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A kind of preparation method of tdi trimer and solvent-containing tdi trimer and its application

A trimer and solvent technology, applied in the field of polyisocyanate, can solve the problems of poor aging resistance and yellowing resistance of paint films or adhesive films

Active Publication Date: 2021-07-23
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation process of TDI trimer curing agent needs to face an important problem, that is, because TDI belongs to aromatic isocyanate, its own yellowing resistance is poor, so the paint film formed when the prepared TDI trimer curing agent is applied downstream Or the aging resistance of the film is also poor

Method used

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  • A kind of preparation method of tdi trimer and solvent-containing tdi trimer and its application
  • A kind of preparation method of tdi trimer and solvent-containing tdi trimer and its application
  • A kind of preparation method of tdi trimer and solvent-containing tdi trimer and its application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] 1. Purification of Mannich base

[0071] The solid Mannich base catalyst based on bisphenol A / formalin / dimethylamine was synthesized with reference to US 4115373.

[0072]At 90°C, gradually add the catalyst to butyl acetate until saturated, quickly transfer the saturated solution of the catalyst to -20°C, and place it for 12 hours, the catalyst precipitates, the solution is filtered to obtain the purified solid catalyst, and in Dry at 30°C / 0.6mbar.

[0073] The dried catalyst (the impurity content of the secondary amine is about 1000ppm) is dissolved in xylene to form a xylene solution for subsequent use.

[0074] 2. Preparation of TDI trimer

[0075] 500g of TDI-80 as the starting diisocyanate and 500 g of butyl acetate were mixed in a 2 L reaction vessel purged with nitrogen to obtain a reaction mixture; the reaction mixture was heated to the required reaction temperature of 75° C. 1.5 g of a polymerization catalyst solution (the solution is a xylene solution of ...

Embodiment 2

[0083] 1. Purification of Mannich base

[0084] The solid Mannich base catalyst based on bisphenol A / formalin / dimethylamine was synthesized with reference to US 4115373.

[0085] At 75°C, gradually add the catalyst to butyl acetate until saturated, quickly transfer the saturated solution of the catalyst to -20°C, and place it for 12 hours, the catalyst precipitates, and the solution is filtered to obtain the purified solid catalyst, and in Dry at 30°C / 0.6mbar.

[0086] Dissolve the dried catalyst (secondary amine impurity content is about 500ppm) in xylene to form a xylene solution for subsequent use.

[0087] 2. Preparation of TDI trimer

[0088] 500g of TDI-80 as the starting diisocyanate and 500 g of butyl acetate were mixed in a 2 L reaction vessel purged with nitrogen to obtain a reaction mixture; the reaction mixture was heated to the required reaction temperature of 75° C. 1.5 g of a polymerization catalyst solution (the solution is a xylene solution of Mannich bas...

Embodiment 3

[0096] 1. Purification of Mannich base

[0097] The liquid Mannich base catalyst based on phenol / formalin / dimethylamine is synthesized with reference to US 4115373.

[0098] The synthesized Mannich base catalyst is subjected to short-path distillation to obtain the purified Mannich base catalyst. Conditions: 180°C / 0.1mbar, feed 0.5Kg / h, evaporation area 0.05m 2 .

[0099] The catalyst (secondary amine impurity content is about 500ppm) collected by distillation was dissolved in butyl acetate to form a butyl acetate solution for subsequent use.

[0100] 2. Preparation of TDI trimer

[0101] 500g of TDI-80 as the starting diisocyanate and 500 g of butyl acetate were mixed in a 2 L reaction vessel purged with nitrogen to obtain a reaction mixture; the reaction mixture was heated to the required reaction temperature of 75° C. 1.5 g of a polymerization catalyst solution (the solution is a butyl acetate solution of Mannich base, the catalyst concentration in which is 40 wt %) wa...

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Abstract

The invention provides a preparation method of TDI trimer, which uses toluene diisocyanate as a monomer raw material, and is prepared by self-polymerization in a solvent under the action of a Mannich base catalyst, wherein the Mannich base The impurity content of the secondary amine structure in the catalyst is ≤1000ppm. The preparation method of the TDI trimer provided by the present invention produces a TDI trimer product with lighter color, better yellowing resistance and more stable storage by controlling the impurity content. The preparation method of the present invention has simple and convenient process, mild reaction conditions, It does not need to consume too much economic cost, and is very valuable for industrial application.

Description

technical field [0001] The invention relates to the field of polyisocyanate, in particular to a preparation method of a TDI trimer, a solvent-containing TDI trimer prepared by the preparation method and an application thereof. Background technique [0002] In the art, the preparation of polyisocyanate compositions based on self-polymerization of isocyanates has been known for a long time, and has been reported in many publications and patent documents, such as patent documents DE 4428107 A1, US2993870 A, DE 1201992B, DE 2452532 A1 and journals Document J. Prakt. Chem. 336, 185-200, 1994. [0003] The preparation method of the commercially common TDI trimer curing agent product mainly is now: by making the toluene diisocyanate raw material available on a large scale in industry and suitable organic solvent in the phenolic catalyst (being that Under the catalysis of Mannich base), self-polymerization is carried out until almost complete conversion, and then the catalyst is de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/02C08G18/79C07D251/34
CPCC07D251/34C08G18/022C08G18/792
Inventor 王暖程李海军王玉启尚永华石滨张谦迟森森苏黎明黎源
Owner WANHUA CHEM GRP CO LTD
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