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Halloysite with modified surface and preparation method for halloysite

A technology for surface modification and modification, applied in the field of halloysite modified by hyperbranched polysiloxane, which can solve the problem of low phosphorus content in hyperbranched polysiloxane, achieve excellent reactivity, adhesion, and operating process The effect of simplicity and high flame retardancy

Inactive Publication Date: 2012-06-13
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hyperbranched polysiloxane is a highly branched product with a three-dimensional spherical structure. It has the advantages of low viscosity, good toughness, and good thermal stability. It can be used as a new type of surface modifier and has potential in the surface modification of halloysite. application value, but so far there is no relevant literature report
Chinese invention patent (CN102199294A) discloses a hyperbranched polysiloxane and its preparation method. The preparation method of the hyperbranched polysiloxane is to first prepare a hyperbranched polymer containing Dotted around the hyperbranched polymer, therefore, the obtained hyperbranched polysiloxane has a low phosphorus content, which is not conducive to obtaining excellent flame retardant efficiency at low content

Method used

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  • Halloysite with modified surface and preparation method for halloysite
  • Halloysite with modified surface and preparation method for halloysite
  • Halloysite with modified surface and preparation method for halloysite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Under nitrogen protection, 1.9g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1.9g of vinyltriethoxysilane, 0.08g of Add nitrogen diisoheptanonitrile and 10ml dimethylformamide into the flask, and react at 120°C for 2 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain the phosphaphenanthrenesilane coupling agent.

[0037] (2) Under the protection of nitrogen, add 3g of phosphaphenanthrenesilane coupling agent, 3g of glycidyl etheroxypropyl trimethoxysilane, 0.1g of 36wt% hydrochloric acid, 20ml of deionized water and 7ml of methanol into the flask, at 55℃ After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a hyperbranched polysiloxane containing phosphaphenanthrene and epoxy groups, with a molecular weight of 3020 g / mol and a phosphorus content of 14.7 wt%.

[0038] (3) Add 20g of 5mol / L hydrochloric acid solution and 10g of halloysite into the flask, react at 6...

Embodiment 2

[0047] (1) Under the protection of argon, 2.4g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.9g vinyltriethoxysilane, 0.08g azobisiso Butyronitrile and 10ml of chloroform were added into the flask, and reacted at 60°C for 20 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a phosphaphenanthrenesilane coupling agent.

[0048] (2) Under the protection of argon, add 3g of phosphaphenanthrenesilane coupling agent, 9g of glycidyl etheroxypropyl trimethoxysilane, 0.1g of 36wt% hydrochloric acid, 20ml of deionized water and 28ml of methanol into the flask, and Reacted at 40°C for 8 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a hyperbranched polysiloxane containing phosphaphenanthrene and epoxy groups with a molecular weight of 2820 g / mol and a phosphorus content of 14.5 wt%.

[0049] (3) Add 50g of 1mol / L hydrochloric acid solution and 10g of halloysite into the flask, react at 80°C for 3 h...

Embodiment 3

[0052] (1) Under nitrogen protection, 2.4g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.9g vinyltriethoxysilane, 0.02g azobisiso Butyronitrile, 0.02g of azobisisoheptanonitrile and 10ml of dichloromethane were added to the flask, and reacted at 60°C for 10 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a phosphaphenanthrenesilane coupling agent.

[0053] (2) Under nitrogen protection, add 3g of phosphaphenanthrenesilane coupling agent, 9g of glycidyl etheroxypropyl trimethoxysilane, 0.1g of 36wt% hydrochloric acid, 20ml of deionized water, 14ml of ethanol and 14ml of propanol The flask was reacted at 60°C for 5 hours. After the reaction was over, the solvent was distilled off under reduced pressure to obtain a hyperbranched polysiloxane containing phosphaphenanthrene and epoxy groups. The molecular weight was 2880 g / mol, and the phosphorus content was 14.5wt. %

[0054](3) Add 50g of 3mol / L hydrochloric acid solution and ...

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Abstract

The invention discloses halloysite with a modified surface and a preparation method for the halloysite. A modification object is hyperbranched polysiloxane containing phosphorus and an epoxy group, and the phosphorus content of the modification object is more than 14.5 weight percent. The preparation method comprises the following steps of: mixing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, a vinyl-containing silane coupling agent, an initiator and a solvent, mixing an obtained phosphaphenanthrene silane coupling agent, a silane coupling agent containing an epoxy resin, a catalyst anda solvent, reacting to obtain hyperbranched polysiloxane containing phosphaphenanthrene and the epoxy group, and reacting activated halloysite and the hyperbranched polysiloxane in a solvent to obtain the halloysite with the modified surface. The halloysite with the modified surface has a large number of active groups and a hyperbranched topological structure, has high dispersity in resin matrixes, and has a broad application prospect in the fields of polymer modification, synthesis and preparation of novel polymer materials and multifunctionalization of nano-clay / polymer composite materials.

Description

technical field [0001] The invention relates to a surface modification technology of halloysite, in particular to a method for modifying halloysite with hyperbranched polysiloxane. Background technique [0002] Halloysite (HNTs) is a natural silicate mineral, which is formed by curling kaolinite sheets under natural conditions. Research findings in recent years (see literature: ①Huang Zhifang, Jia Zhixin, Guo Baochun, Jia Demin. Structure and properties of PBT / halloysite nanotube composites[J]. Plastic Industry, 2008, 36, 29–35. ②Ning, N.Y. ; Yin, Q.J.; Luo, F.; Zhang, Q.; Du, R.N.; Fu, Q. Crystallization behavior and mechanical properties of polypropylene / halloysite composites. Polymer 2007, 48, 7374-7384. BC, Yang BT, Du ML, Jia DM. Reinforcing and flame-rotardant effects of halloysite nanotubes on LLDPE. Polym-Plast Technol Eng 2009;48(6):607-13.), as an abundant and cheap Natural nanotubes, halloysite have broad application prospects in improving and improving the ...

Claims

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Application Information

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IPC IPC(8): C08K9/06C08K3/34C08G77/30C08G77/14C09C1/28C09C3/12
Inventor 梁国正叶菊华顾嫒娟袁莉
Owner SUZHOU UNIV
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