CN101550129B - Method for refining 1,3-Propane sultone - Google Patents
Method for refining 1,3-Propane sultone Download PDFInfo
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- CN101550129B CN101550129B CN2009100680358A CN200910068035A CN101550129B CN 101550129 B CN101550129 B CN 101550129B CN 2009100680358 A CN2009100680358 A CN 2009100680358A CN 200910068035 A CN200910068035 A CN 200910068035A CN 101550129 B CN101550129 B CN 101550129B
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- propane sultone
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Abstract
A method for refining 1,3-propane sultone is characterized by comprising the following steps: firstly circularly infusing refrigerating fluid with temperature of 0-30 DEG C into a crystallizer; then circularly infusing the raw material of 1,3-Propane sultone with the temperature of 32-40 DEG C into the crystallizer for forming a film-shaped crystal in a crystallizing tube; along with the continuously cooling, the film-shaped crystal of 1,3-Propane sultone is gradually thickened, when the crystal layer obtains a preset thickness, discharging the mother solution, increasing the temperature of coolant to 35-50 DEG C for melting the crystal layer; and when the crystal layer is totally dissolved, collecting the refined 1,3-Propane sultone.
Description
Technical field
The present invention relates to a kind of method of refining organic cpds, particularly a kind of method of refining 1.3 propane sultone belongs to the organism purification techniques.
Background technology
1,3 propane sultone (PS) is widely used in fields such as dyestuff, medicine, tensio-active agent, and in the recent period along with the exploitation of green energy resource lithium ion battery, it is widely used as a kind of anti-inflatable functional additive of lithium ion battery organic electrolyte.
Lithium ion battery is the green high-capacity battery of a new generation; Numerous advantages such as have that voltage height, energy density are big, good cycle, self-discharge are little, memory-less effect, operating temperature range are wide are widely used in mobile telephone, notebook, video camera, electronic instrument, weaponry etc.In recent years; The output of lithium ion battery rapidly increases, and Application Areas constantly enlarges, and shows according to market survey; Can reach about 13.5 hundred million to lithium ion battery demand in 2010, become 21st century to national economy and the significant new high-tech product of people's lives.
1.3 propane sultone (PS) is as the basic function additive of preparation lithium ion secondary electrolytic solution; The height of its purity directly has influence on the quality of electrolyte quality; The PS of home market sale at present, purity is many about 99.5%, does not reach cell-grade and requires (purity＞99.9%).1.3 the process for purification of propane sultone (PS), patent CN101157681A is with molecular distillation technique preparation, purification, separation 1.3 propane sultone (PS), and purity can reach 99.5%.State, inside and outside not appearing in the newspapers are exclusively used in the technology of refining 1.3 propane sultone.
Summary of the invention
The object of the present invention is to provide a kind of method that is used for the yellow lactone of refining 1.3 propane, the yellow lactone purity of obtained 1.3 propane is high.
The yellow lactone raw material of used 1.3 propane of the present invention is the Industrial products of purity about 99.5%, can obtain the high purity product greater than 99.9% after making with extra care through present method.
The present invention realizes through following technical proposals.The method of the yellow lactone of a kind of refining 1.3 propane is characterized in that comprising following process:
The refrigerating fulid that at first in mold, circulates and feed 0～30 ℃ with in 32 ℃～40 ℃ the liquid state 1.3 propane sultone raw materials circulation feeding mold, makes raw material in crystallizer, form membranaceous crystallization then; Along with continuing cooling, the membranaceous crystallization progressive additive of 1.3 propane sultone is when crystal layer reaches expectation thickness; Discharge mother liquor; Rising coolant temperature to 35 ℃～50 ℃ of fusing crystal layers treats that crystal layer all after the dissolving, collects purified 1.3 propane sultone.
The method of refining 1.3 propane sultone as described above is characterized in that need not introducing new solvent, for self fusion-crystallization is made solvent.
The method of refining 1.3 propane sultone as described above is characterized in that material and refrigerating fulid all are with falling liquid film state mobile in mold.
The method of refining 1.3 propane sultone as described above is characterized in that material and refrigerating fulid all circulate in mold.
The method of refining 1.3 propane sultone as described above, it is characterized in that can be according to target purity demand crystallization control yield within 20%～80% scope.
The method of refining 1.3 propane sultone as described above is characterized in that the temperature of quench liquid reduces gradually along with the thickening of crystal layer.
The method of refining 1.3 propane sultone as described above, refrigerating fulid can be selected from chilled brine, and water, oil are wherein a kind of as heat-conduction medium.
The characteristics of technology of the present invention are, at first circulation feeds refrigerating fulid precooling mold in mold, refrigerating fulid the crystallizer outer wall with the falling liquid film state flow under, behind the device constant temperature to be crystallized; Liquid 1.3 propane sultone raw materials circulation is fed in the mold, and material becomes the falling liquid film shape to flow down in crystallizer, along with heat spreading out of through refrigerating fulid; 1.3 the yellow lactone of propane forms uniform membranaceous crystallization in crystallizer, along with lasting cooling heat constantly spreads out of, and membranaceous crystallization progressive additive; Cause bulk by the membranaceous sheet that becomes, on the other hand, along with membranaceous crystallization progressive additive; Thermal conduction rate reduces, and for improving heat transfer efficiency, speed that can be certain reduces the temperature of refrigerating fulid; When crystal layer reaches expectation thickness, discharge mother liquor, rising coolant temperature fusing crystal layer; Treat that an amount of back of crystal layer dissolving recycle stock accelerates the crystal layer fusing, treat that crystal layer all after the fusing, collects purified 1.3 propane sultone.
The invention has the advantages that technology, equipment are simple, easy to operate, less investment, environmental protection, energy-conservation, be easy to industriallization.Crystallization process has clear superiority with respect to rectification method, and vaporization heat and melting heat are the multiple relations, say that from energy consumption crystallization process consumes energy well below rectification method, and especially purity requirement is high more, and the crystallization process advantage highlights more.On the liquid-flow mode, the present invention works hard on energy-conservation again, and shell side, tube side are all taked the falling liquid film mode, with respect to mobile energy consumption and the cooling energy consumption that greatly reduces pump of full state.Owing to be that PS self carries out the shortcoming that crystallization has overcome the new impurity of the easy introducing of solvent method crystallization; Also avoided complicated liquid-solid separation device in the operation, simplified the operation, simultaneously because material is mobile at the crystallizer internal recycle; Crystal layer is had scouring effect, guaranteed the densification and the product gas purity of crystalline state.
Embodiment
Below in conjunction with embodiment the present invention is made further detailed description:
Instance 1
Get an amount of 200Kg purity and be 99.8583% PS raw material, 30 ℃ of Control Circulation bath temperatures, 40 ℃ of charge temperatures, 1 ℃/h of circulating water cooling speed; After the circulation crystallization 8 hours, stop, discharging mother liquor; Crystallization 86kg is collected in fusing, and the chromatography of gases purity assay reaches 99.9658%.
Instance 2
Get an amount of 200Kg purity and be 99.8518% PS raw material, 26 ℃ of Control Circulation bath temperatures, 36 ℃ of charge temperatures, 1 ℃/h of circulating water cooling speed; After the circulation crystallization 8 hours, stop, discharging mother liquor; Crystallization 121kg is collected in fusing, and the chromatography of gases purity assay reaches 99.9532%.
Instance 3
Get an amount of 200Kg purity and be 99.8511% PS raw material, 22 ℃ of Control Circulation bath temperatures, 32 ℃ of charge temperatures, 1 ℃/h of circulating water cooling speed; After the circulation crystallization 8 hours, stop, discharging mother liquor; Crystallization 157kg is collected in fusing, and the chromatography of gases purity assay reaches 99.9546%.
Instance 4
Get an amount of 200Kg purity and be 99.8780% PS raw material, 30 ℃ of Control Circulation bath temperatures, 32 ℃ of charge temperatures, 2 ℃/h of circulating water cooling speed; After the circulation crystallization 8 hours, stop, discharging mother liquor; Crystallization 143kg is collected in fusing, and the chromatography of gases purity assay reaches 99.9583%.
Claims (7)
1. make with extra care 1 for one kind, the method for 3-propane sultone is characterized in that comprising following process:
The refrigerating fulid that at first in mold, circulates and feed 0 ℃～30 ℃, with 32 ℃～40 ℃ liquid state 1, the circulation of 3-propane sultone raw material feeds in the mold, makes raw material in crystallizer, form membranaceous crystallization then; Along with continuing cooling, 1, the membranaceous crystallization progressive additive of 3-propane sultone; When crystal layer reaches when estimating thickness, discharge mother liquor, rising coolant temperature to 35 ℃～50 ℃ of fusing crystal layers; After treating that crystal layer all dissolves, collect purified 1,3-propane sultone.
2. as claimed in claim 1 refining 1, the method for 3-propane sultone is characterized in that need not introducing new solvent, for self fusion-crystallization is made solvent.
3. as claimed in claim 1 refining 1, the method for 3-propane sultone is characterized in that material and refrigerating fulid all are with falling liquid film state mobile in mold.
4. as claimed in claim 1 refining 1, the method for 3-propane sultone is characterized in that material and refrigerating fulid all circulate in mold.
5. as claimed in claim 1 refining 1, the method for 3-propane sultone, it is characterized in that can be according to target purity demand crystallization control yield within 20%～80% scope.
6. as claimed in claim 1 refining 1, the method for 3-propane sultone is characterized in that the temperature of quench liquid reduces gradually along with the thickening of crystal layer.
7. as claimed in claim 1 refining 1, the method for 3-propane sultone, refrigerating fulid is selected from chilled brine, water or the oil a kind of as heat-conduction medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100680358A CN101550129B (en) | 2009-03-06 | 2009-03-06 | Method for refining 1,3-Propane sultone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100680358A CN101550129B (en) | 2009-03-06 | 2009-03-06 | Method for refining 1,3-Propane sultone |
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| Publication Number | Publication Date |
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| CN101550129A CN101550129A (en) | 2009-10-07 |
| CN101550129B true CN101550129B (en) | 2012-07-25 |
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| CN2009100680358A Expired - Fee Related CN101550129B (en) | 2009-03-06 | 2009-03-06 | Method for refining 1,3-Propane sultone |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107827865A (en) * | 2017-10-23 | 2018-03-23 | 惠州市宙邦化工有限公司 | A kind of method of purification of 1,3 propane sultone |
| CN112337132A (en) * | 2020-11-20 | 2021-02-09 | 中国有色集团（广西）平桂飞碟股份有限公司 | Ferrous sulfate crystal separation treatment method for titanium dioxide production by sulfuric acid process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85201095U (en) * | 1985-04-01 | 1986-01-01 | 大连工学院 | Evaporated and reacted crystallizer for glucono-delta-lactone |
| CN1568299A (en) * | 2001-10-10 | 2005-01-19 | 巴斯福股份公司 | Method for the isolation of salts of organic acids from a fermentation broth and for releasing the organic acid |
| CN101157681A (en) * | 2007-11-01 | 2008-04-09 | 姜俊 | Method for preparing 1,3 propane sultone |
-
2009
- 2009-03-06 CN CN2009100680358A patent/CN101550129B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85201095U (en) * | 1985-04-01 | 1986-01-01 | 大连工学院 | Evaporated and reacted crystallizer for glucono-delta-lactone |
| CN1568299A (en) * | 2001-10-10 | 2005-01-19 | 巴斯福股份公司 | Method for the isolation of salts of organic acids from a fermentation broth and for releasing the organic acid |
| CN101157681A (en) * | 2007-11-01 | 2008-04-09 | 姜俊 | Method for preparing 1,3 propane sultone |
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| CN101550129A (en) | 2009-10-07 |
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