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Diphenyl ethane diisocyanate trimer as well as preparation method and application thereof

A technology of diphenylethane diisocyanate and diphenylethane, which is applied in the field of polymer material preparation, can solve the problems of poor heat resistance, poor stability, low softening temperature and decomposition temperature, etc.

Inactive Publication Date: 2020-12-04
山东华阳农药化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing PU monomer raw materials have poor stability, and the PU products produced also have obvious shortcomings, such as poor heat resistance, low softening temperature and decomposition temperature, etc., thus limiting the application of PU products in some fields
[0004] Diphenylethane diisocyanate (EDI) is a novel monomer raw material for preparing PU, but the stability of EDI monomer is relatively poor and the storage time is short, which is not conducive to practical application.

Method used

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  • Diphenyl ethane diisocyanate trimer as well as preparation method and application thereof
  • Diphenyl ethane diisocyanate trimer as well as preparation method and application thereof
  • Diphenyl ethane diisocyanate trimer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 250.00L of ethyl acetate into the reaction kettle, blow nitrogen gas to remove water, add 50.00kg of diphenylethane-4,4'-diisocyanate, stir and dissolve at room temperature, heat to 30.0°C and add catalyst N,N-Dimethylbenzylamine 0.05kg, keep warm at 50.0°C for 1h, then take a sample and analyze the mass fraction of isocyanate group (-NCO%) (according to GB / T 13941-92, use di-n-butylamine method-hydrochloric acid titration method ), after that, every 0.5h sampling analysis-NCO%. NCO% reduces along with the carrying out of reaction, determines reaction degree with this, when adjacent 2 times record-NCO% difference value is less than 0.1, adds inhibitor benzoyl chloride 0.10kg to terminate reaction, the colorless or obtained Light yellow transparent liquid, the product detected by FT-IR at 2267cm -1 、1718cm -1 、1419cm-1 3 characteristic absorption peaks appear at , FAB-HRMS (M / e) detection value: 816.7681, molecular formula: C 42 h 36 N 6 o 12 , the product is d...

Embodiment 2

[0037] Add 60.60 L of butyl acetate into the reaction kettle, blow nitrogen gas to remove water, add 50.00 kg of 2,2'-dimethyl-diphenylethane-4,4'-diisocyanate, stir and dissolve at room temperature , add catalyst triethylamine 0.05kg under heating to 30.0°C, keep warm at 60.0°C for 1 hour, then take a sample and analyze the mass fraction of isocyanate group (-NCO%) (according to GB / T 13941-92 with di-n-butylamine method- hydrochloric acid titration), after that, every 0.5h sampling analysis-NCO%. NCO% reduces along with the carrying out of reaction, determines reaction degree with this, when adjacent 2 times record-NCO% difference value is less than 0.1, adds stopper benzoic acid 0.20kg to terminate reaction, obtains colorless or light Yellow transparent liquid, product detected by FT-IR at 2267cm -1 、1718cm -1 、1418cm -1 3 characteristic absorption peaks appear at , FAB-HRMS (M / e) detection value: 844.8212, molecular formula: C 44 h 40 N 6 o 12 , the product is 2,2'-d...

Embodiment 3

[0039] Add 25.50 L of benzyl acetate into the reaction kettle, blow nitrogen gas to remove water, add 50.00 kg of 2,2'-dimethyl-diphenylethane-5,5'-diisocyanate, stir and dissolve at room temperature , add catalyst N, N-diethylbenzylamine 0.05kg under heating to 30.0°C, keep warm at 80.0°C for 1 hour, then sample and analyze isocyanate group mass fraction (-NCO%) (according to GB / T13941-92 with two N-butylamine method-hydrochloric acid titration method), after that, sampling analysis-NCO% was taken every 0.5h. NCO% reduces along with the carrying out of reaction, determines reaction degree with this, when adjacent 2 times record-NCO% difference value is less than 0.1, adds polymerization inhibitor p-toluic acid 0.10kg to terminate reaction, obtains no Color or light yellow transparent liquid, the product is detected by FT-IR at 2264cm -1 、1715cm -1 、1417cm -1 3 characteristic absorption peaks appear at , FAB-HRMS (M / e) detection value: 844.8210, molecular formula: C 44 h ...

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Abstract

The invention discloses a diphenyl ethane diisocyanate tripolymer as well as a preparation method and application thereof, and relates to the technical field of preparation of high polymer materials.Provided is an EDI trimer having a structure represented by a formula in the descriptions of the invention. In a chemical structure in which diphenyl ethane is used as a parent nucleus, R is H or a hydrocarbon group; R is located at the 2-position (2 '-position) or 3-position (3'-position) of the diphenyl ethane structure; and -NCO is located at the 4'-position or 5'-position or 6'-position of diphenyl ethane, and -N- is located at the 4-position or 5-position or 6-position of diphenyl ethane.

Description

technical field [0001] The invention discloses a trimer, its preparation method and application, and relates to the technical field of polymer material preparation, in particular to a diphenylethane diisocyanate trimer, its preparation method and its application. Background technique [0002] Polyurethane (PU for short) is a polymer containing many carbamate groups (-NHCOO-) in the main chain of the polymer structure. Various hydrogen donor compounds (usually such as compounds containing terminal hydroxyl groups) are prepared by reaction. Because isocyanate and polyol compounds have different types of functional groups and different numbers of functional groups, polyurethane products with excellent performance and various forms of expression can be prepared through different synthesis processes and material selection. Widely used products include very soft or hard plastic foam, elastomer rubber with excellent wear resistance, high-gloss paints, coatings, adhesives with exce...

Claims

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Application Information

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IPC IPC(8): C07D251/30C08G18/79
CPCC07D251/30C08G18/79
Inventor 孙绪兵闫新华刘玉法
Owner 山东华阳农药化工集团有限公司
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