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Hyper-branched silicone resin containing active functional group and preparation method thereof

A technology of active functional groups and hyperbranched silicon, which is applied in the field of hyperbranched polymer synthesis, can solve the problems of poor compatibility of thermosetting resins with solubility, limit the application field of hyperbranched polysiloxane, and reduce the storage stability of polymers. Achieve the effects of low production cost, excellent compatibility, and excellent solubility

Inactive Publication Date: 2010-03-03
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to a large amount of alkoxy groups remaining in the resulting hyperbranched polysiloxane, further polymerization tends to occur gradually over time, thereby reducing the storage stability of the polymer; at the same time, a large amount of alkoxy groups The presence of hyperbranched polysiloxane greatly increases the polarity of the hyperbranched polysiloxane, making it less soluble and less compatible with thermosetting resins (such as insoluble in toluene, incompatible with epoxy resin or silicone resin), so , which severely limits the application fields of hyperbranched polysiloxane

Method used

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  • Hyper-branched silicone resin containing active functional group and preparation method thereof
  • Hyper-branched silicone resin containing active functional group and preparation method thereof
  • Hyper-branched silicone resin containing active functional group and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1) Under stirring conditions, after adding 45.00g gamma-glycidoxypropyltrimethoxysilane, 5.15g deionized water and 0.09g tetramethylammonium hydroxide (20% aqueous solution) into the there-necked flask, at 40 Reflux at constant temperature for 2 hours at °C to obtain solution A;

[0038] 2) Under stirring conditions, dissolve 30.89g of trimethylchlorosilane in a mixed solvent of 18.00mL of methanol and 36.00mL of pyridine to obtain solution B;

[0039] 3) Under the conditions of stirring and nitrogen protection, pour solution B into solution A at 60°C, and reflux at constant temperature at 60°C for 6 hours, and obtain the crude product after vacuum distillation;

[0040] 4) After the crude product is dissolved in dichloromethane, the insoluble matter is filtered off, and after vacuum distillation and vacuum drying, the hyperbranched silicone resin containing the active functional group is an epoxy group, and its structural formula is:

[0041]

[0042] Among them, R...

Embodiment 2

[0044] 1) Under stirring conditions, add 45.00g γ-glycidoxypropyltrimethoxysilane, 3.43g deionized water and 0.04g KOH into a three-necked flask, then reflux at 90°C for 8 hours to obtain solution A ;

[0045] 2) Under stirring conditions, dissolve 15.44g of hexamethyldisiloxane in a mixed solvent consisting of 5.00mL of n-butanol and 8.30mL of tetrahydrofuran to obtain solution B;

[0046] 3) Under the conditions of stirring and nitrogen protection, pour solution B into solution A at 60-90°C, and reflux at 90°C for 8 hours, then distill under reduced pressure to obtain the crude product;

[0047] 4) After the crude product is dissolved in dichloromethane, the insoluble matter is filtered off, and after vacuum distillation and vacuum drying, a hyperbranched silicone resin containing an epoxy group as an active functional group is obtained.

Embodiment 3

[0049] 1) Under the conditions of stirring and nitrogen protection, add 45.00g of 3-mercaptopropyltriethoxysilane, 4.46g of deionized water and 0.05g of p-toluenesulfonic acid into a three-necked flask, and then reflux at a constant temperature of 65°C for 4 hours. Obtain solution A;

[0050] 2) Under the conditions of stirring and nitrogen protection, 23.22g of hexamethyldisiloxane was dissolved in a mixed solvent composed of 20.00mL of ethanol and 10.00mL of pyridine to obtain solution B;

[0051] 3) Under the conditions of stirring and nitrogen protection, pour solution B into solution A at 60-65 ° C, reflux at 65 ° C for 7 hours, and obtain the crude product after vacuum distillation;

[0052] 4) After the crude product is dissolved in dichloromethane, the insoluble matter is filtered off, and after vacuum distillation and vacuum drying, a hyperbranched silicone resin containing a mercapto group as an active functional group is obtained.

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Abstract

The invention discloses hyper-branched silicone resin containing active functional group and preparation method thereof. The preparation method comprises following steps : based on mol part, adding 100 parts of alkoxy silanes, 100-150 parts of de-ionized water and 0-0.35 part of catalysts to a reaction container when stirring; reflowing for 2-8h at constant temperature of 40-90 DEG C to obtain solution A; stirring, and dissolving 100-150 parts of blocking agents to a mixed solvent consisting of alcohols and heterocyclic compounds with the volume ratio of 1:2-2:1 to obtain solution B, wherein the volume ratio of the blocking agent to the mixed solvent is 4:6-6:4; stirring, and pouring the solution B to the solution A at 60-90 DEG C, then dissolving a crude product obtained through constant-temperature circumfluence and reduced pressure distillation to aromatics or haloforms solvents, and filtering, carrying out reduced pressure distillation and vacuum drying to obtain the hyper-branchedsilicone resin containing active functional group. The invention has favorable storage stability property, excellent solubility property in low or nonpolar solvents and excellent compatibility with the thermosetting resin, such as epoxy resin, and the like.

Description

technical field [0001] The invention relates to a hyperbranched silicone resin containing active functional groups and a preparation method thereof, belonging to the field of hyperbranched polymer synthesis. Background technique [0002] Silicone resin has the characteristics of both organic resin and inorganic material. Compared with other organic resins, it has excellent heat resistance and weather resistance, excellent electrical insulation, chemical resistance, hydrophobicity and flame retardancy; therefore, Various products such as electrical insulating varnishes, coatings, molding compounds, laminated materials, release agents, and moisture-proof agents prepared with silicone resin as base materials have been widely used in the fields of electronics, electrical appliances, aviation, and construction. [0003] However, the current industrialized silicone resin varieties are only MQ type silicone resin (mainly containing M and Q chain links) and DT type silicone resin (m...

Claims

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Application Information

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IPC IPC(8): C08G77/28C08G77/26C08G77/14C08G77/06
Inventor 梁国正卓东贤顾嫒娟胡江涛
Owner SUZHOU UNIV
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