Acetone purification method, acetone purification equipment, high-purity isopropanol preparation method and application

Abstract

The invention discloses an acetone purification method, acetone purification equipment, and a preparation method and application of high-purity isopropanol, acetone to be purified is contacted with an oxidizing agent in a protective gas atmosphere, dehydration and refining are performed to obtain purified acetone, and high-purity acetone can be obtained.

Description

Technical Field

[0001] The invention relates to an acetone purification method and acetone purification equipment, and a preparation method and application of high-purity isopropanol. Background Art

[0002] Isopropyl alcohol is the most widely used organic solvent in wet electronic chemicals, mainly used for cleaning and drying. Isopropyl alcohol for integrated circuits has strict requirements on trace organic impurity content, metal cation impurity content, particle size and number, anion impurity content, etc. With the intensive production of wafer fabs and the continuous breakthroughs in advanced process nodes of integrated circuits, the demand for G4-G5 high-grade isopropyl alcohol has gradually increased. At the same time, acetone is also a solvent and cleaning reagent that should be extremely widely used. High-purity acetone is an important basic reagent that is indispensable for the production of microelectronics industry and the analysis of food and pesticide residues. At present, the purity of acetone has become one of the constraints for expanding its high-end application. However, the purification effect of existing purification methods is relatively general. Therefore, how to further improve the purity of acetone is a technical problem that needs to be solved at present.

[0003] CN104245655B discloses a method for purifying a crude acetone logistics, wherein the crude acetone logistics is treated with a solid acid catalyst, and acetone is reacted with low-boiling impurities to form high-boiling impurities, which can be used to produce purified isopropanol after separation. As can be seen from the embodiments, by this method, the acetaldehyde content can be reduced by 47-88%, the propionaldehyde content can be reduced by 75-99%, and the isobutyraldehyde content can be reduced by 28-75%. However, this method is not for high-end ultrapure reagents for integrated circuits (purity requirements: single metal impurity ion content is less than 0.1ppb, moisture content is less than 50ppm, and particles greater than 0.2μm are less than 100 / mL), so the removal rate of the above embodiment cannot meet high-end uses, and the method also causes acetone raw material loss while reacting low-boiling impurities, and there are many by-products.

[0004] In addition, acetone has a high saturated vapor pressure and strong volatility. When solid materials are added, a large amount of acetone vapor will overflow, causing safety hazards. Summary of the invention

[0005] The purpose of the present invention is to provide an acetone purification method and acetone purification equipment, a preparation method and application of high-purity isopropanol, which have the advantage of improving the purity of acetone.

[0006] In order to achieve the above object, the present invention provides a method for purifying acetone, wherein the acetone to be purified is contacted with an oxidant under a protective gas atmosphere, dehydrated, and refined to obtain purified acetone.

[0007] Preferably, the protective gas atmosphere is selected from at least one of nitrogen, argon or helium.

[0008] Preferably, the oxidant is selected from one or more of an inorganic oxidant, an organic oxidant and a metal oxygen complex.

[0009] Preferably, the metal oxygen complex is an organic ligand compound with a metal element as the central atom.

[0010] More preferably, the metal oxygen-containing complex has a cyclic ether organic compound as a ligand.

[0011] Preferably, the metal oxygen complex has a structure shown in formula (I),

[0012]

[0013] A second aspect of the present invention provides an acetone purification device, the purification device comprising:

[0014] A reaction unit, comprising an acetone feed port for purification, an acetone discharge port for purification, an oxidant feed bin, a protective gas inlet port and a protective gas outlet port, wherein the reaction unit is used to contact the acetone for purification with the oxidant under a protective gas atmosphere;

[0015] a dehydration unit, connected to the reaction unit, and used to dehydrate the material from the reaction unit;

[0016] The refining unit is connected to the dehydration unit and is used to purify the material from the dehydration unit to obtain purified acetone.

[0017] The present invention discloses a method for preparing high-purity isopropyl alcohol, comprising: (1) purifying acetone using the acetone purification method of the present invention;

[0018] (2) In the presence of a hydrogenation catalyst, the purified acetone obtained in step (1) is subjected to a hydrogenation reaction with hydrogen to obtain crude isopropanol, and the crude isopropanol is refined to obtain high-purity isopropanol.

[0019] The invention discloses a method for preparing high-purity isopropyl alcohol. The high-purity isopropyl alcohol prepared by the method is used in integrated circuits after being deionized and degranulated. The high-purity isopropyl alcohol has an isopropyl alcohol content of more than 99.99%, a total organic impurity content of less than 10 ppm, a metal cation content of less than 10 ppt, and particulate matter of less than 100 pcs / ml.

[0020] Through the above technical scheme, the present invention obtains purified acetone by contacting the acetone to be purified with an oxidant under a protective gas atmosphere, dehydrating, and refining. The obtained purified acetone has high purity, and can realize the industrial production of high-purity acetone and other high-purity reagents prepared by using acetone as a raw material. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1It is a schematic structural diagram of an acetone purification device according to an embodiment of the present invention;

[0022] Figure 2 It is a schematic structural diagram of an acetone purification device according to another embodiment of the present invention.

[0023] Description of Reference Numerals

[0024] 2 oxidant feeding bin; 3 stirring device; 4 purified acetone feeding port; 5 purified acetone discharging port; 6 exhaust port; 7 sealing gasket; 8 baffle; 9 jacket; 10 stirring paddle; 11 heat exchange medium inlet; 12 heat exchange medium outlet; 13 lower bin cover; 16 upper bin cover; 17 protective gas inlet; 18 outlet. DETAILED DESCRIPTION

[0025] The specific implementation of the present invention is described in detail below in conjunction with the accompanying drawings. It should be understood that the specific implementation described here is only used to illustrate and explain the present invention, and is not used to limit the present invention.

[0026] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0027] In the present invention, unless otherwise specified, directional words such as "up, down, left, right" generally refer to up, down, left, right as shown in the reference drawings; "inside and outside" refer to inside and outside relative to the outline of each component itself.

[0028] The first aspect of the present invention discloses a method for purifying acetone, wherein the acetone to be purified is contacted with an oxidant under a protective gas atmosphere, dehydrated, and refined to obtain purified acetone.

[0029] The method of the invention allows the acetone to be purified to contact with an oxidant under a protective gas atmosphere, thereby realizing the industrial production of high-purity acetone and other high-purity reagents prepared by using acetone as a raw material.

[0030] According to a preferred embodiment of the present invention, the protective gas atmosphere is selected from at least one of nitrogen, argon or helium, thereby efficiently realizing the industrial production of high-purity acetone.

[0031] In the present invention, the contact conditions have a wide range of optional conditions. The following exemplary description is provided, but the scope of the present invention is not limited thereby. For the present invention, the contact conditions include: room temperature to 60° C.; and / or, normal pressure to 0.5 MPa. Thus, the industrial production of high-purity acetone can be efficiently realized.

[0032] In the present invention, there are no special requirements for the dehydration conditions, and commonly used dehydrating agents and dehydration steps can be used in the present invention. The following exemplary description does not limit the scope of the present invention. According to one embodiment of the present invention, dehydration includes: dehydrating with a dehydrating agent. The present invention has no special requirements for the dehydrating agent. The dehydrating agent can be selected from one or more of molecular sieves, silica gel, membranes, resins and salts. For example, in the present invention, the molecular sieve can be selected from 4A molecular sieves or 3A molecular sieves, the silica gel can be selected from color-changing silica gel, the membrane can be selected from at least one of ultrafiltration membranes, nanofiltration membranes or ceramic membranes, the resin can be selected from polyacrylic acid-based superabsorbent resins, and the salt is a salt that can form a crystalline hydrate, including but not limited to copper sulfate, calcium sulfate, sodium sulfate or potassium carbonate.

[0033] In the present invention, there is no special requirement for the refining conditions, and commonly used refining steps can be used in the present invention. The following exemplary description is not intended to limit the scope of the present invention. The refining in the present invention includes: distilling the dehydrated product, and during the distillation process, collecting a 54-58° C. fraction as purified acetone.

[0034] In the present invention, there are no special requirements for the source and composition of the raw materials of the acetone to be purified. The following exemplary description is provided, but the scope of the present invention is not limited thereby. According to one embodiment of the present invention, the impurities in the acetone to be purified in the present invention include at least one of aldehydes, alcohols or olefins.

[0035] In the present invention, conventional impurity aldehydes are applicable to the present invention, which are exemplified below, but the scope of the present invention is not limited thereby. According to one embodiment of the present invention, the aldehydes preferably include C2-C3 aldehydes.

[0036] In the present invention, conventional impurity olefins are applicable to the present invention, which are exemplified below, but the scope of the present invention is not limited thereby. According to one embodiment of the present invention, the olefins preferably include C2-C3 olefins.

[0037] According to a preferred embodiment of the present invention, the purified acetone of the present invention comprises: the acetone content in the purified acetone is above 99.99%; the content of total organic impurities in the purified acetone is below 10 ppm.

[0038] In the present invention, the acetone content in the acetone to be purified is ≥99.93%, and the acetone to be purified includes one or more of industrial-grade acetone, analytical-grade acetone and electronic-grade acetone, wherein the purity of industrial-grade acetone is 99.93%; the purity of analytical-grade acetone is 99.98%; and the purity of electronic-grade acetone is 99.98%. In the present invention, the purity of industrial-grade acetone, analytical-grade acetone and electronic-grade acetone refers to the percentage of acetone in total organic components, which is measured by GC using an area normalization method.

[0039] According to a preferred embodiment of the present invention, the amount of the oxidant added is greater than 0.01% by weight of the acetone to be purified, preferably greater than or equal to 0.02%, and more preferably 0.03%-0.1%.

[0040] The oxidant of the present invention is selected from one or more of an inorganic oxidant, an organic oxidant and a metal oxygen-containing complex; for example, the inorganic oxidant can be selected from at least one of potassium permanganate, oxygen or hydrogen peroxide; the organic oxidant can be selected from at least one of a metal oxygen-containing complex, isopropyl benzene peroxide or meta-chloroperbenzoic acid.

[0041] The oxidant in the present invention is a solid oxidant, which is a certain oxidant (such as an inorganic oxidant or an organic oxidant or a metal oxygen-containing complex) or a mixed oxidant including at least two oxidants (such as an inorganic oxidant and a metal oxygen-containing complex).

[0042] According to a preferred embodiment of the present invention, the solid oxidant comprises an inorganic oxidant and a metal oxygen-containing complex, and preferably the mass ratio of the inorganic oxidant to the metal oxygen-containing complex is 1:1-100:1.

[0043] In the present invention, the metal oxygen-containing complex is an organic ligand compound with a metal element as a central atom, which can improve the purity of acetone.

[0044] In the present invention, the cyclic ether organic compound is used as a ligand in the metal oxygen-containing complex.

[0045] In the present invention, the metal element includes at least one of a VIB group metal element, a VIIB group metal element and a VIII group metal element.

[0046] In the present invention, it is preferred that the VIB group metal element include one or more of Cr, Mo and W.

[0047] In the present invention, the Group VIIB metal element includes one or more of Mn, Tc and Re.

[0048] In the present invention, the Group VIII metal element includes one or more of Fe, Co, Ni, Ru, Rh, Pd and Pt.

[0049] According to a preferred embodiment of the present invention, the metal oxygen complex has a structure shown in formula (I):

[0050]

[0051] In formula (I), R1 and R2 are each independently selected from H, C1-C10 alkyl, substituted or unsubstituted benzyl, substituted or unsubstituted aromatic group; M is the metal element; X includes an element or group providing a non-metallic anion; n is an integer of 0-6, wherein when n is 0, the cyclic ether organic compound is a five-membered ring structure, when n is 1, the cyclic ether organic compound is a six-membered ring structure, and so on.

[0052] In some embodiments of the present invention, multiple R1s and multiple R2s are the same or different. According to a preferred embodiment of the present invention, in formula (I), R1 and R2 are each independently selected from H, C1-C3 alkyl, benzyl, C1-C2 alkyl substituted phenyl, C1-C2 alkyl substituted naphthyl; in some embodiments of the present invention, n is an integer of 0-3.

[0053] In some embodiments of the present invention, the element or group providing the non-metallic anion includes at least one of chlorine, iodine and acetate.

[0054] In some embodiments of the present invention, the preparation method of the metal oxygen-containing complex includes: providing a ligand solution of the ligand and a metal salt solution of the central atom for coordination reaction, then performing an oxidation reaction, and after the oxidation reaction, performing desolventizing, extraction, and drying to obtain the metal oxygen-containing complex. The present invention has no special requirements for the oxidant added in the oxidation reaction during the preparation of the metal oxygen-containing complex, and can include one or more of air, oxygen, hydrogen peroxide, isopropyl benzene peroxide, peracetic acid, perchlorate, permanganate and dichromate.

[0055] In some embodiments of the present invention, the coordination reaction and / or oxidation reaction is carried out in an inert atmosphere, wherein the conditions for the coordination reaction include: reaction at room temperature (room temperature in the present invention is 10-30° C.) for 1-10 hours; the conditions for the oxidation reaction include: reaction time of 1-10 hours.

[0056] In some embodiments of the present invention, the molar ratio of the metal salt to the ligand is 1:(1-1.2).

[0057] A second aspect of the present invention discloses an acetone purification device, the purification device comprising:

[0058] The reaction unit comprises a feed port 4 for acetone to be purified, a discharge port 5 for purified acetone, an oxidant feeding bin 2, a protective gas inlet 17 and a gas outlet 18, and the reaction unit is used to contact the acetone to be purified with the oxidant under a protective gas atmosphere;

[0059] A dehydration unit, connected to the reaction unit, for dehydrating the material from the reaction unit;

[0060] The refining unit is connected to the dehydration unit and is used to purify the material from the dehydration unit to obtain purified acetone.

[0061] The acetone purification equipment of the present invention can contact the acetone to be purified with an oxidant under a protective gas atmosphere, and can realize the industrial production of high-purity acetone and other high-purity reagents prepared by using acetone as a raw material.

[0062] In some embodiments of the present invention, the reaction unit includes a reactor, the dehydration unit includes a dehydration tower, and the refining unit includes a distillation device. Along the material flow direction, the reactor, the dehydration tower and the distillation device are connected in sequence. The present invention has no special requirements for the dehydration tower and the distillation device, and no further details are given here.

[0063] In some embodiments of the present invention, Figure 1 or Figure 2 As shown, a jacket 9 is provided outside the reactor, and a heat exchange medium inlet 11 and a heat exchange medium outlet 12 are provided; the reactor comprises a reactor body sleeved in the jacket and a top head with a sealing cover provided on the top of the reactor body, the reactor body and the top head form a closed reaction chamber, a baffle 8 and a stirring device 3 are provided in the reaction chamber, the upper end of the stirring shaft of the stirring device 3 is installed on the top head, and a stirring paddle 10 is installed at the lower end of the stirring shaft for stirring the material in the reaction chamber; a drain port 6 with a valve is provided at the bottom end of the reactor body, and the reactor is provided with a feed pipe for acetone to be purified and a discharge pipe for purified acetone, wherein the bottom ends of the feed pipe for acetone to be purified and the discharge pipe for purified acetone are both extended into the bottom of the reaction chamber, and the top ends of the feed pipe for acetone to be purified and the discharge pipe for purified acetone extend out of the top head to form a feed port 4 for purified acetone and a discharge port 5 for purified acetone (at Figure 1 From the perspective, the purified acetone discharge pipe is located behind the acetone feed pipe to be purified), and the reactor is also provided with a gas outlet and a protective gas inlet 17 for feeding protective gas into the reaction chamber.

[0064] In some embodiments of the present invention, an oxidant feed port is provided on the top cover, and an oxidant feeding bin 2 for storing solid oxidant is sealed and installed on the oxidant feed port, the oxidant feeding bin is connected to the reaction chamber, and an automatically opened and closed lower bin cover 13 is provided in the oxidant feeding bin 2, and an upper bin cover 16 is also provided in the oxidant feeding bin 2, and when the lower bin cover and the upper bin cover are closed, the oxidant feeding bin forms a sealed cavity; a protective gas inlet 17 (a protective gas inlet pipe connected to the installed valve) and an outlet (an outlet pipe connected to the installed valve) can be provided on the upper bin cover 16, and when the lower bin cover is closed, , open the upper bin cover 16 to add solid oxidant to the oxidant feeding bin, introduce protective gas into the oxidant feeding bin 2 to replace the air for multiple times (for example, more than 2 times), and then open the lower bin cover 13 to feed the solid oxidant into the reaction chamber. In order to realize that all the solid oxidant in the oxidant feeding bin 2 is fed into the reaction chamber at one time, the lower bin cover is configured to be able to be fully opened. For example, the lower bin cover can be connected by a hinge in the prior art. In addition, the control component in the prior art is adopted to realize the automatic opening and closing of the lower bin cover 13. The control component of the present invention can be selected from a conventional solenoid valve, and there is no special requirement for this in the present invention.

[0065] It should be noted that the oxidant feed port and the oxidant charging bin 2 can be designed to be sealed with a flange structure equipped with a sealing gasket 7, and the upper bin cover and the oxidant charging bin 2 can also be designed to be a flange structure connection or a quick-opening door structure commonly used in pressure vessels. The present invention has no special requirements for this and will not be elaborated here.

[0066] In the present invention, it is preferred that the oxidant feeding bin 2 is configured to be cylindrical or funnel-shaped.

[0067] The reactor of the present invention can realize sealed feeding, and has the advantages of convenient operation and safety. Specifically, it can well overcome the problem that a large amount of acetone vapor overflows when solid materials are fed due to the high saturated vapor pressure and strong volatility of acetone, thereby causing potential safety hazards.

[0068] The third aspect of the present invention discloses a method for preparing high-purity isopropanol, comprising: (1) purifying acetone using the acetone purification method of the present invention; (2) subjecting the purified acetone obtained in step (1) to a hydrogenation reaction with hydrogen in the presence of a hydrogenation catalyst to obtain crude isopropanol, and refining the crude isopropanol to obtain high-purity isopropanol.

[0069] In the present invention, the hydrogenation reaction conditions include: the molar ratio of purified acetone to hydrogen is 1:(1-30).

[0070] In the present invention, the air velocity of purified acetone is 0.1-1.5h -1 .

[0071] In the present invention, the reaction inlet temperature is 80-120° C. and the reaction pressure is 2.5-6 MPa.

[0072] In the present invention, the hydrogenation catalyst comprises an active component and a carrier; preferably, the content of the active component is 1-10wt% based on the total mass of the hydrogenation catalyst; preferably, the active component comprises one or more of copper, nickel and ruthenium.

[0073] In the present invention, refining crude isopropyl alcohol comprises: passing the crude isopropyl alcohol into a vacuum distillation tower for vacuum distillation to obtain high-purity isopropyl alcohol.

[0074] In the present invention, preferably, the conditions for reduced pressure distillation include: the bottom temperature is 60-74° C.; the vacuum degree is 350-500 mbar; and the fraction at 45-50° C. is collected as high-purity isopropanol.

[0075] The invention discloses a method for preparing high-purity isopropyl alcohol. The prepared high-purity isopropyl alcohol is used in integrated circuits after being deionized and degranulated. The isopropyl alcohol content in the high-purity isopropyl alcohol is greater than 99.99%, the total organic impurity content is less than 10 ppm, the metal cation is less than 10 ppt, and the particulate matter is less than 100 pcs / ml.

[0076] The advantages of the present invention are described below by way of examples, but the present invention is not limited thereto. The results of the examples in the present invention are measured by GC, GC-MS, and ICP. The purity involved in the present invention is measured by GC area normalization method.

[0077] In the following examples, the metal oxygen complex has a structure shown in formula (I):

[0078]

[0079] Example 1

[0080] like Figure 1 or Figure 2 As shown, the upper bin cover 16 of the oxidant charging bin 2 of the reactor is closed, and the atmosphere in the oxidant charging bin 2 and the reactor is replaced three times with analytical pure nitrogen through the protective gas inlet 17 and the gas outlet 18, and the protective gas inlet 17, the gas outlet 18 and the lower bin cover 13 are closed. The upper bin cover 16 is opened, the solid oxidant is added, the upper bin cover is closed, and the atmosphere in the oxidant charging bin is replaced three times with analytical pure nitrogen through the protective gas inlet and the gas outlet, and the protective gas inlet and the gas outlet are closed.

[0081] Analytical grade acetone (purity 99.98%) is used as a raw material (acetone to be purified), which is pressurized by a raw material pump and then enters a reaction chamber of a reactor. After the feeding of the purified acetone is completed, the lower compartment cover is opened, and a solid oxidant in an amount of 0.03% by weight of the analytical grade acetone to be purified is added to the acetone to be purified, and the mixture is stirred and reacted at room temperature and pressure for 2 hours. The effluent after contact is sequentially introduced into a dehydration tower equipped with a 4A molecular sieve, and the flow rate of the effluent is 30 L / h; after dehydration, the effluent is introduced into a distillation device for distillation at normal pressure at a temperature of 74° C., and a fraction of 54-58° C. is collected to obtain purified acetone;

[0082] The solid oxidant includes potassium permanganate and a metal oxygen-containing complex, and the mass ratio of potassium permanganate to the metal oxygen-containing complex is 5:1;

[0083] The preparation of the metal oxygen-containing complex includes mixing a ligand solution providing a ligand and a metal salt solution providing a central atom in an inert atmosphere, wherein the molar ratio of the metal salt to the ligand is 1:1.2, stirring the coordination reaction at room temperature for 5 hours, and then adding potassium permanganate at a molar ratio of 1.5:1 to the metal salt, and performing an oxidation reaction for 2 hours, and then removing the solvent, extracting, and drying to obtain a metal oxygen-containing complex. In the obtained metal oxygen-containing complex, M is Fe, two R1s are CH3, four R2s are H, n is 1, and X is Cl.

[0084] The results are shown in Table 1.

[0085] Example 2

[0086] The difference from Example 1 is that the solid oxidant includes potassium permanganate and does not include a metal oxygen-containing complex. The results are shown in Table 1.

[0087] Example 3

[0088] The difference from Example 1 is that the solid oxidant includes a metal oxygen complex and does not include potassium permanganate. The results are shown in Table 1.

[0089] Example 4

[0090] Different from Example 1, the solid oxidant includes a metal oxygen complex and does not include potassium permanganate, and the reaction time of the solid oxidant and acetone is 4 hours. The results are shown in Table 1.

[0091] Example 5

[0092] Different from Example 1, the purified acetone enters an acetone hydrogenation reactor filled with 5 wt % Cu / SiO2 for hydrogenation reaction, wherein the molar ratio of purified acetone to hydrogen is 1:8, and the space velocity of purified acetone is 0.8 h -1, the reaction inlet temperature is 100°C; the reaction pressure is 6Mpa, and crude isopropanol is obtained after the reaction. The crude isopropanol is then distilled under reduced pressure, the temperature of the bottom of the tower is 72°C, the vacuum degree is 350mbar, and the fraction of 48-50°C is collected to obtain high-purity isopropanol.

[0093] High purity isopropyl alcohol has a purity of 99.999% and a total organic impurity content of <10ppm.

[0094] Example 6

[0095] The difference from Example 1 is that industrial grade acetone (purity 99.93%) is used as the raw material. The results are shown in Table 1.

[0096] Example 7

[0097] The difference from Example 1 is that electronic grade acetone (purity 99.98%) is used as the raw material. The results are shown in Table 1.

[0098] Comparative Example 1

[0099] Different from Example 1, the reactor is not provided with an oxidant feeding bin 2, a protective gas inlet 17 and an outlet 18, and the solid oxidant is directly fed from the oxidant feed port of the top head, that is, the atmosphere in the feeding bin is not replaced. The results are shown in Table 1.

[0100] Comparative Example 2

[0101] Different from Example 5, analytical grade acetone (purity 99.5%) was not purified, and the analytical grade acetone was directly fed into an acetone hydrogenation reactor filled with 5 wt % Cu / SiO2 for hydrogenation reaction, wherein the molar ratio of industrial grade acetone to hydrogen was 1:8, and the space velocity of industrial grade acetone was 0.8 h -1 , the reaction inlet temperature is 100°C; the reaction pressure is 6Mpa, and crude isopropanol is obtained after the reaction. The crude isopropanol is then distilled under reduced pressure, the temperature of the bottom of the tower is 72°C, the vacuum degree is 350mbar, and the fraction of 48-50°C is collected to obtain high-purity isopropanol.

[0102] High purity isopropyl alcohol has a purity of 99.990% and a total organic impurity content of >10ppm.

[0103] Table 1

[0104]

[0105]

[0106] The preferred embodiments of the present invention are described in detail above in conjunction with the accompanying drawings, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various specific technical features in any appropriate manner. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations. However, these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A method for purifying acetone, characterized in that: The acetone to be purified is contacted with an oxidant under a protective gas atmosphere, dehydrated, and refined to obtain purified acetone.

2. The method for purifying acetone according to claim 1, wherein: The protective gas atmosphere is selected from at least one of nitrogen, argon or helium; and / or The contact conditions include: a temperature of room temperature to 60°C; and / or a pressure of normal pressure to 0.5 MPa; and / or The dehydration comprises: dehydration using a dehydrating agent, wherein the dehydrating agent comprises one or more of molecular sieves, silica gel, membranes, resins and salts; and / or The refining comprises: distilling the dehydrated product, and during the distillation process, collecting the 54-58° C. fraction as the purified acetone; and / or The impurities in the acetone to be purified include at least one of aldehydes, alcohols or olefins, and the acetone content in the acetone to be purified is ≥99.93%; Preferably, the aldehydes include C2-C3 aldehydes; and / or Preferably, the olefins include C2-C3 olefins; and / or and / or The purified acetone comprises an acetone content of more than 99.99%; and / or The content of total organic impurities in the purified acetone is below 10 ppm.

3. The method for purifying acetone according to claim 1, wherein: The amount of the oxidant added is greater than 0.01%, preferably greater than or equal to 0.02%, more preferably 0.03%-0.1% by weight of the acetone to be purified; and / or The oxidant is selected from one or more of an inorganic oxidant, an organic oxidant and a metal oxygen complex; and / or The acetone to be purified includes one or more of industrial grade acetone, analytical grade acetone and electronic grade acetone.

4. The method for purifying acetone according to claim 3, wherein: The metal oxygen complex is an organic ligand compound with a metal element as the central atom; Preferably, the metal oxygen-containing complex has a cyclic ether organic compound as a ligand.

5. The method for purifying acetone according to claim 3 or 4, wherein: The metal oxygen-containing complex has a structure shown in formula (I), 6. An acetone purification device, characterized in that: The purification equipment comprises: A reaction unit comprises an acetone feed port (4) for purification, an acetone discharge port (5) for purification, an oxidant feed bin (2), a protective gas inlet port (17) and a gas outlet port (18), wherein the reaction unit is used to contact the acetone for purification with the oxidant under a protective gas atmosphere; a dehydration unit, connected to the reaction unit, and used to dehydrate the material from the reaction unit; The refining unit is connected to the dehydration unit and is used to purify the material from the dehydration unit to obtain purified acetone.

7. The purification device according to claim 6, characterized in that The reaction unit includes a reaction kettle, the dehydration unit includes a dehydration tower, and the refining unit includes a distillation device. Along the material flow direction, the reaction kettle, the dehydration tower and the distillation device are connected in sequence; Preferably, the top cover of the reactor is provided with the oxidant feeding bin (2), and an upper bin cover (16) and a lower bin cover (13) are installed in the oxidant feeding bin (2), wherein the upper bin cover (16) is provided with the protective gas inlet (17) and the gas outlet (18); More preferably, the purification device is equipped with a control member capable of controlling the opening or closing of the lower bin cover (13); and / or Preferably, the oxidant feeding bin (2) is configured as a cylindrical or funnel-shaped bin; and / or Preferably, a stirring device (3) is provided in the reaction chamber of the reactor.

8. A method for preparing high-purity isopropanol, characterized in that: (1) Purifying acetone by the method for purifying acetone according to any one of claims 1 to 5; (2) In the presence of a hydrogenation catalyst, the purified acetone obtained in step (1) is subjected to a hydrogenation reaction with hydrogen to obtain crude isopropanol, and the crude isopropanol is refined to obtain high-purity isopropanol.

9. The preparation method according to claim 8, wherein: The hydrogenation reaction conditions include: The molar ratio of the purified acetone to hydrogen is 1:(1-30); and / or The space velocity of the purified acetone is 0.1-1.5h -1 ; and / or The reaction inlet temperature is 80-120°C; the reaction pressure is 2.5-6Mpa.

10. The high-purity isopropyl alcohol prepared by the method for preparing high-purity isopropyl alcohol according to claim 8 or 9 is used in integrated circuits after being deionized and degranulated, characterized in that: The high-purity isopropyl alcohol has an isopropyl alcohol content of >99.99%, a total organic impurity content of <10ppm, a metal cation content of <10ppt, and particulate matter of <100pcs / ml.

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