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Reactive flame-retardant block copolymer and preparing method thereof

A block copolymer, reactive flame retardant technology, applied in the field of polymer halogen-free flame retardant, can solve the problems of difficult adjustment of silicon content, few functional groups, poor matrix compatibility, etc., to achieve improved compatibility and Effects of flame retardancy, mild reaction conditions, and rich molecular design

Active Publication Date: 2015-08-12
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing phosphorus-containing silicon flame retardants still have disadvantages such as poor compatibility with the matrix, difficulty in adjusting the content of phosphorus and silicon in the product, few functional groups, complex synthesis routes, and high requirements for conditions, which limit their application. used widely

Method used

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  • Reactive flame-retardant block copolymer and preparing method thereof
  • Reactive flame-retardant block copolymer and preparing method thereof
  • Reactive flame-retardant block copolymer and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Preparation of macromolecular chain transfer agent: Dissolve 2.26 g (2.4 mmol) of methacryloxypropyl heptaisobutyl POSS (MAPOSS) in 2 ml of the first solvent toluene, and then add chain transfer agent dithiobenzene Cumyl formate (CDB) 54mg (0.2mmol) and initiator azobisisobutyronitrile (AIBN) 0.0016g (0.01mmol) were placed in a RAFT tube and degassed 3 to 5 times by continuous freezing and thawing. Polymerize at 65°C under the protection of gas argon. After 12-48 hours of reaction, liquid nitrogen is quenched to stop the reaction. The first precipitant is a blend of methanol and ethyl acetate (the volume ratio of methanol to ethyl acetate is 8: 1) Precipitate repeatedly 3 times and dry to obtain a macromolecular chain transfer agent with a degree of polymerization of 12, namely PMAPOSS 12 ;

[0030] 2) Synthesis of reactive flame retardant block copolymer: the PMAPOSS obtained in step 1) 12 0.35g (0.03mmol), methacrylate-2-hydroxyethyl phosphate (MOEP) 0.36g (1.8mm...

Embodiment 2

[0035] 1) Preparation of macromolecular chain transfer agent: the preparation steps are the same as step 1) in Example 1 to obtain macromolecular chain transfer agent PMAPOSS 12 ;

[0036] 2) Synthesis of reactive flame retardant block copolymer: the PMAPOSS obtained in step 1) 12 0.35g (0.03mmol), 0.36g (1.8mmol) of MOEP, 0.31ml (3mmol) of St, 1mg (0.006mmol) of initiator AIBN were dissolved in 3ml of the second solvent anhydrous THF, and degassed by continuous freezing and thawing for 3-5 After the second time, it was polymerized at 65°C under the protection of inert gas argon, and after 24 hours of reaction, it was quenched with liquid nitrogen to stop the reaction, and the second precipitant methanol was used for repeated precipitation twice, and dried to obtain a reactive flame-retardant block copolymer PMAPOSS m -b-P(MOEP n -co-St p ), its chemical structural formula is as shown in (I) formula:

[0037]

[0038] Wherein, m is the total number of units occupied by...

Embodiment 3

[0040] 1) Preparation of macromolecular chain transfer agent: 2.83g (3mmol) of MAPOSS was dissolved in 2ml of the first solvent toluene, then 54mg (0.2mmol) of chain transfer agent CDB and 0.0016g (0.01mmol) of initiator AIBN were added, placed in After continuous freezing and thawing and degassing for 3 to 5 times in the RAFT tube, polymerize at 65°C under the protection of inert gas argon. After reacting for 12 to 48 hours, quench with liquid nitrogen to stop the reaction. Use methanol and ethyl acetate as the first precipitant The ester blend (the volume ratio of methanol to ethyl acetate is 8:1) is precipitated repeatedly 3 times to obtain a macromolecular chain transfer agent with a degree of polymerization of 15, namely PMAPOSS 15 ;

[0041] 2) Synthesis of reactive flame retardant block copolymer: the PMAPOSS obtained in step 1) 15 0.44g (0.03mmol), MOEP 0.48g (2.4mmol), St 0.38ml (3.6mmol), initiator AIBN 1mg (0.006mmol) were dissolved in 3ml of the second solvent anh...

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Abstract

The invention discloses a reactive flame-retardant block copolymer and a preparing method thereof. The preparing method includes: using MA POSS (methacryloxy polyhedral oligomeric silsesquioxane) as a fist block monomer, synthesizing macromolecular chain transfer agent PMAPOSSm by means of RAFT (reversible addition fragmentation transfer) polymerization, and making the macromolecular chain transfer agent into a polymer system with MOEP, monomer styrene and initiator; dissolving the polymer system in solvent for RAFT polymerization so as to obtain the reactive flame-retardant block copolymer containing phosphorus and silicon. The hydroxyethyl methacrylate of flame retardance and oligomeric silasesquioxane of polyhedral structure are added to styrene, phosphorus and silicon are jointly bonded to molecular chains of polystyrene, and the reactive flame-retardant block copolymer is obtained; synergistic flame retardance is achieved; the preparation process has mild conditions, the operating is simple, the content of phosphorus, silicon and styrene can be adjusted through controlling a feed ratio, and after reactively doped with matrix resin, the reactive flame-retardant block copolymer has good application prospect in the fields such as halogen-free flame retardance.

Description

technical field [0001] The invention belongs to the field of polymer halogen-free flame retardant, and relates to a reactive block copolymer, in particular to a reactive flame retardant block copolymer with flame retardant function and a preparation method thereof. Background technique [0002] Although traditional halogenated flame retardants, especially brominated flame retardants, have good flame retardant effects and are widely used, studies have found that brominated dibenzodioxins, polybrominated diphenyl And toxic substances such as furan, which greatly restricts the application and development of halogenated flame retardants. Therefore, in order to protect the environment and people's health, the establishment of a new efficient, halogen-free, non-toxic flame retardant system has become a new direction of flame retardant scientific research. [0003] As we all know, traditional halogen-free flame retardant systems are related to P, Si, and N elements, which can effe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F230/02C08F230/08C08F212/08
Inventor 戴李宗叶华立袁丛辉许一婷李远源陈显明罗伟昂陈国荣毛杰
Owner XIAMEN UNIV
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