Acetone purification system and purification method

Abstract

The present application relates to the field of electronic grade chemical reagent preparation, in particular to a kind of acetone purification system and purification method, the system includes: raw material supply unit, for providing oxidizing reagent stream, acetone crude product and acid remover respectively;Reaction de-aldehyde unit, for oxidizing reagent stream and acetone crude product first contact to obtain effluent;Acid removal unit, for effluent and acid remover second contact to obtain post-acid removal product;Rectification coupled pervaporation unit, for post-acid removal product rectification, dehydration.Use the preparation system of the present application to prepare electronic grade acetone not only preparation method is simple, energy consumption is low, and can realize continuous production, product is stable and high quality.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of electronic-grade chemical reagent preparation, and particularly relates to an acetone purification system and a purification method. BACKGROUND

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

[0003] As a solvent with excellent performance, acetone is widely used in the semiconductor, liquid crystal display and photovoltaic industries, and is often used as a cleaning solvent. However, in the above-mentioned fields, the product requirements for acetone are relatively strict, and it needs to reach the level of electronic grade. In addition to the strict requirements on product purity and water content, the product also has extremely high requirements on metal ion residue and microparticles. And with the improvement of product grade, the requirements for electronic-grade acetone are becoming higher and higher. Therefore, more attention should be paid to the development of electronic-grade acetone preparation process.

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

[0005] In view of the above problems in the preparation process of electronic-grade acetone, it is urgent to develop a preparation technology for obtaining high-quality electronic-grade acetone with low energy consumption and low cost in a continuous manner. SUMMARY

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

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

[0008] The raw material supply unit is used to provide oxidizing agent stream, crude acetone, and deacidifying agent, respectively.

[0009] The reaction dealdehyde unit is used to make the oxidizing reagent stream and crude acetone into the first contact to obtain the extracted liquid;

[0010] The acid removal unit is used to make a second contact between the produced fluid and the acid removal agent to obtain the 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, wherein the method is carried out in the system described herein, and the method includes:

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

[0014] (2) The produced fluid and the deacidifying agent from the raw material supply unit are in a second contact in the reaction dealdehyde unit to obtain the deacidified product;

[0015] (3) After acid removal, 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 benefits;

[0018] 2. Using the system of the present invention to purify acetone can better reduce the aldehyde and water content in crude acetone. The purified acetone product is stable and of high quality, meeting the technical requirements of electronic grade acetone. Attached Figure Description

[0019] Figure 1 This is an acetone purification system in one embodiment of the present invention.

[0020] Explanation of reference numerals in the attached figures

[0021] ① Fixed-bed reactor ② Reactor

[0022] ③ Remove light towers ④ Remove heavy towers

[0023] ⑤ Reheater ⑥ Pervaporation membrane separation unit

[0024] ⑦ Heat exchanger ⑧ Flash tank

[0025] ⑨ Condenser ⑩ Adsorption tower

[0026] Demicronization unit

[0027] 1. Crude acetone 2. Mixed oxidant material

[0028] 3. Oxidizing reagent stream; 4. Collected fluid

[0029] 5. Circulating fluid 6. Acid remover

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

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

[0032] 11. Products from the bottom of the de-weighting tower 12. Products from the top of the de-weighting tower

[0033] 13. Heated product from the top of the heavy removal tower 14. Reflux liquid from the top of the heavy removal tower

[0034] 15. Top product from the deweighting tower 16. Pervaporated permeate

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

[0036] 19. Condensate 20. After deionization

[0037] 21. Acetone products Detailed Implementation

[0038] The endpoints and any values ​​of the ranges disclosed herein 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 the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

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

[0040] The raw material supply unit is used to provide oxidizing agent stream, crude acetone, and deacidifying agent, respectively.

[0041] The reaction dealdehyde unit is used to make the oxidizing reagent stream and crude acetone into the first contact to obtain the extracted liquid;

[0042] The acid removal unit is used to make a second contact between the produced fluid and the acid removal agent to obtain the deacidified product.

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

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

[0045] According to a preferred embodiment of the present invention, the reactive formaldehyde removal unit includes a fixed-bed reactor and a first inlet and a second inlet respectively disposed on the fixed-bed reactor; the first inlet is used for a portion of crude acetone as the first feed, and the second inlet is used for a mixture of another portion of crude acetone and an oxidizing reagent stream as the second feed. Using the aforementioned embodiment, the formaldehyde removal effect can be better increased.

[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; the second feed inlet is located in the upper middle part of the fixed bed reactor.

[0047] According to a particularly preferred embodiment of the present invention, the fixed-bed reactor is equipped with a distributor for distributing the mixture of crude acetone and oxidizing agent streams such that the first feed and the second feed form counter-current contact in the axial direction above the distributor. By employing the aforementioned embodiment, the second feed can be injected into counter-current contact with the first feed, increasing the mixing effect between the two. This ensures better mixing of the oxidizing agent stream and crude acetone even with a small amount of oxidizing agent added, resulting in a better dealdehyde removal effect.

[0048] According to a particularly preferred embodiment of the present invention, the outlet of the reactive formaldehyde removal unit is connected to the inlet of the acid removal unit and the outlet of the raw material supply unit where crude acetone is supplied, respectively. This allows a portion of the collected liquid to enter the acid removal unit, while the other portion is recycled back to the reactive formaldehyde removal unit as a circulating liquid. By employing the aforementioned embodiment, the residence time of crude acetone in the reactive formaldehyde removal unit can be increased, thereby improving the formaldehyde removal effect.

[0049] According to the present invention, in order to increase the mixing between materials, the fixed-bed reactor is preferably filled with packing material, such as at least one of structured wire mesh packing, bulk Pall rings, Sita rings, and triangular spiral packing. Using the aforementioned embodiments, the degree of disorder between materials can be increased, which is beneficial for the mixing between the oxidant and crude acetone, thereby improving the formaldehyde removal effect.

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

[0051] According to a particularly preferred embodiment of the present invention, the reaction vessel is a conical-bottomed reaction vessel. Using the aforementioned embodiment, some solid impurities can be retained at the bottom, facilitating their removal.

[0052] According to a particularly preferred embodiment of the present invention, a vertical plate is provided at the top of the interior of the reactor, dividing the interior of the reactor into a stirring zone and a discharge zone. The vertical plate extends downward and is spaced apart from the bottom of the reactor, so that the bottom of the stirring zone and the bottom of the discharge zone are in communication. Using the aforementioned embodiment, the entire acid removal process is completed within one reactor. Acid removal can be achieved through the stirring zone, and the material after acid removal can continuously flow out through the discharge zone.

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

[0054] According to a particularly preferred embodiment of the present invention, the upper part of the discharge zone is connected to the inlet of a distillation-coupled pervaporation unit, for the deacidified product to enter the distillation-coupled pervaporation unit for distillation and dehydration. A baffle is connected to the inner wall of the discharge zone below the connection point between the discharge zone and the distillation-coupled pervaporation unit. The baffle extends towards the vertical plate, and the gap between the baffle and the vertical plate forms a material passage. This embodiment can reduce the amount of solid impurities such as salt that may be present in the effluent, thereby reducing subsequent energy consumption and increasing the purification effect.

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

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

[0057] According to a particularly preferred embodiment of the present invention, the raw material supply unit provides an outlet for a deacidifying agent that 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-light removal tower, a heavy-light removal tower, and a pervaporation membrane separator connected in series. The light-light removal tower is used for distillation to remove light components from the product after acid removal. The heavy-light removal tower is used for distillation to remove heavy components from the product at the bottom of the light-light removal tower. The pervaporation membrane separator is used for dehydration of the product at the top of the heavy-light removal tower. The concentration-side outlet of the pervaporation membrane separator is connected to a circulation pipeline and a collection pipeline, respectively, and the concentration-side outlet is connected to the top of the heavy-light removal tower through the circulation pipeline. Using the aforementioned embodiment, the coupling of the heavy-light removal tower and the pervaporation membrane separator utilizes the high calorific value of the vapor phase product at the top of the heavy-light removal tower. The coupling process of returning the concentrated liquid from the pervaporation membrane separator to the heavy-light removal tower significantly reduces process energy consumption, improves energy utilization efficiency, and achieves significant dehydration and purification effects.

[0059] According to a particularly preferred embodiment of the present invention, the top of the deweighting tower is connected to the inlet of the pervaporation membrane separation device via a heating device. Using the aforementioned embodiment, during dehydration, the high calorific value of the vapor phase product at the top of the deweighting tower can be utilized, and after further heating to increase the calorific value, the conditions for pervaporation membrane separation can be 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 acid removal and the material at the concentration side outlet of the pervaporation membrane separator. The material at the concentration side after separation by the pervaporation membrane separator has a high calorific value. Using the aforementioned embodiment, the material entering the light-light removal tower (i.e., the product after acid removal) is a cold distillate stream that exchanges heat with the material at the concentration side after separation by the pervaporation membrane separator. This significantly reduces the energy consumption when purifying acetone using the system of the present invention, avoids the waste of high-grade energy and the consumption of large amounts of refrigerant, and improves heat utilization.

[0061] According to a preferred embodiment of the present invention, along the material flow direction, the system further includes: a flash evaporation unit, a condensation heat exchange unit, a deionization unit, and a departicle removal unit, used for flash evaporation followed by condensation, deionization, and departicle removal of the product after distillation and dehydration; the flash evaporation unit is connected to the outlet of the distillation-coupled pervaporation unit. Using the aforementioned embodiment, the flash evaporation unit further reduces the amount of refrigerant used in the subsequent condensation heat exchange unit during the condensation process, and further removes metal ions.

[0062] According to the present invention, the structure of the flash evaporation unit has no special requirements and can be a conventional flash evaporator 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 herein, and the method includes:

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

[0065] (2) The produced fluid and the deacidifying agent from the raw material supply unit are in a second contact in the reaction dealdehyde unit to obtain the deacidified product;

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

[0067] The method in this invention, through steps such as reaction-dealdehydeing-distillation-dehydration, can ultimately obtain high-quality electronic-grade acetone. Furthermore, after acid removal, the product enters a distillation-coupled pervaporation unit for distillation and dehydration, which enables the integration and comprehensive utilization of heat. Under the condition of continuous industrial operation, this further improves product quality and efficiency and reduces energy consumption.

[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 as the first feed through the first inlet of the fixed-bed reactor. The other part of the crude acetone, mixed with the oxidizing agent stream provided by the raw material supply unit, is used as the second feed through the second inlet of the fixed-bed reactor. The mixture then undergoes a first contact reaction with the first feed through a distributor to obtain the produced liquid. By employing the aforementioned embodiment, the mixing of the oxidizing agent stream and the crude acetone can be increased, ensuring dispersion and dealdehyde removal effects.

[0069] According to a preferred embodiment of the present invention, the volume ratio of crude acetone in the first feed to crude acetone in the second feed is (70-99):(1-30). By employing the aforementioned embodiment, the mixing of the oxidizing agent stream and crude acetone can be increased, ensuring dispersion and dealdehyde removal effects.

[0070] According to a preferred embodiment of the present invention, a portion of the collected fluid enters the deacidification unit and undergoes a second contact with the deacidifying agent provided by the raw material supply unit to obtain the deacidified product; the other portion of the collected fluid is recycled back to the reaction dealdehyde removal unit as a circulating liquid. By employing the aforementioned embodiment, the mixing of the oxidizing reagent stream and the crude acetone product can be increased, ensuring 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 any two of the above values. By adopting the aforementioned embodiment, the purity of the acetone product can be better increased.

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

[0073] According to a particularly preferred embodiment of the present invention, a portion of the extracted liquid enters the stirring zone of the reactor through the upper or upper-middle part of the stirring zone, while the acid-removing agent provided by the raw material supply unit enters the stirring zone through the top of the stirring zone. The extracted liquid and the acid-removing agent undergo a second contact within the stirring zone. The deacidified product obtained from this second contact continuously passes through the discharge zone and enters the light-duty removal tower. Using the aforementioned embodiment, the acid removal process can be completed within a single reactor. The extracted liquid and the acid-removing agent can be rapidly mixed in the stirring zone to remove impurities such as acids, and the effluent can continuously flow out through the discharge zone. Simultaneously, impurities such as salts can remain at the bottom of the reactor, increasing the overall purification effect.

[0074] According to a preferred embodiment of the present invention, the product after acid removal passes through a heat exchanger and then enters a light-light removal tower for distillation to remove light-light components. The product at the top of the heavy-light removal tower obtained from the distillation process enters a pervaporation membrane separator for dehydration. The dehydrated material is obtained from the concentration side outlet of the pervaporation membrane separator. The dehydrated material enters a heat exchanger and exchanges heat with the product after acid removal. Part of the dehydrated material after heat exchange is returned to the heavy-light removal tower as reflux liquid through a circulation pipeline, and the other part is collected as the dehydrated product. In the aforementioned embodiment, the pervaporation membrane separator is coupled to the top of the heavy-light removal tower. The coupling process involves the vapor phase at the top of the heavy-light removal tower entering the pervaporation membrane separator for dehydration, and part of the dehydrated material being returned to the heavy-light removal tower as reflux liquid through a circulation pipeline. By adopting the aforementioned embodiment, not only can the process energy consumption be greatly reduced and the energy utilization rate improved, but the acetone purification effect is also significant.

[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, for example, 100 kPa, 150 kPa, 175 kPa, or 200 kPa. Crude acetone contains light components such as propylene. Using the aforementioned positive pressure embodiment ensures that inexpensive ordinary water cooling can be used for the top condenser. Furthermore, under positive pressure, it prevents organic impurities from entering the system, thereby increasing the overall purification effect.

[0076] According to a particularly preferred embodiment of the present invention, the conditions for distillation to remove light components include a reflux ratio of 2-20, for example, 2, 5, 6, 10, 13, 15, or 20, preferably 2-10. By employing the aforementioned embodiment, the overall purification effect of crude acetone can be increased, while simultaneously improving the balance between the recovery rate of the product from the bottom of the light component removal column and the overall operating energy consumption.

[0077] According to a particularly preferred embodiment of the present invention, the conditions for the distillation to remove light components include: the bottom temperature of the light component removal column is 56.6-78.0°C, for example, 56.6°C, 68.7°C, 77.6°C, 78°C, or any combination of two of the aforementioned values. Using the aforementioned embodiment can increase the overall purification effect of crude acetone.

[0078] According to a particularly preferred embodiment of the present invention, the conditions for the distillation deweighting include: an operating pressure of 100-200 kPa, for example, 100 kPa, 150 kPa, 175 kPa, or 200 kPa. Crude acetone contains isopropanol, methanol, isopropyl ether, water, and some inorganic salts soluble in acetone, among other heavy components. Water and acetone have significantly different boiling points and do not exhibit azeotropy. However, experiments have shown that a large amount of water remains in the top product during the deweighting process, indicating incomplete separation of water and acetone. Using the aforementioned embodiment ensures that inexpensive ordinary water cooling can be used for the top condenser, and under positive pressure, it also prevents organic impurities from entering the system.

[0079] According to a particularly preferred embodiment of the present invention, the conditions for the distillation and deweighting process include: a column top temperature of 55.7-77.5°C, for example, 55.7°C, 68°C, 73°C, 77.5°C, or any combination of two of the aforementioned values. Using the aforementioned embodiment can increase the overall purification effect of crude acetone.

[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, or 605 kPa.

[0082] In this invention, the material entering the pervaporation membrane separation device can be heated to reach the required inlet temperature and pressure using a heating device.

[0083] According to a particularly preferred embodiment of the present invention, the mass flow ratio of the reflux liquid at the top of the heavy precipitate removal column to the dehydrated product is (1-5):1, for example, 1:1, 2:1, 3:1, 4:1, 5:1, or any range between two of the above ratios. Using the aforementioned embodiment can increase the overall purification effect of crude acetone, while simultaneously improving the balance between the recovery rate of the product from the bottom of the light precipitate removal column and the overall operating energy consumption.

[0084] In this invention, the conditions for the first contact are not particularly limited as long as the objective of the invention can be achieved. According to a particularly preferred embodiment of the invention, the conditions for the first contact include a temperature of 20-50°C. The research process also found that, using the aforementioned embodiment, the aldehyde removal effect of the oxidant can be maintained at a better level, which can better improve the overall purification effect of crude acetone.

[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 dwell 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 0.5-2 hours.

[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 crude acetone. By employing the aforementioned embodiment, aldehydes in acetone can be removed to a low level without wasting oxidizing agent.

[0091] According to a preferred embodiment of the present invention, the flow rate of the acid removal agent entering the formaldehyde removal unit is 0.001-0.01 times the flow rate of the produced fluid entering the reactive formaldehyde removal unit. By employing the aforementioned embodiment, the content of acidic impurities in the material can be better reduced.

[0092] According to a preferred embodiment of the present invention, the oxidant is selected from hydrogen peroxide aqueous solution and / or potassium permanganate aqueous solution. Using the aforementioned embodiment, the purification effect of acetone can be better improved.

[0093] According to a particularly preferred embodiment of the present invention, the mass concentration of the hydrogen peroxide aqueous solution is 20-40%. Using the aforementioned embodiment, the purification effect of acetone can be better increased.

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

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

[0096] In this invention, "optionally alkaline bicarbonate" refers to the option of adding or not adding alkaline bicarbonate as needed.

[0097] According to a particularly preferred embodiment of the present invention, the mass concentration of the alkaline hydroxide in the aqueous solution is 5-20 wt%. Too high a concentration would be unattainable, exceeding the saturation solubility, while too low a concentration would significantly increase the amount used, raising the water content of the product and increasing the burden on subsequent purification.

[0098] According to the present invention, the type of alkaline hydroxide is not particularly limited as long as the purpose of the present invention can be achieved. 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, the concentration of alkaline bicarbonate in the aqueous solution is 5-20 wt%, for example 5 wt%, 10 wt%, 15 wt%, or 20 wt%.

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

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

[0102] According to a preferred embodiment of the present invention, the method further includes sequentially flashing, condensing, deionizing, and departicle-removing the produced liquid after distillation and dehydration. Preferably, the flashing conditions include a pressure of 0.5-0.8 bar. By employing the aforementioned embodiment, the residual metal ions and particles in the dehydrated produced liquid can be reduced. Simultaneously, the vapor phase heat grade obtained through flashing is further reduced during 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] In this invention, condensation generally refers to condensation to room temperature.

[0105] In this invention, room temperature refers to 20-30℃.

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

[0107] According to the present invention, the method of demicronization is not particularly limited as long as the purpose of the invention can be achieved. For example, the demicronization unit is a plurality of membrane separators connected in series. PTFE, PVDF, and PE membrane separation materials exhibit good particle retention rates and low dissolution rates. The membrane separation material used in the membrane separator is selected from one of PTFE, PVDF, and PE. Preferably, a four-stage membrane separator is used, with filtration specifications of 500 nm, 200 nm, 100 nm, and 50 nm in sequence. Using the aforementioned embodiments, it is possible to remove ≤100 particles (≥0.1 μm) / ml from acetone products.

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

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

[0110] The method includes: acetone crude product 1 from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward by the distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4.

[0111] Part of the extracted liquid 4 enters the stirring zone from the top of the stirring zone of the reactor ②. The deacidifying agent 6 provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of the reactor ②. It makes a second contact with the part of the extracted liquid 4 that has entered the stirring zone to obtain the deacidified product 7. The other part of the extracted liquid 4 is mixed with crude acetone 1 as circulating liquid 5 and then continues to enter the fixed bed reactor ①.

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

[0113] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. After heat exchange, part of the dehydrated material is returned to the heavy-duty tower ④ via the circulation pipeline as the top reflux liquid 14 of the heavy-duty tower ④, and the other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower ⑧ for flash evaporation. The flash liquid phase 17 obtained from flash evaporation is discharged outside the interface for collection. The flash vapor phase 18 obtained from flash evaporation is condensed by condenser ⑨, and the condensate 19 obtained is entered into the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 passes through the departicle unit. After demicronization, acetone product 21 was obtained.

[0114] The present invention will be described in detail below through examples. In the following examples, the purity of the product was detected by HPLC, the moisture content was determined by Karl Fischer titration, the metal ions were determined by ICP-MS, and the particle number was determined by an online particle counter.

[0115] Example 1

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

[0117] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 20℃ and the residence time is 3h.

[0118] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.001 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 0.5h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0120] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0122] Example 2

[0123] Acetone purification methods in, for example Figure 1 The purification process is carried out in the acetone purification system shown: Figure 1 In the system shown, the demicronization unit is a four-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE. The filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with Pall ring bulk packing.

[0124] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 30℃ and the residence time is 3h.

[0125] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (5wt% NaOH aqueous solution, with a mass flow rate 0.01 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio 15) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0127] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.5 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0129] Example 3

[0130] Acetone purification methods in, for example Figure 1 The purification process is carried out in the acetone purification system shown: Figure 1 In the system shown, the demicronization unit is a four-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PE. The filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with Sital ring bulk packing.

[0131] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 5h.

[0132] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 2h, stirring speed 500rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio 20) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0134] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the de-heavy tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the de-heavy tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.8 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the demicronization unit. After demicronization, acetone product 21 was obtained.

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

[0136] Example 4

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

[0138] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 50℃ and the residence time is 3h.

[0139] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0141] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0143] Example 5

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

[0145] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0146] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0148] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0150] Example 6

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

[0152] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0153] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

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

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

[0157] Example 7

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

[0159] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0160] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

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

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

[0164] Example 8

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

[0166] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0167] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

[0168] The deacidified product 7 obtained from the second contact continuously passes through the discharge zone of reactor ② and flows out from the top of the discharge zone. After passing through heat exchanger ⑦, it becomes the deacidified product 8 after heat exchange. The deacidified product 8 enters the light-weight removal tower ③ from the middle and upper part of the light-weight removal tower ③ (the operating pressure of the light-weight removal tower ③ is 150 kPa, the operating reflux ratio is 10, and the temperature of the tower bottom of the light-weight removal tower ③ is controlled at 68.7℃). The top product 9 of the light-weight removal tower is discharged outside the boundary for collection, and the bottom product 10 of the light-weight removal tower enters the heavy-weight removal tower ④ from the middle and lower part of the heavy-weight removal tower. Heavy tower ④ (the operating pressure of heavy tower ④ is 200 kPa, and the vapor phase temperature at the top of heavy tower ④ is controlled at 77.5℃). The product 11 at the bottom of the heavy tower is discharged outside the boundary for collection. The product 12 at the top of the heavy tower is heated to 110℃ by reheater ⑤ to obtain the heated vapor product 13 at the top of the heavy tower. The heated vapor product 13 at the top of the heavy tower enters the pervaporation membrane separation device ⑥ (pressure 478 kPa). The pervaporated permeate 16 at the pervaporation side outlet of the pervaporation membrane separation device ⑥ is discharged outside the boundary for collection.

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

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

[0171] Example 9

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

[0173] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0174] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0176] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the de-heavy tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 (the mass flow ratio of reflux liquid 14 to product 15 is 5:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the demicronization unit. After demicronization, acetone product 21 was obtained.

[0177] The purity of the obtained acetone product 21 was determined to be 99.999%, the water content was 25 ppm, the total aldehyde content was 0.2 ppm, the concentration of single metal ions in acetone product 21 was ≤100 ppt, and the particle count (≥0.1 μm) was ≤100 particles / ml, meeting the technical requirements for electronic grade acetone.

[0178] Example 10

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

[0180] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0181] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

[0182] The deacidified product 7 obtained from the second contact continuously passes through the discharge zone of reactor ② and flows out from the top of the discharge zone. After passing through heat exchanger ⑦, it becomes the deacidified product 8 after heat exchange. The deacidified product 8 enters the light-weight removal tower ③ from the middle and upper part of the light-weight removal tower ③ (the operating pressure of the light-weight removal tower ③ is 150 kPa, the operating reflux ratio is 10, and the temperature of the tower bottom of the light-weight removal tower ③ is controlled at 68.7℃). The top product 9 of the light-weight removal tower is discharged outside the boundary for collection, and the bottom product 10 of the light-weight removal tower enters the heavy-weight removal tower ④ from the middle and lower part of the heavy-weight removal tower. Heavy tower ④ (the operating pressure of heavy tower ④ is 100 kPa, and the vapor phase temperature at the top of heavy tower ④ is controlled at 55.7℃). The product 11 at the bottom of the heavy tower is discharged outside the boundary for collection. The product 12 at the top of the heavy tower is heated to 110℃ by reheater ⑤ to obtain the heated vapor product 13 at the top of the heavy tower. The heated vapor product 13 at the top of the heavy tower enters the pervaporation membrane separation device ⑥ (pressure 478 kPa). The pervaporated permeate 16 at the pervaporation side outlet of the pervaporation membrane separation device ⑥ is discharged outside the boundary for collection.

[0183] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0185] Example 11

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

[0187] The method includes: acetone crude product 1 (purity 99.2%, water content 2700ppm, total aldehyde content 30ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0188] Part of the extracted liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% KOH aqueous solution, with a mass flow rate 0.005 times that of the extracted liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the extracted liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the extracted liquid 4 is used as the circulating liquid 5 (circulation ratio 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0190] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0192] Example 12

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

[0194] The method includes: acetone crude product 1 (purity 99.2%, water content 2700ppm, total aldehyde content 30ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0195] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0197] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0199] Example 13

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

[0201] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0202] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0204] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0206] Example 14

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

[0208] The method includes: acetone crude product 1 (purity 99.2%, water content 2700 ppm, total aldehyde content 30 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0209] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.005 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio of 10) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0211] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0213] Example 15

[0214] Acetone purification methods in, for example Figure 1 The purification process is carried out in the acetone purification system shown: ​ In the system shown, the demicronization unit is a four-stage membrane separator connected in series, and the membrane separation material of the membrane separator is PTFE. The filtration specifications are 500nm, 200nm, 100nm and 50nm respectively; the fixed bed reactor ① is filled with regular wire mesh packing.

[0215] The method includes: acetone crude product 1 (purity 98.5%, water content 3400 ppm, total aldehyde content 166 ppm) from the raw material supply unit is divided into two parts. One part of acetone crude product 1 is used as the first feed and enters the fixed bed reactor 1 from the first feed port at the top of the fixed bed reactor 1. The other part of acetone crude product 1 (the amount used is 25% of the total volume of acetone crude product 1) is used as the second feed and enters the fixed bed reactor 1 from the second feed port at the top of the fixed bed reactor 1. After being injected upward through a distributor, it undergoes a first contact reaction with the first feed to obtain the produced liquid 4. The temperature of the fixed bed reactor 1 is controlled at 40℃ and the residence time is 3h.

[0216] Part of the produced liquid 4 enters the stirring zone from the top of the stirring zone of reactor ②. The acid removal agent 6 (20wt% NaOH aqueous solution, with a mass flow rate 0.01 times that of the produced liquid 4 entering reactor ②) provided by the raw material supply unit enters the stirring zone through the top of the stirring zone of reactor ②. It makes a second contact with the part of the produced liquid 4 entering the stirring zone (residence time 1h, stirring speed 200rpm) to obtain the deacidified product 7. The other part of the produced liquid 4 is used as the circulating liquid 5 (circulation ratio 20) and mixed with crude acetone 1 before continuing to enter the fixed bed reactor ①.

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

[0218] The dehydrated material obtained from the concentration outlet of the pervaporation membrane separation unit ⑥ is exchanged with the deacidified product 7 via heat exchanger ⑦. Part of the dehydrated material after heat exchange is returned to the top of the heavy-duty tower ④ via a circulation pipeline as reflux liquid 14. The other part is entered into the flash tank ⑧ as the top product 15 of the heavy-duty tower (the mass flow ratio of reflux liquid 14 to product 15 is 1:1) for flash evaporation (flash pressure is 0.6 bar). The flash liquid phase 17 is discharged and collected outside the boundary. The flash vapor phase 18 is condensed to room temperature by condenser ⑨, and the resulting condensate 19 enters the adsorption tower ⑩ (filled with a uniformly mixed hydrogen-form strong acid cation exchange resin and hydroxide-form strong base anion exchange resin) for deionization to obtain the deionized product 20. The deionized product 20 then passes through the departicle unit. After demicronization, acetone product 21 was obtained.

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

[0220] Example 16

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

[0222] The purity of the obtained acetone product 21 was determined to be 99.994%, the water content was 50 ppm, the total aldehyde content was less than 0.1 ppm, the concentration of single metal ions in acetone product 21 was ≤100 ppt, and the particle count (≥0.1 μm) was ≤100 particles / ml, meeting the technical requirements for electronic grade acetone.

[0223] Example 17

[0224] Please add: The method of Example 3 is the same as in Example 3, except that the concentration of NaOH in the NaOH and NaHCO3 aqueous solutions is 20 wt% and the concentration of NaHCO3 is 5 wt%.

[0225] The purity of the obtained acetone product 21 was determined to be 99.994%, the water content was 52 ppm, the total aldehyde content was less than 0.1 ppm, the concentration of single metal ions in acetone product 21 was ≤100 ppt, and the particle count (≥0.1 μm) was ≤100 particles / ml, meeting the technical requirements for electronic grade acetone.

[0226] Example 18

[0227] The method of Example 3 was followed, except that the circulation ratio of the circulating liquid was 1, while the rest was the same as in Example 3, and acetone product was finally obtained.

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

[0229] Comparative Example 1

[0230] The method of Example 3 is followed, except that the acid remover 6 is added to the fixed-bed reactor along with the oxidizing agent stream 3. Otherwise, the same as in Example 3 is used to obtain acetone product.

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

[0232] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. An acetone purification system, characterized by, The system comprises: a raw material supply unit for supplying an oxidizing agent stream, crude acetone and an acid-removing agent respectively; a reaction de-aldehyde unit for the first contact of the oxidizing agent stream with the crude acetone to obtain a product stream; an acid-removing unit for the second contact of the product stream with the acid-removing agent to obtain an acid-removed product; a rectification-coupled pervaporation unit for the rectification and dehydration of the acid-removed product; the rectification-coupled pervaporation unit comprises a light-removing column, a heavy-removing column and a pervaporation membrane separation device connected in series; the light-removing column is used for the rectification of the acid-removed product; the heavy-removing column is used for the rectification of the product from the light-removing column; the pervaporation membrane separation device is used for the dehydration of the product from the heavy-removing column, and the top of the heavy-removing column is connected to the inlet of the pervaporation membrane separation device through a heating device; the concentrated side outlet of the pervaporation membrane separation device is connected to a circulating pipeline and a product pipeline respectively, and the concentrated side outlet is connected to the top of the heavy-removing column through the circulating pipeline; the rectification-coupled pervaporation unit further comprises a heat exchange device for the heat exchange of the acid-removed product and the material from the concentrated side outlet of the pervaporation membrane separation device, and the heat-exchanged product enters the inlet of the rectification-coupled pervaporation unit.

2. The system according to claim 1, wherein the reaction de-aldehyde unit comprises a fixed bed reactor and a first feed inlet and a second feed inlet arranged on the fixed bed reactor respectively; the first feed inlet is used for the first feed of part of the crude acetone, and the second feed inlet is used for the second feed of the mixture of another part of the crude acetone and the oxidizing agent stream; and / or the outlet of the reaction de-aldehyde unit is connected to the inlet of the acid-removing unit and the outlet of the raw material supply unit for supplying the crude acetone respectively, so that part of the product stream enters the acid-removing unit, and another part of the product stream circulates back to the reaction de-aldehyde unit as a circulating liquid.

3. The system according to claim 2, wherein the first feed inlet is located at the top of the fixed bed reactor, and the second feed inlet is located at the upper part or the middle-upper part of the fixed bed reactor; and / or a distributor is arranged inside the fixed bed reactor, which is used for the distribution of the mixture of the crude acetone and the oxidizing agent stream so that the first feed and the second feed form a reverse contact in the axial direction above the distributor.

4. The system according to claim 1, wherein the acid-removing unit comprises a reaction kettle.

5. The system according to claim 4, wherein the reaction kettle is a reaction kettle with a conical bottom; and / or a vertical plate is arranged at the top inside the reaction kettle to divide the inside of the reaction kettle into a stirring zone and a discharge zone, the vertical plate extends downward and is arranged spaced apart from the bottom of the reaction kettle, so that the stirring zone is in communication with the bottom of the discharge zone.

6. The system according to claim 5, wherein the upper part of the discharge zone is connected to the inlet of the rectification-coupled pervaporation unit, so that the acid-removed product enters the rectification-coupled pervaporation unit for rectification 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 rectification-coupled pervaporation unit, the baffle extends to the vertical plate and forms a material passing gap between the baffle and the vertical plate.

7. The system of claim 6, wherein, The baffle position is located in the upper part of the discharge area.

8. The system according to claim 1, wherein, the outlet of the reaction de-aldehyde unit is connected with the upper or middle upper part of the stirring area; and / or the outlet of the acid scavenger provided in the raw material supply unit is connected with the top of the stirring area.

9. The system according to any one of claims 1-8, wherein, in the direction of the material flow, the system further comprises a flash unit, a condensation heat exchange unit, a de-ionization unit and a de-particulate unit for condensation, de-ionization and de-particulate of the product after rectification and dehydration; the flash unit is connected with the outlet of the rectification coupled pervaporation unit.

10. A method for purifying acetone, characterized by, The method is carried out in the system according to any one of claims 1-9, and the method comprises: (1) the crude acetone from the raw material supply unit is contacted with the oxidizing agent stream for the first time to obtain a product; (2) the product is contacted with the acid scavenger from the raw material supply unit in the reaction de-aldehyde unit to obtain a product after acid scavenging; (3) the product after acid scavenging is subjected to rectification and dehydration in the rectification coupled pervaporation unit.

11. The method according to claim 10, wherein, 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 of the fixed bed reactor as the first feed, 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 enters the fixed bed reactor from the second feed port of the fixed bed reactor as the second feed and is contacted with the first feed through the distributor to obtain the product.

12. The method according to claim 11, wherein, the volume ratio of the crude acetone in the first feed to the crude acetone in the second feed is (70-99):(1-30).

13. The method according to claim 10, wherein, part of the product enters the acid scavenging unit to be contacted with the acid scavenger provided by the raw material supply unit in the acid scavenging unit to obtain a product after acid scavenging, and the other part of the product is recycled back to the reaction de-aldehyde unit as a circulating liquid.

14. The method of claim 13, wherein, The circulation ratio of the circulating liquid is 2-20.

15. The method according to any one of claims 10-14, wherein, after the product after acid scavenging passes through the heat exchange device, the product enters the light-removing column from the upper part of the light-removing column for rectification and light removal, the column top product obtained by rectification and light removal enters the heavy-removing column from the middle lower part of the heavy-removing column for rectification and heavy removal, the column top product obtained by rectification and heavy removal enters the pervaporation membrane separation device for dehydration, the concentrated side outlet of the pervaporation membrane separation device obtains a dehydrated material, and the dehydrated material enters the heat exchange device to exchange with the product after acid scavenging entering the heat exchange device for heat exchange, and part of the dehydrated material after heat exchange returns to the heavy-removing column as the column top reflux liquid through the circulation pipeline, and the other part is taken out as the dehydrated product.

16. The method according to claim 15, wherein, the conditions of rectification and light removal include: the operating pressure is 100-200 kPa; and / or, the reflux ratio is 2-20; and / or, the column bottom temperature of the light-removing column is 56.6-78.0℃; and / or The conditions of the rectification and heavy component removal include: an operating pressure of 100-200 kPa; and / or, a heavy component removal column overhead temperature of 55.7-77.5℃; and / or The conditions of the dehydration include: an inlet temperature of 60-120℃; and / or a pressure of 115-605 kPa; and / or The mass flow ratio of the heavy component removal column overhead reflux liquid to the dehydrated produced liquid is (1-5):

1.

17. The method of claim 10, wherein, The conditions of the first contact include: a temperature of 20-50℃; and / or, a residence time of 1-5h; and / or The conditions of the second contact 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 of the oxidizing agent stream is 0.001-0.01 times the mass flow of the crude acetone; and / or The flow of the acid removal agent into the de-aldehyde unit is 0.001-0.01 times the flow of the produced liquid into the reaction de-aldehyde unit; and / or The oxidizing agent is a hydrogen peroxide solution and / or a potassium permanganate solution; and / or The acid removal agent includes an aqueous solution of a basic hydroxide and a basic bicarbonate; and / or The crude acetone has a purity of 98.5-99.9%, and / or the crude acetone contains aldehyde 20-500ppm; and / or The method further includes that the produced liquid after the rectification and dehydration is sequentially subjected to flashing, condensing, de-ionization, and de-particle.

18. The method of claim 17, wherein, 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 In the aqueous solution, the mass concentration of the basic hydroxide is 5-20wt%; and / or, the basic hydroxide is sodium hydroxide and / or potassium hydroxide; and / or, the concentration of the basic bicarbonate in the aqueous solution is 5-20wt% and / or, the basic bicarbonate is sodium bicarbonate and / or potassium bicarbonate; and / or The conditions of the flashing include: a pressure of 0.5-0.8bar.

Images