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Synthetic method of compound blocked polyisocyanates by using multiple sealants to compound and block terminal groups

A technology of polyisocyanate and synthesis method, which is applied in the field of composite polyisocyanate block synthesis, to achieve the effects of reasonable cost, improved performance, and improved stone chipping resistance

Active Publication Date: 2010-08-04
WUHAN RES INST OF MATERIALS PROTECTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] Aiming at the various problems mentioned above in the preparation of isocyanate blockers by a single blocking agent, the present invention proposes a compound polyisocyanate blocker synthetic method that is compound-blocked with multiple blocking agents. , the same below), 50 to 350 parts of active methylene compounds, 290 to 335 parts of solvents, and stirred at 50 to 90°C for 1 to 3 hours; add another active methylene that is different from the previous one 50-350 parts of pyrazole-based compounds, stirred at 50-90°C for about 1-2 hours; then added 20-130 parts of pyrazole-derived compounds in batches, stirred at 50-85°C until no NCO groups or NCO groups could be detected % is not higher than 0.2% (about 0.5 to 2 hours).

Method used

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  • Synthetic method of compound blocked polyisocyanates by using multiple sealants to compound and block terminal groups
  • Synthetic method of compound blocked polyisocyanates by using multiple sealants to compound and block terminal groups
  • Synthetic method of compound blocked polyisocyanates by using multiple sealants to compound and block terminal groups

Examples

Experimental program
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Effect test

Embodiment 1

[0052] 468 grams of liquefied diphenylmethane-4,4'-diisocyanate, 160 grams of diethyl malonate, 133 grams of propylene glycol methyl ether acetate, 192 grams of naphtha 100 # Add the mixture to the container, stir at 70°C for about 2 hours; add 130 grams of ethyl acetoacetate, stir at 70°C for about 2 hours; add 109 grams of 3,5-dimethylpyrazole in batches, and stir at 80°C , and stir until no NCO groups are detected (about 1 hour).

[0053] The molar ratio of active methylene compound blocking agent (diethyl malonate and ethyl acetoacetate) to pyrazole blocking agent (3,5-dimethylpyrazole) is 2:1.

[0054] Compared with the prior art, the technical progress and advantages of the present invention are obvious, and it solves many problems that have plagued the synthesis of isocyanate blockers with a single blocking agent for a long time.

Embodiment 2

[0056] 386 grams of liquefied diphenylmethane-4,4'-diisocyanate (NCO% is 29%) and 147 grams of hexamethylene diisocyanate biuret, 80 grams of diethyl malonate, 142 grams of methyl isobutyl Base Ketone, 185g Naphtha 100 # Add the mixture to the container, stir for about 2 hours at 75°C; add 182 grams of ethyl acetoacetate, stir for about 2 hours at 75°C; add 120 grams of 3,5-dimethylpyrazole in batches, °C, stir until no NCO groups are detected (about 1 hour).

[0057] The molar ratio of the active methylene compound blocking agent (diethyl malonate and ethyl acetoacetate) to the pyrazole blocking agent (3,5-dimethylpyrazole) was 1.7:1.

[0058] Compared with the prior art, the invention has obvious technical progress and advantages, and solves many problems that have been perplexing the synthesis of isocyanate blockers with a single blocking agent for a long time.

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Abstract

The invention relates to a synthetic method of compound blocked polyisocyanates by using multiple sealants to compound and block terminal groups, which is characterized in that 300-600 parts of polyisocyanate ( by mass part, the same below), 50-350 parts of active methylene compound and 290-335 parts of solvent are stirred for 1-3 hours at a temperature of 50-90 DEG C; 50-350 parts of another active methylene compound is added to be stirred for 1-2 hours at a temperature of 50-90 DEG C; 20-130 parts of pyrazole derivative compound is added to be stirred at a temperature of 50-85 DEG C in batches until NCO groups can not be detected or NCO% is not higher than 0.2% (about 0.5-2 hours). Compared with the prior art, the invention has improved technology and obvious advantages.

Description

technical field [0001] The present invention relates to polyisocyanate for end-blocking, in particular to a synthetic method for compound polyisocyanate blocker which is compound-blocked with multiple blocking agents. Background technique [0002] In many application fields, single-package polyurethane coatings are gradually replacing two-package polyurethane coatings, and have formed a complete application system. Single-package polyurethane coatings include thermosetting, room temperature curing, light curing and blocked isocyanate types. In single packaging In the coating system, blocked isocyanate has been widely used, especially polyurethane car bottom coating is increasingly in urgent need of appropriate blocked isocyanate. The polymer material in polyurethane car bottom coating has viscoelasticity, which can convert vibration energy into heat energy dissipation, It can effectively reduce structural vibration and noise, and its high attenuation coefficient can reduce t...

Claims

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Application Information

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IPC IPC(8): C07D231/14
Inventor 廖有为李健吴勇钟萍
Owner WUHAN RES INST OF MATERIALS PROTECTION
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