CN106045889A - Novel mercaptopropionic acid pressurized hydrolysis process - Google Patents
Novel mercaptopropionic acid pressurized hydrolysis process Download PDFInfo
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- CN106045889A CN106045889A CN201610427487.0A CN201610427487A CN106045889A CN 106045889 A CN106045889 A CN 106045889A CN 201610427487 A CN201610427487 A CN 201610427487A CN 106045889 A CN106045889 A CN 106045889A
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- China
- Prior art keywords
- hydrolysis
- mercaptopropionic acid
- temperature
- heating
- new technology
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
Abstract
The invention relates to a novel mercaptopropionic acid pressurized hydrolysis process which is efficient in energy saving and short in hydrolysis time. The process includes: feeding acidified hydrolysate into a hydrolysis kettle, stirring, heating to 65-75 DEG C, and closing a tail gas system; heating until hydrolysis temperature reaches 90-110 DEG C, keeping the temperature and the pressure, and stirring for hydrolysis. Due to continue of reaction, the hydrolysis temperature can automatically rise to 120 DEG C even heating is stopped when the hydrolysis temperature reaches 90-110DEG C, and then the temperature and the pressure and kept to continue to stir for hydrolysis. Consumption of cooling water is avoided on the premise of guarantee of hydrolysis conversion rate, loss of mercaptopropionitrile is prevented, hydrolysis time is greatly shortened, and manpower and resources are saved.
Description
Technical field
The present invention relates to a kind of pressurized hydrolysis technique, be specifically related to a kind of mercaptopropionic acid pressurized hydrolysis new technology.
Background technology
Mercaptopropionic acid (CAS NO.:107-96-0) is a kind of poisonous transparency liquid, has strong sulphide smell, and it is other
Name have β-mercaptopropionic acid, sulfur for lactic acid, 3-mercaptopropionic acid, Β-sulfur for lactic acid, Β-sulfydryl propanoic acid, 3-mercaptopropionic acid,
BETA-mercaptopropionic acid, 3-2-mercaptopropionic acid, 3-thiohydracrylic acid etc..Mercaptopropionic acid is a kind of important organic synthesis raw material, is doctor
The intermediate of medicine chlomezanone, is also the stabilizer of pvc material.
In prior art, in mercaptopropionic acid production process, meeting acid hydrolysis after acrylonitrile and NaHS additive reaction, and
Generally hydrolysis can use reflux technique, whole hydrolytic process must control cooling down operation well, it is ensured that sulfydryl propionitrile will not be evaporated
Loss.If cooling water system goes wrong, it is also possible to cause material loss.Hydrolyzed solution maintains the temperature at during acid adding
Between 45-55 DEG C, after acid adding, start with enamel still and add set and carry out the heating of logical steam.When temperature rises, and return duct occurs
Substantially during backflow, start timing and carry out back hydrolysis operation.And, whole hydrolytic process is time-consuming relatively big, and hydrolysis operation is general
Need more than 8 hours.Such as number of patent application is entitled " a kind of high-purity 3-mercaptopropionic acid producer of CN201510856250
Method " patent, its reflux technique is specific as follows: squeeze in reactor by the hydrochloric acid of metering, close exhaust-valve, open absorption tower also
Open reactor, start stirring, in specify 50 DEG C slowly dropping step one reaction solutions, about 3 hours titration after, be brought rapidly up to
Backflow, after back flow reaction 3h, is cooled to 80-90 DEG C, has both obtained 3-mercaptopropionic acid and the mixture solution of dithio malonic acid.
Summary of the invention
The invention aims to provide a kind of energy-conservation, mercaptopropionic acid pressurized hydrolysis new technology that hydrolysis time is short.
For achieving the above object, the technical solution used in the present invention is: mercaptopropionic acid pressurized hydrolysis new technology includes step:
A. the hydrolyzed solution after acid adding is sent into hydrolysis kettle, be stirred heating, be warming up to 65-75 DEG C, be then shut off tail gas
System；Close exhaust system and exactly hydrolysis kettle is converted into seal pattern, along with temperature raises further, in hydrolysis kettle from open
Pressure can increase therewith.
B. under air-proof condition, continue heat temperature raising, when hydrolysis temperature reaches 90-110 DEG C, stop heating, keep temperature pressure
Power continues stirring hydrolysis.When hydrolysis temperature reaches 90-110 DEG C, although stop heating, owing to its temperature of carrying out of reaction can be automatically
Rise to 120 DEG C, at this moment keep temperature, pressure to continue stirring hydrolysis.
Further, exhaust system is closed after described step A being warming up to 70 DEG C.That is hydrolyze after being warming up to 70 DEG C
Still seals and carries out heating nature supercharging again.
During it is further preferred that hydrolysis temperature reaches 100 DEG C in described step B, stop heating.
Further, in described step A, before closedown exhaust system, the heating-up time is 0.5-1h.
Further, in described step B, heat time heating time is 0.5-1h.
Further, keeping temperature, pressure to continue stirring hydrolysis time in described step B is 2.5-4h.
The present invention can need not cool down water, prevent sulfydryl propionitrile from losing, improve on the premise of ensureing hydrolysis conversion
Reaction yield, is greatly shortened hydrolysis time, and saves manpower and the energy.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.The described embodiment only present invention is preferable to carry out
Example, is not limited to the present invention, and for a person skilled in the art, the present invention can have various change and change
Change.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention
Protection domain within.
Embodiment one
Hydrolyzed solution after acid adding is sent into hydrolysis kettle, is stirred heating, is warming up to 70 DEG C in 0.6h, is then shut off tail gas
System；When hydrolysis temperature being risen to 100 DEG C in continuing heat temperature raising, 1h under air-proof condition, stop heating, keep temperature, pressure
Continue stirring hydrolysis 2.5h.
Embodiment two
Hydrolyzed solution after acid adding is sent into hydrolysis kettle, is stirred heating, is warming up to 75 DEG C in 0.5h, is then shut off tail gas
System；When hydrolysis temperature being risen to 95 DEG C in continuing heat temperature raising, 1h under air-proof condition, stop heating, keep temperature, pressure
Continue stirring hydrolysis 4h.
Embodiment three
Hydrolyzed solution after acid adding is sent into hydrolysis kettle, is stirred heating, is warming up to 65 DEG C in 0.5-1h, is then shut off tail
Gas system；When hydrolysis temperature being risen to 105 DEG C in continuing heat temperature raising, 0.5h under air-proof condition, stop heating, keep temperature
Pressure continues stirring hydrolysis 3h.
Claims (6)
1. mercaptopropionic acid pressurized hydrolysis new technology, it is characterised in that: include step:
A. the hydrolyzed solution after acid adding is sent into hydrolysis kettle, be stirred heating, be warming up to 65-75 DEG C, be then shut off exhaust system；
B. under air-proof condition, continue heat temperature raising, when hydrolysis temperature reaches 90-110 DEG C, stop heating, keep temperature, pressure to continue
Continuous stirring hydrolysis.
Mercaptopropionic acid pressurized hydrolysis new technology the most according to claim 1, it is characterised in that: described step A is warming up to
Exhaust system is closed after 70 DEG C.
Mercaptopropionic acid pressurized hydrolysis new technology the most according to claim 1, it is characterised in that: hydrolysis temperature in described step B
When degree reaches 100 DEG C, stop heating.
Mercaptopropionic acid pressurized hydrolysis new technology the most according to claim 1, it is characterised in that: described step A is closed tail
Before gas system, the heating-up time is 0.5-1h.
Mercaptopropionic acid pressurized hydrolysis new technology the most according to claim 1, it is characterised in that: in described step B during heating
Between be 0.5-1h.
Mercaptopropionic acid pressurized hydrolysis new technology the most according to claim 1, it is characterised in that: described step B keeps temperature
It is 2.5-4h that degree pressure continues stirring hydrolysis time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610427487.0A CN106045889A (en) | 2016-06-16 | 2016-06-16 | Novel mercaptopropionic acid pressurized hydrolysis process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610427487.0A CN106045889A (en) | 2016-06-16 | 2016-06-16 | Novel mercaptopropionic acid pressurized hydrolysis process |
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| Publication Number | Publication Date |
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| CN106045889A true CN106045889A (en) | 2016-10-26 |
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| CN201610427487.0A Pending CN106045889A (en) | 2016-06-16 | 2016-06-16 | Novel mercaptopropionic acid pressurized hydrolysis process |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3280163A (en) * | 1963-05-06 | 1966-10-18 | Phillips Petroleum Co | Production of mercapto-substituted nitriles |
| JPS58135852A (en) * | 1982-02-08 | 1983-08-12 | Mitsui Toatsu Chem Inc | Preparation of beta-mercaptopropionic acid derivative |
| CN102575273A (en) * | 2009-04-30 | 2012-07-11 | 三井化学株式会社 | Process for production of 3-mercaptopropionic acid or salt thereof |
| CN105085344A (en) * | 2015-09-10 | 2015-11-25 | 山西其右建材科技有限公司 | Synthesis method of beta-mercaptopropionic acid |
| CN105348158A (en) * | 2015-11-26 | 2016-02-24 | 安徽省宁国市朝农化工有限责任公司 | Method for producing high-purity 3-thiohydracrylic acid |
-
2016
- 2016-06-16 CN CN201610427487.0A patent/CN106045889A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3280163A (en) * | 1963-05-06 | 1966-10-18 | Phillips Petroleum Co | Production of mercapto-substituted nitriles |
| JPS58135852A (en) * | 1982-02-08 | 1983-08-12 | Mitsui Toatsu Chem Inc | Preparation of beta-mercaptopropionic acid derivative |
| CN102575273A (en) * | 2009-04-30 | 2012-07-11 | 三井化学株式会社 | Process for production of 3-mercaptopropionic acid or salt thereof |
| CN105085344A (en) * | 2015-09-10 | 2015-11-25 | 山西其右建材科技有限公司 | Synthesis method of beta-mercaptopropionic acid |
| CN105348158A (en) * | 2015-11-26 | 2016-02-24 | 安徽省宁国市朝农化工有限责任公司 | Method for producing high-purity 3-thiohydracrylic acid |
Non-Patent Citations (4)
| Title |
|---|
| 宫贵贞: "巯基酸及其酯和取代苯酚的合成研究", 《山东师范大学硕士学位论文》 * |
| 张圣光 等: "硫氢化钠法合成β-巯基丙酸的工艺研究", 《精细与专用化学品》 * |
| 张家骅 等: "加压水解法处理含氰废水", 《环境科学与技术》 * |
| 李铭新 等: "硫代二丙酸的合成", 《山东化工》 * |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161026 |
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| RJ01 | Rejection of invention patent application after publication |