Acetone refining method and electronic-grade acetone product thereof

By contacting the crude acetone product with a mixed solution containing an oxidant and a strong alkali, and undergoing distillation, dehydration, deionization and departiculation treatment, the problem of difficulty in removing aldehyde impurities in the prior art is solved, and a high-purity electronic grade acetone product is obtained, which is suitable for semiconductor applications with higher requirements.

CN119841723AActive Publication Date: 2025-04-18CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202311348720.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-18
Publication Date
2025-04-18
Estimated Expiration
2043-10-18

AI Technical Summary

Technical Problem

The prior art is difficult to effectively remove aldehyde impurities in acetone raw materials, affecting the purity of acetone and unable to meet the higher requirements of semiconductor application scenarios.

Method used

The purification method of contacting the crude acetone product with a mixed solution containing oxidizing agent and a strong alkali is obtained by distillation, dehydration, deionization and departiculate steps, and electronic grade acetone products with a purity of no less than 99.99%.

Benefits of technology

It achieves high purity of acetone products, and the content of aldehyde compounds and evaporated residues are very low, which is suitable for semiconductor application scenarios with higher requirements.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of electronic-grade reagents, in particular to an acetone refining method and an electronic-grade acetone product thereof. The purity of the acetone product is not lower than 99.99%, and in the acetone product, the water content is not higher than 100 ppm, the content of aldehyde compounds is not higher than 3 ppm, and the content of evaporation residues is not higher than 1 ppm; the refining method of acetone comprises the following steps: contacting an acetone crude product with a mixed solution containing an oxidizing agent and a strong base, and then carrying out rectification, dehydration, deionization and particle removal to obtain an electronic-grade acetone product. According to the refining method of the acetone, an electronic-grade acetone product suitable for semiconductor application scenes with higher requirements can be obtained; the electronic-grade acetone product is good in quality and high in purity, the content of aldehyde compounds and the content of evaporation residues in the acetone product are very low, and the electronic-grade acetone product can be suitable for semiconductor application scenes with higher requirements.
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Description

Technical Field

[0001] The invention relates to the technical field of electronic-grade reagents, and in particular to a method for refining acetone and an electronic-grade acetone product thereof. Background Art

[0002] Acetone, also known as dimethyl ketone, is the simplest ketone in the saturated fatty ketone series, with a melting point of -95°C and a boiling point of 56°C at normal pressure. It is highly volatile and flammable, soluble in water, ethanol and ether, and has active chemical properties. It can undergo halogenation, addition, condensation and other reactions, and can be used as a solvent for artificial fibers, explosives, grease, acetylene, etc.

[0003] In the semiconductor field, acetone also plays an important role, such as cleaning and drying in the process of large-scale integrated circuit processing. Electronic grade acetone has very strict requirements on product purity, water content, metal cations, anions and residual particles. Therefore, higher requirements are put forward for the purification and refining process of acetone.

[0004] The existing reported patent literature information is relatively small, and the purification methods and effects are also relatively general. For example, CN201317750Y, CN104030903A and CN114344932A do not consider the removal of aldehyde impurities in the acetone raw material, which will affect the purity of acetone. Therefore, developing a high-purity electronic-grade acetone suitable for semiconductor application scenarios with higher requirements is an important technical problem that needs to be solved. Summary of the invention

[0005] The object of the present invention is to provide a method for refining acetone and an electronic-grade acetone product thereof, wherein the electronic-grade acetone product is suitable for semiconductor application scenarios with higher requirements.

[0006] The first aspect of the present invention provides an electronic grade acetone product, wherein the purity of the acetone product is not less than 99.99%, and the water content of the acetone product is not higher than 100 ppm, the aldehyde compound content is not higher than 3 ppm, and the evaporation residue content is not higher than 1 ppm.

[0007] The second aspect of the present invention provides a method for refining acetone, which comprises: contacting a crude acetone product with a mixed solution containing an oxidant and a strong base, and then performing rectification, dehydration, deionization, and degranulation to obtain an electronic-grade acetone product; the purity of the electronic-grade acetone product is not less than 99.99%, and the acetone product has: a water content of not more than 100 ppm, an aldehyde compound content of not more than 3 ppm, and an evaporation residue content of not more than 1 ppm.

[0008] Compared with the prior art, the present invention has at least the following advantages:

[0009] 1. The electronic-grade acetone product of the present invention has good quality and high purity, and the aldehyde compound content and evaporation residue content in the acetone product are both very low, and can be applied to semiconductor application scenarios with higher requirements;

[0010] 2. The acetone refining method of the present invention can obtain electronic-grade acetone products suitable for semiconductor application scenarios with higher requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 It is a schematic flow diagram of a method for refining acetone in one embodiment of the present invention.

[0012] Description of Reference Numerals

[0013] 1. Acetone crude product 2. Mixed solution 3. Reaction material

[0014] 4. Tower bottom products 5. Coarse filtration products 6. Tower top products

[0015] 7. Concentrate 8. Deionized liquid 9. Acetone products

[0016] ①、Stirring kettle ②、Distillation and light removal tower ③、Centrifugal filtration equipment

[0017] ④、Distillation deweighting tower ⑤、Pervaporation membrane equipment ⑥、Deionization tower

[0018] ⑦. Filtration equipment DETAILED DESCRIPTION

[0019] 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.

[0020] The first aspect of the present invention provides an electronic grade acetone product, wherein the purity of the acetone product is not less than 99.99%, and the water content of the acetone product is not higher than 100 ppm, the aldehyde compound content is not higher than 3 ppm, and the evaporation residue content is not higher than 1 ppm.

[0021] The electronic-grade acetone product of the present invention has good quality and high purity, and the aldehyde compound content and evaporation residue content in the acetone product are both very low, and can be suitable for semiconductor application scenarios with higher requirements.

[0022] According to the present invention, the purity of the acetone product provided by the present invention is generally 99.99-99.997%, preferably 99.993-99.997%, more preferably 99.994-99.997%, and further preferably 99.996-99.997%. The purity in the present invention refers to the weight percentage.

[0023] According to the present invention, in some embodiments, the aldehyde compound includes C1-C6 aldehydes, such as formaldehyde, acetaldehyde, propionaldehyde, butyraldehyde, valeraldehyde, etc.

[0024] According to the present invention, in some preferred embodiments, the water content in the acetone product is 55-100 ppm, preferably 55-75 ppm, more preferably 55-66 ppm, and even more preferably 55-58 ppm.

[0025] According to the present invention, in some preferred embodiments, in the acetone product: the content of aldehyde compounds is 0.1-3 ppm, preferably 0.1-0.9 ppm, more preferably 0.1-0.5 ppm, and even more preferably 0.1-0.2 ppm.

[0026] According to the present invention, in some preferred embodiments, in the acetone product: the evaporation residue content is 0.4-1 ppm, preferably 0.4-0.8 ppm, more preferably 0.4-0.6 ppm, and even more preferably 0.4-0.5 ppm.

[0027] According to the present invention, in some preferred embodiments, in the acetone product: the content of a single metal ion is not higher than 100 ppt, for example, not higher than 80 ppt, not higher than 60 ppt, not higher than 52 ppt, not higher than 50 ppt, not higher than 30 ppt, not higher than 28 ppt, etc.

[0028] According to the present invention, in some preferred embodiments, in the acetone product: the content of particles with an average particle size greater than 0.1 μm is not higher than 100 particles / ml, for example, 50 particles / ml, 53 particles / ml, 55 particles / ml, 56 particles / ml, 89 particles / ml, 97 particles / ml, preferably 50-56 particles / ml, further preferably 50-55 particles / ml, and even more preferably 50-53 particles / ml.

[0029] The second aspect of the present invention provides a method for refining acetone, comprising: contacting a crude acetone product with a mixed solution containing an oxidant and a strong base, and then performing rectification, dehydration, deionization, and degranulation to obtain an electronic-grade acetone product; the purity of the electronic-grade acetone product is not less than 99.99%, and the electronic-grade acetone product has: a water content of not more than 100 ppm, an aldehyde compound content of not more than 3 ppm, and an evaporation residue content of not more than 1 ppm.

[0030] The prior art does not consider the removal of aldehyde impurities in the acetone raw material. The acetone refining method of the present invention can obtain an electronic-grade acetone product suitable for semiconductor application scenarios with higher requirements, with a purity of not less than 99.99%, a water content of not more than 100 ppm, an aldehyde compound content of not more than 3 ppm, and an evaporation residue content of not more than 1 ppm.

[0031] According to the present invention, the weight content of acetone in the crude acetone product of the present invention is 98.0-99.9%. The refining method of the present invention is used to purify the crude acetone product to obtain an acetone product with higher purity.

[0032] According to the present invention, the crude acetone contains some other impurities. In some embodiments, the crude acetone further contains at least one of water, C1-C6 alcohols (such as methanol, ethanol, isopropanol, butanol, etc.), C1-C6 aldehydes, C2-C6 olefins (such as propylene, butene, etc.) and C2-C6 ethers (such as diethyl ether, isopropyl ether, etc.).

[0033] According to the present invention, the content of specific impurities in the crude acetone is not particularly limited, for example, the content of C1-C6 alcohols is 0.01-0.50wt%; for example, the content of C1-C6 aldehydes is 0.002-0.20wt%; for example, the content of C2-C6 olefins is 0.001-0.10%; for example, the content of C2-C6 ethers is 0.001-0.20%.

[0034] According to the present invention, as long as the purpose of the present invention can be achieved, when the crude acetone product contacts with the mixed solution containing the oxidant and the strong base, the amount of the mixed solution is not particularly limited. In some preferred embodiments, the mass of the mixed solution is 0.001-0.01 times of the crude acetone product, for example, 0.001 times, 0.002 times, 0.003 times, 0.004 times, 0.005 times, 0.007 times, 0.01 times, or a range consisting of any two of the above values. By adopting the above embodiment, the crude acetone product can be better refined to obtain a high-purity, low-aldehyde content and low-water content acetone product.

[0035] According to the present invention, the mixed solution containing an oxidant and a strong base refers to a mixed solvent formed by a reagent such as an oxidant, a strong base and water. In some embodiments, in the mixed solution, the content of the oxidant is 0.5-20wt%, such as 0.5wt%, 1wt%, 2wt%, 2.5wt%, 3wt%, 4wt%, 5wt%, 7wt%, 10wt%, 15wt%, 20wt%, or a range consisting of any two of the above values. By adopting the above embodiment, the crude acetone can be better refined to obtain a high-purity, low-aldehyde and low-water acetone product.

[0036] According to the present invention, in some preferred embodiments, the content of the oxidant in the mixed solution is 0.5-10wt%, preferably 0.5-5wt%. The above embodiment can better purify the crude acetone to obtain a high-purity acetone product with low aldehyde content and low water content.

[0037] According to the present invention, in some embodiments, the content of the strong base in the mixed solution is 1-4 mol / L, for example, 1 mol / L, 2 mol / L, 3 mol / L, 4 mol / L, or a range consisting of any two of the above values. By adopting the above embodiment, the crude acetone can be better refined to obtain an acetone product with high purity, low aldehyde content, low water content and low evaporation residue.

[0038] According to the present invention, as long as the purpose of the present invention can be achieved, the type of the oxidant is not particularly limited. In some embodiments, the oxidant is selected from one or more of a neutral oxidant, an acidic oxidant and an alkaline oxidant.

[0039] According to the present invention, in some preferred embodiments, the oxidant is selected from one or more of potassium permanganate, potassium dichromate, potassium perchlorate, potassium chlorite, potassium chlorate and potassium hypochlorite.

[0040] According to the present invention, in some preferred embodiments, the strong base is selected from one or more of sodium hydroxide, potassium hydroxide and ammonium hydroxide, preferably sodium hydroxide and / or potassium hydroxide. By adopting the above-mentioned embodiment, the crude acetone can be better refined to obtain an acetone product with high purity, low aldehyde content, low water content and low evaporation residue.

[0041] According to the present invention, in some preferred embodiments, the mixed solution further contains a stabilizer, and the stabilizer in the present invention refers to a reagent that can promote the interaction between the oxidant and the strong base in the mixed solution and the impurities in the crude acetone product, especially the aldehyde impurities; in some preferred embodiments, the stabilizer is selected from one or more of sodium pyrophosphate, sodium tripolyphosphate, sodium polyacrylate, sodium polymethacrylate, sodium gluconate and sodium metasilicate. By adopting the above-mentioned embodiment, the crude acetone product can be better refined to obtain an acetone product with high purity, low aldehyde content, low water content and low evaporation residue.

[0042] According to the present invention, in some preferred embodiments, the stabilizer is selected from sodium pyrophosphate and / or sodium polyacrylate. By adopting the above-mentioned embodiment, an acetone product with higher purity and lower total aldehyde content, single metal ion and evaporation residue content can be obtained.

[0043] According to the present invention, in some more preferred embodiments, the stabilizer is a combination of sodium pyrophosphate and sodium polyacrylate, and preferably the mass ratio of sodium pyrophosphate to sodium polyacrylate is 1:(1-5), for example, 1:1, 1:2, 1:2.5, 1:3, 1:4, 1:5, or a range consisting of any two of the above ratios. By adopting the aforementioned embodiment, an acetone product with higher purity and lower total aldehyde content, single metal ion content, and evaporation residue content can be refined.

[0044] According to the present invention, in some preferred embodiments, in the mixed solution, the content of the stabilizer is 0.5-20wt%, for example, 0.5wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 13wt%, 15wt%, 20wt%, or a range consisting of any two of the above values. By adopting the above embodiment, an acetone product with higher purity and lower total aldehyde content, single metal ion and evaporation residue content can be refined.

[0045] According to the present invention, in some more preferred embodiments, in the mixed solution, the content of the stabilizer is 1-10 wt %, preferably 2-7 wt %.

[0046] According to the present invention, as long as the purpose of the present invention can be achieved, the manner in which the crude acetone product is contacted with the mixed solution containing an oxidant and a strong base is not particularly limited. Preferably, the mixed solution containing an oxidant and a strong base is sprayed to contact the crude acetone product, that is, the mixed solution containing an oxidant and a strong base is sprayed into a reaction device containing the crude acetone product to contact the crude acetone product. By adopting the above-mentioned embodiment, the mixed solution can better interact with impurities in the crude acetone product, reduce the content of impurities, and finally purify and obtain an acetone product with higher purity, lower total aldehyde content, single metal ion, and evaporation residue content.

[0047] The reaction equipment for contacting the crude acetone with the mixed solution containing the oxidant and the strong base in the present invention is not particularly limited and can be a conventional stirred tank in the art. In order to spray the mixed solution containing the oxidant and the strong base into the stirred tank containing the crude acetone, a spray head can be provided at the bottom of the stirred tank.

[0048] According to the present invention, as long as the purpose of the present invention can be achieved, the contact conditions are not particularly limited. Preferably, the contact conditions include: room temperature (20-30° C.); preferably, the contact conditions include: time of 2-7 hours.

[0049] According to the present invention, the purpose of distillation is to remove light components and heavy components in the contacted material. In some embodiments, the distillation method includes: distilling the contacted material to remove light components and heavy components.

[0050] According to the present invention, in some preferred embodiments, the conditions for distillation to remove light substances include: an operating pressure of 100-200 kPa (absolute pressure).

[0051] According to the present invention, in some preferred embodiments, the conditions for distillation to remove light substances include: a reflux ratio of 2-20, for example, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12, 15, 17, 20, or a range consisting of any two of the above values, preferably 8-15.

[0052] According to the present invention, in some preferred embodiments, the conditions for the rectification and weight removal include: an operating pressure of 100-200 kPa (absolute pressure).

[0053] According to the present invention, in some preferred embodiments, the conditions for distillation weight removal include: a reflux ratio of 0.2-5.

[0054] According to the present invention, in some preferred embodiments, the conditions for distillation weight removal include: the tower top temperature is 55.7-77.5°C.

[0055] According to the present invention, the crude acetone product is contacted with a mixed solution containing an oxidant and a strong base to produce salt impurities. In some preferred embodiments, the distillation to remove light and heavy substances further includes a desalting step. By adopting the above-mentioned embodiment, an acetone product with higher purity and lower total aldehyde content, single metal ion, particulates, and evaporation residue content can be finally refined.

[0056] According to the present invention, as long as the purpose of the present invention can be achieved, the desalination method includes centrifugal treatment and / or filtering using a filtering device with a specification of less than 1 micron.

[0057] According to the present invention, in some embodiments, the dehydration method includes: pervaporation membrane separation method.

[0058] According to the present invention, the pervaporation membrane separation method refers to separation using a membrane. In some preferred embodiments, the membrane in the pervaporation membrane separation method is a molecular sieve membrane.

[0059] According to the present invention, in some preferred embodiments, the operating conditions of the pervaporation membrane separation method include: an operating temperature of 80°C-140°C.

[0060] According to the present invention, in some preferred embodiments, the operating conditions of the pervaporation membrane separation method include: the operating pressure of the pervaporation membrane separation method is 2-9 bar.

[0061] According to the present invention, in some preferred embodiments, the operating conditions of the pervaporation membrane separation method include: the operating pressure on the permeation side is 0-20 kPa (absolute pressure).

[0062] According to the present invention, as long as the purpose of the present invention can be achieved, the deionization method is not particularly limited. In some embodiments, the deionization method includes: ion exchange adsorption removal method.

[0063] According to the present invention, the ion exchange adsorption removal method refers to treating the material in an ion tower filled with adsorption material to remove metal cation and anion impurities in the material. Preferably, the adsorption material used in the ion exchange adsorption removal method includes a mixed bed resin composed of a hydrogen-type strong acid cation exchange resin and a hydroxide-type strong base anion exchange resin. The mixed bed resin 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. The mixed bed resin can remove metal cations and anions in the material.

[0064] According to the present invention, in some preferred embodiments, the degranulation method comprises: a filtration method.

[0065] According to the present invention, in some preferred embodiments, the material of the filter element in the filtration method is at least one of PTFE, PVDF and PE.

[0066] According to the present invention, in some preferred embodiments, at least 4 filter elements with gradually increasing filtration accuracy are used in series, for example, PTFE filter elements with filtration specifications of 500nm, 200nm, 100nm and 50nm are used for particle removal.

[0067] According to the present invention, Figure 1As shown, in some embodiments, the method for refining acetone includes: adding a mixed solution containing an oxidant and a strong base to the industrial-grade acetone crude product 1 in the stirring tank ① for contact, and the reaction material 3 after contact enters the distillation and de-lightening tower ② for distillation and de-lightening; the bottom product 4 of the distillation and de-lightening tower ② first enters the centrifugal filtration equipment ③ for coarse filtration, and the obtained coarse filtration product 5 enters the distillation and de-weighting tower ④ for distillation and de-weighting; the top product 6 obtained by distillation and de-weighting enters the pervaporation membrane equipment ⑤ for pervaporation membrane separation and dehydration; the concentrated liquid 7 separated and dehydrated by the pervaporation membrane enters the deionization tower ⑥ filled with a mixed bed resin of a uniformly mixed hydrogen-type strong acid cation exchange resin and a hydroxyl-type strong basic anion exchange resin for deionization, and the bottom material 8 of the deionization tower ⑥ enters the filtration equipment ⑦ for filtration and de-particle removal to obtain an acetone product 9.

[0068] The present invention will be described in detail below through examples. In the following examples, the purity of the products is tested by HPLC; the water content is determined by Karl Fischer titrator; the metal ions are determined by ICP-MS; the number of particles is determined online by a particle counter; the aldehyde compound content (total aldehyde content) is determined by HPLC; and the evaporation residue is determined by the general method of national standard GB / T 9740-2008.

[0069] Example 1

[0070] To the industrial grade acetone crude product 1 (measured purity of 99.0%, total aldehyde content of 35ppm, water content of 3500ppm) in the stirred tank ①, 0.01 times the mass of a mixed solution 2 containing 1wt% potassium permanganate, 2mol / L sodium hydroxide and 2wt% sodium pyrophosphate (the solvent is water) is directly added, and then the reaction material 3 after stirring at room temperature for 5h is entered into the distillation and light removal tower ② for distillation and light removal, the operating pressure of the distillation and light removal is 100kPa, the operating reflux ratio is 10, and the tower bottom temperature is controlled to be 56.6°C;

[0071] The bottom product 4 of the distillation and light removal tower ② first enters the centrifugal filtration device ③ for coarse filtration, and the obtained coarse filtration product 5 enters the distillation and heavy removal tower ④ for distillation and heavy removal. The operating pressure of the distillation and heavy removal is 100 kPa, the operating reflux ratio is 1, and the tower top temperature is controlled to be 55.7°C;

[0072] The top product 6 obtained by distillation and deweighting enters the pervaporation membrane device ⑤ for pervaporation membrane separation and dehydration. The operating temperature of the membrane separation is 120°C, the operating pressure is 6 bar, and the operating pressure on the permeate side is 0.1 kPa (absolute pressure);

[0073] The concentrated liquid 7 separated by the membrane enters the deionization tower ⑥ filled with a mixed bed resin of a uniformly mixed hydrogen-type strongly acidic cation exchange resin and a hydroxide-type strongly basic anion exchange resin for deionization. The bottom material 8 of the deionization tower ⑥ enters the filtering device ⑦ and is filtered through a PTFE filter element with filtration specifications of 500nm, 200nm, 100nm and 50nm respectively for degranulation to obtain the acetone product 9.

[0074] Example 2

[0075] The method of Example 1 is followed, except that the purity of the crude industrial-grade acetone is 98.5%, the total aldehyde content is 240 ppm, and the water content is 8200 ppm; the rest is the same as Example 1, and the acetone product is finally obtained.

[0076] Example 3

[0077] The method of Example 1 is followed, except that the amount of the mixed solution added is 0.002 times the amount of crude acetone added; the rest is the same as Example 1, and finally an acetone product is obtained.

[0078] Example 4

[0079] The method of Example 1 is followed, except that: the mixed solution also contains 5wt% of sodium polyacrylate; the mixed solution enters the stirring tank through the nozzle at the bottom of the stirring tank and is stirred and reacted with the crude acetone in the stirring tank for 5 hours; the rest is the same as Example 1, and finally an acetone product is obtained.

[0080] Example 5

[0081] The method of Example 1 is followed, except that the mixed solution further contains 5 wt % of sodium polyacrylate; the rest is the same as Example 1, and finally an acetone product is obtained.

[0082] Example 6

[0083] The method of Example 1 is followed, except that the mixed solution contains 1wt% potassium permanganate, 2mol / L sodium hydroxide and 7wt% sodium polyacrylate; the rest is the same as Example 1, and finally an acetone product is obtained.

[0084] Example 7

[0085] The method of Example 4 is different from that:

[0086] The bottom product 4 of the distillation and light removal tower directly enters the distillation and heavy removal tower for subsequent steps; the rest is the same as in Example 1, and finally an acetone product is obtained.

[0087] Comparative Example 1

[0088] The method of Example 1 is different from that of Example 1:

[0089] The mixed solution contains only 1 wt % potassium permanganate; the rest is the same as in Example 1, and finally an acetone product is obtained.

[0090] Comparative Example 2

[0091] The method of Example 1 is followed, except that the mixed solution contains only 2 mol / L sodium hydroxide; the rest is the same as Example 1, and finally an acetone product is obtained.

[0092] Table 1

[0093]

[0094]

[0095] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. An electronic grade acetone product, characterized in that: The purity of the acetone product is not less than 99.99%. In the acetone product, the water content is not higher than 100 ppm, the aldehyde compound content is not higher than 3 ppm, and the evaporation residue content is not higher than 1 ppm.

2. The acetone product according to claim 1, wherein The aldehyde compound comprises C1-C6 aldehyde; and / or In the acetone product: The content of a single metal ion is not more than 100ppt; and / or The content of particles with an average particle size greater than 0.1 μm is not higher than 100 particles / ml.

3. A method for refining acetone, characterized in that: The method includes: The crude acetone product is contacted with a mixed solution containing an oxidant and a strong base, and then distilled, dehydrated, deionized, and degranulated to obtain an electronic grade acetone product; The purity of the electronic-grade acetone product is not less than 99.99%. In the electronic-grade acetone product, the water content is not higher than 100 ppm, the aldehyde compound content is not higher than 3 ppm, and the evaporation residue content is not higher than 1 ppm.

4. The method according to claim 3, wherein: The weight content of acetone in the crude acetone product is 98.0-99.9%; and / or The crude acetone also contains at least one of water, C1-C6 alcohols, C1-C6 aldehydes, C2-C6 olefins and C2-C6 ethers.

5. The preparation method according to claim 3 or 4, wherein The mass of the mixed solution is 0.001-0.01 times that of the crude acetone; and / or In the mixed solution, the content of the oxidant is 0.5-20wt%, preferably 0.5-10wt%; and / or In the mixed solution, the content of the strong base is 1-4 mol / L; and / or The oxidant is selected from one or more of a neutral oxidant, an acidic oxidant and an alkaline oxidant, preferably one or more of potassium permanganate, potassium dichromate, potassium perchlorate, potassium chlorite, potassium chlorate and potassium hypochlorite; and / or The strong base is selected from one or more of sodium hydroxide, potassium hydroxide and ammonium hydroxide, preferably sodium hydroxide and / or potassium hydroxide.

6. The method according to any one of claims 3 to 5, wherein: The mixed solution also contains a stabilizer; Preferably, the stabilizer is selected from one or more of sodium pyrophosphate, sodium tripolyphosphate, sodium polyacrylate, sodium polymethacrylate, sodium gluconate and sodium metasilicate; and / or In the mixed solution, the content of the stabilizer is 0.5-20wt%, preferably 1-10wt%.

7. The method according to any one of claims 3 to 5, wherein: The mixed solution containing the oxidant and the strong base is sprayed to contact with the crude acetone product; and / or The contact conditions include: room temperature and / or a contact time of 2-7 hours.

8. The method according to any one of claims 3 to 7, wherein: The distillation method comprises: distilling the obtained material after contact to remove light and heavy substances; Preferably, the conditions for distillation and light removal include: an operating pressure of 100-200 kPa; and / or a reflux ratio of 2-20; and / or a bottom temperature of 56.6-78.0°C; and / or The conditions for the rectification and de-weighting include: an operating pressure of 100-200 kPa; and / or a reflux ratio of 0.2-5; and / or a tower top temperature of 55.7-77.5° C.; and / or The step of desalting is further included between the distillation for light removal and the distillation for heavy removal. Preferably, the desalting method includes centrifugal treatment and / or filtering using a filtering device with a specification of less than 1 micron.

9. The method according to any one of claims 3 to 8, wherein: The dehydration method includes: pervaporation membrane separation method; Preferably, the membrane in the pervaporation membrane separation method is a molecular sieve membrane; and / or The pervaporation membrane separation process operating conditions include: Operating temperature is 80℃-140℃, and / or The operating pressure of the pervaporation membrane separation method is 2-9 bar; and / or The operating pressure on the permeate side is 0-20 kPa.

10. The method according to any one of claims 3 to 9, wherein: The deionization method includes: ion exchange adsorption removal method, preferably the adsorption material used in the ion exchange adsorption removal method includes a mixed bed resin composed of a hydrogen-type strongly acidic cation exchange resin and a hydroxide-type strongly basic anion exchange resin; and / or The method for removing particles comprises: a filtration method, wherein the material of the filter element in the filtration method is preferably at least one of PTFE, PVDF and PE; and / or at least four filter elements with gradually increasing filtration accuracy are used in series.

Citation Information

Patent Citations

  • Continuous production method of ultra-clean high-purity acetone

    CN104030903A

  • Preparing system for ultra-clean and high-purity electronic grade acetone

    CN201317750Y

  • Method for purifying acetone

    CN102245553A

  • Method for purifying acetone

    CN102245554A

  • Continuous production method of semiconductor-grade acetone

    CN113735697A