Solid acid catalyst and use thereof in synthesizing 1,6-hexamethylene diisocyanate

A technology of hexamethylene diisocyanate and solid acid catalyst, which is applied in the direction of urethane preparation, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of high price, high cost of HDI, unsatisfactory, etc., and achieve high Reactivity and selectivity, increase product yield, reduce the effect of side reactions

Active Publication Date: 2009-01-07
JIANGSU GUOLI CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material butyl hexamethylenedicarbamate is more expensive, and the cost of synthesizing HDI is still relatively high
[0009] The above-mentioned green preparation of 1,6-hexamethylene diisocyanate, if the lower price dimethyl carbonate raw material is used, not only the pyrolysis temperature is high, but also the yield is low, which is extremely unsatisfactory

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Add 500ml deionized water to a 1000ml reaction bottle, then add 118gZnSO 4 ·7H 2 O(0.413mol), 15g Al(NO 3 ) 3 9H 2 O (0.040mol) and 19.7g ZrOCl 2 ·8H 2 O, (0.061mol) and stir to dissolve, after cooling to 5°C, slowly drop 70g of ethyl titanate (0.304mol), continue to keep warm and stir for 60 minutes, then adjust the pH value to 6.5 with 10% ammonia water. After standing still for 24 hours, filter and wash, dry at 70°C for 24 hours, and cool to obtain white solid A. 10g ZrOCl 2 ·8H 2 O (0.031mol) zirconium oxychloride was dissolved in 296g of 5% sulfuric acid aqueous solution (0.151mol), and the resulting white solid A was impregnated with this solution for 4 hours, dried at 100°C for 4 hours, and then calcined at 550°C for 4 hours. A solid acid catalyst is prepared.

Embodiment 2

[0021] Embodiment 2: add 500ml deionized water in 1000ml reaction bottle, then add 76.3g ZnCl 2 (0.56mol), 17.6g AlCl 3 ·6H 2 O (0.073mol) and 41.8g ZrOCl 2 ·8H 2 O (0.13 mol) was stirred and dissolved, and after cooling down to 5°C, 21.7 g of ethyl titanate (0.095 mol) was slowly added dropwise, kept stirring for 60 minutes, and then adjusted the pH value to 6.5 with 10% ammonia water. After standing still for 24 hours, filter and wash, dry at 70°C for 24 hours, and cool to obtain white solid A. 10g ZrOCl 2 ·8H 2 O (0.031mol) was dissolved in 218g of 5% sulfuric acid aqueous solution (0.111mol), impregnated with this solution to obtain a white solid A for 4 hours, dried at 100°C for 4 hours, and then calcined at 550°C for 4 hours to obtain solid acid catalyst.

Embodiment 3

[0022] Embodiment 3: add 500ml deionized water in 1000ml reaction bottle, then add 92.5gZn (NO 3 ) 2 ·6H 2 O(0.311mol), 20.5g Al(NO 3 ) 3 9H 2 O(0.055mol) and 25gZr(SO 4 ) 2 (0.088mol), and stir to dissolve, after cooling to 5°C, slowly drop 99.7g of ethyl phthalate (0.437mol), continue to insulate and stir for 60 minutes, then adjust the pH value to 6.5 with 10% ammonia water. After standing still for 24 hours, filter and wash, dry at 70°C for 24 hours, and cool to obtain white solid A. 8.8gZr(SO 4 ) 2 (0.031mol) was dissolved in 152g of 5% sulfuric acid aqueous solution (0.078mol), impregnated with this solution to obtain a white solid A for 4 hours, dried at 100°C for 4 hours, and then calcined at 550°C for 4 hours to obtain a solid acid catalyst.

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PUM

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Abstract

The invention relates to a solid-acid catalyst, and the application thereof in the synthesis of 1, 6-hexamethylene diisocyanate (HDI). The solid-acid catalyst of the invention is characterized in that SO4<2-> / TiO2-ZnO-ZrO2-Al2O3 is prepared by the reaction of phthalate ester, water soluble zinc salt, water soluble aluminum salt, water soluble zirconium salt and H2SO4; the mole fraction of the phthalate ester is 8-45 percent; the mole fraction of the zinc salt is 30-60 percent; the mole fraction of the zirconium salt is 3-10 percent; and the mole fraction of the H2SO4 is 6-18 percent. The catalyst is applicable to the preparation of the 1, 6-hexamethylene diisocyanate (HDI), has higher reaction activity and higher selectivity, and can adopt the cheaper dimethyl carbonate as the raw material, besides, the aminolysis yield is as high as 95 percent, the pyrolysis yield can reach 88 percent, and the catalytic pyrolysis temperature is especially lower, and can decrease to be not higher than 230 DEG C, thereby obviously reducing the occurrence of side reactions, improving the yielding rate of the product, and enabling the total yielding rate of the product to be 83.6 percent.

Description

technical field [0001] The invention relates to a solid acid catalyst and its application in synthesizing 1,6-hexamethylene diisocyanate (HDI). Background technique [0002] 1,6--Hexamethylene diisocyanate (HDI) is an important aliphatic diisocyanate species, which is widely used in the aviation industry, automobile industry and shipbuilding industry, as well as for the production of alcohol due to its many outstanding properties. Acid resin paint, polyurethane leather finishing agent, clothing fabric finishing agent, transparent polyurethane coating (crystal slurry), imitation enamel coating, polymer bandage material, plastic additives and polyurethane elastomer, etc. HDI has become the isocyanate with the largest demand after MDI (diphenylmethane diisocyanate), PAPI (polymethyl polyphenylene isocyanate) and TDI (toluene diisocyanate), and is an important species in the diisocyanate family. [0003] The earlier preparation method of HDI is the phosgene method, for example:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C265/14C07C263/04
Inventor 陈光炎胡立新郎旭东
Owner JIANGSU GUOLI CHEM TECH
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