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Hyperbranched polysiloxane and preparation method thereof

A technology of polysiloxane and trialkoxysilane is applied in the field of hyperbranched polymer and preparation thereof, modified hyperbranched polysiloxane and preparation thereof, can solve problems such as unreported technology, and achieve operation Simple process, broad application potential, wide applicability effect

Inactive Publication Date: 2011-09-28
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, no relevant technology has been reported

Method used

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  • Hyperbranched polysiloxane and preparation method thereof
  • Hyperbranched polysiloxane and preparation method thereof
  • Hyperbranched polysiloxane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 4.7g of distilled water and 47.5g of 3-glycidyl etheroxypropyltrimethoxysilane and mix evenly, then slowly add 1mL of HCl with a concentration of 36.5% dropwise at room temperature and under stirring; React for 4 hours; after the reaction is complete, vacuum-dry to obtain transparent and viscous hyperbranched polysiloxane containing epoxy groups.

[0028] Take 20g of the above-mentioned epoxy-containing hyperbranched polysiloxane, mix 7.5g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with 120mL propanol, add triphenyl Base phosphorus 0.3g, heated to 97°C and continued to react for 12 hours, then raised the temperature to 99°C, kept the temperature for 5 hours, and distilled under reduced pressure to obtain the crude product;

[0029] Purify the crude product, first dissolve it in a mixture of toluene, carbon tetrachloride, chloroform and dichloromethane, filter to remove the insoluble matter, then distill under reduced pressure and vacuum dry to obtain a Hyp...

Embodiment 2

[0040] Take 4.7g of distilled water and 47.5g of 3-glycidyl etheroxypropyltrimethoxysilane and mix evenly, slowly add 1mL of 33.5% H 2 SO 4 After the dropwise addition, the temperature was raised to 55° C. to continue the reaction for 4 hours; after the reaction was completed, vacuum drying was carried out to obtain a transparent and viscous hyperbranched polysiloxane containing epoxy groups.

[0041] Take 20g of the above-mentioned epoxy-containing hyperbranched polysiloxane, mix 7.5g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with 120mL propanol, add triphenyl Base phosphorus 0.3g, heated to 97°C and continued to react for 12 hours, then raised the temperature to 95°C, kept the temperature for 8 hours, and distilled under reduced pressure to obtain the crude product;

[0042] After the crude product is purified, filtered, distilled under reduced pressure and dried in vacuum, the hyperbranched polysiloxane containing phosphaphenanthrene structure and epoxy group is o...

Embodiment 3

[0044] Take 4.7g of distilled water and 47.5g of 3-glycidoxypropyltrimethoxysilane and mix evenly, then slowly add 1mL of HCl with a concentration of 36.5% dropwise at room temperature and under stirring; React for 4 hours; after the reaction is complete, vacuum-dry to obtain transparent and viscous hyperbranched polysiloxane containing epoxy groups.

[0045] Take 20g of the above-mentioned hyperbranched polysiloxane containing epoxy groups, mix 7.5g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with 120mL methanol, add triphenyl Phosphorus 0.6g, heated to 97°C and continued to react for 12 hours, then raised the temperature to 95°C, kept the temperature for 8 hours, and distilled under reduced pressure to obtain the crude product;

[0046] Dissolve the crude product in a mixture of toluene and chloroform, filter to remove insoluble matter, and then distill under reduced pressure and dry in vacuum to obtain a hyperbranched polysiloxane containing a phosphaphenanthrene str...

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Abstract

The invention discloses hyperbranched polysiloxane and a preparation method thereof. The hyperbranched polysiloxane contains a phosphaphenanthrene structure and an epoxy group simultaneously. The preparation method comprises the following steps of: mixing distilled water and epoxy group-containing trialkoxysilane uniformly according to a molar ratio, adding a catalyst A slowly and dropwise under the condition of stirring, and performing a reaction to obtain epoxy group-containing hyperbranched polysiloxane; mixing the epoxy group-containing hyperbranched polysiloxane and a certain amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide; and mixing the mixture and a catalyst B and alcohol solvent, and purifying, filtering and vacuumizing a crude product to obtain the hyperbranched polysiloxane containing the phosphaphenanthrene structure and the epoxy group. The hyperbranched polymer integrates the molecular characteristics of the hyperbranched polysiloxane, the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the epoxy group, and has the huge application potential in the modification aspect. The preparation method has the characteristics of wide applicability and simpleoperational process.

Description

technical field [0001] The invention relates to a hyperbranched polymer and a preparation method thereof, in particular to a modified hyperbranched polysiloxane and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] In terms of improving the flame retardancy of polymers, at present, adding halogen-free flame retardants is a general and effective method. See the literature "A new intumescent flame-retardant: preparation, surface modification, and its application in polypropylene" (X.Y.Wang, Y.Li, W.W.Liao, J.Gu, Polym.Adv.Technol., 2008, 19, 1055-1061. ) and "On the intumescence of ethylene-acrylate copolymers blended with chalk and silicone" (R.H. Kra¨mer, Blomqvi st., Polym. Degrad. Stab., 2007, 92: 1899-1910.), reported that the main chain is composed of silicon, It is a cross-linked semi-inorganic polymer organosilicon composed of elements such as carbon, oxygen and nitrogen, and connected with organic group...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/395C08G77/14
Inventor 顾嫒娟张志勇梁国正卓东贤袁莉
Owner SUZHOU UNIV
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