CN115197193B - Preparation method of electronic-grade 1, 4-butane sultone - Google Patents
Preparation method of electronic-grade 1, 4-butane sultone Download PDFInfo
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- CN115197193B CN115197193B CN202210838681.3A CN202210838681A CN115197193B CN 115197193 B CN115197193 B CN 115197193B CN 202210838681 A CN202210838681 A CN 202210838681A CN 115197193 B CN115197193 B CN 115197193B
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- butane sultone
- water content
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- MHYFEEDKONKGEB-UHFFFAOYSA-N oxathiane 2,2-dioxide Chemical compound O=S1(=O)CCCCO1 MHYFEEDKONKGEB-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 106
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 52
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002808 molecular sieve Substances 0.000 claims abstract description 17
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 7
- 230000001502 supplementing effect Effects 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 230000000630 rising effect Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000010926 purge Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 8
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D327/00—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
- C07D327/02—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms one oxygen atom and one sulfur atom
- C07D327/06—Six-membered rings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of electronic grade 1, 4-butane sultone, which comprises the following steps: s1, directly filling 1, 4-butane sultone subjected to rectification treatment on a factory production line into a reaction kettle filled with a molecular sieve, standing for 8-16h, and obtaining a product with an acid value and water content primarily reduced; s2, injecting the product processed in the step S1 into each open tank body in a closed container in a dry and clean environment to form a layer of liquid film at the tank bottom, slowly cooling to below 12.5 ℃ after standing, circularly introducing nitrogen with the water content of below 15ppm into the closed container by using a circulation pipeline to take away moisture and impurities, and continuously circulating until the water content of the nitrogen is not more than 5ppm for more than 24 hours; s3, standing and rising to room temperature, and collecting liquid in each open groove body. The method has the advantages that the molecular sieve, the low temperature and nitrogen purging water carrying technology are combined, the process is relatively simple, and the acid value and the water content of the product can be remarkably reduced.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a preparation method of electronic grade 1, 4-butane sultone.
Background
Sulfonate is an organic film-forming additive with good effect, the electronegativity of the central sulfur atom is stronger, the reducibility of the sulfonate in a graphite negative electrode is stronger than that of carbonate, and a more stable solid electrolyte phase interface film is formed in preference to the interface of an electrode. 1, 3-propane sultone and 1, 4-butane sultone are generally used as stabilizers in an electrolyte to improve thermal stability and cycle life of a battery because of their good film forming property and high and low temperature properties. However, the addition of the above sulfonate species to the electrolyte is highly required for purity, wherein the acid value and moisture requirement for 1, 3-propane sultone should generally be 50ppm or less, and the smaller the acid value and moisture of 1, 4-butane sultone is, the better the corresponding battery performance is.
The Chinese patent No. 107043365A discloses an effective method for reducing acid value and water content of 1, 3-propane sultone, which is characterized in that molecular sieve is utilized to carry out primary purification on the 1, 3-propane sultone, and then distillation, nanofiltration membrane and reverse osmosis membrane are sequentially utilized to carry out treatment to obtain electronic grade 1, 3-propane sultone, wherein the acid value and water content are reduced to below 50ppm, and the use requirement of electrolyte is met. However, when the purification treatment and refining of 1, 4-propane sultone are attempted by the same method, the ideal effect cannot be obtained after multiple key parameter adjustment, so that a method for effectively reducing the acid value and the moisture of 1, 4-butane sultone to achieve the electronic grade additive standard is required to be developed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of electronic grade 1, 4-butane sultone, which aims to solve the problems in the prior art.
The technical scheme for solving the technical problems is as follows: a method for preparing electronic grade 1, 4-butane sultone, which comprises the following steps:
s1, directly filling 1, 4-butane sultone subjected to rectification treatment on a factory production line into a reaction kettle filled with a molecular sieve, standing for 8-16h to obtain 1, 4-butane sultone with an acid value of 0-64ppm and a water mass content of 0-120ppm for later use;
s2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film at the groove bottom, standing for more than 3 hours, slowly cooling to below 12.5 ℃, circularly introducing nitrogen with the water content of below 15ppm into the closed container by using a circulation pipeline, continuously circulating and monitoring the water content of the nitrogen, discharging at least half of the molar amount of nitrogen in the closed container and supplementing new nitrogen with the water content of below 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24 hours, and continuously circulating until the water content of the nitrogen is increased by more than 24 hours and is not increased by more than 5 ppm;
s3, standing and raising the temperature to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 0-30ppm and the water content of 0-40 ppm.
On the basis of the technical scheme, the invention can be further specifically selected as follows.
Specifically, the standing temperature of the 1, 4-butane sultone in the step S1 in the reaction kettle is controlled to be 25-35 ℃.
Specifically, the molecular sieve in the reaction kettle in the step S1 is a 4A molecular sieve or a 5A molecular sieve.
Specifically, the open groove body in the step S2 is a rectangular groove or a round groove, the opening area is more than 2.5m 2, the groove depth is 5-10cm, and the liquid film thickness is 1-3cm.
Specifically, in the step S2, a plurality of open groove bodies are stacked and placed through a bracket, and the interval distance between two adjacent open groove bodies is 20-50cm.
Specifically, an air pipe for slowly feeding nitrogen gas flow to the solid 1, 4-butane sultone in the tank is arranged above or at one side of each layer of the open tank body, and the air pipe is communicated with the circulating pipeline.
Specifically, in the step S2, before 1, 4-butane sultone is injected into an open tank body, nitrogen with the water content of less than 15ppm is used for purging the closed container, after 1, 4-butane sultone is injected into the open tank body, a certain amount of nitrogen with the water content of less than 15ppm is injected into the closed container through a circulating pipeline and circulated, and the air pressure of the closed container is kept at 1.1-1.2atm in the circulating process.
Specifically, the cooling speed is controlled to be 0.5-1 ℃/10min when the temperature is reduced in the step S2.
The method utilizes the effect of molecular sieve to adsorb water molecules and small molecular organic impurities to primarily purify the 1, 4-butane sultone with higher water content and acid value after rectification, then solidifies a liquid film formed by the 1, 4-butane sultone at a temperature slightly lower than the melting point of the 1, 4-butane sultone, and has certain effect of promoting the movement of water to an upper layer after the liquid film is formed and is stood for a period of time and in the subsequent slow cooling solidification process, and finally takes away the water on the surface layer under the circulation effect of nitrogen with low water content, and some unset small organic molecular impurities can be taken away by nitrogen in the process, so that the purity of the 1, 4-butane sultone is further obviously improved.
Drawings
FIG. 1 is a process flow diagram corresponding to the preparation method of electronic grade 1, 4-butane sultone.
Detailed Description
The invention is described in further detail below with reference to the drawings and to specific embodiments, which are given for illustration only and are not intended to limit the scope of the invention.
The medicines and devices used in the following examples are commercially available products or devices which can be assembled by one of ordinary skill in the art if necessary, and the methods used are conventional in the art if not specified.
As shown in FIG. 1, the invention provides a preparation method of electronic grade 1, 4-butane sultone, which takes 1, 4-butane sultone (the acid value is about 120ppm and the water content is about 360 ppm) with quite high purity (more than 99.9 percent) obtained after rectification as a raw material, and further refines and purifies the raw material to achieve the aim of obviously reducing the acid value and the water content. In the following embodiment, the open groove body in the step S2 is a rectangular groove, the opening area is more than 2.5m 2, and the groove depth is 5cm; the plurality of open groove bodies are stacked and placed through the support, and the interval distance between two adjacent open groove bodies is 25cm; the closed container is a stainless steel box body, which is purged, dried and purified in advance by nitrogen with the water content of 15 ppm.
Example 1
A preparation method of electronic grade 1, 4-butane sultone comprises the following steps:
s1, directly filling 1, 4-butane sultone (acid value is 108ppm, water content is 345 ppm) subjected to rectification treatment on a factory production line into a reaction kettle filled with a 4A molecular sieve, standing at 25 ℃ for 16 hours to obtain 1, 4-butane sultone with acid value of 57ppm and water content of 103ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film with the thickness of 1cm at the groove bottom, standing for 3h, slowly cooling to 12.5 ℃ (the cooling speed is 0.5 ℃/10 min), circularly introducing nitrogen with the water content of 15ppm into the closed container by using a circulation pipeline to enable the air pressure in the closed container to reach 1.1atm, continuously circulating and monitoring the water content of the nitrogen, discharging half of the molar amount of nitrogen in the closed container (the air pressure is halved and the same applies) and supplementing new nitrogen with the water content of 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24h, and repeating for several times until the water content of the nitrogen is increased by no more than 5 ppm;
s3, standing and rising to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 16ppm and the water content of 24 ppm.
Example 2
A preparation method of electronic grade 1, 4-butane sultone comprises the following steps:
s1, directly filling 1, 4-butane sultone (acid value 116ppm, moisture content 371 ppm) subjected to rectification treatment on a factory production line into a reaction kettle filled with a 4A molecular sieve, standing at 25 ℃ for 16 hours to obtain 1, 4-butane sultone with acid value 53ppm and moisture mass content 112ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film with the thickness of 1cm at the groove bottom, standing for 3h, slowly cooling to 12.5 ℃ (the cooling speed is 0.5 ℃/10 min), circularly introducing nitrogen with the water content of 15ppm into the closed container by using a circulation pipeline to enable the air pressure in the closed container to reach 1.1atm, continuously circulating and monitoring the water content of the nitrogen, discharging half of the molar amount of nitrogen in the closed container (the air pressure is halved and the same applies) and supplementing new nitrogen with the water content of 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24h, and repeating for several times until the water content of the nitrogen is increased by no more than 5 ppm;
S3, standing and rising to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 24ppm and the water content of 31 ppm.
Example 3
A preparation method of electronic grade 1, 4-butane sultone comprises the following steps:
S1, directly filling 1, 4-butane sultone (acid value is 129ppm and water content is 338 ppm) subjected to rectification treatment on a factory production line into a reaction kettle filled with a 4A molecular sieve, standing at 25 ℃ for 16 hours to obtain 1, 4-butane sultone with acid value of 61ppm and water content of 84ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film with the thickness of 1cm at the groove bottom, standing for 5 hours, slowly cooling to 12.5 ℃ (the cooling speed is 0.5 ℃/10 min), circularly introducing nitrogen with the water content of 15ppm into the closed container by using a circulation pipeline to enable the air pressure in the closed container to reach 1.1atm, continuously circulating and monitoring the water content of the nitrogen, discharging half of the molar amount of nitrogen in the closed container (the air pressure is halved and the same applies) and supplementing new nitrogen with the water content of 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24 hours, and repeating for several times until the water content of the nitrogen is increased by no more than 5 ppm;
S3, standing and rising to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 18ppm and the water content of 21 ppm.
Example 4
A preparation method of electronic grade 1, 4-butane sultone comprises the following steps:
S1, directly filling 1, 4-butane sultone (acid value 135ppm, water content 391 ppm) subjected to rectification treatment on a factory production line into a reaction kettle filled with a 5A molecular sieve, standing for 10 hours at 35 ℃ to obtain 1, 4-butane sultone with acid value 56ppm and water content 98ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film with the thickness of 2cm at the groove bottom, standing for 8 hours, slowly cooling to 12.5 ℃ (the cooling speed is 1 ℃/10 min), circularly introducing nitrogen with the water content of 15ppm into the closed container by using a circulation pipeline to enable the air pressure in the closed container to reach 1.2atm, continuously circulating and monitoring the water content of the nitrogen, discharging half molar amount of nitrogen in the closed container (the air pressure is halved and the same as the description below) and supplementing new nitrogen with the water content of 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24 hours, and repeating for several times until the water content of the nitrogen is increased by no more than 5 ppm;
S3, standing and rising to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 24ppm and the water content of 34 ppm.
Example 5
A preparation method of electronic grade 1, 4-butane sultone comprises the following steps:
S1, directly filling 1, 4-butane sultone (acid value 115ppm, water content 324 ppm) subjected to rectification treatment on a factory production line into a reaction kettle filled with a 5A molecular sieve, standing for 10 hours at 35 ℃ to obtain 1, 4-butane sultone with acid value 45ppm and water content 85ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film with the thickness of 2cm at the groove bottom, standing for 8 hours, slowly cooling to 12.5 ℃ (the cooling speed is 1 ℃/10 min), circularly introducing nitrogen with the water content of 15ppm into the closed container by using a circulation pipeline to enable the air pressure in the closed container to reach 1.2atm, continuously circulating and monitoring the water content of the nitrogen, discharging half molar amount of nitrogen in the closed container (the air pressure is halved and the same as the description below) and supplementing new nitrogen with the water content of 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24 hours, and repeating for several times until the water content of the nitrogen is increased by no more than 5 ppm;
S3, standing and rising to room temperature, and collecting liquid in each open groove body to obtain the electronic grade 1, 4-butane sultone with the acid value of 19ppm and the water content of 28 ppm.
From the above examples, the preparation method provided by the invention can remarkably reduce the acid value and the water content of the 1, 4-butane sultone to achieve the electronic grade, and meets the requirement of adding and using in the electrolyte.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The preparation method of the electronic grade 1, 4-butane sultone is characterized by comprising the following steps:
s1, directly filling 1, 4-butane sultone subjected to rectification treatment on a factory production line into a reaction kettle filled with a molecular sieve, standing for 8-16h to obtain 1, 4-butane sultone with an acid value of 0-64ppm and a water mass content of 0-120ppm for later use;
S2, injecting the 1, 4-butane sultone processed in the step S1 into each open groove body in a closed container in a dry and clean environment to form a layer of liquid film at the groove bottom, standing for more than 3 hours, cooling to below 12.5 ℃, circularly introducing nitrogen with the water content of below 15ppm into the closed container by using a circulation pipeline, continuously circulating and monitoring the water content of the nitrogen, discharging at least half of the molar amount of nitrogen in the closed container and supplementing new nitrogen with the water content of below 15ppm when the water content of the nitrogen is increased by more than 5ppm in 24 hours, and then continuously circulating until the water content of the nitrogen is increased by more than 24 hours and is not more than 5 ppm;
S3, standing and raising the temperature to room temperature, and collecting liquid in each open groove body to obtain electronic grade 1, 4-butane sultone with an acid value of 0-30ppm and a moisture content of 0-40 ppm;
And in the step S2, the cooling speed is controlled to be 0.5-1 ℃/10min when the temperature is reduced.
2. The method for preparing electronic grade 1, 4-butane sultone according to claim 1, wherein the standing temperature of 1, 4-butane sultone in step S1 in the reaction kettle is controlled to 25-35 ℃.
3. The method for preparing electronic grade 1, 4-butane sultone according to claim 1, wherein the molecular sieve in the reaction kettle in the step S1 is 4A molecular sieve or 5A molecular sieve.
4. The method for preparing electronic grade 1, 4-butane sultone according to claim 1, wherein the open groove body in the step S2 is a rectangular groove or a round groove, the opening area is more than 2.5m 2, the groove depth is 5-10cm, and the liquid film thickness is 1-3cm.
5. The method for preparing electronic grade 1, 4-butane sultone according to claim 4, wherein a plurality of open grooves are formed in the step S2 and are stacked by a bracket, and the interval distance between two adjacent open grooves is 20-50cm.
6. The method for preparing electronic grade 1, 4-butane sultone according to claim 5, wherein an air pipe for slowly feeding nitrogen gas flow to the solid 1, 4-butane sultone in the tank is arranged above or at one side of each layer of the open tank body, and the air pipe is communicated with the circulating pipeline.
7. The process for producing electronic grade 1, 4-butane sultone as claimed in any one of claims 1 to 6, wherein in step S2, the gas in the closed vessel is purged with nitrogen having a water content of 15ppm or less before 1, 4-butane sultone is injected into the open vessel, and after 1, 4-butane sultone is injected into the open vessel, a certain amount of 15ppm or less of nitrogen is injected into the closed vessel through the circulation line and circulated, and the pressure of the closed vessel is maintained at 1.1 to 1.2atm during the circulation.
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| CN202210838681.3A CN115197193B (en) | 2022-07-18 | 2022-07-18 | Preparation method of electronic-grade 1, 4-butane sultone |
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| CN115197193B true CN115197193B (en) | 2024-06-25 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177326A (en) * | 2014-08-07 | 2014-12-03 | 武汉中德远东精细化工有限公司 | Preparation method of electronic grade 1, 3-propanesultone |
| CN114247172A (en) * | 2020-09-23 | 2022-03-29 | 四川大学 | Method and device for removing water solution volatile impurities and preparing crystallized product by air circulation gas stripping concentration |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10338653A (en) * | 1997-06-06 | 1998-12-22 | Jiyunsei Kagaku Kk | Dehydration of liquid |
| CN107043365A (en) * | 2017-04-26 | 2017-08-15 | 武汉松石科技股份有限公司 | A kind of embrane method preparation method of the propane sultone of electron level 1,3 |
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2022
- 2022-07-18 CN CN202210838681.3A patent/CN115197193B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177326A (en) * | 2014-08-07 | 2014-12-03 | 武汉中德远东精细化工有限公司 | Preparation method of electronic grade 1, 3-propanesultone |
| CN114247172A (en) * | 2020-09-23 | 2022-03-29 | 四川大学 | Method and device for removing water solution volatile impurities and preparing crystallized product by air circulation gas stripping concentration |
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| CN115197193A (en) | 2022-10-18 |
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