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Production of tri(4-isocyanate benzyl) thiophosphate

A technology of triaminotriphenyl phosphorothioate and phosphorothioate, which is applied in the field of industrial production of phosphorothioate, can solve the problems of complex process, pollution, harsh reaction conditions and the like, and achieves low operating cost and easy operation. Safe, short response time effect

Active Publication Date: 2010-05-26
山东崇舜新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problems of complex process, harsh reaction conditions and serious pollution in the prior art, thereby providing a tris(4-isocyanate) with simple and safe process, mild reaction conditions, high yield and no environmental pollution The production method of phosphorothioate (hereinafter referred to as TPTI)

Method used

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  • Production of tri(4-isocyanate benzyl) thiophosphate
  • Production of tri(4-isocyanate benzyl) thiophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Put 200kg of 1,2-dichloroethane and 25kg of TPTA into a 500L enamel reaction kettle, heat up and dissolve for later use.

[0030] In a 1000L enamel reaction kettle, put 200kg of 1,2-dichloroethane and 50kg of BTC into it, stir to dissolve, add 9kg of triethylamine in 1,2-dichloroethane (containing 0.8kg of triethylamine), and feed nitrogen. Then slowly add the 1,2-dichloroethane solution of TPTA from the 500L kettle, and then raise the temperature and reflux for 2 hours. The 1,2-dichloroethane was distilled off by passing nitrogen gas to obtain 29.1 kg of a light yellow solid with a melting point of 82.5-84.5°C and a content of 3% of 1,2-dichloroethane. After refining, 27.6kg of white solid was obtained, with a yield of 92.0%. Melting point 83.5~86.0℃, isocyanate content 27.0%. The solid can be directly added to an appropriate solvent to prepare a polyisocyanate adhesive with a corresponding concentration.

[0031] In the embodiment, the ratio of TPTI to BTC is 0.38...

Embodiment 2

[0033] In 1000L reactor, drop into 200kg isoamyl acetate and 60kg BTC, stir and dissolve. 10 kg of isoamyl acetate solution of triethylamine (containing 0.9 kg of triethylamine) was added, and nitrogen gas was introduced. Slowly add the isoamyl acetate solution 235kg of the TAPA prepared with embodiment 1 then. Subsequent operations are the same as in Example 1. Yield 96.4%.

[0034] In the embodiment, the ratio of TPTI to BTC is 0.32:1.

Embodiment 3

[0036] Operation with embodiment 1, the difference is that the inert organic solvent is chlorobenzene. Yield 98.0%.

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Abstract

Production of trithiophosphate (4-isocyanic ester group phenyl ) achieves simple and safety process, high production efficiency and no environmental pollution.

Description

technical field [0001] The invention belongs to a production method of tris(4-isocyanatophenyl)phosphorothioate, in particular to a method for industrial production by reacting triaminotriphenylphosphorothioate with bis(trichloromethyl)carbonate Tris(4-isocyanatophenyl) phosphorothioate method. Background technique [0002] Polyisocyanate adhesive is widely used because of its high bonding strength, especially suitable for bonding metal to rubber, fiber, etc. Such as Desmodur RF and Desmodur RFE adhesives of Bayer Company in Germany, Hartdur E333, Hartdur F256, Hartdur F215 and other adhesives of Hangzhou Chongshun Chemical Co., Ltd. Tris (4-isocyanatophenyl) phosphorothioate (English name Tris-(4-Isocyanatophenyl)-Thiophosphate, referred to as TPTI) is the main component of this type of polyisocyanate adhesive, which is mentioned in patents GB930918, GB1094321, and US5576558 There are elaborations. [0003] At present, the industrial production of TPTI has been using the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/165
Inventor 俞介兵聂天明钟文清
Owner 山东崇舜新材料科技有限公司