CN108997303A - A kind of preparation method of 1,3- propane sultone - Google Patents
A kind of preparation method of 1,3- propane sultone Download PDFInfo
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- CN108997303A CN108997303A CN201810625698.4A CN201810625698A CN108997303A CN 108997303 A CN108997303 A CN 108997303A CN 201810625698 A CN201810625698 A CN 201810625698A CN 108997303 A CN108997303 A CN 108997303A
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Abstract
The invention discloses one kind 1, the preparation method of 3- propane sultone, the following steps are included: preparing calcium chloride solution first, then citric acid is added, mixed solution A is made, and it is mixed with mixed solution B with sodium polyacrylate solution, it is then quickly added into sodium carbonate liquor and precipitates, prepare porous calcium carbonate, be impregnated in benzoyl hydroperoxide solution and catalyst is made；Sodium Allyl Sulfonate and sulfuric acid solution are mixed, catalyst reaction is added, the ethanol solution reaction of sodium hydroxide is added, is eventually adding hydrochloric acid acidification, 3- hydroxy-propanesulfonic acid is made；3- hydroxy-propanesulfonic acid obtained and n-hexane are mixed to join in three-necked flask, is stirred to react, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3-propane sultone is made.This method is easy to operate, and low energy consumption, product yield high.
Description
Technical field:
The present invention relates to organic synthesis fields, are specifically related to a kind of preparation method of 1,3-propane sultone.
Background technique:
1,3- propane sultone belongs to functional form fine chemistry industry new material.The compound of its energy and numerous species is in non-room temperature
It is reacted under conditions of, sulfonic acid group is accurately provided, to assign the new performance of these compounds (as there is hydrophily, resist
The features such as static behaviour), it is excellent universal sulfonating agent, and the important electroplating additive intermediate PPS, UPS of synthesis,
The critical materials of the products such as DPS, MPS, ZPS, POPS, SP.It is a kind of important medicine intermediate, is also applied to brightener, dye
Material, double ion surfactant, sulfonating agent, lithium battery etc..
The preparation method of production 1,3-propane sultone mainly includes following several at present: (1) using propenyl as raw material,
1,3- propane sultone is generated after reacting under sodium peroxydisulfate catalyst action with sodium sulfite after peracid, ring-closure reaction.(2)
It is reacted with the mixed liquor dissolved with the aqueous solution of sodium sulfite and sodium hydrogensulfite, propenyl and tert-butyl hydroperoxide and 3- hydroxyl is made
Base propanesulfonate solution, then after obtaining 3- hydroxy-propanesulfonic acid with acid acidification, then under the action of catalyst, carried out at 80-100 DEG C
Dehydration 3 hours is less than 1.066kPa in air pressure, and the rectifying between 147-150 DEG C of liquid temperature temperature obtains 1,3-propane sultone.But
It is the above method using propenyl as raw material, it is at high cost, and reaction condition the high requirements on the equipment.
Summary of the invention:
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of preparation methods of 1,3-propane sultone, should
Method is easy to operate, low for equipment requirements, and product obtained is easily isolated, high income.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, calcium chloride solution is made；Into calcium chloride solution
Citric acid is added, continues stirring to solid and dissolves, mixed solution A is made；
(2) Sodium Polyacrylate is dissolved in stir in deionized water and sodium polyacrylate solution is made, and be slowly added into
In mixed solution A obtained above, 30-50min is stirred in the state of 3000-5000 revs/min after being added dropwise, mixing is made
Solution B；
(3) sodium carbonate liquor is prepared, then mixed solution B obtained above is added rapidly in sodium carbonate liquor,
Precipitating is stirred in the state of 5000 revs/min, is filtered after precipitating, precipitating is washed with deionized, and porous carbonic acid is made in drying
Calcium；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 50-70 DEG C to dissolve, porous carbon is then added
Sour calcium, impregnation 3-6h, then cools to room temperature, dry, and catalyst is made；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 10-30min, catalyst obtained above is then added, is to slowly warm up to 80-100 DEG C, is stirred to react 1-4h, instead
It is cooled to room temperature after answering, the ethanol solution of sodium hydroxide is added, be stirred 30-50min, hydrochloric acid acidification is then added,
3- hydroxy-propanesulfonic acid is made；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 100-200 DEG C,
It is stirred to react 3-15h under conditions of 3000 revs/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- is made
Propane sultone.
As a preferred embodiment of the above technical solution, in step (1), the mass concentration of the calcium chloride solution is 15-35%.
As a preferred embodiment of the above technical solution, in step (1), the calcium chloride, citric acid mass ratio be (5-7):
0.3。
As a preferred embodiment of the above technical solution, in step (2), the mass concentration of the sodium polyacrylate solution is 3-8%.
As a preferred embodiment of the above technical solution, in step (2), the rate of addition of the sodium polyacrylate solution is 1-5ml/
L。
As a preferred embodiment of the above technical solution, in step (2), Sodium Polyacrylate, calcium chloride mass ratio be (0.1-
0.6):1。
As a preferred embodiment of the above technical solution, in step (3), the mass concentration of the sodium carbonate liquor is 20%.
As a preferred embodiment of the above technical solution, in step (4), benzoyl hydroperoxide, porous calcium carbonate mass ratio be 1:
(15-45)。
As a preferred embodiment of the above technical solution, in step (5), the Sodium Allyl Sulfonate, catalyst mass ratio be
(10-30): 1.
As a preferred embodiment of the above technical solution, in step (5), in the ethanol solution of the sodium hydroxide, sodium hydroxide, second
The mass ratio of alcohol is 5:(15-20).
The invention has the following advantages:
The method comprises the steps of firstly, preparing calcium chloride solution, citric acid, Sodium Polyacrylate is then added, it can effectively and calcium ion
Complex compound is formed, to effectively control the settling velocity of subsequent calcium ion, porous calcium carbonate stable lattice obtained, porosity is steady
It is fixed, using the method for dipping, catalyst is made, catalytic activity is high, can effectively facilitate reaction；
The present invention effectively adjusts preparation process condition, and target product yield obtained is high, and purity is good, and this method operation letter
It is single, it is low for equipment requirements.
Specific embodiment:
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 15% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 5:0.3；
(2) Sodium Polyacrylate is dissolved in stirring in deionized water and the sodium polyacrylate solution that mass concentration is 3% is made, and
It is slowly added into mixed solution A obtained above, stirs 30min in the state of 3000 revs/min after being added dropwise,
Mixed solution B is made；Wherein, the rate of addition of the sodium polyacrylate solution is 1ml/L；The matter of Sodium Polyacrylate, calcium chloride
Amount is than being 0.1:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 50 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 3h, then cools to room temperature, dry, and catalyst is made；Wherein, the quality of benzoyl hydroperoxide, porous calcium carbonate
Than for 1:15；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 10min, catalyst obtained above is then added, is to slowly warm up to 80 DEG C, is stirred to react 1h, it is cold after reaction
But to room temperature, the ethanol solution of sodium hydroxide is added, is stirred 30min, hydrochloric acid acidification is then added, the third sulphur of 3- hydroxyl is made
Acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 10:1；In the ethanol solution of the sodium hydroxide, hydroxide
Sodium, ethyl alcohol mass ratio be 5:15；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 100 DEG C, 3000
It is stirred to react 3h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane sulphur is made
Lactone.
Embodiment 2
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 35% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 7:0.3；
(2) Sodium Polyacrylate is dissolved in stirring in deionized water and the sodium polyacrylate solution that mass concentration is 8% is made, and
It is slowly added into mixed solution A obtained above, stirs 50min in the state of 5000 revs/min after being added dropwise,
Mixed solution B is made；Wherein, the rate of addition of the sodium polyacrylate solution is 5ml/L；The matter of Sodium Polyacrylate, calcium chloride
Amount is than being 0.6:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 70 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 6h, then cools to room temperature, dry, and catalyst is made；Wherein, the quality of benzoyl hydroperoxide, porous calcium carbonate
Than for 1:45；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 30min, catalyst obtained above is then added, is to slowly warm up to 100 DEG C, is stirred to react 4h, after reaction
It is cooled to room temperature, the ethanol solution of sodium hydroxide is added, be stirred 50min, hydrochloric acid acidification is then added, 3- hydroxyl third is made
Sulfonic acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 30:1；In the ethanol solution of the sodium hydroxide, hydrogen-oxygen
Change sodium, the mass ratio of ethyl alcohol is 5:20；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 200 DEG C, 3000
It is stirred to react 15h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane is made
Sultone.
Embodiment 3
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 20% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 5.5:0.3；
(2) Sodium Polyacrylate is dissolved in stirring in deionized water and the sodium polyacrylate solution that mass concentration is 4% is made, and
It is slowly added into mixed solution A obtained above, stirs 35min in the state of 3500 revs/min after being added dropwise,
Mixed solution B is made；Wherein, the rate of addition of the sodium polyacrylate solution is 2ml/L；The matter of Sodium Polyacrylate, calcium chloride
Amount is than being 0.2:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 55 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 4h, then cools to room temperature, dry, and catalyst is made；Wherein, the quality of benzoyl hydroperoxide, porous calcium carbonate
Than for 1:20；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 15min, catalyst obtained above is then added, is to slowly warm up to 85 DEG C, is stirred to react 2h, it is cold after reaction
But to room temperature, the ethanol solution of sodium hydroxide is added, is stirred 35min, hydrochloric acid acidification is then added, the third sulphur of 3- hydroxyl is made
Acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 15:1；In the ethanol solution of the sodium hydroxide, hydroxide
Sodium, ethyl alcohol mass ratio be 5:16；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 120 DEG C, 3000
It is stirred to react 5h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane sulphur is made
Lactone.
Embodiment 4
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 25% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 6:0.3；
(2) Sodium Polyacrylate is dissolved in stirring in deionized water and the sodium polyacrylate solution that mass concentration is 5% is made, and
It is slowly added into mixed solution A obtained above, stirs 40min in the state of 4500 revs/min after being added dropwise,
Mixed solution B is made；Wherein, the rate of addition of the sodium polyacrylate solution is 3ml/L；The matter of Sodium Polyacrylate, calcium chloride
Amount is than being 0.3:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 60 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 4.5h, then cools to room temperature, dry, and catalyst is made；Wherein, the matter of benzoyl hydroperoxide, porous calcium carbonate
Amount is than being 1:25；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 20min, catalyst obtained above is then added, is to slowly warm up to 90 DEG C, is stirred to react 2h, it is cold after reaction
But to room temperature, the ethanol solution of sodium hydroxide is added, is stirred 40min, hydrochloric acid acidification is then added, the third sulphur of 3- hydroxyl is made
Acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 20:1；In the ethanol solution of the sodium hydroxide, hydroxide
Sodium, ethyl alcohol mass ratio be 5:17；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 140 DEG C, 3000
It is stirred to react 10h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane is made
Sultone.
Embodiment 5
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 30% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 6.5:0.3；
(2) Sodium Polyacrylate is dissolved in stirring in deionized water and the sodium polyacrylate solution that mass concentration is 6% is made, and
It is slowly added into mixed solution A obtained above, stirs 40min in the state of 4000 revs/min after being added dropwise,
Mixed solution B is made；Wherein, the rate of addition of the sodium polyacrylate solution is 3ml/L；The matter of Sodium Polyacrylate, calcium chloride
Amount is than being 0.4:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 60 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 5h, then cools to room temperature, dry, and catalyst is made；Wherein, the quality of benzoyl hydroperoxide, porous calcium carbonate
Than for 1:30；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 20min, catalyst obtained above is then added, is to slowly warm up to 90 DEG C, is stirred to react 3h, it is cold after reaction
But to room temperature, the ethanol solution of sodium hydroxide is added, is stirred 30min, hydrochloric acid acidification is then added, the third sulphur of 3- hydroxyl is made
Acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 20:1；In the ethanol solution of the sodium hydroxide, hydroxide
Sodium, ethyl alcohol mass ratio be 5:18；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 100-200 DEG C,
It is stirred to react 9h under conditions of 3000 revs/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- third is made
Alkane sultone.
Embodiment 6
A kind of preparation method of 1,3-propane sultone, comprising the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, it is molten that the calcium chloride that mass concentration is 33% is made
Liquid；Citric acid is added into calcium chloride solution, continues stirring to solid and dissolves, mixed solution A is made；Wherein, the calcium chloride,
The mass ratio of citric acid is 6.5:0.3；
(2) Sodium Polyacrylate is dissolved in stir in deionized water and the sodium polyacrylate solution that mass concentration is 7.5% is made,
And be slowly added into mixed solution A obtained above, it is stirred in the state of 4500 revs/min after being added dropwise
Mixed solution B is made in 40min；Wherein, the rate of addition of the sodium polyacrylate solution is 4.5ml/L；Sodium Polyacrylate, chlorine
The mass ratio for changing calcium is 0.55:1；
(3) mixed solution B obtained above, is then added rapidly to by the sodium carbonate liquor that preparation mass concentration is 20%
In sodium carbonate liquor, precipitating is stirred in the state of 5000 revs/min, filters after precipitating, precipitating is washed with deionized, it is dry
Porous calcium carbonate is made；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 65 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 5h, then cools to room temperature, dry, and catalyst is made；Wherein, the quality of benzoyl hydroperoxide, porous calcium carbonate
Than for 1:41；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, under 1500 revs/min of speed of agitator
It is stirred 20min, catalyst obtained above is then added, is to slowly warm up to 95 DEG C, is stirred to react 3h, it is cold after reaction
But to room temperature, the ethanol solution of sodium hydroxide is added, is stirred 45min, hydrochloric acid acidification is then added, the third sulphur of 3- hydroxyl is made
Acid；Wherein, the Sodium Allyl Sulfonate, catalyst mass ratio be 30:1；In the ethanol solution of the sodium hydroxide, hydroxide
Sodium, ethyl alcohol mass ratio be 5:19；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 180 DEG C, 3000
It is stirred to react 12h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane is made
Sultone.
Comparative example 1
Catalyst is not added in (5) in step, other reaction conditions and embodiment 6 are identical.
The purity of target product 1,3-propane sultone made from embodiment 1-6 is greater than 99%, and yield is 93.5% or more；
Target product purity made from comparative example is 75%, yield 80.5%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of 1,3-propane sultone, which comprises the following steps:
(1) calcium chloride is dissolved in stirring to solid in deionized water to dissolve, calcium chloride solution is made；It is added into calcium chloride solution
Citric acid continues stirring to solid and dissolves, mixed solution A is made；
(2) Sodium Polyacrylate is dissolved in stir in deionized water and sodium polyacrylate solution is made, and be slowly added into above-mentioned
In mixed solution A obtained, 30-50min is stirred in the state of 3000-5000 revs/min after being added dropwise, mixed solution is made
B；
(3) sodium carbonate liquor is prepared, then mixed solution B obtained above is added rapidly in sodium carbonate liquor, 5000 turns/
Precipitating is stirred in the state of point, is filtered after precipitating, and precipitating, dry obtained porous calcium carbonate is washed with deionized；
(4) benzoyl hydroperoxide and deionized water are blended in stirring to solid at 50-70 DEG C to dissolve, porous carbonic acid is then added
Calcium, impregnation 3-6h, then cools to room temperature, dry, and catalyst is made；
(5) Sodium Allyl Sulfonate and sulfuric acid solution are mixed to join in three-necked flask, are stirred under 1500 revs/min of speed of agitator
10-30min is mixed, catalyst obtained above is then added, is to slowly warm up to 80-100 DEG C, is stirred to react 1-4h, reaction knot
It is cooled to room temperature after beam, the ethanol solution of sodium hydroxide is added, be stirred 30-50min, hydrochloric acid acidification is then added, is made
3- hydroxy-propanesulfonic acid；
(6) 3- hydroxy-propanesulfonic acid obtained above and n-hexane are mixed to join in three-necked flask, at 100-200 DEG C, 3000
It is stirred to react 3-15h under conditions of rev/min, is cooled to room temperature after reaction, is evaporated under reduced pressure, target product 1,3- propane is made
Sultone.
2. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (1)
The mass concentration of calcium chloride solution is 15-35%.
3. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (1)
Calcium chloride, citric acid mass ratio be (5-7): 0.3.
4. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (2)
The mass concentration of sodium polyacrylate solution is 3-8%.
5. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (2)
The rate of addition of sodium polyacrylate solution is 1-5ml/L.
6. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: in step (2), poly- third
Olefin(e) acid sodium, calcium chloride mass ratio be (0.1-0.6): 1.
7. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (3)
The mass concentration of sodium carbonate liquor is 20%.
8. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: in step (4), peroxide
Benzoic acid, porous calcium carbonate mass ratio be 1:(15-45).
9. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: described in step (5)
Sodium Allyl Sulfonate, catalyst mass ratio be (10-30): 1.
10. a kind of preparation method of 1,3-propane sultone as described in claim 1, it is characterised in that: in step (5), institute
State in the ethanol solution of sodium hydroxide, sodium hydroxide, ethyl alcohol mass ratio be 5:(15-20).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677651A (en) * | 2022-12-08 | 2023-02-03 | 青岛科技大学 | Preparation method of alkyl sultone |
| CN115947713A (en) * | 2022-11-26 | 2023-04-11 | 青岛科技大学 | Preparation method of 1,3-propane sultone |
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| CN104803967A (en) * | 2015-04-20 | 2015-07-29 | 荣成青木高新材料股份有限公司 | Method for preparing 1,3-propane sultone |
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| CN115677651B (en) * | 2022-12-08 | 2023-11-14 | 青岛科技大学 | Preparation method of alkyl sultone |
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