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Hyperbranched polysiloxane and preparation method thereof

A technology of polysiloxane and trialkoxysilane, which is applied in the fields of hyperbranched polymers and their synthesis, hyperbranched polysiloxanes and their preparation, can solve the problem of limited improvement in flame retardancy and reduction in mechanical properties and other properties. , flame retardant performance and other issues, to achieve the effects of improved mechanical properties, improved limiting oxygen index, and wide applicability

Inactive Publication Date: 2013-05-22
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods of preparing silicon-phosphorus synergistic flame retardants include physical blending or intrinsic type. The disadvantage of the former is that it has poor compatibility with polymers, which not only reduces mechanical properties, but also leads to limited improvement in flame retardancy.
For example, Chinese invention patents "flame retardant polymer composition" (CN1143658) and "flame retardant polycarbonate composition with phosphorus-silicon compound" (CN1720293) disclose methods for preparing phosphorus-containing silicon flame retardants, but due to Poor compatibility affects its flame retardant performance

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
Comparison scheme
Effect test

Embodiment 1

[0026] After mixing 1.98g of distilled water with 28.0g of vinyl-tris(2-methoxyethoxy)silane (0.1mol vinyl content), slowly add 1mL of 36.5% mass concentration of HCl; After the dropwise addition, the temperature was raised to 50° C. to continue the reaction for 4 hours; after the reaction was completed, vacuum drying was carried out to obtain a transparent and viscous vinyl-containing hyperbranched polysiloxane.

[0027] The prepared vinyl-containing hyperbranched polysiloxane (vinyl content 0.1mol), 2.16g (0.01mol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxidized After the compound was mixed evenly with 120mL of propanol, 0.4g of azobisisobutyronitrile was added, heated to 95°C and continued to react for 5 hours, and the crude product was obtained by distillation under reduced pressure.

[0028] After the crude product is purified, filtered, vacuum-distilled, and vacuum-dried, a hyperbranched polysiloxane containing a phosphaphenanthrene structure and a vinyl group i...

Embodiment 2

[0046] Take 3.24g of distilled water and 28.0g (0.1mol vinyl content) of vinyl-tris(2-methoxyethoxy)silane and mix evenly, then slowly add 1mL of 36.5% HCl dropwise at room temperature with stirring; After the dropwise addition, the temperature was raised to 70° C. to continue the reaction for 4 hours; after the reaction was completed, vacuum drying was carried out to obtain a transparent and viscous vinyl-containing hyperbranched polysiloxane.

[0047] Get all the above-mentioned vinyl-containing hyperbranched polysiloxanes (0.1mol vinyl content), 18.44g (0.09mol) 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and After mixing 120mL of ethanol evenly, add 0.6g of azobisisoheptanonitrile, heat to 100°C and continue the reaction for 10 hours, and distill under reduced pressure to obtain the crude product;

[0048] After the crude product is purified, filtered, distilled under reduced pressure and dried in vacuum, the hyperbranched polysiloxane containing phosphaphenanthrene...

Embodiment 3

[0050] Take 2.34g of distilled water and 28.0g (0.1mol vinyl content) of vinyl-tris(2-methoxyethoxy)silane and mix evenly, then slowly add 1mL of 36.5% HCl dropwise at room temperature with stirring; After the dropwise addition, the temperature was raised to 55° C. to continue the reaction for 5 hours; after the reaction was completed, vacuum drying was carried out to obtain a transparent and viscous vinyl-containing hyperbranched polysiloxane.

[0051] Take all the above vinyl-containing hyperbranched polysiloxane (0.1mol vinyl content), 8.44g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and mix with 120mL propanol After uniformity, add 0.1 g of azobisisobutylcyanide, heat to 100°C and continue the reaction for 7 hours, and distill under reduced pressure to obtain the crude product;

[0052] After the crude product is purified, filtered, distilled under reduced pressure and dried in vacuum, the hyperbranched polysiloxane containing phosphaphenanthrene structure and viny...

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Abstract

The invention discloses a phosphaphenanthrene structure and vinyl containing-hyperbranched polysiloxane and a preparation method thereof. The preparation method comprises the steps of evenly mixing distilled water with vinyl-containing trialkoxysilane, dropwise adding catalyst slowly under the stirring condition, and increasing temperature to 50-60 DEG C, thus obtaining vinyl-containing hyperbranched polysiloxane; and mixing the vinyl-containing hyperbranched polysiloxane with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, adding initiator and alcohol solvent, increasing temperature to 95-100 DEG C, and carrying out purification, filtering, reduced pressure distillation and vacuum drying after reaction is finished, thus obtaining phosphaphenanthrene structure and vinyl containing-hyperbranched polysiloxane. The phosphaphenanthrene structure and vinyl containing-hyperbranched polysiloxane integrates molecular properties of hyperbranched polysiloxane, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and vinyl, thus having wide application prospects on polymer modification aspect. The preparation method adopted has the advantages of wide applicability and simple operation process.

Description

technical field [0001] The invention relates to a hyperbranched polymer and its synthesis, in particular to a hyperbranched polysiloxane containing a phosphaphenanthrene structure and a vinyl group and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Flame-retardant polymer materials occupy an important position in today's industrial field. Flame-retardant polymer materials are divided into intrinsic type and additive type. The former refers to starting from the structural design and synthesis of polymer chains, so that the polymer itself has good flame retardancy. However, this flame-retardant polymer It is difficult to prepare and the research and development cycle is long. The additive polymer material is the method of adding a flame retardant to the polymer. It has the advantages of short development cycle and strong designability. Therefore, it has become a common method for the research and development ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/395C08G77/20
Inventor 顾嫒娟张志勇梁国正徐静冒飞燕卓东贤袁莉
Owner SUZHOU UNIV
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