Preparing method of POSS modified poly-butylene succinate

A polybutylene succinate and modification technology is applied in the field of preparation of biodegradable modified polyester, can solve the problems of heat resistance, poor water resistance and stain resistance, etc., and achieves good heat resistance, The effect of excellent wear resistance and high flexural strength

Inactive Publication Date: 2017-04-19
SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The problem solved by the present invention is PBS polyester mechanical properties, heat resistance and water resistance, poor prob...

Method used

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  • Preparing method of POSS modified poly-butylene succinate
  • Preparing method of POSS modified poly-butylene succinate
  • Preparing method of POSS modified poly-butylene succinate

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preparation example Construction

[0019] The preparation method of the POSS modified polybutylene succinate that the embodiment of the present invention provides comprises:

[0020] Step 1, under normal temperature trihydroxy heptapolycrate siloxane R 7 Si 8 o 9 (OH) 3 with SiCl 4 React in the solution of THF for more than 12h, then filter and dry to obtain POSS(R 7 Si 8 o 12 Cl) (wherein R is i-C 4 h 9 、CH 3 、C 6 h 5 One of them), during the reaction R 7 Si 8 o 9 (OH) 3 with SiCl 4 The molar ratio is set to 1:(1~1.3); among them, trihydroxyheptapolysiloxane R 7 Si 8 o 9 (OH) 3 The molecular structure is:

[0021]

[0022] Chlorinated POSS(R 7 Si 8 o 12 The molecular structure of Cl) is:

[0023]

[0024] Step 2, the chlorinated POSS powder is refluxed 100h in tetrahydrofuran and water mixed solvent, after rotary evaporation back drying, obtain hydroxylated POSS (R 7 Si 8 o 12 (OH)); molecular structure is:

[0025]

[0026] Step 3. Under the protection of nitrogen, react t...

Embodiment 1

[0035] Trihydroxyheptaisobutyl polycrate siloxane (i-C 4 h 9 ) 7 Si 8 o 9 (OH) 3 with SiCl 4 React in a tetrahydrofuran solution at a ratio of 1:1 for more than 12h, filter and dry to obtain the chlorinated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 Cl); The chlorinated POSS powder is refluxed 100h in tetrahydrofuran and water mixed solvent, makes hydroxylation POSS ((i-C 4 h 9 ) 7 Si 8 o 12 (OH)); Under the protection of nitrogen, the hydroxylated POSS and dimethyl monochlorosilane were reacted with triethylamine at 60° C. as a catalyst for 20 h at a ratio of 1:1, and then deionized water, 5% hydrochloric acid solution Wash with saturated NaCl solution, and obtain alkylated POSS ((i-C 4 h 9 ) 7 Si 8 o 12 Si(CH 3 ) 2 H); the toluene solution of alkylated POSS and tetrahydrophthalic anhydride THPA (the molar ratio is 1:1) is mixed, and Pt is used as a catalyst, reacted for 60h at 60°C, then rotary steamed, reflux washed, and dried to prepare Acid anhydride POSS ((i-C ...

Embodiment 2

[0038] Trihydroxyheptamethyl clathrosiloxane (CH 3 ) 7 Si 8 o 9 (OH) 3 with SiCl 4 With the ratio of 1:1.3, react in tetrahydrofuran solution for more than 12h, filter and dry to obtain chlorinated POSS ((CH 3 ) 7 Si 8 o 12 Cl); The chlorinated POSS powder is refluxed 100h in tetrahydrofuran and water mixed solvent, makes hydroxylated POSS ((CH 3 ) 7 Si 8 o 12 (OH)); Under the protection of nitrogen, the hydroxylated POSS and dimethyl monochlorosilane were reacted with triethylamine as a catalyst for 20 h at 70 ° C in a ratio of 1:1.2, and then deionized water, 5% hydrochloric acid solution Wash with saturated NaCl solution, and obtain alkylated POSS ((CH 3 ) 7 Si 8 o 12 Si(CH 3 ) 2 H); Mix the toluene solution of alkylated POSS and tetrahydrophthalic anhydride THPA (the molar ratio is 1:1.05), use Pt as the catalyst, react for 60h at 70°C, then rotary steam, reflux washing, and drying to prepare Acid anhydride POSS ((CH 3 ) 7 Si 8 o 12 Si(CH 3 ) 2 THPA...

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Abstract

The invention relates to a preparing method of polyhedral oligomeric silsesquioxane(POSS) modified poly-butylene succinate (PBS). 3-hydroxy siloxane heptamer cage-like siloxane, triethylamine, tetrahydrofuran, SiCl4, dimethyl chlorosilane, tetralin phthalic anhydride, LiAlH4 and potassium sodium tartrate are used for preparing POSS dihydric alcohol; and the POSS dihydric alcohol, succinic acid and butanediol are subject to esterification-polycondensation, and POSS modified PBS polyester is obtained. In the preparing method, the POSS dihydric alcohol is prepared, the hydroxyl reaction activity is achieved, and the problem about consistency in common inorganic substance modification can be effectively solved. The modified material has the mechanical property better than that of original PBS, for example, the tensile strength, the impact strength and the bending strength are high; and the preparing method has the beneficial effects that the surface energy is low, the heat resistance is good, and the abrasive resistance is excellent.

Description

technical field [0001] The invention relates to a preparation method of biodegradable modified polyester, in particular to a preparation method of POSS modified polybutylene succinate. Background technique [0002] Polybutylene succinate (PBS) is a linear high polymer with succinic acid and butanediol as the basic synthetic raw materials and a large number of ester groups in the main chain. The raw materials of PBS can be completely obtained from nature, and its products can be completely degraded under the action of moisture and mold in nature, and have excellent biodegradable properties. In the degradable polyester family, PBS has good mechanical properties and crystallization properties, and can replace traditional plastics such as polypropylene and polyethylene in many areas of life. At present, PBS has been widely used in the fields of film, fiber, plate, coating and so on. However, compared with traditional plastics, the melting point of PBS is only 115°C, the heat r...

Claims

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Application Information

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IPC IPC(8): C08G63/695C08G77/38C08G77/04
CPCC08G63/6956C08G77/045C08G77/38
Inventor 张崇印龚菊贤何腾锋连爱珍堵同亮于文凯徐世俊郝冬冬韩亚刚玉钰奉
Owner SHANGHAI AEROSPACE EQUIP MFG GENERAL FACTORY
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