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

Intumescent flame retardant of star-shaped boric acid ester derivative and preparation method of intumescent flame retardant

A technology of intumescent flame retardant and borate ester, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problems of weak flame retardancy and toxicity, and achieve Prevent burning, prevent dripping, and solve the effect of easy dripping

Active Publication Date: 2017-01-04
SOUTH CHINA UNIV OF TECH
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Boron, phosphorus and nitrogen are all flame retardant elements. Although organic phosphorus flame retardants containing flame retardant phosphorus in the organic molecular structure have good flame retardant properties, they have certain toxicity.
While the organic nitrogen flame retardant containing only one flame retardant element nitrogen in the organic molecular structure is non-toxic, but its flame retardant performance is relatively weak.

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
  • Intumescent flame retardant of star-shaped boric acid ester derivative and preparation method of intumescent flame retardant
  • Intumescent flame retardant of star-shaped boric acid ester derivative and preparation method of intumescent flame retardant
  • Intumescent flame retardant of star-shaped boric acid ester derivative and preparation method of intumescent flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step: 2.58g phloroglucinol and 9.11gN, N-diisopropylethylamine are dissolved in 40ml tetrahydrofuran solution (mixture 1), 16.79g cyanuric chloride is dissolved in 80ml tetrahydrofuran solution, and Fully stir in an ice-water bath for 31 minutes (mixed solution 2), add mixed solution 1 dropwise to mixed solution 2, stir at 5°C for 3 hours, and filter;

[0031] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0032] Step 3: Add 7.5ml of ethylene glycol and 20ml of toluene (as a water-carrying agent) solution into a three-necked flask, stir and gradually heat up to 42°C, add 7.34g of boric acid, continue to heat up to 88°C, and stir for 47 minutes until the boric acid is completely Dissolve; continue to react for 2.5 hou...

Embodiment 2

[0040] The first step: 5.23g phloroglucinol and 18.37gN, N-diisopropylethylamine are dissolved in 80ml tetrahydrofuran solution (mixture 1), 35.31g cyanuric chloride is dissolved in 80ml tetrahydrofuran solution, and Fully stir in an ice-water bath for 31 minutes (mixed solution 2), add mixed solution 1 dropwise to mixed solution 2, stir at 5°C for 3 hours, and filter;

[0041] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0042] Step 3: Add 14ml of ethylene glycol and 40ml of toluene (as a water-carrying agent) solution into the three-necked flask, stir and gradually heat up to 42°C, add 14.89g of boric acid, continue to heat up to 88°C, and stir for 47 minutes until the boric acid is completely dissolved ; When the moisture in the...

Embodiment 3

[0046] The first step: 7.76g phloroglucinol and 27.29gN, N-diisopropylethylamine are dissolved in 120ml tetrahydrofuran solution (mixture 1), 49.63g cyanuric chloride is dissolved in 240ml tetrahydrofuran solution, and Fully stir in an ice-water bath for 37 minutes (mixed solution 2), add mixed solution 1 dropwise to mixed solution 2, stir at 3°C ​​for 5 hours, and filter;

[0047] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0048] Step 3: Add 20.5ml of ethylene glycol and 60ml of toluene (as a water-carrying agent) solution into a three-necked flask, stir and gradually heat up to 47°C, add 22.67g of boric acid, continue to heat up to 70°C, and stir for 55 minutes until the boric acid is completely Dissolve; continue to react for ...

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
heat release rateaaaaaaaaaa
Login to View More

Abstract

The invention discloses an intumescent flame retardant of a star-shaped boric acid ester derivative and a preparation method of the intumescent flame retardant. The star-shaped boric acid ester derivative is 1,3,5-three-{4,6-two-([1,3,2] dioxaborolane-2-oxo)-1,3,5-triazine-2-oxo} benzene. When the intumescent flame retardant is prepared, phloroglucinol and N, N-diisopropylethylamine are added into tetrahydrofuran solution; mixed solution is dripped into tetrahydrofuran solution of cyanuric chloride, stirred, filtered and separated to obtain intermediate products 1; ethylene glycol and methylbenzene are stirred and mixed, temperature is gradually risen, boric acid is added, the temperature continues to be risen, and backflow and reaction are performed; the methylbenzene is removed, and drying is performed to obtain intermediate products 2; the intermediate products 2 are dissolved in the tetrahydrofuran solution under protection of nitrogen, sodium hydroxide is added, the tetrahydrofuran solution with the intermediate products 1 is added in batches, and continuous reaction is performed for 3-6 hours; purification is performed to obtain target products. The obtained products can serve as excellent environment-friendly organic flame retardants.

Description

technical field [0001] The invention relates to an environment-friendly flame-retardant polymer material, in particular to an intumescent flame retardant based on a star-shaped borate ester derivative and a preparation method thereof. Background technique [0002] Compared with traditional inorganic metal materials, polymer materials have their own unique advantages, and they play an increasingly important role in the national economy and people's lives. However, most polymer materials are flammable materials, which will pose a huge threat to people's property and life, so flame retardants are very important. Flame retardants can be divided into inorganic flame retardants and organic flame retardants according to their attributes. Inorganic flame retardants have the advantages of low smoke, low toxicity, halogen-free, good stability, and low price. The disadvantages such as poor capacitance and reduced material performance are limited to a certain extent. Although the trad...

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): C07F5/04C08K5/55C08L63/02
CPCC07F5/04C08K5/55C08L2201/02C08L63/00
Inventor 曾金明陈珊珊刘平刘伟时张铁潘永红刘东发徐添贵
Owner SOUTH CHINA UNIV OF TECH
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

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com