CN109678842A - A kind of production technology of 944 intermediate of continuous production light stabilizer - Google Patents
A kind of production technology of 944 intermediate of continuous production light stabilizer Download PDFInfo
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- CN109678842A CN109678842A CN201910100580.4A CN201910100580A CN109678842A CN 109678842 A CN109678842 A CN 109678842A CN 201910100580 A CN201910100580 A CN 201910100580A CN 109678842 A CN109678842 A CN 109678842A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/14—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing three or more hetero rings
Abstract
The present invention relates to a kind of production technologies of 944 intermediate of continuous production light stabilizer, specific step is as follows: Cyanuric Chloride being added and obtains reaction solution A into organic solvent, reaction solution A and t-octanylamine solution are pumped into level-one tubular reactor simultaneously, and carry out continuous reaction, obtains reaction solution B；Reaction solution B is pumped into second level tubular reactor, while being pumped into liquid alkaline and carrying out neutralization reaction, obtains reaction liquid C；Reaction liquid C is pumped into washing kettle washed, filters pressing, obtain intermediate 2- t-octanylamine base -4,6- bis- chloro- 1,3,5 triazine solution, gained intermediate can be directly used for the polymerization of back segment 944；Gained intermediate and hexamethylene diamine piperidines carry out polymerization reaction and obtain light stabilizer 944；The present invention substitutes the synthetic reaction that traditional kettle reactor carries out 944 intermediates using pipe reaction device, substantially reduces the synthesis cycle of light stabilizer 944, while to realize that serialization, intelligent production are laid a good foundation.
Description
Technical field
The present invention relates to a kind of production technologies of 944 intermediate of continuous production light stabilizer, belong in light stabilizer 944
The preparation process field of mesosome.
Background technique
Light stabilizer 944 is a kind of aggretion type high molecular weight hindered amine light stabilizer, the low, thermal stability with volatility
It is high, resistant to extraction is good, with erect it is good to compatibility, it is not easy to migrate, nonirritant the advantages that.
The comparison reported in the literature of the synthetic route of light stabilizer 944 is more, mainly include two step method, three-step approach and four step rule,
Regardless of for which kind of synthetic route, the monobasic Cyanuric Chloride of t-octanylamine is all most important one of step.
Current existing commercial synthesis is mostly with batch-type still reaction, and there is equipment energy consumption height, stable product qualities
It is influenced by factors such as artificial, equipment bigger.Process control automation is the inexorable trend of traditional chemical company's future transition, intelligence
Equipment can be changed gradually to react by traditional batch to continuous production technology transition and development, can significantly save labour at
Sheet improves work situation, is energy-saving.In recent years, market is gradually proposed the reactor of a variety of automations, there is autoclave series connection
Reactor, tubular reactor, it is more high-end have high throughput-microchannel continuous flow reactor etc., micro passage reaction is using spy
The materials such as kind glass, special cermacis or stainless steel are made, and processing technology is more complicated, and price is somewhat expensive, are suitble to some amount small, attached
Value added high reaction.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provides a kind of 944 intermediate of continuous production light stabilizer
Production technology, to solve problems of the prior art.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of production technology of 944 intermediate of continuous production light stabilizer, the specific steps are as follows:
(1) Cyanuric Chloride is added and obtains reaction solution A into organic solvent, reaction solution A and t-octanylamine solution are pumped into simultaneously
Level-one tubular reactor, and continuous reaction is carried out, obtain reaction solution B；
(2) reaction solution B is pumped into second level tubular reactor, while is pumped into liquid alkaline and carries out neutralization reaction, obtain reaction liquid C；
(3) reaction liquid C is pumped into washing kettle washed, filters pressing, obtain intermediate 2- t-octanylamine base -4,6- bis- chloro- 1
, 3,5 triazine solution, gained intermediate and hexamethylene diamine piperidines carry out polymerization reaction and obtain light stabilizer 944.
As an improvement of the present invention, organic solvent is in toluene, dimethylbenzene or C6-C15 alkane in the step (1)
Any one.
As an improvement of the present invention, the mass fraction of reaction solution A is 10-50% in the step (1).
As an improvement of the present invention, the molar ratio of Cyanuric Chloride and t-octanylamine is 1:1-1.5 in the step (1).
As an improvement of the present invention, the reaction temperature of continuous reaction is -10-50 DEG C in the step (1), reaction
Time is 1-60min.
As an improvement of the present invention, the molar ratio of liquid alkaline and Cyanuric Chloride in step (1) is 1- in the step (2)
2:1.
As an improvement of the present invention, reaction temperature is 0-50 DEG C in the step (2), reaction time 1-30min.
As an improvement of the present invention, reaction solution B is passed through in washing kettle in the step (3) in being washed to
Property.
As an improvement of the present invention, level-one tubular reactor long 1-100m, diameter 1- in the step (1)
30cm；Second level tubular reactor long 1-50m, diameter 1-10cm in the step (2).
Due to using the above technology, the present invention compared with the prior art, is had the advantage that as follows:
The present invention provides a kind of production technology of 944 intermediate of continuous production light stabilizer, the present invention uses pipe reaction
Device accurately controls response parameter, changes the operation of autoclave discontinuity, under conditions of ensuring that quality is stablized, the company of realizing
The production method of continuousization, substantially increases the rate of coming into force；The present invention using pipe reaction device substitute traditional kettle reactor into
The synthetic reaction of 944 intermediate of row substantially reduces the synthesis cycle of light stabilizer 944, while to realize serialization, intelligence
Production is laid a good foundation.
Specific embodiment
With reference to embodiment, the present invention is furture elucidated.
Embodiment 1:
It is made into 30% Cyanuric Chloride solution with dimethylbenzene, is pumped into tubular reactor with metering pump, flow 3kg/h, and meanwhile it is continuous
It is passed through t-octanylamine, flow 0.6kg/h, (Cyanuric Chloride is 1:1 with t-octanylamine molar ratio) stops 20min at 30 DEG C of temperature,
First-stage reactor long 2m, diameter 5cm.The above reaction solution is directly entered second reactor, while being passed through 20% with flow 1.5kg/h
Liquid alkaline, (Cyanuric Chloride with liquid alkaline molar ratio be 1:1.5) reacts 10min, the long 2m of second reactor, diameter at 30 DEG C of temperature
6cm.Material after reaction is delivered directly to washing kettle, washes 3 times, filters pressing, and it is 99.35% that GC, which detects intermediate purity,.
Embodiment 2:
It is made into 40% Cyanuric Chloride solution with toluene, is pumped into tubular reactor, flow 4kg/h with metering pump, while continuously leading to
Enter t-octanylamine, flow 1.3kg/h, (Cyanuric Chloride is 1:1.2 with t-octanylamine molar ratio) stops 15min at 40 DEG C of temperature,
First-stage reactor long 2m, diameter 5cm.The above reaction solution is directly entered second reactor, while being passed through 30% with flow 2.3kg/h
Liquid alkaline, (Cyanuric Chloride with liquid alkaline molar ratio be 1:2) reacts 8min, the long 2m of second reactor, diameter at 40 DEG C of temperature
6cm.Material after reaction is delivered directly to washing kettle, washes 5 times, filters pressing, and it is 99.01% that GC, which detects intermediate purity,.
Embodiment 3:
It is made into 30% Cyanuric Chloride solution with dimethylbenzene, is pumped into tubular reactor with metering pump, flow 3kg/h, and meanwhile it is continuous
It is passed through t-octanylamine, flow 0.9kg/h, (Cyanuric Chloride is 1:1.5 with t-octanylamine molar ratio) stops at 10 DEG C of temperature
30min, first-stage reactor long 2m, diameter 5cm.The above reaction solution is directly entered second reactor, while logical with flow 0.6kg/h
Enter 30% liquid alkaline, (Cyanuric Chloride is 1:1 with liquid alkaline molar ratio) reacts 30min, the long 2m of second reactor at 10 DEG C of temperature,
Diameter 6cm.Material after reaction is delivered directly to washing kettle, washes 5 times, filters pressing, and it is 99.13% that GC, which detects intermediate purity,.
Above-described embodiment is only the preferred technical solution of the present invention, and is not construed as limitation of the invention, the present invention
Protection scope should with claim record technical solution, including claim record technical solution in technical characteristic etc.
It is protection scope with alternative, i.e., equivalent replacement within this range is improved, also within protection scope of the present invention.
Claims (9)
1. a kind of production technology of 944 intermediate of continuous production light stabilizer, which is characterized in that specific step is as follows:
(1) Cyanuric Chloride is added and obtains reaction solution A into organic solvent, reaction solution A and t-octanylamine solution are pumped into simultaneously
Level-one tubular reactor, and continuous reaction is carried out, obtain reaction solution B；
(2) reaction solution B is pumped into second level tubular reactor, while is pumped into liquid alkaline and carries out neutralization reaction, obtain reaction liquid C；
(3) reaction liquid C is pumped into washing kettle washed, filters pressing, obtain intermediate 2- t-octanylamine base -4,6- bis- chloro- 1
, 3,5 triazine solution, gained intermediate and hexamethylene diamine piperidines carry out polymerization reaction and obtain light stabilizer 944.
2. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: organic solvent is any one in toluene, dimethylbenzene or C6-C15 alkane in the step (1).
3. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: the mass fraction of reaction solution A is 10-50% in the step (1).
4. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: the molar ratio of Cyanuric Chloride and t-octanylamine is 1:1-1.5 in the step (1).
5. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: the reaction temperature of continuous reaction is -10-50 DEG C in the step (1), reaction time 1-60min.
6. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: the molar ratio of liquid alkaline and Cyanuric Chloride in step (1) is 1-2:1 in the step (2).
7. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: reaction temperature is 0-50 DEG C in the step (2), reaction time 1-30min.
8. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: reaction solution B is passed through in the step (3) and carries out being washed to neutrality in washing kettle.
9. a kind of production technology of 944 intermediate of continuous production light stabilizer according to claim 1, feature exist
In: level-one tubular reactor long 1-100m, diameter 1-30cm in the step (1)；Second level pipe reaction in the step (2)
Device long 1-50m, diameter 1-10cm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507216A (en) * | 2022-03-08 | 2022-05-17 | 河南省化工研究所有限责任公司 | Preparation method of hindered amine light stabilizer 944 |
| CN115975189A (en) * | 2022-12-26 | 2023-04-18 | 江苏富比亚化学品有限公司 | Synthesis method of hindered amine light stabilizer 944 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744127A (en) * | 1996-09-13 | 1998-04-28 | 3V Inc. | Derivatives of benzoxazole useful as UV filters |
| CN108623566A (en) * | 2018-04-28 | 2018-10-09 | 宿迁联盛科技有限公司 | A kind of synthesis technology of hindered amine light stabilizer 944 |
| CN109251313A (en) * | 2018-10-29 | 2019-01-22 | 北京天罡助剂有限责任公司 | A kind of hindered amine light stabilizer and preparation method thereof |
-
2019
- 2019-01-31 CN CN201910100580.4A patent/CN109678842A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744127A (en) * | 1996-09-13 | 1998-04-28 | 3V Inc. | Derivatives of benzoxazole useful as UV filters |
| CN108623566A (en) * | 2018-04-28 | 2018-10-09 | 宿迁联盛科技有限公司 | A kind of synthesis technology of hindered amine light stabilizer 944 |
| CN109251313A (en) * | 2018-10-29 | 2019-01-22 | 北京天罡助剂有限责任公司 | A kind of hindered amine light stabilizer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 温飞: "《受阻胺光稳定剂 Chimassorb 944 的合成及其工艺优化》", 《中国优秀硕士学位论文全文数据库（电子期刊）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507216A (en) * | 2022-03-08 | 2022-05-17 | 河南省化工研究所有限责任公司 | Preparation method of hindered amine light stabilizer 944 |
| CN115975189A (en) * | 2022-12-26 | 2023-04-18 | 江苏富比亚化学品有限公司 | Synthesis method of hindered amine light stabilizer 944 |
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Effective date of registration: 20190515 Address after: 223800 No. 22 Nanhua Road, Suqian Eco-chemical Science and Technology Industrial Park, Suqian City, Jiangsu Province Applicant after: Suqian Liansheng Auxiliaries Co.,Ltd. Address before: 223800 No. 88 Yangtze Road, Suqian Eco-chemical Science and Technology Industrial Park, Suqian City, Jiangsu Province Applicant before: SUQIAN UNITECHEM Co.,Ltd. |
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Application publication date: 20190426 |
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