Catalyst for preparing polymercaptan curing agent and application thereof

A technology for a polythiol curing agent and a catalyst, which is applied in the field of polythiol compounds, can solve the problems of large industrial-scale production and application limitations, high production and separation costs, difficult recovery of catalysts, etc., and achieves good industrial application prospects and halogen residues. Low, reduced wastewater discharge effect

Active Publication Date: 2020-09-25
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But, the polythiol curing agent that above-mentioned preparation method obtains, product is mostly yellow-green or light yellow, and transparency is poor, and mostly used in the above-mentioned preparation method is quaternary ammonium salt type phase-transfer catalyst, can remain in the product after use. Excessive residues of halogens, etc., such as the high content of chloride ions in the obtained product, do not meet the requirements of green environmental protection; and the catalyst is not easy to recycle, the cost of production and separation is high, and the limitations of industrial-scale production and application are large

Method used

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  • Catalyst for preparing polymercaptan curing agent and application thereof
  • Catalyst for preparing polymercaptan curing agent and application thereof
  • Catalyst for preparing polymercaptan curing agent and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of catalyst QA-SBA-15:

[0052] (1) Halogenated SBA-15 process: in N 2 Under the atmosphere, add 2g of SBA-15 to a solution of 50mM 3-chloropropyltriethoxysilane (2g) in absolute ethanol, and after reflux for 24h, filter the mixture with suction and wash with absolute ethanol at 80°C. Dry overnight under vacuum, and the obtained solid is halogenated SBA-15.

[0053] (2) Synthesis of QA-SBA-15: 2 g of dried halogenated SBA-15 was placed in a 150 mL three-necked flask, and a mixed solvent of 50 mL of 1,2-dichloroethane and 50 mL of absolute ethanol was added. Add tri-n-butylamine according to the molar ratio n(Cl):n(amine)=1:3, reflux for 12 hours, separate by suction filtration, wash with ethanol, and dry in the air. Then use a Soxhlet extractor to add absolute ethanol to extract for 12 hours to remove unreacted tertiary amines in the pores, and finally vacuum-dry at room temperature to constant weight to obtain catalyst QA-SBA-15.

Embodiment 2

[0055] Catalyst QA-SBA-15 is prepared with reference to Example 1, the halogenation reagent is selected from 3-bromopropyltriethoxysilane (1.2), and during QA-SBA-15 synthesis, n(Cl):n(amine)=1:4.2 , and the rest of the reaction conditions remained unchanged.

Embodiment 3

[0057] Catalyst QA-SBA-15 was prepared with reference to Example 1, and the halogenation reagent was selected from 3-chloropropyltriethoxysilane (3.2g). When QA-SBA-15 was synthesized, n(Cl):n(amine)=1: 2.7, choose tri-n-propane as the tertiary amine, and keep the rest of the reaction conditions unchanged.

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Abstract

The invention relates to the technical field of polythiol compounds, in particular to a catalyst for preparing polythiol curing agents and its application. In the invention, a quaternary ammonium salt three-phase phase transfer catalyst is obtained by halogenating and modifying the mesoporous molecular sieve and reacting with a tertiary amine, and applying it to the preparation of a polythiol curing agent. The catalyst obtained by the method not only has high catalytic activity, but also can prepare a high-quality polythiol curing agent that is colorless and transparent and has low halogen residues, and the catalyst is easy to recycle, has low separation cost, and has very good industrial application prospects.

Description

technical field [0001] The invention relates to the technical field of polythiol compounds, in particular to a catalyst for preparing polythiol curing agents and its application. Background technique [0002] The preparation method of known thiol compound has many kinds, for example: (1) disulfide compound reduction method; (2) use organic halide or alcohols to react with thiourea earlier to generate isothiourea salt, then isothiourea The method of urea hydrolysis; (3) the method via Bunte salt; (4) the method of using organic halides to react with metal salts such as sodium hydrogensulfide and potassium hydrogensulfide; (5) the method of hydrolysis by dithiocarbamate (6) A method of adding alkenes to hydrogen sulfide or thioacetic acid, etc. Among them, method (2) and method (4) are the most commonly used preparation methods of mercaptan compounds by organic halides as starting materials. Compared with other methods, these two methods have high yield, few by-products, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/04C08G59/66
CPCC08G59/66C08G75/04
Inventor 梁万根费潇瑶崔卫华张超宋吻吻孙志利
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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