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Sulfonate flame retardant with high nitrogen and phosphorus content, preparation method and application

A sulfonate and flame retardant technology, applied in the field of flame retardant synthesis, can solve the problems of easy-to-corrode molds, large amount of flame retardants, environmental hazards, etc. Efficient effect

Active Publication Date: 2016-06-29
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the many reported commercial flame retardants for PC modification, although some flame retardants have achieved different degrees of flame retardant effects, there are still many defects in the application process, such as halogen flame retardants. Flame retardants are gradually eliminated by people because they produce a lot of smoke and corrosive gases when they burn, and some even produce carcinogenic dioxins, which cause serious environmental hazards; , environmental protection, high efficiency and other advantages, but this kind of flame retardants are expensive, and the product performance stability needs to be improved; the addition of phosphorus-nitrogen flame retardants will lead to a decrease in the mechanical properties and mechanical properties of the material, and it is easy to corrode the mold; Sulfonate flame retardants are expensive, and the synthesis process route and post-treatment are complicated and will affect the performance, color, etc. of the product

Method used

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  • Sulfonate flame retardant with high nitrogen and phosphorus content, preparation method and application
  • Sulfonate flame retardant with high nitrogen and phosphorus content, preparation method and application
  • Sulfonate flame retardant with high nitrogen and phosphorus content, preparation method and application

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preparation example Construction

[0031] The embodiment of the present invention provides a preparation method of the above-mentioned high nitrogen-containing phosphorus-containing sulfonate flame retardant, comprising the following steps:

[0032] Step 1, using polycyanogen chloride as a matrix and sodium p-aminobenzenesulfonate as a nucleophile to synthesize compound II, said compound II has the following structure:

[0033]

[0034] Step 2, triphenylphosphine oxide is nitrated into compound III with a nitrating agent, and the compound III has the following structure:

[0035]

[0036] Step 3, the compound III is reduced to generate compound IV, and the compound IV has the following structure:

[0037]

[0038] Step 4, using the compound II as the matrix and the compound IV as the nucleophile to synthesize the compound I as the target product.

[0039] Concrete reaction process is as follows:

[0040]

[0041] Preferably, the specific process of said step 1 is: adding cyanuric chloride into a t...

Embodiment

[0052]First, stir and dissolve 18.40g (0.1mol) of cyanuric chloride in a 1000ml four-neck flask in 300ml of industrial acetone, then place the aqueous solution containing 36.8g (0.1mol) of sodium p-aminobenzenesulfonate in a constant pressure dropping funnel , slowly drop into the four-neck flask. A large amount of white precipitate was produced during the reaction. During the reaction process, adjust the pH value with a sodium hydroxide solution with a concentration of 1 mol / L to about 7 to 8, and react for 2 hours. After the reaction is completed, filter under reduced pressure, take out the filter cake, and wash with industrial acetone (50mL×3) repeatedly. . Filter and dry. The developer was methanol:toluene=1:1, and dried to obtain compound II as a white solid.

[0053] 0.1 mol of triphenylphosphine oxide was stirred and dissolved in 400 ml of 95-98% concentrated sulfuric acid in a 1000 ml four-necked flask at -5°C to obtain a colorless transparent liquid. Nitrating age...

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Abstract

The invention relates to the technical field of synthesis of a flame retardant and provides a sulfonate flame retardant with high nitrogen and phosphorus content. The sulfonate flame retardant comprises a compound I with a structure shown in the specification. The invention further provides a preparation method of the sulfonate flame retardant with high nitrogen and phosphorus content. According to the preparation method, cyanuric chloride, triphenylphosphine oxide, sodium sulfanilate, concentrated nitric acid and concentrated sulfuric acid are taken as raw materials, and the compound I is synthesized through four steps of reactions. The invention further provides an application of the sulfonate flame retardant with high nitrogen and phosphorus content in addition to polycarbonate. The sulfonate flame retardant, the preparation method and the application have the beneficial effects that the flame retardant is non-toxic, smoke-suppressing, droplet-resisting, good in thermal stability, high in flame retardant efficiency and low in cost; the usability and color of a product are not affected when the sulfonate flame retardant is added to the material, a nitrogen and phosphorus synergistic flame retardant effect can be realized, and a synthesis process is simple and suitable for popularization and application.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis, in particular to a high-nitrogen-containing phosphorus-containing sulfonate flame retardant, a preparation method and an application. Background technique [0002] Compared with ordinary engineering plastics, polycarbonate (PC) has higher flame retardancy, but it is still difficult to meet the application requirements in the field of flame retardancy, and flame retardants are aimed at improving the fire and flame retardancy of materials A chemical compound. Among the many reported commercial flame retardants for PC modification, although some flame retardants have achieved different degrees of flame retardant effects, there are still many defects in the application process, such as halogen flame retardants. Flame retardants are gradually eliminated by people because they produce a lot of smoke and corrosive gases when they burn, and some even produce carcinogenic dioxins, which...

Claims

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Application Information

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IPC IPC(8): C08K5/5397C08L69/00C07F9/6521
CPCC07F9/6521C08K5/5397C08L2201/02C08L2201/08C08L69/00
Inventor 胡志勇张旭东蒋俊奎宁娟霞朱海林贺圣龙马忠平曹端林郭建峰
Owner ZHONGBEI UNIV
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