Preparation method of POSS modified polyurethane resin

A polyurethane resin and modification technology, which is applied in the field of preparation of POSS modified polyurethane resin, can solve the problems of affecting physical and mechanical properties, destroying polyurethane crystallization, insufficient wear resistance, etc., and achieves overcoming compatibility problems and high tensile strength , the effect of high impact strength

Inactive Publication Date: 2015-05-06
JIAXING HEXIN CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ordinary polyurethane resins often have problems such as insufficient wear resistance and poor heat resistance, and compatibility problems are likely to occur when inorganic nanoparticles such as silica are used for modification, and silicone modification will destroy polyurethane molecules. Crystallization, affecting its physical and mechanical properties

Method used

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  • Preparation method of POSS modified polyurethane resin
  • Preparation method of POSS modified polyurethane resin
  • Preparation method of POSS modified polyurethane resin

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preparation example Construction

[0014] The preparation method of this POSS modified polyurethane resin comprises the following steps:

[0015] (1) Under the protection of nitrogen, add trihydroxy heptapolysiloxane (R 7 Si 7 o 9 (OH) 3 ), triethylamine and tetrahydrofuran, and then slowly inject SiCl 4 After stirring overnight, the Et was removed by filtration 3 NHCl, the filtrate rotary evaporation, obtains compound 1 chloride POSS ((i-C 4 h 9 ) 7 Si 7 o 12 Cl). Its reaction formula is as follows:

[0016]

[0017] where R is i-C 4 h 9 、CH 3 、C 6 h 5

[0018] (2) Compound 1 (R 7 Si 8 o 12 Cl) in THF / H 2 O mixed solution was refluxed for 72-90h, and after the solvent was removed by rotary evaporation, compound 2 hydroxylated POSS (R 7 Si 8 o 12 (OH)). Its reaction formula is as follows:

[0019]

[0020] (3) Under nitrogen protection, compound 2 hydroxylated POSS (R 7 Si 8 o 12 (OH)), tetrahydrofuran, triethylamine, and then slowly add dimethyl monochlorosilane, a white preci...

Embodiment 1

[0038] (1) Under the protection of nitrogen, add trihydroxyheptaisobutyl heptapolysiloxane (i-C 4 h 9 ) 7 Si 8 o 9 (OH) 3 (97g, 100mmol), triethylamine (30.3g, 100mmol) and tetrahydrofuran (250ml), then slowly inject SiCl 4 (17g, 100mmol) After stirring overnight, the precipitate was removed by filtration, and the filtrate was rotary evaporated to obtain 73g of compound 1 POSS chloride ((i-C 4 h 9 ) 7 Si 8 o 12 Cl).

[0039] (2) 73g compound 1 chloride POSS ((i-C 4 h 9 ) 7 Si 8 o 12 Cl) in a mixed solution of tetrahydrofuran (100ml) and water (200ml) was refluxed for 78h, and after the solvent was removed by rotary evaporation, 68g of compound 2 hydroxylated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 (OH)).

[0040] (3) Under nitrogen protection, compound 2 hydroxylated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 (OH)) (65g, 78mmol), tetrahydrofuran (250ml), triethylamine (23g, 230mmol), then slowly add dimethyl monochlorosilane (7.38g, 78mmol), it can be seen that a white pre...

Embodiment 2

[0047] (1) Under the protection of nitrogen, add trihydroxyheptaisobutyl heptapolysiloxane (i-C 4 h 9 ) 7 Si 8 o 9 (OH) 3 (79g, 100mmol), triethylamine (33.3g, 110mmol) and tetrahydrofuran (250ml), then slowly inject SiCl 4 (20.4g, 120mmol) After stirring overnight, the precipitate was removed by filtration, and the filtrate was rotary evaporated to obtain 78g of compound 1 POSS chloride ((i-C 4 h 9 ) 7 Si 8 o 12 Cl).

[0048] (2) 78g compound 1 chloride POSS ((i-C 4 h 9 ) 7 Si 8 o 12 Cl) in a mixed solution of tetrahydrofuran (100ml) and water (200ml) was refluxed for 90h, and after the solvent was removed by rotary evaporation, 74g of compound 2 hydroxylated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 (OH)).

[0049](3) Under nitrogen protection, compound 2 hydroxylated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 (OH)) (65g, 78mmol), tetrahydrofuran (250ml), triethylamine (23g, 230mmol), and then slowly add dimethyl monochlorosilane (8.86g, 93.6mmol), a white precipitate can ...

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Abstract

A preparation method of POSS (polyhedral oligomeric silsesquioxane) modified polyurethane resin comprises the following steps: preparing POSS diol by using trihydroxy cage-like siloxane heptamer, triethylamine, tetrahydrofuran, SiCl4, dimethylchlorosilane, tetrahydrophthalic anhydride, LiAlH4 and potassium sodium tartrate; and polymerizing the POSS diol, polyether diol, polyester diol and isocyanate to obtain the POSS modified polyurethane resin. The method allows the novel POSS modified polyurethane resin to be obtained by using the POSS diol, and can effectively overcome the compatibility problem existing in the modification of common inorganic substances; and the obtained POSS modified polyurethane resin has large tensile strength, impact strength, shearing strength and other mechanical performances, and also has the advantages of low surface energy, good heat resistance and good wear resistance.

Description

technical field [0001] The invention relates to a preparation method of polyurethane resin, in particular to a preparation method of POSS modified polyurethane resin. Background technique [0002] Polyurethane is the abbreviation of polyurethane, which means that the main chain of the macromolecule contains repeated urethane units. In addition to containing a large number of urethane bonds, it may also contain ester bonds, ether bonds, urea bonds, and allophanic acid. Ester bonds, isocyanurate bonds, hydrogen bonds between macromolecules, etc. Polyurethane is a block polymer composed of flexible soft segments composed of polyester or polyether and rigid hard segments such as carbamate and urea groups alternately connected; due to the thermodynamic incompatibility of soft and hard segments, soft Segment and hard segment aggregate in the polymer respectively to form soft segment phase and hard segment phase, and microphase separation occurs. Due to the unique microphase sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/61C08G18/48C08G18/42C08G18/12
CPCC08G18/12C08G18/4009C08G18/4238C08G18/44C08G18/4854C08G18/61C08G18/6511C08G18/664
Inventor 沈连根郦聪张勇徐欣欣石磊纪尚超沈建峰沈雁宾李寿伟息锁柱赵磊
Owner JIAXING HEXIN CHEM IND
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