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Isocyanate with inflaming retarding characteristic and preparation method and application thereof

A technology of isocyanate and diisocyanate, applied in the field of isocyanate and its preparation, can solve problems such as the flame retardancy of modified isocyanate, and achieve the effects of increasing flame retardancy, novel structure and less by-products

Inactive Publication Date: 2019-07-05
苏州塔霍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

However, this patent does not substantially modify the flame retardancy of isocyanate

Method used

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  • Isocyanate with inflaming retarding characteristic and preparation method and application thereof
  • Isocyanate with inflaming retarding characteristic and preparation method and application thereof
  • Isocyanate with inflaming retarding characteristic and preparation method and application thereof

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preparation example Construction

[0037] There is the preparation method of the isocyanate of flame retardant characteristic among the present invention, comprises the following steps:

[0038] (1) Preparation of 5-bromo-isophthaloyl chloride: 5-bromo-isophthalic acid in SOCl 2 Medium reflux reaction, and then evaporated under reduced pressure to remove SOCl 2 , to obtain 5-bromo-isophthaloyl chloride;

[0039] (2) Preparation of 5-bromo-isophthaloyl diazide: Dissolve 5-bromo-isophthaloyl dichloride in THF, then add NaN 3 , then add saturated NaHCO to the mixed solution 3 , extracted with toluene, the organic layer was dried and evaporated under reduced pressure to obtain a toluene solution of 5-bromo-m-dibenzoyldiazide;

[0040] (3) Preparation of 1-bromo-3,5-diisocyanatobenzene: reflux the toluene solution of 5-bromo-m-dibenzoyldiazide obtained in the above step (2), remove toluene, and obtain 1-Bromo-3,5-diisocyanatobenzene.

[0041] However, the inventor found in the synthesis process that the purity ...

Embodiment 1

[0043] An isocyanate with flame retardant properties, its structural name is 1-bromo-3,5-diisocyanatobenzene, and its structural formula is:

[0044]

[0045] The preparation method of the above-mentioned isocyanate with flame retardant properties, its preparation steps are:

[0046](1) Preparation of 5-bromo-isophthaloyl chloride: 5-bromo-isophthalic acid in SOCl 2 Medium (the mass concentration of 5-bromo-isophthaloyl chloride is 0.067mol / L) was refluxed for 2 hours, and the SOCl was distilled off under reduced pressure. 2 , to obtain the product 5-bromo-isophthaloyl chloride.

[0047] (2) Preparation of 5-bromo-isophthaloyl diazide: Dissolve 5-bromo-isophthaloyl chloride in THF (short for tetrahydrofuran) (it can be completely dissolved), and add NaN to the mixed solution 3 (NaN 3 The concentration of the substance is 0.07mol / L). Then add saturated NaHCO to the mixed solution 3 , extracted 3 times with toluene, and the organic layer was washed with MgSO 4 Drying an...

Embodiment 2

[0050] First, the preparation of 5-bromo-isophthalic acid in the present embodiment, using isophthalic acid as a raw material, utilizes liquid bromine to carry out bromination reaction to obtain 5-bromo-isophthalic acid (see Mark Gelmont for specific steps and Jakob Oren, Organic Process Research & Development 2002, 6, 591-596).

[0051] Such as figure 2 Shown is the mass spectrum of 5-bromo-isophthalic acid. Wherein the highest peak is at 244.9, which is the molecular weight of 5-bromo-isophthalic acid, indicating that the product 5-bromo-isophthalic acid has been successfully prepared. In addition, some miscellaneous peaks are ion fragments, and the peak at 322.8 is Bromine disubstitution.

[0052] In this embodiment, the isocyanate with flame retardant properties, that is, the preparation steps of 1-bromo-3,5-diisocyanatobenzene are as follows:

[0053] (1) Preparation of 5-bromo-isophthaloyl chloride: 5-bromo-isophthalic acid in SOCl 2 Medium (the mass concentration o...

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Abstract

The invention discloses isocyanate with an inflaming retarding characteristic and a preparation method and application thereof, and belongs to the technical field of inflaming retarding coatings. Isophthalic acid is taken as a raw material, and the 1-bromine-3,5-diisocyanate benzene with the inflaming retarding characteristic is synthesized. The preparation method comprises the following steps of(1) preparation of 5-bromine-isophthalyl chloride; (2) preparation of 5-bromine 2-nitrine; (3) preparation of the 1-bromine-3,5-diisocyanate benzene. According to the preparation method, based on thephysicochemical property of an original coating, the non-toxic and fire-proof effects are added for the coating, a production technology and the preparation method are simple, there are no complex processes, the quality of the prepared product is stable, and the isocyanate is suitable for large-scale production, wide in market prospect and high in social and economic benefits.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant coatings, and more specifically relates to a flame-retardant isocyanate and its preparation method and application. Background technique [0002] With the development of my country's economic construction and the rapid development of the coating industry, people's awareness of the safety of coatings has gradually become stronger. The coating industry is everywhere, from people's interior decoration to automobile spraying to national defense, the coating industry is everywhere, especially polyurethane coatings. [0003] Along with the construction of the national economy, along with the development of coating industry, as people pay more and more attention to health, fireproof and non-toxic coatings are just becoming more and more important. At present, the flame retardant properties of coatings are mainly started from the formulation point of view, and some flame retardants (such as phosp...

Claims

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Application Information

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IPC IPC(8): C07C265/14C07C263/12C07C51/363C07C63/68C09D175/02C09D5/18C08G18/77
CPCC07C51/363C07C265/14C08G18/773C09D5/18C09D175/02C07C63/68
Inventor 李净植梅泽群
Owner 苏州塔霍新材料科技有限公司
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