Ultra-clean high-purity acetone as well as preparation method and application thereof

By contacting the crude acetone product with an oxidant-containing mixture, combined with a pH adjuster and multi-step treatment, high-purity ultra-clean and high-purity acetone is prepared, which solves the problem of poor removal of organic impurities in the prior art, and achieves product quality with high purity and low impurities.

CN119841722AActive Publication Date: 2025-04-18CHINA PETROLEUM & CHEMICAL CORP +1
View PDF 16 Cites 0 Cited by

Patent Information

Application Number
CN202311353011.3
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 existing ultra-clean high-purity acetone preparation method has poor effect on removing organic impurities, resulting in poor product quality, especially in the integrated circuit industry, which requires high purity and low impurities.

Method used

The crude acetone product is used to contact with the mixed material containing an oxidant, and then contact it with the pH adjuster. After steps such as lightness, dehydration, deionization and filtration, high-purity ultra-clean and high-purity acetone are prepared.

Benefits of technology

The ultra-clean high-purity acetone prepared by this method has low organic impurity content, low acid value and high chemical purity, and can meet the high purity and low impurity requirements of the integrated circuit industry for cleaning solvents.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119841722A_ABST
    Figure CN119841722A_ABST
Patent Text Reader

Abstract

The invention relates to the field of preparation of cleaning solvents for the integrated circuit industry, in particular to ultra-clean high-purity acetone as well as a preparation method and application thereof. The chemical purity of the ultra-clean high-purity acetone is larger than or equal to 99.99%, the chromaticity is smaller than or equal to 10 Hazen, and the acid value is smaller than or equal to 10 ppm; the content of organic impurities is less than or equal to 20ppm. The preparation method of the ultra-clean high-purity acetone comprises the following steps: (1) contacting an acetone crude product with a mixed material containing an oxidizing agent to obtain a first material; (2) contacting the first material with a pH regulator to obtain a second material; and (3) sequentially carrying out light component removal, heavy component removal, dehydration, deionization and filtration on the second material. The ultra-clean high-purity acetone is low in organic impurity content and low in acid value, the ultra-clean high-purity acetone with the low organic impurity content and the low acid value content can be obtained through the preparation method, and the prepared ultra-clean high-purity acetone can meet the requirements of cleaning solvents for the integrated circuit industry.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the field of preparation of cleaning solvents for the integrated circuit industry, and in particular to ultra-clean high-purity acetone and a preparation method and application thereof. Background Art

[0002] Acetone, also known as dimethyl ketone, has a molecular formula of C 3 H 6 O is the simplest saturated ketone, easily soluble in water and organic solvents such as methanol, ethanol, ether, chloroform, pyridine, etc. In industry, it is an excellent solvent, mainly used in explosives, plastics, rubber, fiber, leather, grease, spray paint and other industries.

[0003] In the field of chip semiconductors, acetone is also an important solvent. With its low boiling point, it is often used as a cleaning agent and desiccant. Acetone used in semiconductors, namely ultra-clean high-purity acetone, has a great impact on the yield rate of semiconductors. Therefore, it has very high requirements for the quality of the product, especially the organic impurities, water content, metal ions and particulate residues in the product. Compared with traditional acetone products, in order to ensure the high quality requirements of the product, the preparation process of ultra-clean high-purity acetone is more cumbersome and strict. And with the further development of the integrated circuit industry and the precision and miniaturization of chips, the requirements for ultra-clean high-purity acetone will become higher and higher. Therefore, the development of the preparation process of ultra-clean high-purity acetone is extremely urgent.

[0004] However, there are few patents and literature reports on existing ultra-clean high-purity acetone, especially for the removal of organic impurities in acetone. For example, CN201317750Y reports a method for obtaining ultra-clean high-purity acetone by only using one distillation, but the removal effect of this method on organic impurities is limited, and some aldehyde materials will still remain in the product, affecting the product quality of ultra-clean high-purity acetone; for example, CN103601624B uses an oxidation method to oxidize acetone first and then distill to remove organic impurities, but this method will cause the acid value in the product to be higher, which will also affect the quality of the product.

[0005] Therefore, in view of the problems arising in the preparation process of the ultra-clean high-purity acetone, especially the problem of poor product quality caused by poor removal effect during the removal of organic impurities, it is necessary to develop a better ultra-clean high-purity acetone and a method for purifying ultra-clean high-purity acetone. Summary of the invention

[0006] The purpose of the present invention is to provide a novel ultra-clean high-purity acetone, which can be used as a cleaning solvent for the integrated circuit industry.

[0007] The first aspect of the present invention provides an ultra-clean high-purity acetone with a chemical purity of ≥99.99%, a chromaticity of ≤10 Hazen, an acid value of ≤10 ppm, and an organic impurity content of ≤20 ppm.

[0008] The second aspect of the present invention provides a method for preparing the ultra-clean high-purity acetone of the present invention, the preparation method comprising:

[0009] (1) contacting the crude acetone with a mixture containing an oxidant to obtain a first material;

[0010] (2) contacting the first material with a pH adjuster to obtain a second material;

[0011] (3) The second material is sequentially subjected to light removal, heavy removal, water removal, deionization and filtration.

[0012] The third aspect of the present invention provides the use of the ultra-clean high-purity acetone of the present invention, and / or the ultra-clean high-purity acetone prepared by the preparation method of the present invention in integrated circuits.

[0013] Through the above technical scheme, the ultra-clean high-purity acetone of the present invention has not only a low organic impurity content but also a low acid value, and the preparation method of the present invention can obtain ultra-clean high-purity acetone with low organic impurity content and acid value, and the prepared ultra-clean high-purity acetone can meet the requirements of cleaning solvents used in the integrated circuit industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 The present invention is a schematic flow diagram of a method for preparing ultra-clean high-purity acetone in one embodiment of the present invention.

[0015] Description of Reference Numerals

[0016] 1. Acetone crude product 2. Mixed material 3. First material

[0017] 4. Alkali solution 5. Second material 6. Light component

[0018] 7. Tower bottom product 8. Heavy component 9. Tower top distillate

[0019] 10. Water 11. Concentration side product 12. Bottom material

[0020] 13. Ultra-clean high-purity acetone product ①, first stirring kettle ②, second stirring kettle

[0021] ③、Light component removal tower ④、Heavy component removal tower ⑤、Pervaporation device

[0022] ⑥. Deionization tower ⑦. Filtration system DETAILED DESCRIPTION

[0023] 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.

[0024] The "purity" in the present invention is measured in terms of mass percentage; the unit "ppm" refers to mass content.

[0025] The first aspect of the present invention provides an ultra-clean high-purity acetone with a chemical purity of ≥99.99%, a chromaticity of ≤10 Hazen, an acid value of ≤10 ppm, and an organic impurity content of ≤30 ppm.

[0026] The ultra-clean high-purity acetone of the present invention has not only a low content of organic impurities but also a low acid value.

[0027] According to the present invention, in some embodiments, the chemical purity of ultra-clean high-purity acetone is 99.9972-99.9991%, preferably 99.9985-99.9991%, and further preferably 99.9989-99.9991%.

[0028] According to the present invention, in some embodiments, the acid value of ultra-clean high-purity acetone is 4-10 ppm, preferably 4-6 ppm.

[0029] According to the present invention, in some embodiments, the content of organic impurities in the ultra-clean high-purity acetone is ≤20 ppm, preferably 9-15 ppm, and preferably 9-11 ppm.

[0030] According to the present invention, in some embodiments, the organic impurities include at least one of isopropyl alcohol, acetaldehyde, propionaldehyde, propylene, isopropyl ether and methanol.

[0031] According to the present invention, in some embodiments, the water content in the ultra-clean high-purity acetone is ≤100 ppm, preferably 50-78 ppm, more preferably 50-65 ppm, and even more preferably 50-60 ppm.

[0032] According to the present invention, in some embodiments, the content of a single metal ion in the ultra-clean high-purity acetone is ≤50ppt.

[0033] According to the present invention, in some embodiments, in the ultra-clean high-purity acetone, the number of particles larger than 0.5 μm is ≤10 / ml, for example, 5 / ml, 6 / ml, 7 / ml or 8 / ml.

[0034] According to the present invention, in some embodiments, the evaporation residue content in the ultra-clean high-purity acetone is ≤1 ppm, for example, 0.2 ppm, 0.3 ppm, 0.4 ppm, 0.5 ppm, 0.6 ppm, 0.7 ppm or 0.8 ppm.

[0035] A second aspect of the present invention provides a method for preparing ultra-clean high-purity acetone, the preparation method comprising:

[0036] (1) the crude acetone product is brought into first contact with a mixture containing an oxidant to obtain a first material;

[0037] (2) contacting the first material with a pH adjuster for a second time to obtain a second material;

[0038] (3) De-lightening, de-heaving, dehydrating, deionizing, and filtering the second material.

[0039] The preparation method of the present invention can obtain ultra-clean high-purity acetone with low organic impurity content and acid value content, and the prepared ultra-clean high-purity acetone can meet the requirements of cleaning solvents used in the integrated circuit industry.

[0040] According to the present invention, in step (1), the conditions for the first contact include: the crude acetone product and the mixed material containing the oxidant are firstly mixed in a static mixer, and the mixed materials are then mixed in a stirring tank. By adopting the above-mentioned embodiment, the mixed material can better interact with the impurities in the crude acetone product, and finally an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chroma can be obtained.

[0041] According to the present invention, in some embodiments, the second mixing conditions include: a mixing temperature of 15-50°C, such as 15°C, 25°C, 35°C, 40°C, 45°C or 50°C, preferably 35-50°C.

[0042] According to the present invention, in some embodiments, the second mixing condition includes: the mixing time is 1-4h.

[0043] According to the present invention, in some embodiments, in step (2), the conditions of the second contact include: the first material and the pH regulator first enter the static mixer for the third mixing, and then enter the stirring tank for the fourth mixing after the mixing. By adopting the above embodiment, an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity can be finally obtained.

[0044] According to the present invention, the conditions for the first mixing and the third mixing are not particularly limited, and are generally carried out at room temperature (10-30° C.) and are uniformly mixed. No further details are given in the present invention. Among them, the structure of the static mixer is not particularly limited, and it is a conventional static mixer in the art.

[0045] According to the present invention, in some embodiments, the fourth mixing conditions include: a mixing temperature of 15-50°C, such as 15°C, 25°C, 35°C, 40°C, 45°C or 50°C, preferably 20-30°C.

[0046] According to the present invention, in some embodiments, the fourth mixing condition includes: the mixing time is 0.5h-1h.

[0047] According to the present invention, the mixed material containing an oxidant refers to a mixed material formed by mixing an oxidant and other reagents with water. In some embodiments, the oxidant is selected from at least one of potassium permanganate, hydrogen peroxide, potassium dichromate, potassium perchlorate, potassium chlorite, potassium chlorate and potassium hypochlorite, preferably potassium permanganate and / or hydrogen peroxide. By adopting the above-mentioned embodiment, an acetone product with higher purity and lower organic impurity content can be prepared.

[0048] According to the present invention, in some embodiments, the content of the oxidant in the mixed material is 1-20wt%. By adopting the above embodiment, an acetone product with higher purity and lower organic impurity content can be prepared.

[0049] According to the present invention, in some preferred embodiments, when the oxidant is hydrogen peroxide, the content of the oxidant in the mixture is 2-20wt%, for example, 2.5wt%, 5wt%, 10wt%, 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 organic impurity content and evaporation residue content can be prepared.

[0050] According to the present invention, in some preferred embodiments, when the oxidant is hydrogen peroxide, the content of the oxidant in the mixture is 1-10wt%, for example, 1wt%, 1.5wt%, 2.5wt%, 5wt%, 7wt%, 10wt%, or a range consisting of any two of the above values. By adopting the above embodiment, an acetone product with higher purity and lower organic impurity content and evaporation residue content can be prepared.

[0051] According to the present invention, in some preferred embodiments, when the oxidant is potassium permanganate, the content of the oxidant in the mixture is 1.5-4wt%, for example, 1.5wt%, 2.5wt%, 4wt%, or a range consisting of any two of the above values.

[0052] According to the present invention, in some embodiments, the mixed material containing the oxidant further contains a stabilizer. By adopting the above-mentioned embodiment, the oxidant in the mixed material can act more stably with some impurities in the crude acetone product, and the subsequent steps can be stably performed, and finally an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity is obtained.

[0053] According to the present invention, in some embodiments, the stabilizer is selected from at least one of sodium tripolyphosphate, sodium polymethacrylate, sodium gluconate and sodium metasilicate. By adopting the above-mentioned embodiment, the oxidant in the mixture can act more stably with some impurities in the crude acetone product, and the subsequent steps can be stably carried out, and finally an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity is obtained.

[0054] According to the present invention, in some preferred embodiments, the stabilizer is selected from sodium tripolyphosphate. By adopting the above embodiment, an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity can be finally obtained.

[0055] According to the present invention, as long as the purpose of the present invention can be achieved, the amount of the mixed material is not particularly limited, and preferably the mass ratio of the crude acetone to the mixed material is (0.001-0.01):1, for example, 0.001:1, 0.003:1, 0.005:1, 0.007:1 or 0.01:1. By adopting the above-mentioned embodiment, an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity can be finally obtained.

[0056] According to the present invention, in some embodiments, the chemical purity of the crude acetone product is 98.5-99.9%. The preparation method of the present invention can better improve the chemical purity of the crude acetone product.

[0057] According to the present invention, as long as the purpose of the present invention can be achieved, the amount of the pH adjuster used in step (2) is not particularly limited. Preferably, the amount of the pH adjuster added is such that the pH value of the second material is 7-10.

[0058] According to the present invention, in some fourteen modes, the pH regulator is selected from alkali solution, wherein the alkali solution refers to a solution formed by an alkaline substance and water, preferably the content of the alkaline substance in the alkali solution is 0.5-5 mol / L, and preferably the alkaline substance in the alkali solution is selected from at least one of sodium hydroxide, potassium hydroxide and ammonium hydroxide. By adopting the above-mentioned embodiment, an acetone product with higher purity, lower organic impurity content, evaporation residue content, single metal ion, water content and chromaticity can be finally obtained.

[0059] According to the present invention, in order to remove impurity components with a lower boiling point than acetone during light removal, in some embodiments, the conditions for light removal include: an operating pressure of 0-50 kPa (gauge pressure).

[0060] According to the present invention, in some embodiments, the conditions for removing light 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. The purity of the acetone product finally prepared can be better increased.

[0061] According to the present invention, in some preferred embodiments, the light removal condition includes: a reflux ratio of 8 to 15. The above embodiment can better increase the purity of the acetone product finally prepared and increase the recovery rate of the acetone product.

[0062] According to the present invention, in some preferred embodiments, the conditions for removing light substances include: the bottom temperature of the tower is 56.6-68.1°C.

[0063] According to the present invention, the de-weighting treatment is mainly for removing impurity components having a boiling point higher than that of the acetone product. As long as the purpose of the present invention can be achieved, the conditions of the de-weighting treatment are not particularly limited. In some embodiments, the de-weighting conditions include: an operating pressure of 0 kPa-50 kPa (absolute pressure).

[0064] According to the present invention, in some preferred embodiments, the weight removal conditions include: a reflux ratio of 0.2-5, for example, 0.2, 1, 2, 3, 4, 5, or a range consisting of any two of the above values.

[0065] According to the present invention, in some embodiments, the weight removal conditions include: the tower top temperature is 55.7-68.0°C.

[0066] According to the present invention, in some preferred embodiments, a coarse filtration step is provided between the light removal and the heavy removal; the coarse filtration is performed by a filter with a filtration specification of no more than 1 micron. By adopting the above embodiment, an acetone product with higher purity, lower evaporation residue content, particles (≥0.5 μm), and lower water content can be obtained.

[0067] According to the present invention, in some preferred embodiments, the dehydration method is pervaporation.

[0068] According to the present invention, the pervaporation separation method refers to separation using a membrane. In some preferred embodiments, the operating conditions of the pervaporation membrane separation method include: an operating pressure of 0-8 bar.

[0069] According to the present invention, in some preferred embodiments, the operating conditions of the pervaporation membrane separation method include: an operating temperature of 56.6-138.2° C., wherein the operating temperature refers to the corresponding pre-membrane temperature.

[0070] According to the present invention, in some preferred embodiments, the conditions of pervaporation include: the operating pressure on the permeate side is -100 to -80 kPa (absolute pressure).

[0071] According to the present invention, as long as the purpose of the present invention can be achieved, the method of deionization is not particularly limited. In some embodiments, the deionization is carried out in the presence of an ion exchange resin, wherein the ion exchange resin can be a hydrogen-type strongly acidic cation exchange resin and / or a hydroxide-type strongly basic anion exchange resin. In the present invention, an ion exchange resin model AmberjetUP6040 is used to illustrate the example, but the present invention is not limited to this.

[0072] According to the present invention, the filtration system used for filtration includes: a multi-stage series filter element made of PTFE, preferably, the filtration accuracy of the multi-stage series filter element increases step by step, for example, 4-stage filter elements with increasing filtration accuracy are used in series, specifically, PTFE filter elements with filtration specifications of 500nm, 200nm, 100nm and 50nm are used for filtration.

[0073] The third aspect of the present invention provides the use of the ultra-clean high-purity acetone of the present invention and / or the ultra-clean high-purity acetone prepared by the preparation method of the present invention in integrated circuits.

[0074] The ultra-clean high-purity acetone of the present invention can meet the requirements of cleaning solvents used in the integrated circuit industry.

[0075] According to the present invention, Figure 1As shown, in some embodiments, the preparation method of ultra-clean high-purity acetone includes: a batch of industrial-grade acetone crude product 1, this part of the acetone crude product 1 and the mixed material 2 containing an oxidant (the balance is water) are mixed through a static mixer (not shown) and then pumped into a first stirring tank ①, and mixed for 3 hours to obtain a first material 3; the first material 3 and the pH regulator are first mixed through a static mixer (not shown) and then pumped into a second stirring tank ②, and a second material 5 is obtained after mixing; the second material 5 enters a light component removal tower ③, and a light component 6 is obtained at the top of the tower, and the bottom product 7 is first filtered through a 1-micron filter (not shown) and then enters a heavy component removal tower ④, and the bottom of the heavy component removal tower ④ obtains a heavy component 8; the top distillate 9 obtained from the heavy component removal tower ④ enters a pervaporation device ⑤ for pervaporation, and water 10 is obtained on the permeate side, and the product 11 on the concentrated side enters a condenser filled with Amberjet The ion exchange resin of UP6040 is deionized in the deionization tower ⑥; the bottom material 12 of the deionization tower ⑥ is passed through the filtering system ⑦ to obtain the ultra-clean high-purity acetone product 13.

[0076] The present invention will be described in detail below through examples. In the following examples, the purity of the ultra-clean high-purity acetone product is measured by HPLC and the content of organic impurities is measured by ICP-MS; the single metal ion is measured by ICP-MS; the particles (≥0.5 μm) are measured online by a counter; the chromaticity is measured by a colorimeter; the acid value (converted into acetic acid) is measured by a titrator; the water content is measured by a Karl Fischer titrator; and the evaporation residue is measured by the general method of the national standard GB / T 9740-2008.

[0077] Example 1

[0078] A batch of high-quality industrial-grade crude acetone 1 (chemical purity of 99.5%, water content of 2560ppm, total aldehyde impurities of 35ppm) is mixed with a mixture 2 containing 2.5wt% potassium permanganate and 2.5wt% sodium tripolyphosphate (the balance is water) in a static mixer (not shown) and then pumped into a first stirring tank ①. The amount of the mixture 2 added is 0.005 times the mass of the crude acetone 1. The mixture is mixed at 40°C for 3h to obtain a first material 3.

[0079] The first material 3 and the alkali solution 4 containing 2 mol / L potassium hydroxide are first mixed in a static mixer (not shown) and then pumped into the second stirring tank ②, the pH value in the second stirring tank ② is controlled to be 8, and the second material 5 is obtained after mixing for 0.5 h at 25° C.;

[0080] The second material 5 enters the light component removal tower ③, the operating pressure of the light component removal tower ③ is 25kPa, the reflux ratio is 10, the tower bottom temperature is controlled to be 62.8°C, and the light component 6 is obtained at the tower top. The tower bottom product 7 is first filtered through a 1 micron filter (not shown) and then enters the heavy component removal tower ④. The operating pressure of the heavy component removal tower ④ is 25kPa, the reflux ratio is 2, the tower top temperature is controlled to be 62.4°C, and the heavy component 8 is obtained at the tower bottom;

[0081] The top distillate 9 obtained from the heavy component removal tower ④ enters the pervaporation device ⑤ for pervaporation, the operating pressure is 5 bar, the corresponding pre-membrane temperature is 120°C, the operating pressure on the permeation side is -99 kPa, water 10 is obtained on the permeation side, and the product 11 on the concentration side enters the deionization tower ⑥ filled with an ion exchange resin of model Amberjet UP6040 for deionization; the bottom material 12 of the deionization tower ⑥ passes through the filtration system ⑦ (composed of a four-stage series filter element made of PTFE; the specifications of the four-stage series filter element are 200nm, 100nm, 50nm and 15nm respectively) to obtain an ultra-clean high-purity acetone product 13.

[0082] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0083] Example 2

[0084] The method of Example 1 is followed, except that pervaporation is carried out in the pervaporation device ⑤, and the operating pressure is 2 bar; the rest is the same as in Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0085] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0086] Example 3

[0087] The method of Example 1 is followed, except that the operating reflux ratio of the heavy component removal tower ④ is 0.5; the rest is the same as Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0088] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0089] Example 4

[0090] The method of Example 1 is followed, except that 2.5 wt % hydrogen peroxide is used to replace the mixed material containing 2.5 wt % potassium permanganate; the rest is the same as Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0091] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0092] Example 5

[0093] The method of Example 1 is followed, except that 10 wt % hydrogen peroxide is used to replace the mixed material containing 2.5 wt % potassium permanganate; the rest is the same as Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0094] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0095] Example 6

[0096] The method of Example 1 is followed, except that the first material 3 is obtained after mixing at 5° C. for 0.5 h; the rest is the same as Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0097] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0098] Example 7

[0099] The method of Example 1 is followed, except that the bottom product 7 directly enters the heavy component removal tower ④ without being filtered through a 1-micron filter (not shown); the rest is the same as Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0100] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0101] Example 8

[0102] The method of Example 1 is followed, except that there is no sodium tripolyphosphate in the mixed material 2; the rest is the same as in Example 1, and an ultra-clean high-purity acetone product 13 is obtained.

[0103] The characteristics of the ultra-clean high-purity acetone product 13 are shown in Table 1.

[0104] Comparative Example 1

[0105] The method of Example 1 is different from that of Example 1:

[0106] The first material 3 directly enters the light component removal tower ③ for subsequent operation; the rest is the same as in Example 1 to obtain acetone product.

[0107] The characteristics of the acetone product are shown in Table 1.

[0108] Table 1

[0109]

[0110] 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 ultra-clean high-purity acetone, characterized in that: Chemical purity ≥99.99%, color ≤10Hazen, acid value ≤10ppm; organic impurity content ≤30ppm.

2. The ultra-clean high-purity acetone according to claim 1, wherein Ultra-clean high-purity acetone: Organic impurities ≤ 20ppm; and / or The organic impurities include at least one of isopropanol, acetaldehyde, propionaldehyde, propylene, isopropyl ether and methanol; and / or Moisture content ≤ 100 ppm; and / or Single metal ion content ≤ 50ppt; and / or Particles larger than 0.5 μm ≤ 10 / ml; and / or Evaporation residue content ≤1ppm.

3. A method for preparing ultra-clean high-purity acetone according to claim 1 or 2, characterized in that: The preparation method comprises: (1) the crude acetone product is brought into first contact with a mixture containing an oxidant to obtain a first material; (2) contacting the first material with a pH adjuster for a second time to obtain a second material; (3) De-lightening, de-heaving, dehydrating, deionizing, and filtering the second material.

4. The preparation method according to claim 3, wherein In step (1), the conditions for the first contact include: the crude acetone and the mixture containing the oxidant are first mixed in a static mixer, and the mixed materials are then mixed in a stirred tank. Preferably, the conditions for the second mixing include: a mixing temperature of 15-50° C., and / or a mixing time of 1-4 h; and / or In step (2), the conditions for the second contact include: the first material and the pH adjuster first enter the static mixer for the third mixing, and then enter the stirring tank for the fourth mixing after mixing. Preferably, the conditions for the fourth mixing include: the mixing temperature is 15-50°C, and / or the mixing time is 0.5h-1h.

5. The preparation method according to claim 3 or 4, wherein The pH value of the second material is 7-10; and / or The pH adjusting agent is selected from alkali solution; Preferably, the content of alkaline substances in the alkali solution is 0.5-5 mol / L; and / or The alkaline substance in the alkali solution is selected from at least one of sodium hydroxide, potassium hydroxide and ammonium hydroxide.

6. The preparation method according to any one of claims 3 to 5, wherein: The oxidant is selected from at least one of potassium permanganate, hydrogen peroxide, potassium dichromate, potassium perchlorate, potassium chlorite, potassium chlorate and potassium hypochlorite, and the content of the oxidant in the mixture is preferably 1-20wt%; and / or The oxidant-containing mixture further contains a stabilizer, preferably the stabilizer is selected from at least one of sodium tripolyphosphate, sodium polymethacrylate, sodium gluconate and sodium metasilicate, and the content of the stabilizer in the mixture is preferably 1-20wt%; and / or The mass ratio of the crude acetone to the mixed material is (0.001-0.01):1; and / or The chemical purity of the crude acetone is 98.5-99.9%.

7. The preparation method according to any one of claims 3 to 6, wherein: The conditions for removing light include: an operating pressure of 0-50 kPa; and / or a reflux ratio of 2-20 and / or a bottom temperature of 56.6-68.1° C.; and / or The conditions for weight removal include: an operating pressure of 0 kPa-50 kPa; and / or a reflux ratio of 0.2-5; and / or a tower top temperature of 55.7-68.0°C.

8. The preparation method according to any one of claims 3 to 7, wherein: A coarse filtration step is provided between the light removal and the heavy removal; the coarse filtration is performed using a filter with a filtration specification not greater than 1 micron.

9. The preparation method according to any one of claims 3 to 8, wherein: The dehydration method is pervaporation, and preferably the pervaporation conditions include: the pervaporation operating pressure is 0-8 bar; and / or, the operating temperature is 56.6-138.2° C.; and / or, the operating pressure on the permeate side is -100 to -80 kPa; and / or The deionization is carried out in the presence of an ion exchange resin; and / or The filtering system used for the filtering comprises: a multi-stage series filter element made of PTFE, and preferably the filtering accuracy of the multi-stage series filter element increases step by step.

10. Use of the ultra-clean high-purity acetone according to any one of claims 1 or 2, and / or the ultra-clean high-purity acetone prepared by the preparation method according to any one of claims 3 to 9 in integrated circuits.

Citation Information

Patent Citations

  • A method for preparing acetone

    CN103601624B

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

    CN201317750Y

  • System for producing ultra-clean high-purity electronic grade acetone

    CN101445439A

  • Method and device for preparing ultrapure acetone

    CN101973859A

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

    CN104030903A