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Method for preparing ethylenediamine esilate

A technology of ethylenediaminoethanesulfonate and ethylenediaminoethanesulfonate, applied in the direction of sulfonate preparation, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problem of harsh reaction conditions and conversion rate Not high, high reaction temperature and other problems, to achieve the effect of mild reaction conditions, high controllability, excellent activity and stability, and improved sulfonic acid resistance

Active Publication Date: 2016-12-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional preparation process of sodium ethylenediaminoethanesulfonate is more complicated. Taking the sodium chloroethylsulfonate method to prepare sodium ethylenediaminoethanesulfonate as an example, there is incomplete conversion of raw materials, and it is difficult to contain sodium chloride in the product. and product separation
[0005] Chinese published patent CN101240057 discloses a sulfonic acid type hydrophilic chain extender and its preparation method, using polyamines and alkenyl sulfonates as raw materials, and the market price of alkenyl sulfonates is relatively high, so the sulfonic acid produced by this method Type hydrophilic chain extenders do not have a cost advantage; GB1336050 discloses a method for preparing ethylenediaminoethylsulfonate, but the reaction temperature is as high as 1000-3000 °C, and the special reaction conditions of high temperature and high pressure are not conducive to large-scale chemical production. Reaction energy consumption is high
[0006] Therefore, it is necessary to find a new production method of sodium ethylenediaminoethanesulfonate to solve the defects of low conversion rate, harsh reaction conditions, high energy consumption and high cost in the traditional process

Method used

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  • Method for preparing ethylenediamine esilate
  • Method for preparing ethylenediamine esilate
  • Method for preparing ethylenediamine esilate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1), 75.82 grams of bauxite, 9 grams of cellulose derivative compounds, and 4.5 grams of nitric acid solution were mixed and kneaded until plastic, dried and roasted after extrusion to obtain a catalyst carrier;

[0058] (2) 19.42 grams of nickel nitrate, 19.46 grams of cobalt nitrate, 1.03 grams of manganese nitrate, 0.74 grams of molybdenum nitrate, and 0.34 grams of technetium nitrate are added to deionized water to obtain a co-impregnation solution, and trimethylamine is used to adjust pH=10.5, and then the The carrier was impregnated for 3 hours at a temperature of 25°C; the drying time was 10 hours at a drying temperature of 95°C; the firing temperature was 450°C for 1.5 hours. The active component in the obtained hydrogenation catalyst is NiO 5wt%, CoO5wt%, Mo 2 o 3 0.2wt%, MnO 2 0.5wt%,Tc 2 0 7 0.1wt%, others as a carrier of 100 g pre-reforming hydrogenation catalyst 1.

[0059] (3) Fill the pre-reforming hydrogenation catalyst into a 400 milliliter hydr...

Embodiment 2-5

[0061] Change the ratio of nickel nitrate, cobalt nitrate, manganese nitrate, molybdenum nitrate and technetium nitrate, and the carrier, other conditions are basically the same as in the examples, and catalyst 2-5 is prepared. The content of active components is shown in Table 1, and the content is based on The total mass of the catalyst, and the rest of the components are carriers.

[0062] Table 1 Catalyst 1-5 Composition Table

[0063]

Embodiment 6

[0065] 147 grams of sodium taurine (1mol) are placed in the there-necked flask equipped with stirrer, thermometer, dropping funnel, slowly drip 114 grams (1mol) of 50wt% hydroxyacetonitrile aqueous solution by dropping funnel under stirring, keep reaction The temperature was at 30°C, the time for dropping was 30 minutes, and then the reaction was incubated for 20 minutes. The reaction liquid was removed by rotary evaporation under reduced pressure to remove water, and dried at 90°C for 3 hours to obtain 183.21 grams of light yellow crystal sodium cyanoethyl taurate. The yield was 98.5%.

[0066] Get 100 grams of sodium cyanoethyl taurate and dissolve it in 870 grams of dioxane, and add 30 grams of liquid ammonia using a high-pressure pump,

[0067] Fill 100 grams of hydrogenation catalyst 1 into a high-pressure hydrogenation fixed bed, press it to 10 MPa (gauge pressure) after hydrogen replacement, keep warm at a temperature of 120 ° C, and start feeding, and the feeding amoun...

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Abstract

The invention relates to a method for preparing ethylenediamine esilate. The method comprises the steps that glycolonitrile and taurine salt serve as raw materials, or glycolonitrile, taurine and alkali metal hydroxide serve as raw materials, and cyanoethyl taurine salt is obtained through a dehydration condensation reaction; then, under the action of a hydrogenation catalyst, an ethylenediamine esilate hydrogenation solution is obtained through hydrogenation; a solvent is removed, and then the product ethylenediamine esilate is obtained. According to the catalyst, aluminum oxide and / or silicon oxide serve / serves as a carrier, and NiO, CoO, MoO3, MnO2 and Tc2O7 serve as active components. According to the method, ethylenediamine esilate can be obtained with a high conversion rate and high selectivity as long as light components such as the solvent in the hydrogenation solution are removed, the method is environmentally friendly in process, economical, safe and high in product yield, and has the industrialization amplification prospects, and purification is easy.

Description

technical field [0001] The invention relates to a method for preparing ethylenediaminoethanesulfonate, in particular to a method for preparing ethylenediaminoethanesulfonate from hydroxyacetonitrile and taurine as raw materials, and belongs to the field of organic chemical synthesis. Background technique [0002] As an environmentally friendly polymer material, waterborne polyurethane has been widely used in adhesives, coatings and other fields due to its excellent mechanical properties, cold resistance, and non-toxicity. At present, the research and development of water-based polyurethane is very active, but most of the synthesized water-based polyurethane is carboxylic acid type, and there is still a certain gap between its performance and solvent-based polyurethane. The reason is that in the preparation of water-based polyurethane, besides the raw material polyol and diisocyanate process conditions, the hydrophilic chain extender is the key to determine its performance. ...

Claims

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Application Information

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IPC IPC(8): C07C303/32C07C309/14B01J23/889
CPCB01J23/002B01J23/8898B01J37/0213B01J37/0236B01J37/082B01J2523/00C07C303/32C07C309/14B01J2523/31B01J2523/68B01J2523/72B01J2523/73B01J2523/845B01J2523/847
Inventor 何光文黎源丛鑫崔乾王鹏
Owner WANHUA CHEM GRP CO LTD
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