CN106187987A - A kind of environmental protection method of purification of acrylic 1,3 sultones - Google Patents
A kind of environmental protection method of purification of acrylic 1,3 sultones Download PDFInfo
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- CN106187987A CN106187987A CN201610545725.8A CN201610545725A CN106187987A CN 106187987 A CN106187987 A CN 106187987A CN 201610545725 A CN201610545725 A CN 201610545725A CN 106187987 A CN106187987 A CN 106187987A
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- propenyl
- sulfonic acid
- acid lactone
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- 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
- C07D327/04—Five-membered rings
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Abstract
The invention belongs to lithium battery electrolytes additive technology field, be specifically related to the environmental protection method of purification of a kind of acrylic 1,3 sultones.The method comprising the steps of: 1) by acrylic 1, and 3 sultones crude products join in aqueous solvent, is heated to 25～75 DEG C of stirring and dissolving, acrylic 1, and 3 sultones crude products are 1:20～1:10 with the mass ratio of water；2) to step 1) aqueous solution that obtains adds activated carbon decolour, rear filtered while hot of having decoloured, obtain filtrate；3) by step 2) filtrate that obtains is cooled to 0～15 DEG C and separates out crystal, isolated crystal and mother solution；4) by step 3) crystal that obtains is dried at 0～82 DEG C, obtains acrylic 1, the 3 thin product of sultones.Equipment and technique needed for the method are simpler, it is not necessary to use organic solvent to purify acrylic 1, the method for 3 sultoness, and adaptation can repeatedly circulate purification, purification process is prone to industrialization, is the environmental protection method of purification of simple acrylic 1,3 sultones.
Description
Technical field
The invention belongs to lithium battery electrolytes additive technology field, be specifically related to a kind of propenyl-1,3-sulfonic acid lactone
Environmental protection method of purification.
Background technology
Propenyl-1,3-sulfonic acid lactone is a kind of important chemical intermediate, electrochemistry, dyestuff, medicine, brightener,
The fields such as surfactant have a wide range of applications, particularly moisture high-purity propylene base-1 less than 200ppm, in 3-sulfonic acid
Ester can be used as lithium battery electrolytes additive, in order to improve life-span and the safety of battery.
Propenyl-1,3-sulfonic acid lactone, molecular formula C3H4O3S, molecular weight 120.13, off-white color crystal, fusing point 82～83
DEG C, boiling point 257 DEG C, density 1.508, flash-point 109 DEG C.
In document, " preparation method of PST " (publication number: 101456856A) and " acrylic-1,
The preparation method of 3-sultones " (publication number: CN 101659653A), utilize organic solvent such as: benzene, toluene, ethyl acetate and
Dichloromethane etc. carry out crystallization and purification to propenyl-1,3-sulfonic acid lactone, carry out crystallization and purification with organic solvent, and not only cost is relatively
Height, and to environment, the health of operator is damaged.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides the environmental protection purification side of a kind of propenyl-1,3-sulfonic acid lactone
Method.Equipment and technique needed for the method are simpler, it is not necessary to use organic solvent to purify propenyl-1,3-sulfonic acid lactone
Method, and use repeatedly circulate purification, purification process is prone to industrialization, is simple propenyl-1,3-sulfonic acid lactone
Environmental protection method of purification.
A kind of acrylic-1, the method for purification of 3-propane sultone, comprise the following steps:
1) propenyl-1,3-sulfonic acid lactone crude product is joined in aqueous solvent, be heated to 25～75 DEG C of stirring and dissolving, obtain
Aqueous solution, wherein, propenyl-1,3-sulfonic acid lactone crude product is 1:20～1:10 with the mass ratio of water.
Further, propenyl-1,3-sulfonic acid lactone crude product from the preparation process of propenyl-1,3-sulfonic acid lactone, third
The purity of thiazolinyl-1,3-sultones crude product is 85～90%.
Preferably, the mass ratio of propenyl-1,3-sulfonic acid lactone crude product and water is 1:15～1:10, solution temperature be 45～
65℃。
2) to step 1) aqueous solution that obtains adds activated carbon decolour, rear filtered while hot of having decoloured, obtain filtrate.
3) by step 2) filtrate that obtains is cooled to 0～15 DEG C and separates out crystal, isolated crystal and mother solution.
Further, step 3) in the mother solution that obtains use step 1 as recycling design, set) before acrylic-1,3-
In the preparation process of sultones crude product.
Preferably, crystallization temperature is 0～10 DEG C.
4) by step 3) crystal that obtains is dried at 0～82 DEG C, obtains the thin product of propenyl-1,3-sulfonic acid lactone.
Preferably, baking temperature is 60～80 DEG C, and drying pressure is-0.5～-0.1Mpa.
Further, after separating out based on crystal, the mother solution of isolated returns the preparation of propenyl-1,3-sulfonic acid lactone
Journey, the environmental protection method of purification of propenyl-1,3-sulfonic acid lactone comprises the following steps:
1) acrylic-1,3-sultones crude product is prepared；
2) propenyl-1,3-sulfonic acid lactone crude product is joined in aqueous solvent, be heated to 25～75 DEG C of stirring and dissolving, obtain
Aqueous solution, wherein, propenyl-1,3-sulfonic acid lactone crude product is 1:20～1:10 with the mass ratio of water；
3) to step 2) aqueous solution that obtains adds activated carbon decolour, rear filtered while hot of having decoloured, obtain filtrate；
4) by step 3) filtrate that obtains is cooled to 0～15 DEG C and separates out crystal, isolated crystal and mother solution, mother solution conduct
Step 1 used by solvent set) in, wherein, step 4) consumption of mother solution that obtains and step 1) in preparation process in solvent
The volume ratio of consumption be 0.3:1～0.8:1；
5) step 1 is repeated) to step 4), obtain total crystal；
6) by step 5) total crystal of obtaining is dried at 0～82 DEG C, obtains propenyl-1,3-sulfonic acid lactone thin
Product.
Other acrylic-1 in the prior art that compares, the method for purification of 3-propane sultone, provided by the present invention
Method of purification is made solvent with water and is carried out crystallization and purification, on the one hand can reduce cost, reduces the pollution to environment and avoid behaviour
Making the somatic damage of personnel, on the other hand, Dan Yishui is as solvent, and the system of the mother solution after crystallization and purification is simpler, and then
Directly overlap to use in early stage preparation technology again and be circulated, it is ensured that after cycling during being prepared into purification, all the time
Be in a simplest dicyandiamide solution, thus avoid the solvent that multi-solvent system usually needs to face extract and separate or
The problems such as separated.Prior, carry out crystallization and purification using water as solvent, although yield decreases, but the lowest
Cost obtain more than 99.6% acrylic-1,3-propane sultone, and further refined being purified to of being more convenient for
99.9%.And relative to the reduction of yield, the added value brought to product that improves further of purity is but greatly promoted.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
1. in 2000mL four-hole boiling flask, add propenyl-1,3-sulfonic acid lactone crude product 100g, water 1000g.It is warmed up to 50
DEG C stirring makes solid dissolve；
2. add 1g activated carbon to decolour, rear filtered while hot of having decoloured；
3. after filtrate cools to 10 DEG C, crystal filter pressing is separated, after filtrate collection, treat use next time；
4. propenyl-1,3-sulfonic acid lactone crystal is vacuum dried 12h at 60 DEG C, obtains propenyl-1,3-sulfonic acid lactone
73g, content 99.63%.
Embodiment 2
1. in 2000mL four-hole boiling flask, add propenyl-1,3-sulfonic acid lactone crude product 100g, water 1000g.It is warmed up to 55
DEG C stirring makes solid dissolve；
2. add 1g activated carbon to decolour, rear filtered while hot of having decoloured；
3. after filtrate cools to 5 DEG C, crystal filter pressing is separated, after filtrate collection, treat use next time；
4. propenyl-1,3-sulfonic acid lactone crystal is vacuum dried 12h at 60 DEG C, obtains propenyl-1,3-sulfonic acid lactone
68g, content 99.67%.
Embodiment 3
1. adding propenyl-1,3-sulfonic acid lactone crude product 80g, water 140g in 2000mL four-hole boiling flask, embodiment one is pressed
The mother solution 860mL that filter obtains.Being warmed up to 50 DEG C of stirrings makes solid dissolve；
2. add 1g activated carbon to decolour, rear filtered while hot of having decoloured；
3. after filtrate cools to 10 DEG C, crystal filter pressing is separated, after filtrate collection, treat use next time；
4. propenyl-1,3-sulfonic acid lactone crystal is vacuum dried 12h at 60 DEG C, obtains propenyl-1,3-sulfonic acid lactone
62g, content 99.59%.
Embodiment 4
1. in 2000mL four-hole boiling flask, add propenyl-1,3-sulfonic acid lactone crude product 80g, the last filter pressing of embodiment two
Mother solution.Being warmed up to 55 DEG C of stirrings makes solid dissolve；
2. add 1g activated carbon to decolour, rear filtered while hot of having decoloured；
3. after filtrate cools to 5 DEG C, crystal filter pressing is separated, after filtrate collection, treat use next time；
4. propenyl-1,3-sulfonic acid lactone crystal is vacuum dried 12h at 60 DEG C, obtains propenyl-1,3-sulfonic acid lactone
59g, content 99.62%.
Embodiment 5
With embodiment 1, carry out step 1 and arrive step 4, then carry out following operation:
5. adding propenyl-1,3-sulfonic acid lactone crude product 100g, water 200g in 2000mL four-hole boiling flask, step 3 is collected
The mother solution 800mL obtained, is warmed up to 50 DEG C of stirrings and makes solid dissolve；
6. add 1g activated carbon to decolour, rear filtered while hot of having decoloured；
7. after filtrate cools to 10 DEG C, crystal filter pressing is separated, after filtrate collection, treat use next time；
8. propenyl-1,3-sulfonic acid lactone crystal is vacuum dried 12h at 60 DEG C, obtains propenyl-1,3-sulfonic acid lactone
73g, content 99.58%.
The foregoing is only the better embodiment of the present invention, not in order to limit the present invention, all spirit in the present invention
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. the environmental protection method of purification of a propenyl-1,3-sulfonic acid lactone, it is characterised in that comprise the following steps:
1) propenyl-1,3-sulfonic acid lactone crude product is joined in aqueous solvent, be heated to 25～75 DEG C of stirring and dissolving, obtain water-soluble
Liquid, wherein, propenyl-1,3-sulfonic acid lactone crude product is 1:20～1:10 with the mass ratio of water；
2) to step 1) aqueous solution that obtains adds activated carbon decolour, rear filtered while hot of having decoloured, obtain filtrate；
3) by step 2) filtrate that obtains is cooled to 0～15 DEG C and separates out crystal, isolated crystal and mother solution；
4) by step 3) crystal that obtains is dried at 0～82 DEG C, obtains the thin product of propenyl-1,3-sulfonic acid lactone.
The environmental protection method of purification of propenyl-1,3-sulfonic acid lactone the most according to claim 1, it is characterised in that step 1)
In: acrylic-1,3-sultones crude product is 1:15～1:10 with the mass ratio of water.
The environmental protection method of purification of propenyl-1,3-sulfonic acid lactone the most according to claim 1, it is characterised in that: step 1)
In, solution temperature is 45～65 DEG C.
The environmental protection method of purification of propenyl-1,3-sulfonic acid lactone the most according to claim 1, it is characterised in that: step 3)
In, crystallization temperature is 0～10 DEG C.
The environmental protection method of purification of propenyl-1,3-sulfonic acid lactone the most according to claim 1, it is characterised in that: step 4)
In, baking temperature is 60～80 DEG C, and drying pressure is-0.5～-0.1Mpa.
6. according to the environmental protection method of purification of the arbitrary described propenyl-1,3-sulfonic acid lactone of claim 1 to 5, it is characterised in that:
Step 1) in, propenyl-1,3-sulfonic acid lactone crude product is from the preparation process of propenyl-1,3-sulfonic acid lactone, acrylic-1,3-
The purity of sultones crude product is 85～90%；Step 3) in, the mother solution obtained uses step 1 as recycling design, set) before
Acrylic-1,3-sultones crude product preparation process in.
The environmental protection method of purification of propenyl-1,3-sulfonic acid lactone the most according to claim 6, it is characterised in that include with
Lower step:
1) acrylic-1,3-sultones crude product is prepared；
2) propenyl-1,3-sulfonic acid lactone crude product is joined in aqueous solvent, be heated to 25～75 DEG C of stirring and dissolving, obtain water-soluble
Liquid, wherein, propenyl-1,3-sulfonic acid lactone crude product is 1:20～1:10 with the mass ratio of water；
3) to step 2) aqueous solution that obtains adds activated carbon decolour, rear filtered while hot of having decoloured, obtain filtrate；
4) by step 3) filtrate that obtains is cooled to 0～15 DEG C and separates out crystal, and isolated crystal and mother solution, mother solution is as solvent
Step 1 used by set) in, wherein, step 4) consumption of mother solution that obtains and step 1) in the volume ratio of consumption of solvent be
0.3:1～0.8:1；
5) step 1 is repeated) to step 4), obtain total crystal；
6) by step 5) total crystal of obtaining is dried at 0～82 DEG C, obtains the thin product of propenyl-1,3-sulfonic acid lactone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610545725.8A CN106187987B (en) | 2016-07-12 | 2016-07-12 | A kind of environmentally friendly method of purification of acrylic -1,3- sultones |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610545725.8A CN106187987B (en) | 2016-07-12 | 2016-07-12 | A kind of environmentally friendly method of purification of acrylic -1,3- sultones |
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| CN106187987A true CN106187987A (en) | 2016-12-07 |
| CN106187987B CN106187987B (en) | 2019-01-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114149404A (en) * | 2020-09-07 | 2022-03-08 | 石家庄圣泰化工有限公司 | Purification method of 1-propylene-1, 3-sultone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456856A (en) * | 2009-01-07 | 2009-06-17 | 石家庄圣泰化工有限公司 | Preparation method of 1-propylene-1, 3-sultone |
| CN101659653A (en) * | 2009-08-28 | 2010-03-03 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of propenyl-1, 3-sulfonic acid lactone |
| CN104557853A (en) * | 2013-10-25 | 2015-04-29 | 石家庄圣泰化工有限公司 | Refining and purifying method of prop-1-ene-1, 3-sultone |
-
2016
- 2016-07-12 CN CN201610545725.8A patent/CN106187987B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456856A (en) * | 2009-01-07 | 2009-06-17 | 石家庄圣泰化工有限公司 | Preparation method of 1-propylene-1, 3-sultone |
| CN101659653A (en) * | 2009-08-28 | 2010-03-03 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of propenyl-1, 3-sulfonic acid lactone |
| CN104557853A (en) * | 2013-10-25 | 2015-04-29 | 石家庄圣泰化工有限公司 | Refining and purifying method of prop-1-ene-1, 3-sultone |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114149404A (en) * | 2020-09-07 | 2022-03-08 | 石家庄圣泰化工有限公司 | Purification method of 1-propylene-1, 3-sultone |
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