CN105218416A - The preparation method of Thiovanic acid - Google Patents
The preparation method of Thiovanic acid Download PDFInfo
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- CN105218416A CN105218416A CN201410311809.6A CN201410311809A CN105218416A CN 105218416 A CN105218416 A CN 105218416A CN 201410311809 A CN201410311809 A CN 201410311809A CN 105218416 A CN105218416 A CN 105218416A
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Abstract
The present invention relates to a kind of preparation method of Thiovanic acid, at normal temperatures and pressures, chloroacetic acid solution is dripped in sodium hydrosulfide, continue to pass into a certain amount of H during dropping and in reaction process subsequently
2s gas.Higher product yield can be obtained by such method.This method instrument and supplies is simple, raw materials cost is low, and Synthesis conversion is greater than 90%.
Description
Technical field
The present invention relates to a kind of preparation method of Thiovanic acid.
Background technology
Under normal circumstances, the main path adopting sodium hydrosulfide to produce Thiovanic acid has two kinds: one is low temperature process, and one is high-pressure process.
In low temperature process, Sodium sulfhydrate and Mono Chloro Acetic Acid initial reaction temperature are 5 ~ 10 DEG C, time for adding 1 hour.Drip temperature after l hour and rise to about 20 DEG C, and then be warming up to 35 DEG C through 1 hour, insulation is to having reacted at such a temperature.Because this reaction starting stage will react for some time at low temperatures, therefore be unfavorable for production operation.This kind of method reaction times is also longer.Therefore, this technological process is implemented more difficult in suitability for industrialized production.
In high-pressure process, because building-up reactions will be carried out under pressure, and reaction raw materials has very strong corrodibility, therefore just has very high requirement to the material of reactor.In the industrial production, adopt this technique to increase facility investment, and there is potential safety hazard in production run process.
Summary of the invention
The object of the invention is the preparation difficulty overcoming current Thiovanic acid, the shortcoming of poor stability.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of preparation method of Thiovanic acid is provided, at normal temperatures and pressures, chloroacetic acid solution is dripped in sodium hydrosulfide, and stirs, in conversion zone, pass into H simultaneously
2s gas, reacted solution, through acidifying, extraction, distillation, obtains Thiovanic acid product.
Temperature of reaction 10 DEG C-25 DEG C, is preferably 20 DEG C.
Sodium hydrosulfide concentration is 15%, chloroacetic acid solution concentration 20%, time for adding 1 hour, and temperature of reaction is 15-25 DEG C, drips after terminating and reacts l hour again.
Logical H in conversion zone
2s gas passes into continuously in dropping and reaction process subsequently.
In reaction process, after Mono Chloro Acetic Acid and Sodium sulfhydrate reaction generate Thioglycolic acid sodium salt, Thioglycolic acid sodium salt can continue to react with the Sodium sulfhydrate in reaction solution, generates by product NaSCH
2cOONa, releases hydrogen sulfide simultaneously.Therefore, if there is a large amount of hydrogen sulfide in reaction system, the generation suppressing side reaction can be conducive to.Because side reaction all can occur when reinforced and after feeding in raw material, therefore need to continue to pass into hydrogen sulfide.
In above-mentioned reaction, sodium hydrosulfide concentration about 15%, chloroacetic acid solution concentration about 20%.Reactant concn is too high, and Synthesis conversion declines; Reactant concn is too low, can make resultant density loss, increases the loss in subsequent processes.
Method of the present invention is carried out at normal temperatures and pressures, simple and easy to do, and security is high, has hydrogen sulfide to generate in Sodium sulfhydrate and chloroacetate reaction process, this part collection and confinement of gases can be used at basin internal recycle.Can obtain higher product yield by such method, raw materials cost is low, and Synthesis conversion is greater than 90%.
Embodiment
Embodiment 1
Reaction is carried out in the 1L four-hole boiling flask that stirring arm, thermometer and dropping funnel are housed: temperature of reaction is controlled by water-bath.First prepare the sodium hydrosulfide 467 grams of 15%, the chloroacetic acid solution of 20% 237 grams.Sodium sulfhydrate is all put into four-hole boiling flask, in dropping funnel, adds chloroacetic acid solution, dripped by Mono Chloro Acetic Acid in sodium hydrosulfide, temperature of reaction about 20 DEG C, time for adding 1 hour, dropwises, and reaction soln was warming up to 35 DEG C in 0.5 hour.In whole reaction process, pass into hydrogen sulfide in conversion zone, tolerance is about 0.4-0.6L/min.
It is 2 that above-mentioned reaction solution concentrated hydrochloric acid is acidified to pH value, with extraction agent extraction, steams solvent at ambient pressure, then underpressure distillation, and collect the cut under 104 ~ 110 DEG C/2.13kPa, the yield of product is greater than 90%, and purity is greater than 99%.
Embodiment 2
Solution preparation and dropping process, with embodiment 10 dropping temperature about 25 DEG C, dropwise, and continue reaction about 1 hour at same temperature.In whole reaction process, pass into hydrogen sulfide in conversion zone, tolerance is about 0.4-0.6L/min.
Acidifying, extraction, still-process are the same, and the yield of product is greater than 90%, and purity is greater than 99%.
Claims (5)
1. a preparation method for Thiovanic acid, is characterized in that, at normal temperatures and pressures, is dripped by chloroacetic acid solution, and stir in sodium hydrosulfide, passes into H in conversion zone simultaneously
2s gas, reacted solution, through acidifying, extraction, distillation, obtains Thiovanic acid product.
2. the preparation method of the Thiovanic acid as described in claim l, is characterized in that, temperature of reaction 10 DEG C-25 DEG C.
3. the preparation method of Thiovanic acid as claimed in claim 2, is characterized in that, temperature of reaction 20 DEG C.
4. the preparation method of Thiovanic acid as claimed in claim 1, it is characterized in that, sodium hydrosulfide concentration is 15%, chloroacetic acid solution concentration 20%, time for adding 1 hour, and temperature of reaction is 15-25 DEG C, drips after terminating and reacts l hour again.
5. the preparation method of Thiovanic acid as claimed in claim 1, is characterized in that, logical H in conversion zone
2s gas passes into continuously in dropping and reaction process subsequently.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410311809.6A CN105218416A (en) | 2014-07-03 | 2014-07-03 | The preparation method of Thiovanic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410311809.6A CN105218416A (en) | 2014-07-03 | 2014-07-03 | The preparation method of Thiovanic acid |
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| Publication Number | Publication Date |
|---|---|
| CN105218416A true CN105218416A (en) | 2016-01-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410311809.6A Pending CN105218416A (en) | 2014-07-03 | 2014-07-03 | The preparation method of Thiovanic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047867A (en) * | 2020-09-24 | 2020-12-08 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
-
2014
- 2014-07-03 CN CN201410311809.6A patent/CN105218416A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047867A (en) * | 2020-09-24 | 2020-12-08 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
| CN112047867B (en) * | 2020-09-24 | 2023-02-03 | 湖北犇星新材料股份有限公司 | Method for purifying sodium thioglycolate |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160106 |