Block copolymer of polyolefine and phosphorus-containing alkene and preparation method thereof

An olefin block and polyolefin technology, applied in the field of block copolymer and its preparation, can solve the problem of less phosphorus-containing block polymer, and achieve the effects of low cost, wide source of raw materials and excellent flame retardant performance

Inactive Publication Date: 2015-04-29
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies on phosphorus-containing block polymers, and the synthesis methods are basically prepared by the ATRP method.

Method used

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  • Block copolymer of polyolefine and phosphorus-containing alkene and preparation method thereof
  • Block copolymer of polyolefine and phosphorus-containing alkene and preparation method thereof
  • Block copolymer of polyolefine and phosphorus-containing alkene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] In a 100ml three-necked bottle, add 0.300g (0.018mmol) Mn=1.7×10 4 After the benzyl chloride-terminated polypropylene was vacuum-dried at 60°C for 4 hours, 20 ml of toluene was added and stirred to fully dissolve the benzyl chloride-terminated polypropylene, and then 20.1 mg (0.203 mmol) of cuprous chloride, 1,1,4,7,10,10-Hexamethyltriethylenetetramine 45ul (0.17mmol), 5ml (24mmol) comonomer DEVBP, fully deoxygenated, reacted at 90°C for 4h under nitrogen protection. The reaction was quenched by bubbling air and the polymer was precipitated with hexane or heptane. The polyolefin / phosphorus-containing olefin block copolymer is obtained by repeatedly adding dichloromethane or trichloromethane and other halogenated hydrocarbons to dissolve, then precipitating and washing the polymer with hexane or heptane to remove unreacted monomers, filtering and drying.

[0062] 1 H-NMR characterization confirmed that the molar content of phosphorus-containing olefin segments in the c...

Embodiment 2

[0066] In a 100ml three-necked bottle, add 0.300g (0.018mmol) Mn=1.7×10 4 After the benzyl chloride-terminated polypropylene was vacuum-dried at 60°C for 4 hours, 20ml of toluene was added and stirred to fully dissolve the benzyl chloride-terminated polypropylene, and then 20.1mg (0.20mmol) of cuprous chloride (0.20mmol) was added successively. 1,1,4,7,10,10-Hexamethyltriethylenetetramine 45ul (0.19mmol), 5ml (24mmol) comonomer DEVBP, fully deoxygenated, reacted at 90°C for 12h under nitrogen protection. The reaction was quenched by bubbling air and the polymer was precipitated with hexane or heptane. The polyolefin / phosphorus-containing olefin block copolymer is obtained by repeatedly adding dichloromethane or trichloromethane and other halogenated hydrocarbons to dissolve, then precipitating and washing the polymer with hexane or heptane to remove unreacted monomers, filtering and drying.

[0067] 1 H-NMR characterization confirmed that the molar content of phosphorus-cont...

Embodiment 3

[0070] In a 100ml three-necked bottle, add 0.300g (0.018mmol) Mn=1.7×10 4 After the benzyl chloride-terminated polypropylene was vacuum-dried at 60°C for 4 hours, 20ml of toluene was added and stirred to fully dissolve the benzyl chloride-terminated polypropylene, and then 20.1mg (0.20mmol) of cuprous chloride (0.20mmol) was added successively. 1,1,4,7,10,10-Hexamethyltriethylenetetramine 45ul (0.19mmol), 5ml (24mmol) comonomer DEVBP, fully deoxygenated, reacted at 90°C for 18h under nitrogen protection. The reaction was quenched by bubbling air and the polymer was precipitated with hexane or heptane. The polyolefin / phosphorus-containing olefin block copolymer is obtained by repeatedly adding dichloromethane or trichloromethane and other halogenated hydrocarbons to dissolve, then precipitating and washing the polymer with hexane or heptane to remove unreacted monomers, filtering and drying.

[0071] 1 H-NMR characterization confirmed that the molar content of phosphorus-cont...

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Abstract

The invention discloses a block copolymer of polyolefine and phosphorus-containing alkene and a preparation method thereof. The block copolymer has the structural formula (I), wherein R is H or C1-C8 alkyl; when the phosphorus-containing group has the formula (II), R1 and R2 are H or C1-C8 alkyl, and R3, R4 and R5 are all H, C1-C8 alkyl, hydroxyl, carboxyl, nitryl, amino or substitutional groups in the formula (III), and at least one of R3, R4 and R5 is the substitutional group in the formula (III); in the formula (III), Ra is C1-C6 alkyl, alkoxyl or azanyl, Rb and Rc are both C1-C6 alkyl or C6-C18 aryl; and when the phosphorus-containing group has the formula (III), R1 is H or C1-C8 alkyl, R2 is H, C1-C8 alkyl or a C1-C8 ester group, Ra is C1-C6 alkyl, an ester group, alkoxyl or azanyl, and Rb and Rc are both C1-C8 alkyl. The copolymer is obtained by polymerization of phosphorus-containing alkene using polyolefine which acts as a polymer initiator. The block polymer of polyolefine and phosphorus-containing alkene has broad application prospects in the aspect of improving flame retardancy and adhesion property of polyolefine.

Description

technical field [0001] The invention relates to a block copolymer of polyolefin and phosphorus-containing olefin and a preparation method thereof. Background technique [0002] Polyolefins are widely used in daily life, home appliances, textiles, automobiles, construction, agriculture and military due to their rich raw materials, excellent mechanical properties, easy processing, strong electrical insulation, stable chemical properties, low density, and light weight. Applications. However, since the polyolefin macromolecular chain is mainly composed of C and H atoms, it is a non-polar chain, and the semi-crystalline characteristics of polyolefin make its surface energy extremely low, so it is different from most polymers or inorganic materials. It is difficult for fillers to achieve effective compatibility, and it is difficult to ensure the performance of blends or composite materials. In addition, polyolefins belong to hydrocarbon materials and are easy to burn. The oxygen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F230/02
Inventor 董金勇王洪振秦亚伟黄英娟牛慧
Owner INST OF CHEM CHINESE ACAD OF SCI
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