Acetone purification system and purification method

Abstract

The invention relates to the field of preparation of electronic-grade chemical reagents, in particular to an acetone purification system and method, and the system comprises a raw material supply unit which is used for respectively providing an oxidation reagent material flow, an acetone crude product and a deacidification agent; the reaction dealdehyding unit is used for carrying out first contact on the oxidizing reagent material flow and an acetone crude product to obtain produced liquid; the deacidification unit is used for performing second contact on the produced liquid and a deacidification agent to obtain a deacidified product; and the rectification coupling pervaporation unit is used for rectifying and dehydrating the deacidified product. When the preparation system is used for preparing the electronic-grade acetone, the preparation method is simple, energy consumption is low, continuous production can be achieved, and the product is stable and high in quality.

Description

Technical Field

[0001] The present invention relates to the technical field of electronic-grade chemical reagent preparation, and in particular to an acetone purification system and a purification method. Background Art

[0002] Acetone is an important chemical raw material. It is colorless and transparent, easily soluble in water and organic solvents such as methanol, ethanol, ether, and chloroform. It plays an important role in the fields of plastics, rubber, fiber, oils, etc.

[0003] As a solvent with excellent performance, acetone is also widely used in the semiconductor, liquid crystal display and photovoltaic industries, and is often used as a cleaning solvent. However, in the above fields, the product requirements for acetone are relatively strict and need to reach the electronic grade level. In addition to strict requirements on product purity and water content, there are extremely high requirements for the residual metal ions and particles in the product. And with the improvement of product grade, the requirements for electronic grade acetone are also getting higher and higher. Therefore, the development of electronic grade acetone preparation process should receive more attention.

[0004] However, it can be seen from the existing reported patents and documents on the preparation of electronic-grade acetone that the research content is relatively small. Among them, CN201317750Y reports a method for obtaining ultra-clean high-purity acetone by only one distillation, the adjustability of the invention is relatively poor, and the stability of the product is seriously insufficient; another example is patent CN105175236A reports a method for finally obtaining ultra-clean high-purity acetone by two-stage dehydration-oxidation-distillation-microfiltration, the invention contains an intermittent step, and the material needs to be collected by color judgment, which greatly affects the efficiency; another example is patent CN104030903A and CN114344932A both report a method for preparing ultra-clean high-purity and electronic-grade acetone, but neither of them considers removing aldehyde impurities in acetone, and the presence of the above impurities will greatly affect the product quality; and CN113636922A also reports a method for preparing ultra-clean high-purity acetone by generating acetone azine, the process uses hydrazine water as a reactant, and the overall cost is relatively high.

[0005] In view of the problems arising in the preparation process of electronic-grade acetone, it is very urgent to develop a preparation technology for obtaining high-quality electronic-grade acetone with low consumption, low cost and continuous production. Summary of the invention

[0006] The purpose of the present invention is to overcome the problems of high production cost, low production efficiency and poor product grade in the prior art when preparing electronic-grade acetone, and to provide a system and method for preparing electronic-grade acetone. The preparation of electronic-grade acetone using the preparation system of the present invention not only has a simple preparation method and low energy consumption, but also can realize continuous production, and the product is stable and of high quality.

[0007] A first aspect of the present invention provides an acetone purification system, the system comprising:

[0008] A raw material supply unit, used for respectively providing an oxidizing agent flow, a crude acetone product and an acid scavenger;

[0009] A reaction dealdehyde unit, used for first contacting the oxidation reagent stream with the crude acetone product to obtain a produced liquid;

[0010] A deacidification unit, used for the second contact between the produced liquid and the deacidifier to obtain a deacidified product;

[0011] The distillation-coupled pervaporation unit is used for distillation and dehydration of the product after acid removal.

[0012] A second aspect of the present invention provides a method for purifying acetone, which is carried out in the system described in the method, and the method comprises:

[0013] (1) the crude acetone from the raw material supply unit is first contacted with the oxidizing agent stream to obtain a produced liquid;

[0014] (2) the produced liquid is contacted with the deacidifier from the raw material supply unit for a second time in the reaction dealdehyde unit to obtain a deacidified product;

[0015] (3) After deacidification, the product enters the distillation-coupled pervaporation unit for distillation and dehydration.

[0016] Through the above technical solution, the present invention has at least the following beneficial effects:

[0017] 1. The system of the present invention can realize continuous purification of crude acetone and has good economic effect;

[0018] 2. The system of the present invention is used to purify acetone, which can better reduce the aldehyde content and water content in the crude acetone product. The purified acetone product is stable and of high quality, and can meet the technical index requirements of electronic grade acetone. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The invention relates to a system for purifying acetone in one embodiment of the present invention.

[0020] Description of Reference Numerals

[0021] ①、Fixed bed reactor ②、Reaction kettle

[0022] ③、Light-removing tower ④、Heavy-removing tower

[0023] ⑤、Reheater ⑥、Pervaporation membrane separation device

[0024] ⑦、Heat exchanger ⑧、Flash tank

[0025] ⑨、Condenser ⑩、Adsorption tower

[0026] De-particle unit

[0027] 1. Acetone crude product 2. Remove mixed oxidant materials

[0028] 3. Oxidation reagent logistics 4. Produced liquid

[0029] 5. Circulating fluid 6. Acid scavenger

[0030] 7. Product after deacidification 8. Product after deacidification after heat exchange

[0031] 9. Top product of light removal tower 10. Bottom product of light removal tower

[0032] 11. Products from the kettle of the deweighting tower 12. Products from the top of the deweighting tower

[0033] 13. Heating of the top steam product of the de-weighting tower 14. Top reflux liquid of the de-weighting tower

[0034] 15. Liquid produced from the top of the deweighting tower 16. Permeation liquid from pervaporation

[0035] 17. Flash liquid phase 18. Flash steam phase

[0036] 19. Condensate 20. After deionization

[0037] 21. Acetone products DETAILED DESCRIPTION

[0038] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0039] A first aspect of the present invention provides an acetone purification system, the system comprising:

[0040] A raw material supply unit, used for respectively providing an oxidizing agent flow, a crude acetone product and an acid scavenger;

[0041] A reaction dealdehyde unit, used for first contacting the oxidation reagent stream with the crude acetone product to obtain a produced liquid;

[0042] A deacidification unit, used for the second contact between the produced liquid and the deacidifier to obtain a deacidified product;

[0043] The distillation-coupled pervaporation unit is used for distillation and dehydration of the product after acid removal.

[0044] In the present invention, the acetone purification system of the present invention is used to purify acetone, which can achieve simple operation, low energy consumption, and continuous production, and the purified acetone product is stable and of high quality.

[0045] According to a preferred embodiment of the present invention, the reaction dealdehyde unit comprises a fixed bed reactor and a first feed port and a second feed port respectively arranged on the fixed bed reactor; the first feed port is used for a part of the crude acetone as a first feed, and the second feed port is used for a mixed solution of another part of the crude acetone and the oxidizing agent stream as a second feed. The above embodiment can better increase the effect of dealdehyde.

[0046] According to a particularly preferred embodiment of the present invention, the first feed inlet is located at the top of the fixed bed reactor; and the second feed inlet is located at the upper middle portion of the fixed bed reactor.

[0047] According to a particularly preferred embodiment of the present invention, a distributor is provided inside the fixed bed reactor for distributing the mixed solution of the crude acetone product and the oxidizing agent flow so that the first feed and the second feed form reverse contact in the axial direction above the distributor. By adopting the aforementioned embodiment, the second feed can be injected into reverse contact with the first feed, thereby increasing the mixing effect of the two, ensuring that when the amount of oxidizing agent flow added is very small, the mixing of the oxidizing agent flow and the crude acetone product can be better ensured, so that the dealdehyde effect is better.

[0048] According to a particularly preferred embodiment of the present invention, the outlet of the reaction dealdehyde unit is respectively connected to the inlet of the acid removal unit and the outlet of the raw material supply unit for providing crude acetone, so that part of the produced liquid enters the acid removal unit, and the other part of the produced liquid is circulated back to the reaction dealdehyde unit as a circulating liquid. By adopting the above embodiment, the residence time of the crude acetone in the reaction dealdehyde unit can be increased, and the dealdehyde effect can be improved.

[0049] According to the present invention, in order to increase the mixing between materials, the fixed bed reactor is preferably filled with fillers, such as at least one of regular wire mesh fillers, bulk ball rings, theta rings and triangular spiral fillers. The above-mentioned embodiment can increase the degree of confusion between materials, which is beneficial to the mixing between the oxidant and the crude acetone product and improves the effect of dealdehyde removal.

[0050] According to a preferred embodiment of the present invention, the acid removal unit comprises a reaction kettle.

[0051] According to a particularly preferred embodiment of the present invention, the reactor is a reactor with a conical bottom. By adopting the above embodiment, some solid impurities can be retained at the bottom for easy removal.

[0052] According to a particularly preferred embodiment of the present invention, a vertical plate is provided at the top of the reactor to divide the reactor into a stirring zone and a discharging zone, and the vertical plate extends downward and is spaced apart from the bottom of the reactor so that the stirring zone is connected to the bottom of the discharging zone. With the aforementioned embodiment, the entire deacidification process is completed in one reactor, and deacidification can be achieved in the stirring zone, and the material after deacidification can flow out continuously through the discharging zone.

[0053] According to the present invention, stirring can be achieved by installing a stirrer in the stirring zone.

[0054] According to a particularly preferred embodiment of the present invention, the upper portion of the discharge zone is connected to the inlet of the distillation-coupled pervaporation unit, so that the product after deacidification enters the distillation-coupled pervaporation unit for distillation and dehydration, and a baffle is connected to the inner side wall of the discharge zone below the connection between the discharge zone and the distillation-coupled pervaporation unit, and the baffle extends toward the vertical plate and the gap between the baffle and the vertical plate forms a material port. The above embodiment can reduce solid impurities such as salt that may exist in the effluent, reduce subsequent energy consumption, and increase the purification effect.

[0055] According to a particularly preferred embodiment of the present invention, the baffle is located in the upper middle portion of the discharge zone.

[0056] According to a particularly preferred embodiment of the present invention, the outlet of the reactive dealdehyde unit is connected to the upper part or the upper middle part of the stirring zone.

[0057] According to a particularly preferred embodiment of the present invention, the outlet for providing the acid scavenger in the raw material supply unit is connected to the top of the stirring zone.

[0058] According to a preferred embodiment of the present invention, the distillation-coupled pervaporation unit includes a light-removal tower, a heavy-removal tower, and a pervaporation membrane separation device connected in series; the light-removal tower is used for distillation and light-removal of the product after acid removal; the heavy-removal tower is used for distillation and heavy-removal of the product in the kettle of the light-removal tower; the pervaporation membrane separation device is used for the product at the top of the heavy-removal tower to enter the pervaporation membrane separation device for dehydration; the outlet of the concentration side of the pervaporation membrane separation device is respectively connected to a circulation pipeline and a production pipeline, and the outlet of the concentration side is connected to the top of the heavy-removal tower through a circulation pipeline. Using the aforementioned embodiment, the heavy-removal tower is coupled with the pervaporation membrane separation device, which can utilize the higher thermal grade of the vapor phase product at the top of the heavy-removal tower. The coupling process of the concentrated side liquid of the pervaporation membrane separation device returning to the heavy-removal tower can greatly reduce the process energy consumption, improve the utilization rate of energy consumption, and has obvious dehydration and purification effects.

[0059] According to a particularly preferred embodiment of the present invention, the top of the dehydration tower is connected to the inlet of the pervaporation membrane separation device through a heating device. By adopting the above embodiment, the higher heat grade of the vapor phase product at the top of the dehydration tower can be utilized during dehydration, and after further heating to increase the heat grade, the pervaporation membrane separation conditions are met for dehydration.

[0060] According to a particularly preferred embodiment of the present invention, the distillation-coupled pervaporation unit further includes a heat exchange device for exchanging heat between the product after deacidification and the material at the outlet of the concentration side of the pervaporation membrane separation device. The material on the concentration side separated by the pervaporation membrane separation device has a high thermal grade. By adopting the aforementioned embodiment, the material entering the lightness removal tower (i.e., the product after deacidification) is a cold distillate and heat exchanged with the material on the concentration side separated by the pervaporation membrane separation device can significantly reduce the energy consumption when using the system of the present invention to purify acetone, avoid the waste of high-grade energy consumption and the consumption of a large amount of refrigerant, and improve the utilization rate of heat.

[0061] According to a preferred embodiment of the present invention, along the material flow direction, the system further includes: a flash unit, a condensation heat exchange unit, a deionization unit and a particle removal unit, which are used for condensing, deionizing and particle removal of the product after distillation and dehydration after flash evaporation; the flash unit is connected to the outlet of the distillation coupling pervaporation unit. By adopting the above embodiment, the refrigerant consumption in the condensation process in the subsequent condensation heat exchange unit can be further reduced through the flash unit, and the metal ions therein can be further removed.

[0062] According to the present invention, there is no special requirement for the structure of the flash unit, and it can be a conventional flash tank in the art.

[0063] A second aspect of the present invention provides a method for purifying acetone, which is carried out in the system described in the present invention, and comprises:

[0064] (1) the crude acetone from the raw material supply unit is first contacted with the oxidizing agent stream to obtain a produced liquid;

[0065] (2) the produced liquid is contacted with the deacidifier from the raw material supply unit for a second time in the reaction dealdehyde unit to obtain a deacidified product;

[0066] (3) After deacidification, the product enters the distillation-coupled pervaporation unit for distillation and dehydration.

[0067] The method of the present invention can finally obtain high-quality electronic-grade acetone through the steps of reaction dealdehyde removal, distillation, dehydration, etc., and the product after acid removal enters a distillation-coupled pervaporation unit for distillation and dehydration, which can realize the integration and comprehensive utilization of heat, further improve product quality and efficiency, and reduce energy consumption under the condition of realizing industrial continuity.

[0068] According to a preferred embodiment of the present invention, the crude acetone provided by the raw material supply unit is divided into two parts, one part of the crude acetone enters the fixed bed reactor from the first feed port on the fixed bed reactor as the first feed, and the other part of the crude acetone is mixed with the oxidizing agent flow provided by the raw material supply unit to obtain a mixed liquid, which enters the fixed bed reactor from the second feed port on the fixed bed reactor as the second feed and undergoes a first contact reaction with the first feed through a distributor to obtain a produced liquid. By adopting the above embodiment, the mixing of the oxidizing agent flow and the crude acetone can be increased to ensure the dispersion and dealdehyde effect.

[0069] According to a preferred embodiment of the present invention, the volume ratio of the crude acetone in the first feed to the crude acetone in the second feed is (70-99): (1-30). The above embodiment can increase the mixing of the oxidizing agent flow and the crude acetone to ensure the dispersion and dealdehyde effect.

[0070] According to a preferred embodiment of the present invention, part of the produced liquid enters the acid removal unit and undergoes a second contact with the acid removal agent provided by the raw material supply unit in the acid removal unit to obtain a deacidified product, and another part of the produced liquid is circulated back to the reaction dealdehyde removal unit as a circulating liquid. By adopting the aforementioned embodiment, the mixing of the oxidizing agent flow and the crude acetone product can be increased to ensure the dispersion and dealdehyde removal effects.

[0071] According to a particularly preferred embodiment of the present invention, the circulation ratio of the circulating liquid is 2-20, for example, 2, 3, 5, 10, 13, 15, 20, or a range consisting of any two of the above values. By adopting the above embodiment, the purity of the obtained acetone product can be better increased.

[0072] The circulation ratio mentioned in the present invention refers to the ratio of the circulating liquid flow rate to the flow rate of the produced liquid entering the acid removal unit.

[0073] According to a particularly preferred embodiment of the present invention, part of the produced liquid enters the stirring zone through the upper part or the upper middle part of the stirring zone of the reactor, and the deacidifier provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor, and part of the produced liquid and the deacidifier are subjected to a second contact in the stirring zone, and the deacidified product obtained by the second contact continuously passes through the discharge zone and enters the lightness removal tower. With the aforementioned embodiment, the deacidification process can be completed in one reactor, part of the produced liquid and the deacidifier can be quickly mixed in the stirring zone to remove impurities such as acid, and the effluent can flow out continuously through the discharge zone, while impurities such as salts can remain at the bottom of the reactor to increase the overall purification effect.

[0074] According to a preferred embodiment of the present invention, the deacidified product passes through a heat exchange device and then enters a deacidifying tower from the top of a deacidifying tower for distillation and delightening; the deacidifying tower top product obtained by distillation and deheaving enters a pervaporation membrane separation device for dehydration; the concentrated side outlet of the pervaporation membrane separation device obtains the dehydrated material, and the dehydrated material enters the heat exchange device for heat exchange with the deacidified product entering the heat exchange device, and a part of the dehydrated material after heat exchange is returned to the deacidifying tower through a circulation pipeline as the deacidifying tower top reflux liquid, and the other part is produced as the dehydrated produced liquid. In the aforementioned embodiment, the pervaporation membrane separation device is coupled with the deacidifying tower top, and the coupling process is that the vapor phase at the top of the deacidifying tower enters the pervaporation membrane separation device for dehydration, and a part of the dehydrated material is returned to the deacidifying tower through a circulation pipeline as the deacidifying tower top reflux liquid. The aforementioned embodiment can not only greatly reduce the process energy consumption and improve the energy consumption utilization rate, but also have a significant acetone purification effect.

[0075] According to a particularly preferred embodiment of the present invention, the conditions for distillation to remove light components include: an operating pressure of 100-200 kPa, such as 100 kPa, 150 kPa, 175 kPa or 200 kPa. The crude acetone contains light components such as propylene. The positive pressure embodiment can ensure that the top condensation can be done with cheap ordinary water cooling. Also, under the positive pressure condition, it can ensure that organic impurities outside the system do not enter the system, which can increase the overall purification effect.

[0076] According to a particularly preferred embodiment of the present invention, the conditions for distillation light removal include: a reflux ratio of 2-20, for example, 2, 5, 6, 10, 13, 15 or 20, preferably 2-10. The above embodiment can increase the purification effect of the overall crude acetone product, while increasing the recovery rate of the bottom product of the light removal tower and the overall operating energy consumption to better balance.

[0077] According to a particularly preferred embodiment of the present invention, the conditions for distillation and light removal include: the temperature of the bottom of the light removal tower is 56.6-78.0°C, for example, 56.6°C, 68.7°C, 77.6°C, 78°C, or a range consisting of any two of the foregoing values. The foregoing embodiment can increase the purification effect of the overall crude acetone product.

[0078] According to a particularly preferred embodiment of the present invention, the conditions for the rectification and de-weighting include: an operating pressure of 100-200 kPa, for example, 100 kPa, 150 kPa, 175 kPa or 200 kPa. The crude acetone contains heavy components such as isopropanol, methanol, isopropyl ether, water and some inorganic salts soluble in acetone. The boiling points of water and acetone are quite different, and there is no azeotropy. However, experiments have found that there is still a large amount of water in the top product of the de-weighting process, indicating that the separation of water and acetone is not complete. The above-mentioned embodiment can ensure that the top condensation can be cooled by cheap ordinary water, and under the condition of positive pressure, it can ensure that organic impurities outside the system do not enter the system.

[0079] According to a particularly preferred embodiment of the present invention, the conditions for the rectification and de-weighting include: the top temperature of the de-weighting tower is 55.7-77.5°C, for example, 55.7°C, 68°C, 73°C, 77.5°C, or a range consisting of any two of the foregoing values. The foregoing embodiment can increase the purification effect of the overall crude acetone product.

[0080] According to a particularly preferred embodiment of the present invention, the dehydration conditions include: an inlet temperature of 60-120°C, for example, 60°C, 90°C, 100°C or 120°C.

[0081] According to a particularly preferred embodiment of the present invention, the dehydration conditions include: a pressure of 115-605 kPa (absolute pressure), for example, 115 kPa, 159 kPa, 478 kPa, 605 kPa.

[0082] In the present invention, the heating device can be used to make the material entering the pervaporation membrane separation device reach the required inlet temperature and pressure.

[0083] According to a particularly preferred embodiment of the present invention, the mass flow ratio of the reflux liquid from the top of the dehydration tower to the produced liquid after dehydration is (1-5):1, for example, 1:1, 2:1, 3:1, 4:1, 5:1, or a range between any two of the above ratios. The above embodiment can increase the purification effect of the overall crude acetone product, while increasing the recovery rate of the dehydration tower kettle product and the overall operating energy consumption to better balance.

[0084] In the present invention, as long as the purpose of the present invention can be achieved, the conditions of the first contact are not particularly limited. According to a particularly preferred embodiment of the present invention, the conditions of the first contact include: a temperature of 20-50° C. The research process also found that by adopting the above embodiment, the dealdehyde effect of the oxidant can be maintained at a better level, which can better improve the overall purification effect of the crude acetone product.

[0085] According to a particularly preferred embodiment of the present invention, the conditions for the first contact include: a temperature of 20-50°C.

[0086] According to a particularly preferred embodiment of the present invention, the conditions for the first contact include: a residence time of 1-5 hours.

[0087] According to a particularly preferred embodiment of the present invention, the conditions for the second contact include: room temperature.

[0088] According to a particularly preferred embodiment of the present invention, the conditions for the second contact include: a residence time of 0.5-2h.

[0089] According to a particularly preferred embodiment of the present invention, the conditions for the second contact include: a stirring speed of 100-1000 rpm.

[0090] According to a preferred embodiment of the present invention, the mass flow rate of the oxidizing agent stream is 0.001-0.01 times the mass flow rate of the crude acetone. By adopting the above embodiment, the aldehydes in the acetone can be removed to a lower level without wasting the oxidizing agent.

[0091] According to a preferred embodiment of the present invention, the flow rate of the acid scavenger entering the dealdehyde removal unit is 0.001-0.01 times the flow rate of the produced liquid entering the reaction dealdehyde removal unit. The above embodiment can better reduce the content of acidic impurities in the material.

[0092] According to a preferred embodiment of the present invention, the oxidant is selected from a hydrogen peroxide solution and / or a potassium permanganate solution. The above embodiment can better improve the effect of acetone purification.

[0093] According to a particularly preferred embodiment of the present invention, the mass concentration of the hydrogen peroxide solution is 20-40%. The above embodiment can better improve the effect of acetone purification.

[0094] According to a preferred embodiment of the present invention, the mass concentration of the potassium permanganate aqueous solution is 1.5-4%. The above embodiment can better increase the effect of acetone purification.

[0095] According to a preferred embodiment of the present invention, the acid scavenger comprises an aqueous solution of an alkaline hydroxide and optionally an alkaline bicarbonate.

[0096] In the present invention, "optionally alkaline bicarbonate" means adding or not adding alkaline bicarbonate as required.

[0097] According to a particularly preferred embodiment of the present invention, the mass concentration of the alkaline hydroxide in the aqueous solution is 5-20wt%. Too high a concentration cannot be achieved and exceeds the saturated solubility, while too low a concentration will result in a significant increase in usage, increase the water content of the product and increase the burden of subsequent purification.

[0098] According to the present invention, as long as the purpose of the present invention can be achieved, the type of the alkaline hydroxide is not particularly limited. From the perspective of solubility, the alkaline hydroxide is sodium hydroxide and / or potassium hydroxide.

[0099] According to a particularly preferred embodiment of the present invention, in the aqueous solution, the concentration of the alkaline bicarbonate is 5-20wt%, such as 5wt%, 10wt%, 15wt% or 20wt%.

[0100] According to a particularly preferred embodiment of the present invention, the alkaline bicarbonate is selected from sodium bicarbonate and / or potassium bicarbonate.

[0101] The crude acetone generally contains at least one impurity of water, isopropanol, acetaldehyde, propionaldehyde, propylene, isopropyl ether and methanol. According to a preferred embodiment of the present invention, the purity of the crude acetone is 98.5-99.9%, and the crude acetone contains 20-500 ppm of aldehydes.

[0102] According to a preferred embodiment of the present invention, the method further comprises flashing, condensing, deionizing and degranulating the produced liquid after distillation and dehydration, and the flashing conditions preferably include: pressure 0.5-0.8 bar. The above embodiment can reduce the residual metal ions and particles in the produced liquid after dehydration, and the vapor phase thermal grade obtained by flashing is further reduced in the flashing process, which will reduce the amount of refrigerant used in the condensation process.

[0103] According to a particularly preferred embodiment of the present invention, the flash evaporation conditions include: a pressure of 0.5-0.8 bar.

[0104] The condensation described in the present invention generally refers to condensation to room temperature.

[0105] Room temperature in the present invention refers to 20-30°C.

[0106] According to the present invention, as long as the purpose of the present invention can be achieved, the deionization method is not particularly limited. For example, the deionization unit is an adsorption tower filled with adsorption material, and deionization is performed by ion exchange adsorption removal. Preferably, the adsorption material is a mixed bed resin, and the mixed bed resin refers to a hydrogen-type strong acid cation exchange resin and a hydroxide-type strong base anion exchange resin that are uniformly mixed and filled in the adsorption tower. The mixed bed resin can remove metal cations and anions in the solution, and the replaced hydrogen ions and hydroxide ions eventually form a small amount of water in the solution.

[0107] According to the present invention, as long as the purpose of the present invention can be achieved, the method of degranulation is not particularly limited. For example, the degranulation unit is a plurality of membrane separators connected in series, and the three membrane separation materials of PTFE, PVDF and PE show good particle retention rate and low solubility. The membrane separation material used in the membrane separator is selected from one of PTFE, PVDF and PE. Preferably, a 4-stage membrane separator connected in series is used, and the filtration specifications are 500nm, 200nm, 100nm and 50nm, respectively. By adopting the above-mentioned embodiment, the particles (≥0.1μm) in the acetone product can be ≤100 / ml.

[0108] According to a particularly preferred embodiment of the present invention, the acetone purification method is as follows Figure 1 The acetone purification system shown is carried out:

[0109] Figure 1 In the system shown, the particle removal unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively.

[0110] The method comprises: a crude acetone product 1 from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters the fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, and the other part of the crude acetone product 1 is used as a mixed oxidant material 2 and mixed with an oxidizing agent flow 3 provided by the raw material supply unit to obtain a mixed liquid, which is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor, and then the mixed liquid is subjected to a first contact reaction with the first feed to obtain a produced liquid 4;

[0111] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone to obtain the deacidified product 7; another part of the produced liquid 4 is used as the circulating liquid 5 and mixed with the crude acetone 1 and then continues to enter the fixed bed reactor ①;

[0112] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone and passes through the heat exchanger ⑦ to obtain the deacidified product 7 after heat exchange. The deacidified product 8 after heat exchange enters the lightness removal tower ③ from the middle and upper part of the lightness removal tower ③. The lightness removal tower top product 9 is discharged out of the boundary for collection. The lightness removal tower bottom product 10 enters the heavyness removal tower ④ from the middle and lower part of the heavyness removal tower ④. The heavyness removal tower bottom product 11 is discharged out of the boundary for collection. The heavyness removal tower top product 12 is heated by the reheater ⑤ to obtain the heated heavyness removal tower top steam product 13. The heated heavyness removal tower top steam product 13 enters the pervaporation membrane separation device ⑥. The pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection.

[0113] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 for flash evaporation, and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is obtained by condensing in a condenser ⑨ to obtain a condensate 19, which enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0114] The present invention will be described in detail below through examples. In the following examples, the product purity is detected by HPLC, the water content is determined by Karl Fischer titrator, the metal ions are determined by ICP-MS, and the particle number is determined online by a particle counter.

[0115] Example 1

[0116] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0117] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 20° C., and the residence time is 3 hours;

[0118] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.001 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 0.5h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio is 10) and is mixed with the crude acetone 1 and then continues to enter the fixed bed reactor ①;

[0119] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0120] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0121] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 44 ppm, the total aldehyde content was 0.7 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0122] Example 2

[0123] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with ball ring bulk filler;

[0124] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters the fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.001 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 30° C., and the residence time is 3 hours;

[0125] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (5wt% NaOH aqueous solution, the mass flow rate is 0.01 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 15) and then continues to enter the fixed bed reactor ①;

[0126] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0127] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.5 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is obtained by flash evaporation. After condensing to room temperature by a condenser ⑨, the condensate 19 obtained enters an adsorption tower ⑩ (filled with uniformly mixed hydrogen-type strong acid cation exchange resin and hydrogen-oxygen-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0128] It was determined that the purity of the obtained acetone product 21 was 99.996%, the water content was 60 ppm, the total aldehyde content was 0.3 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0129] Example 3

[0130] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with theta ring bulk filler;

[0131] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.01 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 5 hours;

[0132] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 2h, stirring speed is 500rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 20) and then continues to enter the fixed bed reactor ①;

[0133] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 20, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0134] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash pressure is 0.8 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash vapor phase 18 obtained by flash evaporation is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0135] It was determined that the purity of the obtained acetone product 21 was 99.994%, the water content was 58 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0136] Example 4

[0137] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PVDF, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with triangular spiral bulk filler;

[0138] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 50° C., and the residence time is 3 hours;

[0139] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0140] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 2, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection. The tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. Tower ④ (the operating pressure of the deweighting tower ④ is 150 kPa, and the vapor phase temperature of the top of the deweighting tower ④ is controlled to be 68.0° C.), the deweighting tower kettle product 11 is discharged out of the boundary for collection, the deweighting tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated deweighting tower top vapor product 13, the heated deweighting tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0141] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0142] It was determined that the purity of the obtained acetone product 21 was 99.998%, the water content was 36 ppm, the total aldehyde content was 0.1 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0143] Example 5

[0144] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0145] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0146] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0147] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 200 kPa, the operating reflux ratio is 6, and the tower bottom temperature of the delightening tower ③ is controlled to be 78.0°C). The top product 9 of the delightening tower is discharged out of the boundary for collection. The tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part. Tower ④ (the operating pressure of the deweighting tower ④ is 150 kPa, and the vapor phase temperature of the top of the deweighting tower ④ is controlled to be 68.0° C.), the deweighting tower kettle product 11 is discharged out of the boundary for collection, the deweighting tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated deweighting tower top vapor product 13, the heated deweighting tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0148] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0149] It was determined that the purity of the obtained acetone product 21 was 99.998%, the water content was 40 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0150] Example 6

[0151] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0152] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0153] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0154] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 175 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 73.6°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0155] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:5) for flash evaporation (the flash pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash vapor phase 18 obtained by flash evaporation is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0156] It was determined that the purity of the obtained acetone product 21 was 99.994%, the water content was 70 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0157] Example 7

[0158] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0159] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0160] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0161] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 100 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 56.6°C). The top product 9 of the delightening tower is discharged out of the boundary for collection. The tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0162] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:2) for flash evaporation (the flash pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash vapor phase 18 obtained by flash evaporation is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0163] It was determined that the purity of the obtained acetone product 21 was 99.996%, the water content was 55 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0164] Example 8

[0165] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0166] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0167] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0168] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. De-weighting tower ④ (the operating pressure of de-weighting tower ④ is 200 kPa, and the vapor phase temperature of the top of de-weighting tower ④ is controlled to be 77.5° C.), the de-weighting tower kettle product 11 is discharged out of the boundary for collection, the de-weighting tower top product 12 is heated to 110° C. by a reheater ⑤ to obtain a heated de-weighting tower top vapor product 13, and the heated de-weighting tower top vapor product 13 enters a pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0169] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 2:1) for flash evaporation (the flash pressure is 0.6 bar), and the flash liquid phase 17 obtained by flash evaporation is discharged out of the boundary for collection, and the flash vapor phase 18 obtained by flash evaporation is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0170] It was determined that the purity of the obtained acetone product 21 was 99.998%, the water content was 32 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0171] Example 9

[0172] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0173] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0174] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0175] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 175 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 73.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0176] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 5:1) for flash evaporation (the flash pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash vapor phase 18 is obtained by flash evaporation. After condensing to room temperature by a condenser ⑨, the condensate 19 obtained enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0177] It has been determined that the purity of the obtained acetone product 21 is 99.999%, the water content is 25 ppm, the total aldehyde is 0.2 ppm, the concentration of single metal ions in the acetone product 21 is ≤100 ppt, and the particles (≥0.1 μm) are ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0178] Example 10

[0179] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0180] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0181] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0182] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. De-weighting tower ④ (the operating pressure of de-weighting tower ④ is 100 kPa, and the vapor phase temperature of the top of de-weighting tower ④ is controlled to be 55.7° C.), the de-weighting tower kettle product 11 is discharged out of the boundary for collection, the de-weighting tower top product 12 is heated to 110° C. by a reheater ⑤ to obtain a heated de-weighting tower top vapor product 13, and the heated de-weighting tower top vapor product 13 enters a pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0183] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0184] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 44 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0185] Embodiment 11

[0186] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0187] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (hydrogen peroxide with a concentration of 30 wt%, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ① and then sprays the feed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C. and the residence time is 3 hours;

[0188] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% KOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0189] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0190] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0191] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 59 ppm, the total aldehyde content was 0.5 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the number of particles (≥0.1 μm) was ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0192] Example 12

[0193] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0194] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a mixed oxidant material 2 and mixed with an oxidizing agent stream 3 (hydrogen peroxide with a concentration of 30 wt%, which is 0.01 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ① and then sprays the feed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C. and the residence time is 3 hours;

[0195] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0196] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0197] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0198] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 57 ppm, the total aldehyde content was 0.4 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0199] Embodiment 13

[0200] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0201] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0202] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0203] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 120° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 605 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0204] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0205] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 22 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0206] Embodiment 14

[0207] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0208] The method comprises: a crude acetone product 1 (with a purity of 99.2%, a water content of 2700 ppm, and a total aldehyde content of 30 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.005 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0209] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.005 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 10) and then continues to enter the fixed bed reactor ①;

[0210] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 70° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 159 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0211] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0212] It was determined that the purity of the obtained acetone product 21 was 99.997%, the water content was 99 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0213] Embodiment 15

[0214] Acetone purification method Figure 1 The acetone purification system shown is carried out: Figure 1 In the system shown, the demicronizing unit is a 4-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE, and the filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh filler;

[0215] The method comprises: a crude acetone product 1 (with a purity of 98.5%, a water content of 3400 ppm, and a total aldehyde content of 166 ppm) from a raw material supply unit is divided into two parts, one part of the crude acetone product 1 is used as a first feed and enters a fixed bed reactor ① from a first feed port at the top of the fixed bed reactor ①, another part of the crude acetone product 1 (with a dosage of 25% of the total volume of the crude acetone product 1) is used as a demixed oxidant material 2 and mixed with an oxidizing agent stream 3 (a 2.5 wt % potassium permanganate aqueous solution, which is 0.01 times the mass flow rate of the total crude acetone product 1) provided by the raw material supply unit to obtain a mixed liquid, and the mixed liquid is used as a second feed and enters the fixed bed reactor ① from a second feed port at the upper middle part of the fixed bed reactor ①, and then the feed is sprayed upward through a distributor to carry out a first contact reaction with the first feed to obtain a produced liquid 4, and the temperature of the fixed bed reactor ① is controlled to be 40° C., and the residence time is 3 hours;

[0216] Part of the produced liquid 4 enters the stirring zone from the upper part of the stirring zone of the reactor ②, and the deacidifier 6 (20wt% NaOH aqueous solution, the mass flow rate is 0.01 times the mass flow rate of the produced liquid 4 entering the reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②, and makes a second contact with the part of the produced liquid 4 entering the stirring zone in the stirring zone (residence time 1h, stirring speed is 200rmp) to obtain the deacidified product 7; another part of the produced liquid 4 is mixed with the acetone crude product 1 as the circulating liquid 5 (circulation ratio is 20) and then continues to enter the fixed bed reactor ①;

[0217] The deacidified product 7 obtained by the second contact continuously passes through the discharge zone of the reactor ② and then flows out from the upper part of the discharge zone to pass through the heat exchanger ⑦ to obtain the deacidified product 8 after heat exchange. The deacidified product 8 after heat exchange enters the delightening tower ③ from the middle and upper part of the delightening tower ③ (the operating pressure of the delightening tower ③ is 150 kPa, the operating reflux ratio is 10, and the tower bottom temperature of the delightening tower ③ is controlled to be 68.7°C). The top product 9 of the delightening tower is discharged out of the boundary for collection, and the tower bottom product 10 of the delightening tower enters the deweighting tower ④ from the middle and lower part of the deweighting tower ④. The weight removal tower ④ (the operating pressure of the weight removal tower ④ is 150 kPa, and the vapor phase temperature of the top of the weight removal tower ④ is controlled to be 68.0° C.), the weight removal tower kettle product 11 is discharged out of the boundary for collection, the weight removal tower top product 12 is heated to 110° C. by the reheater ⑤ to obtain the heated weight removal tower top vapor product 13, the heated weight removal tower top vapor product 13 enters the pervaporation membrane separation device ⑥ (pressure 478 kPa), and the pervaporated permeate 16 at the permeation side outlet of the pervaporation membrane separation device ⑥ is discharged out of the boundary for collection;

[0218] The dehydrated material obtained at the concentration outlet of the pervaporation membrane separation device ⑥ is exchanged with the deacidified product 7 through a heat exchanger ⑦ for heat exchange; a part of the dehydrated material after heat exchange is returned to the dehydration tower ④ from the upper part of the dehydration tower ④ through a circulation pipeline as the dehydration tower top reflux liquid 14, and the other part is entered into a flash tank ⑧ as the dehydration tower top produced liquid 15 (the mass flow ratio of the dehydration tower top reflux liquid 14 to the dehydration tower top produced liquid 15 is 1:1) for flash evaporation (the flash evaporation pressure is 0.6 bar), and the flash evaporation liquid phase 17 is discharged out of the boundary for collection, and the flash evaporation flash vapor phase 18 is condensed to room temperature by a condenser ⑨ to obtain a condensate 19 that enters an adsorption tower ⑩ (filled with a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin) for deionization to obtain a deionized product 20, and the deionized product 20 passes through a demicronization unit After degranulation, the acetone product 21 is obtained.

[0219] It was determined that the purity of the obtained acetone product 21 was 99.992%, the water content was 95 ppm, the total aldehyde content was 2.5 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0220] Example 16

[0221] The method of Example 3 is followed, except that the acid scavenger is an aqueous solution of NaOH and NaHCO3, the concentration of NaOH is 20wt%, the concentration of NaHCO3 is 20wt%, and the rest is the same as Example 3.

[0222] It has been determined that the purity of the obtained acetone product 21 is 99.994%, the water content is 50 ppm, the total aldehyde is less than 0.1 ppm, the concentration of a single metal ion in the acetone product 21 is ≤100 ppt, and the number of particles (≥0.1 μm) is ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0223] Embodiment 17

[0224] Please add: According to the method of Example 3, the difference is: NaOH and NaHCO3 aqueous solution, the concentration of NaOH is 20wt%, the concentration of NaHCO3 is 5wt%, and the rest is the same as Example 3.

[0225] It has been determined that the purity of the obtained acetone product 21 is 99.994%, the water content is 52 ppm, the total aldehyde is less than 0.1 ppm, the concentration of a single metal ion in the acetone product 21 is ≤100 ppt, and the particles (≥0.1 μm) are ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0226] Embodiment 18

[0227] The method of Example 3 is followed, except that the circulation ratio of the circulating liquid is 1, and the other aspects are the same as those of Example 3, to finally obtain an acetone product.

[0228] It was determined that the purity of the obtained acetone product 21 was 99.991%, the water content was 64 ppm, the total aldehyde content was 3.5 ppm, the concentration of single metal ions in the acetone product 21 was ≤100 ppt, and the particles (≥0.1 μm) were ≤100 / ml, meeting the technical index requirements of electronic grade acetone.

[0229] Comparative Example 1

[0230] The method of Example 3 is followed, except that the acid scavenger 6 is added to the fixed bed reactor together with the oxidizing agent stream 3. The other steps are the same as those of Example 3, and finally an acetone product is obtained.

[0231] The obtained acetone product has a purity of 99.988%, a water content of 65 ppm, a total aldehyde content of 4.2 ppm, a single metal ion concentration of ≤100 ppt, and particles (≥0.1 μm) of ≤100 / ml.

[0232] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. An acetone purification system, characterized in that: The system includes: A raw material supply unit, used for respectively providing an oxidizing agent flow, a crude acetone product and an acid scavenger; A reaction dealdehyde unit, used for first contacting the oxidation reagent stream with the crude acetone product to obtain a produced liquid; A deacidification unit, used for the second contact between the produced liquid and the deacidifier to obtain a deacidified product; The distillation-coupled pervaporation unit is used for distillation and dehydration of the product after acid removal.

2. The system according to claim 1, wherein: The reaction dealdehyde unit comprises a fixed bed reactor and a first feed port and a second feed port respectively arranged on the fixed bed reactor; the first feed port is used for a part of the crude acetone as a first feed, and the second feed port is used for a mixed solution of another part of the crude acetone and an oxidizing agent stream as a second feed; Preferably, the first feed inlet is located at the top of the fixed bed reactor; the second feed inlet is located at the upper part or the upper middle part of the fixed bed reactor; and / or A distributor is provided inside the fixed bed reactor for distributing the mixture of the crude acetone product and the oxidizing agent stream so that the first feed and the second feed are in counter-contact in the axial direction above the distributor; and / or The outlet of the reaction dealdehyde unit is respectively connected to the inlet of the acid removal unit and the outlet of the raw material supply unit for providing crude acetone, so that part of the produced liquid enters the acid removal unit and the other part of the produced liquid is circulated back to the reaction dealdehyde unit as a circulating liquid.

3. The system according to claim 1 or 2, wherein: The acid removal unit comprises a reaction kettle; Preferably, the reactor is a reactor with a conical bottom; and / or A vertical plate is provided at the top of the reactor to divide the reactor into a stirring zone and a discharging zone. The vertical plate extends downward and is spaced apart from the bottom of the reactor so that the stirring zone is connected to the bottom of the discharging zone. More preferably, the upper portion of the discharge zone is connected to the inlet of the distillation-coupled pervaporation unit, so that the product after deacidification enters the distillation-coupled pervaporation unit for distillation and dehydration, and a baffle is connected to the inner side wall of the discharge zone below the connection between the discharge zone and the distillation-coupled pervaporation unit, and the baffle extends toward the vertical plate, and the gap between the baffle and the vertical plate forms a material port; More preferably, the baffle is located in the upper middle part of the discharge area; and / or The outlet of the reaction dealdehyde unit is connected to the upper part or the upper middle part of the stirring zone; and / or The outlet of the acid scavenger provided in the raw material supply unit is connected to the top of the stirring zone.

4. The system according to any one of claims 1 to 3, wherein: The distillation-coupled pervaporation unit comprises a light removal tower, a heavy removal tower, and a pervaporation membrane separation device connected in series; Light removal tower, used for distillation and light removal of products after acid removal; De-heavy tower, used for distillation and de-heavy removal of the product in the kettle of light tower; A pervaporation membrane separation device, used for the top product of the dehydration tower to enter the pervaporation membrane separation device for dehydration, preferably the top of the dehydration tower is connected to the inlet of the pervaporation membrane separation device through a heating device; The outlet of the concentration side of the pervaporation membrane separation device is connected to a circulation pipeline and a production pipeline respectively, and the outlet of the concentration side is connected to the top of the deweighting tower through the circulation pipeline; Preferably, the distillation-coupled pervaporation unit further comprises a heat exchange device for exchanging heat between the deacidified product and the material at the outlet of the concentration side of the pervaporation membrane separation device and then entering the inlet of the distillation-coupled pervaporation unit.

5. The system according to any one of claims 1 to 4, wherein: Along the material flow direction, the system also includes: a flash unit, a condensation heat exchange unit, a deionization unit and a particle removal unit, which are used for condensing, deionizing and particle removal of the product after the distillation and dehydration after flashing; The flash unit is connected to the outlet of the distillation-coupled pervaporation unit.

6. A method for purifying acetone, characterized in that: The method is carried out in a system according to any one of claims 1 to 5, and the method comprises: (1) the crude acetone from the raw material supply unit is first contacted with the oxidizing agent stream to obtain a produced liquid; (2) the produced liquid is contacted with the deacidifier from the raw material supply unit for a second time in the reaction dealdehyde unit to obtain a deacidified product; (3) After deacidification, the product enters the distillation-coupled pervaporation unit for distillation and dehydration.

7. The method according to claim 6, wherein: The crude acetone provided by the raw material supply unit is divided into two parts, one part of the crude acetone is used as a first feed and enters the fixed bed reactor from a first feed port on the fixed bed reactor, and the other part of the crude acetone is mixed with the oxidizing agent stream provided by the raw material supply unit to obtain a mixed liquid, which is used as a second feed and enters the fixed bed reactor from a second feed port on the fixed bed reactor, and undergoes a first contact reaction with the first feed through a distributor to obtain a produced liquid; Preferably, the volume ratio of the crude acetone in the first feed to the crude acetone in the second feed is (70-99):(1-30).

8. The method according to claim 6 or 7, wherein: Part of the produced liquid enters the acid removal unit and undergoes a second contact with the acid removal agent provided by the raw material supply unit in the acid removal unit to obtain a deacidified product, and another part of the produced liquid is circulated back to the reaction dealdehyde unit as a circulating liquid. Preferably, the circulation ratio of the circulating liquid is 2-20.

9. The method according to any one of claims 6 to 8, wherein: The deacidified product passes through a heat exchange device and enters a lightness removal tower from the middle and upper part thereof for distillation and lightness removal. Preferably, the distillation and lightness removal conditions include: an operating pressure of 100-200 kPa; and / or a reflux ratio of 2-20; and / or a temperature of the bottom of the lightness removal tower of 56.6-78.0°C; The product of the de-lightening tower kettle obtained by distillation and de-lightening enters the de-weighting tower from the middle and lower part of the de-weighting tower for distillation and de-weighting. Preferably, the conditions for distillation and de-weighting include: an operating pressure of 100-200 kPa; and / or a de-weighting tower top temperature of 55.7-77.5°C; The top product of the dehydration tower obtained by distillation dehydration enters the pervaporation membrane separation device for dehydration. Preferably, the dehydration conditions include: an inlet temperature of 60-120° C.; and / or a pressure of 115-605 kPa; The dehydrated material is obtained at the outlet of the concentration side of the pervaporation membrane separation device. The dehydrated material enters the heat exchange device and exchanges heat with the deacidified product entering the heat exchange device. A part of the dehydrated material after the heat exchange is returned to the dehydration tower through the circulation pipeline as the top reflux liquid of the dehydration tower, and the other part is produced as the dehydrated produced liquid. The mass flow ratio of the top reflux liquid of the dehydration tower to the dehydrated produced liquid is preferably (1-5):

1.

10. The method according to any one of claims 6 to 8, wherein: The conditions of the first contact include: a temperature of 20-50° C.; and / or a residence time of 1-5 h; and / or The second contact conditions include: room temperature; and / or, a residence time of 0.5-2h; and / or, a stirring speed of 100-1000rmp; and / or The mass flow rate of the oxidizing reagent stream is 0.001-0.01 times the mass flow rate of the crude acetone; and / or The flow rate of the acid scavenger entering the dealdehyde removal unit is 0.001-0.01 times the flow rate of the produced liquid entering the reaction dealdehyde removal unit; and / or The oxidant is selected from a hydrogen peroxide solution and / or a potassium permanganate solution; preferably, the mass concentration of the hydrogen peroxide solution is 20-40%; and / or, the mass concentration of the potassium permanganate solution is 1.5-4%; and / or The acid scavenger comprises an aqueous solution of an alkaline hydroxide and optionally an alkaline bicarbonate, preferably in the aqueous solution, the mass concentration of the alkaline hydroxide is 5-20wt%; and / or, the alkaline hydroxide is sodium hydroxide and / or potassium hydroxide; and / or, the concentration of the alkaline bicarbonate in the aqueous solution is 5-20wt% and / or, the alkaline bicarbonate is selected from sodium bicarbonate and / or potassium bicarbonate; and / or The purity of the crude acetone is 98.5-99.9%, and / or the crude acetone contains 20-500 ppm of aldehydes; and / or The method further comprises flashing, condensing, deionizing and removing microparticles of the produced liquid after distillation and dehydration, and preferably the flashing conditions include: pressure 0.5-0.8 bar.

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