Preparation method for series of polyurethane catalysts

A technology of polyurethane catalyst and solid acid catalyst, which is applied in the field of preparation of a series of polyurethane catalysts, can solve problems such as inability to prepare THBA, and achieve the effects of low equipment operation requirements, easy handling, and good selectivity

Active Publication Date: 2016-02-24
恒光新材料(江苏)股份有限公司
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  • Abstract
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  • Claims
  • Application Information

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[0016] Neither of the above tw...

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  • Preparation method for series of polyurethane catalysts
  • Preparation method for series of polyurethane catalysts
  • Preparation method for series of polyurethane catalysts

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preparation example Construction

[0052] Mode 1, the preparation method of a silicon-aluminum supported solid acid catalyst with a silicon-aluminum ratio of 1:1, using SiO 2 / Al 2 o 3 =The mass ratio of 1:1 is carrier, carries out following steps successively:

[0053] (1) Dipping:

[0054] Immerse 50g of the carrier in 150ml of ammonium sulfate aqueous solution with a mass concentration of 25%, filter after 25 hours, and dry at 65-75°C to constant weight;

[0055] Repeat the above-mentioned soaking, filtering and drying twice more to obtain the precipitate I;

[0056] (2) Roasting:

[0057] Calcining the precipitate I at 400-420° C. for 3 hours to obtain a silica-alumina supported solid acid catalyst.

Embodiment 1

[0058] Example 1, a silicon-aluminum supported solid acid catalyst with a silicon-aluminum ratio of 1:1 (prepared in the above method 1), using N,N-dimethylethanolamine and N-methyldiethanolamine as starting materials, Follow the steps in order:

[0059] 1) synthesis

[0060] Add 356g (4mol) N,N-dimethylethanolamine, 476g (4mol) N-methyldiethanolamine, 40g silica-alumina supported solid acid catalyst into a 1000ml stainless steel autoclave, and replace the air in the autoclave with nitrogen for 2 minutes. Lower the temperature to 145-155°C and react for 15 hours. After the reaction time is up, stop heating, cool down to 30°C, vent, filter, and take the filtrate for rectification in the following steps. The filter cake is used as a silica-alumina supported solid acid catalyst for the next batch of reactions.

[0061] 2) Distillation and separation

[0062] The filtrate is transferred to a 1000ml single-necked flask equipped with a 30cm packed rectification column (using Rasc...

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Abstract

The invention discloses a preparation method for a series of polyurethane catalysts. The preparation method comprises the following steps: SioO2 and Al2O3 with different ratios are employed as carriers, soaked in an ammonium sulfate aqueous solution, dried and roasted, and a silicon-aluminum-loaded solid acid catalyst is prepared; then a mixture of N,N-dimethyl ethanolamine and N-methyl diethanolamine is employed as a raw material, the raw materials and the silicon-aluminum-loaded solid acid catalyst accounting for 1-10% of the total weight of the raw material are added in an autoclave and a reaction is carried out; the filtrate after the reaction is subjected to rectification separation and therefore N-methyl morpholine, 2-dimethylaminoethyl ether and N,N,N'-trimethyl-N'-hydroxyethyl-bis-amino ethyl ether are obtained respectively.

Description

technical field [0001] The invention relates to a preparation method of a series of polyurethane catalysts, specifically preparing N,N,N'-trimethyl-N'-hydroxyethyl-bis-aminoethyl ether, by-products N-methylmorpholine, bis The synthetic method of (2-dimethylaminoethyl) ether, these 3 kinds of compounds all can be used as polyurethane catalyst. Background technique [0002] N-methylmorpholine (abbreviated as NMM), whose general structural formula is shown in S-1, is an important class of organic chemical intermediates, which can be used as catalysts, spinning aids, solvents, etc. for polyurethane foam synthesis. [0003] [0004] Bis(2-dimethylaminoethyl) ether (abbreviated as A-1), whose general structural formula is shown in S-2, is an important polyurethane catalyst, which has the characteristics of high catalytic foaming reactivity and strong selectivity, and is commonly used It is used in the production of soft bulk foam and high resilience foam. [0005] [0006]...

Claims

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Application Information

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IPC IPC(8): C07C217/08C07C213/06C07D295/03C07D295/023B01J27/053
CPCB01J27/053C07C213/06C07D295/023C07D295/03C07C217/08
Inventor 张琪叶小明张超张华叶开天张依
Owner 恒光新材料(江苏)股份有限公司
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