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Catalyst formula for synthesizing thiobisethylamine and preparation process thereof

A preparation technology of ethyl sulfide, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve environmental pollution, long product production cycle, reaction Long time and other problems, to achieve the effect of shortening the process time, low equipment material requirements, and easy continuous production

Inactive Publication Date: 2013-09-18
盐城美茵新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the existing aminoethyl sulfide synthesis process, there are problems such as long reaction time, many reaction steps, harsh reaction conditions, and long product production cycle.
A large amount of acid and alkali are used in the synthesis process [2 Guo Yonghua et al.: Chinese patent application 200810070087.4], and finally discharged with waste water, which not only increases the cost but also pollutes the environment
Ultimately lead to low production efficiency, poor product quality and high cost
The total yield of the existing synthetic process is between 49% and 77%

Method used

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  • Catalyst formula for synthesizing thiobisethylamine and preparation process thereof
  • Catalyst formula for synthesizing thiobisethylamine and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Catalyst preparation

[0020] Preparation of Catalyst 1: Take 100 ml of 0.1 mol / L AlCl 3 The solution is dissolved in ethanol, according to Al 3+ The amount of substance: ethyl orthosilicate: absolute ethanol: water = 1:8:70:100 (molar ratio) ratio, first dissolve ethyl orthosilicate in absolute ethanol, slowly drop under stirring Add deionized water to the ethanol solution of ethyl orthosilicate, stir for 24 hours, age at 110° C. for 24 hours, and roast at 500° C. for 6 hours to obtain catalyst 1.

[0021] Synthesis of Aminoethyl Sulfide

[0022] At room temperature, add 155 grams (1.0 moles) of 5-(dimethylamino) methyl-2-furan methanol, 60 grams of 90% sulfuric acid, 113 grams (1.0 moles) of cysteamine hydrochloride, add 20.2 g catalyst 1. At 40°C, react for 8 hours, neutralize with 30% sodium hydroxide solution until the pH value is between 11-12, then let stand to separate layers, distill the separated oil layer under reduced pressure, and collect the vacuum deg...

Embodiment 2

[0024] Catalyst preparation

[0025] Preparation of Catalyst 2: Take 100 ml of 0.1 mol / L FeCl 3 The solution is dissolved in ethanol, according to Fe 3+ The amount of substance: ethyl orthosilicate: absolute ethanol: water = 1: 10: 50: 120 (molar ratio) ratio, first dissolve ethyl orthosilicate in absolute ethanol, slowly drop under stirring Add deionized water to the ethanol solution of ethyl orthosilicate, stir for 24 hours, age at 110°C for 24 hours, and calcinate at 500°C for 6 hours to obtain catalyst 2.

[0026] Synthesis of Aminoethyl Sulfide

[0027] At room temperature, add 155 grams (1.0 moles) of 5-(dimethylamino) methyl-2-furan methanol, 60 grams of 90% sulfuric acid, 113 grams (1.0 moles) of cysteamine hydrochloride, add 16.4 g catalyst 2. At 38°C, react for 7 hours, neutralize with 30% sodium hydroxide solution until the pH value is between 11-12, then stand to separate layers, distill the separated oil layer under reduced pressure, and collect the vacuum deg...

Embodiment 3

[0029] Catalyst preparation

[0030] Preparation of Catalyst 3: Take 50 ml of 0.1 mol / L FeCl 3 and 50 ml of 0.1 mol / L Cu(NO 3 ) 2 The solution is dissolved in ethanol, according to Fe 3+ and Cu 2+ The amount of the total substance: orthosilicate ethyl ester: absolute ethanol: the proportioning ratio of water=1: 10: 50: 100 (molar ratio), first tetraethyl orthosilicate is dissolved in absolute ethanol, under stirring slowly Deionized water was added dropwise into the ethanol solution of ethyl orthosilicate, stirred for 24 hours, aged at 110°C for 24 hours, and calcined at 500°C for 6 hours to obtain catalyst 3.

[0031] Synthesis of Aminoethyl Sulfide

[0032] At room temperature, add 155 grams (1.0 moles) of 5-(dimethylamino) methyl-2-furan methanol, 70 grams of 90% sulfuric acid, 113 grams (1.0 moles) of cysteamine hydrochloride, add 19.6 g catalyst 3. At 37°C, react for 7 hours, neutralize with 30% sodium hydroxide solution until the pH value is between 11-12, then st...

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Abstract

The invention discloses a catalyst formula for synthesizing thiobisethylamine and a preparation process thereof. The thiobisethylamine catalyst is prepared by performing a reaction on 5-(dimethylamino) methyl-2-furfuryl alcohol and cysteamine hydrochloride. The thiobisethylamine catalyst is prepared from the following components by mass percent: the ratio of the total mass of one or more of Al3<+>, La3<+>, Fe3<+> and Cu2<+> to tetraethoxysilane to absolute ethyl alcohol to water is 1: (5-50): (30-200): (50-200), wherein the parent bodies of the Al3<+>, the La3<+>, the Fe3<+> and the Cu2<+> with metal slats are AlCl3, Al(NO3)3, La(NO3)3, FeCl3, Fe(NO3)3 and Cu(NO3)2. The preparation process comprises the following steps: firstly, dissolving one or several kinds of the AlCl3, the Al(NO3)3, the La(NO3)3, the FeCl3, the Fe(NO3)3 and the Cu(NO3)2 in the water; adding a solution required for enabling the tetraethoxysilane to be dissolved in the absolute ethyl alcohol; slowly dripping deionized water in a stirring manner; stirring for 18 to 26 hours; aging for 18 to 36 hours at the temperature of 100 to 120 DEG C; roasting for 4 to 8 hours at the temperature of 450 to 600 DEG C, thereby obtaining the corresponding catalyst. The catalyst has the good activity in the reaction of the 5-(dimethylamino) methyl-2-furfuryl alcohol and the cysteamine hydrochloride for preparing the thiobisethylamine. The preparation process is an environmentally-friendly synthesizing process; the highest yield of the thiobisethylamine product can reach 84.1%.

Description

a technical field [0001] The invention relates to a catalyst formula and a preparation process for synthesizing aminoethyl sulfide, belonging to the technical field of chemical material preparation. This method is suitable for the occasion of preparing aminoethyl sulfide catalyst by reacting 5-(dimethylamino)methyl-2-furan methanol and cysteamine hydrochloride. Two background technology [0002] Aminoethyl sulfide [chemical name: 2-[[[(5-dimethylamino-2-furyl] methyl] thio] ethylamine, CAS number: 66356-53-4, is the stomach drug Raney The intermediate of titin.At present, the synthetic route that aminoethyl sulfide realizes industrialization is divided into two steps: [0003] The first step: the preparation of intermediate A [0004] [0005] The second step: the synthesis of aminoethyl sulfide [0006] [0007] The intermediate A obtained in the first step is: 5-(dimethylamino)methyl-2-furanmethanol, which is the synthesis of H 2 -Important intermediate of recept...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07D307/52
Inventor 朱其军茆福林谢毅
Owner 盐城美茵新材料有限公司