Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of flame retardant for inflammable hazardous chemical plastic products

A technology for flame retardants and hazardous chemicals, applied in the field of chemical preparation preparation, can solve the problem of easily turning yellow, orange or even purple in severe cases, product strength, hardness, elasticity, and active ingredient content of flame retardants. Advanced problems, to achieve the effect of strong flame retardancy, easy rubber mixing, and good compatibility

Inactive Publication Date: 2017-08-29
刘新智 +1
View PDF2 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the known flammable and dangerous plastic halophosphorus composite flame retardants mainly include liquids such as dihalogen (chlorine, bromine) propyl triphosphate, chloroalkyl polyphosphate, chlorobromoalkyl phosphate, etc. Although it can meet the requirements of flame retardancy in practical applications, it has a negative impact on the strength, hardness, and elasticity of the product; another example is the well-known bromophosphorous compound such as S6000, SW-B80, (tribromoneopentyl) triphosphate, etc. Flame retardants, Yuyao high-efficiency BPN and many brominated powder flame retardants have no plasticizing effect on nitrocellulose and polymer plastics, and have extremely poor tolerance with nitrocellulose; in addition, the above-mentioned known flame retardants are used due to Large amount of addition, high cost, and the use of auxiliary flame retardant Sb 2 o 3 (antimony white), the key is that after adding these flame retardants, the performance of the product will deteriorate, which is the main reason why the known flame retardant plastics are difficult to popularize and promote; in 2009, the flame retardant developed by Sun Jialong et al. As the main raw material, aliphatic halogenated derivatives are used as solvents and triethylamine is used as a catalyst. Although some progress has been made in the experimental range, the reaction of the prepared product is too intense due to the direct addition of triethylamine in the pre-treatment and post-treatment. ——Washed and refined products have poor whiteness, free bromine (Br free radicals and HBr have a very decomposing and catalytic effect on the flame retardant itself and the plastic polymer base material, which can cause chain reactions and automatic oxidation, resulting in The active ingredients of flame retardants are extremely lost) and the content is high. During the thermal processing of flame-retardant plastics, it is easy to turn yellow, and in severe cases, it can turn orange or even purple, and the bromination of the glare and the pungent odor of the respiratory system are emitted in the workshop. Hydrogen gas also deteriorates the mechanical properties, appearance and flame retardancy of the product, thus losing its practicability

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of flame retardant for inflammable hazardous chemical plastic products
  • Preparation method of flame retardant for inflammable hazardous chemical plastic products
  • Preparation method of flame retardant for inflammable hazardous chemical plastic products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for preparing a plastic flame retardant for flammable hazardous chemicals based on (2,4-dibromophenyl) phosphate triester, comprising the following process steps:

[0029] 1. Synthesis of 2,4-dibromophenol

[0030] Required equipment: clean four-necked glass reaction bottle, return pipe and matching external vacuum exhaust gas absorption bottle.

[0031] 1. Add 28.2g (0.3 mole) of dry industrial phenol and 300ml of chloroform to the four-necked bottle successively, then stir to dissolve, and control the temperature below 30°C;

[0032] 2. Slowly add 96g (0.6 mole) of dried industrial bromine dropwise to the reaction bottle, control the feeding speed for about 2 hours, control the reaction temperature not to exceed 30°C, after the dropwise addition is completed, then continue the reflux reaction in a boiling state 1.5h to obtain 2,4-dibromophenol solution;

[0033] 3. The reaction tail gas is absorbed by water to produce hydrobromic acid, which is sold as a by...

Embodiment 2

[0045] A method for preparing a plastic flame retardant for flammable hazardous chemicals based on (2,4-dibromophenyl) phosphate triester, comprising the following process steps:

[0046] 1. Synthesis of 2,4-dibromophenol

[0047] 1. In a 2000ml four-necked bottle, add 112.8g (1.2 moles) of dry industrial phenol and 1200ml chloroform to dissolve it under stirring;

[0048] 2. Control the reaction temperature below 30°C, slowly add 384g (2.4 moles) of industrial bromine dropwise under stirring, control the addition in 1 hour, control the reaction temperature not to exceed 30°C, and continue the reflux reaction for 1.5h to obtain 2,4― Dibromophenol solution;

[0049] 3. The reaction tail gas is made into hydrobromic acid as a by-product through the water absorption device.

[0050] 2. Synthesis of (2,4-dibromophenyl) phosphate triester

[0051] 1. The above-mentioned product 2,4-dibromophenol chloroform solution, keep the temperature below 25°C, slowly add 60.5g (0.395mol) of...

Embodiment 3

[0061] A method for preparing a plastic flame retardant for flammable hazardous chemicals based on (2,4-dibromophenyl) phosphate triester, comprising the following process steps:

[0062] 1. Synthesis of 2,4-dibromophenol

[0063] 1. In a 2000ml four-necked bottle, add 112.8g (1.2 moles) of industrial phenol, and dissolve it with 1200ml carbon tetrachloride under stirring;

[0064] 2. Control the reaction temperature below 30°C, slowly add 384g (2.4 moles) of industrial bromine dropwise under stirring, and finish the addition in about 2 hours. After the addition, keep the temperature below 30°C and continue the reflux reaction for 1 hour to obtain 2,4- Dibromophenol solution;

[0065] 3. The reaction tail gas is made into hydrobromic acid as a by-product through the water absorption device.

[0066] 2. Synthesis of (2,4-dibromophenyl) phosphate triester

[0067] 1. The above product 2,4-dibromophenol carbon tetrachloride solution, keep the temperature below 25°C, slowly add...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
breaking strengthaaaaaaaaaa
tensile strengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of a flame retardant for inflammable hazardous chemical plastic products. The method includes the steps of: 1) in an aliphatic-series halogenated solvent, dissolving phenol, performing a dropwise-adding reaction under stirring with bromine, slowly increasing the temperature until the boiling range of the solvent, and performing reflux to prepare a dibromo (tribromo) phenol aliphatic-series halogenated solution; 2) slowly dropwise adding a newly distilled industrial product phosphorus oxychloride, and slowly dropwise adding diluted triethylamine into the reaction bottle, and then slowly increasing the temperature so as to perform a reaction to the solvent at boiling temperature; 3) maintaining stable reflux to prepare tri(2,4-dibromophenyl) phosphate or tri(2,4,6-tribromophenyl) phosphate; and 4) water-washing and re-crystallizing the product to obtain the flame retardant. The flame retardant is toxic-free, is low in melt point, has good thermostability and compatibility, is good in flame retarding effect, and can be widely used in engineering plastics and alloys, such as nitro-cotton, celluloid and the like.

Description

technical field [0001] The content of the present invention belongs to the technical field of preparation of chemical preparations, and relates to a method for preparing a plastic flame retardant for flammable and dangerous chemicals. Flame retardant for nitrocellulose. Background technique [0002] Celluloid products, as the early "King of Plastics", once played an important role in human life. Table tennis, which is well known and proud of the Chinese people, is made of synthetic plastic celluloid. Because celluloid has the advantages of high hardness, good elasticity, strength and dyeability, despite the development of many new plastics for more than a hundred years, celluloid has always been recognized as the best choice for making table tennis balls. Decorative materials for making buttons, hair clips, glasses frames, organs, pianos, keys of percussion instruments, etc. However, since the main raw material of celluloid is the sister material of smokeless gunpowder - n...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12C08K5/523
CPCC07F9/12C08K5/523
Inventor 刘新智张汝冰李刘洋马春江
Owner 刘新智
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products