CN1036338C - Method of preparing N,N-dimethyl cyclohexylamine catalyst - Google Patents
Method of preparing N,N-dimethyl cyclohexylamine catalyst Download PDFInfo
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- CN1036338C CN1036338C CN93110708A CN93110708A CN1036338C CN 1036338 C CN1036338 C CN 1036338C CN 93110708 A CN93110708 A CN 93110708A CN 93110708 A CN93110708 A CN 93110708A CN 1036338 C CN1036338 C CN 1036338C
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- China
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- dimethylcyclohexylamine
- dimethyl cyclohexylamine
- present
- water
- thick product
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Abstract
The present invention relates to a method for producing N, N-dimethyl cyclohexylamine catalysts in production of chemical engineering, particularly in the production of hard polyurethane foam plastic. Chemical material which is easy to obtain is treated by a scientific and simple method to prepare N, N-dimethyl cyclohexylamine through one step reaction, and the content reaches more than 99%. The N, N-dimethyl cyclohexylamine produced by the method of the present invention fills the vacancy in China and can replace imported products. Compared with foreign methods, the method of the present invention has the advantages of simple technology, easy reaction control, high content of finished products, favorable product quality, low cost, etc.
Description
The present invention relates to N in a kind of polyurethane rigid foam plastic production, the production method of N-dimethylcyclohexylamine.
At present, in polyurethane rigid foam plastic is produced, mostly adopt potassium oleate and trimerization to make catalyzer, not only increase operation, made technology loaded down with trivial details, and existed the difficult grasp of proportioning in the production process, quality product is uncontrollable, and physicals is poor, staging life is short, problems such as the three wastes are arranged.Some enterprise has to spend huge foreign exchange import N in order to guarantee quality product, the N-dimethyl cyclohexylamine catalyst, and domesticly also do not have a manufacturer production.
Purpose of the present invention will overcome above-mentioned defective exactly, develops the N that is fit to China's national situation, the new production process of N-dimethyl cyclohexylamine catalyst.
Technical scheme of the present invention is:
Its production method:
1, raw material pimelinketone, dimethylamine are dropped in the reactor;
2, add palladium catalyst charcoal Pd/c;
3, feed high pressure hydrogen, pressure is 2.5-3.5MPa;
4, fully reaction, its chemical equation is:
Temperature of reaction is 100-140 ℃, and the time is 3-8 hour, obtains N, N-dimethylcyclohexylamine and water (thick product);
5, leave standstill 4-6 hour, remove the water of lower floor, obtain N, N-dimethylcyclohexylamine (still being thick product);
6, above-mentioned thick product is put into still kettle, be heated to 100 ℃, the remainder water vaporization;
7, continue to be heated to 150-160 ℃, N, the vaporization of N-dimethylcyclohexylamine receives by condensing works, obtains N, N-dimethylcyclohexylamine (smart product).
Effect of the present invention is to have filled up domestic production N, the blank of N-dimethylcyclohexylamine, import substitutes, for country saves a large amount of foreign exchanges, method of the present invention is compared with the method that overseas enterprise produces like product, has the advantage that technology is simple, single step reaction makes, cost is low, use N of the present invention, the N-dimethylcyclohexylamine has the effect of foaming and gel, homemade polyurethane rigid foam plastic quality is guaranteed, yield rate height, physicals are strong, and it is also long not have the three wastes, staging life.
Other advantage of the present invention will further be set forth in the following description.
Embodiment:
With content is that 98% 330 kilograms of pimelinketone, content are that 370 kilograms of 40% dimethylamine agueous solutions drop in the autoclave of 1000 liters, add an amount of palladium charcoal again and make catalyzer, mix, in reactor, feed high pressure hydrogen again, optimal pressure range is 2.5-3.5MPa, optimum temperature range is 120-130 ℃, produces chemical reaction, and its reaction formula is:
Wherein, mole ratio is:
Pimelinketone: dimethylamine=1: 1.1
Fully reaction is 5-6 hour, obtains thick product N, and N-dimethylcyclohexylamine and water stop hydrogenation then, leaves standstill 5 hours, and the upper strata is N in the reactor, the N-dimethylcyclohexylamine, and lower floor is a water, and water is removed.The upper strata also has remainder water and N, the N-dimethylcyclohexylamine is miscible in together, and this solution is put into still kettle, is heated to 100 ℃, the remainder water carburation by evaporation, reach the purpose of dehydration, continue to be heated to 157 ℃ again, N, the vaporization of N-dimethylcyclohexylamine, by condenser condenses and receive, obtain content and be the smart product N more than 99%, 418 kilograms of N-dimethylcyclohexylamines.Calculate by cyclohexanone content in whole process of production, its transformation efficiency reaches 100%, and product yield reaches 98%.
The N that the present invention produces, the N-dimethylcyclohexylamine also can be applicable to others, as makes oil oxidation inhibitor, stablizer etc.
Claims (1)
1, N during polyurethane rigid foam plastic is produced, the production method of N-dimethyl cyclohexylamine catalyst is characterized in that:
(1) raw material pimelinketone, dimethylamine are dropped in the reactor;
(2) add palladium catalyst charcoal Pd/c;
(3) feed high pressure hydrogen, pressure is 2.5-3.5MPa;
(4) fully reaction, its chemical equation is:
Temperature of reaction is 100-140 ℃, and the time is 3-9 hour, obtains N, N-dimethylcyclohexylamine and water (thick product);
(5) leave standstill 4-6 hour, remove the water of lower floor, obtain N, N-dimethylcyclohexylamine (still being thick product);
(6) above-mentioned thick product is put into still kettle, be heated to 100 ℃, the remainder water vaporization;
(7) continue to be heated to 150-160 ℃, N, the vaporization of N-dimethylcyclohexylamine receives by condensing works, obtains N, N-dimethylcyclohexylamine (smart product).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110708A CN1036338C (en) | 1993-03-10 | 1993-03-10 | Method of preparing N,N-dimethyl cyclohexylamine catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110708A CN1036338C (en) | 1993-03-10 | 1993-03-10 | Method of preparing N,N-dimethyl cyclohexylamine catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1092061A CN1092061A (en) | 1994-09-14 |
| CN1036338C true CN1036338C (en) | 1997-11-05 |
Family
ID=4988543
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93110708A Expired - Fee Related CN1036338C (en) | 1993-03-10 | 1993-03-10 | Method of preparing N,N-dimethyl cyclohexylamine catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1036338C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460445B (en) | 2006-05-31 | 2013-06-05 | 巴斯夫欧洲公司 | Process for the preparation of an amine |
| CN101619026B (en) * | 2009-07-29 | 2013-01-09 | 浙江新化化工股份有限公司 | Synthesis method for continuously producing N,N-dimethyl cyclohexyl amine |
| CN115947660A (en) * | 2022-12-19 | 2023-04-11 | 江苏万盛大伟化学有限公司 | Preparation method of high-purity dimethyl cyclohexylamine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4020059A (en) * | 1975-06-02 | 1977-04-26 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Process for preparing tertiary amines |
| US4521624A (en) * | 1984-04-16 | 1985-06-04 | Ethyl Corporation | Process for making cyclic amines |
| US4954654A (en) * | 1988-08-29 | 1990-09-04 | Phillips Petroleum Company | Process for the preparation of secondary and tertiary amines |
-
1993
- 1993-03-10 CN CN93110708A patent/CN1036338C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4020059A (en) * | 1975-06-02 | 1977-04-26 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Process for preparing tertiary amines |
| US4521624A (en) * | 1984-04-16 | 1985-06-04 | Ethyl Corporation | Process for making cyclic amines |
| US4954654A (en) * | 1988-08-29 | 1990-09-04 | Phillips Petroleum Company | Process for the preparation of secondary and tertiary amines |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1092061A (en) | 1994-09-14 |
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