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Preparation method of plant-oil-based polyurethane composites modified by dual-layer cage type silsesquioxane

A technology of silsesquioxane and modified vegetable oil, which is applied in the field of preparation of double-layer cage silsesquioxane modified vegetable oil-based polyurethane composite materials, can solve the problems of difficult biodegradation and toxicity, and achieve thermal stability And the effect of water resistance improvement

Active Publication Date: 2016-08-17
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthetic raw materials of traditional polyurethane come from petrochemical products, which will inevitably bring about some environmental and product safety problems in the production process, such as toxicity, refractory biodegradation, etc.

Method used

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  • Preparation method of plant-oil-based polyurethane composites modified by dual-layer cage type silsesquioxane
  • Preparation method of plant-oil-based polyurethane composites modified by dual-layer cage type silsesquioxane
  • Preparation method of plant-oil-based polyurethane composites modified by dual-layer cage type silsesquioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of soybean oil polyol: Add 100g of soybean oil and 43.4g of ethylene glycol into a 250mL single-necked flask, and add 0.14g of fluoboric acid while stirring. After reacting at 98°C for 2 hours, cool to room temperature, extract with ethyl acetate, wash the upper layer solution with saturated NaCl solution and deionized water for 3 times, and evaporate the obtained solution in vacuum at 0.8MPa and 80°C to obtain the desired soybean oil polyols;

[0029] According to the measuring method of hydroxyl value, record its hydroxyl value to be 192mg KOH / g.

[0030] (2) Preparation of double cage silsesquioxane DDSQ:

[0031] Hydrolysis of phenyltrimethoxysilane under alkaline conditions to generate incompletely condensed DDSQ tetraol sodium salt Na 4 o 14 Si 8 (C 6 h 5 ) 8 : Add 35g of phenyltrimethoxysilane, 150mL of isopropanol, 5g of deionized water and 6g of solid NaOH in sequence in a flask equipped with a condenser and magnetic stirring, reflux at 7...

Embodiment 2

[0060] (1) Preparation of vegetable oil-based polyol: the same as in Example 1.

[0061] (2) Preparation of double cage silsesquioxane DDSQ: the same as in Example 1.

[0062] (3) Preparation of vegetable oil-based polyurethane composite material: 4 g of soybean oil polyol, 1.98 mL of IPDI and 160 μL of stannous octoate were added to a 100 mL three-neck flask, and 30 mL of ethyl acetate was added under stirring. Install the condenser tube, in N 2 Under the atmosphere, after reacting at 80°C for 2 hours, the isocyanate value after the reaction was titrated by the di-n-butylamine toluene method. After calculating the chain extension coefficient of 1.05, add 0.2g DDSQ and 0.844g chain extender 1,4-butanediol, 80 The reaction was continued for 2 h at ℃ to obtain a polyurethane composite solution.

[0063] (4) Drying to form a film: apply the polyurethane composite solution prepared in step (3) on a polytetrafluoroethylene board and let it stand for 10 hours. Let the solvent ethy...

Embodiment 3

[0065] (1) Preparation of vegetable oil-based polyol: the same as in Example 1.

[0066] (2) Preparation of double cage silsesquioxane DDSQ: the same as in Example 1.

[0067] (3) Preparation of vegetable oil-based polyurethane composite material: 4 g of soybean oil polyol, 1.98 mL of IPDI and 160 μL of stannous octoate were added to a 100 mL three-neck flask, and 30 mL of ethyl acetate was added under stirring. Install the condenser tube, in N 2 Under the atmosphere, after reacting at 80°C for 2 hours, the isocyanate value after the reaction was titrated by the di-n-butylamine toluene method. After calculating the chain extension coefficient of 1.05, add 0.4g DDSQ and 0.704g chain extender 1,4-butanediol, 80 The reaction was continued for 2 h at ℃ to obtain a polyurethane composite solution.

[0068] (4) Drying to form a film: apply the polyurethane composite solution prepared in step (3) on a polytetrafluoroethylene board and let it stand for 12 hours, let the solvent ethy...

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Abstract

The invention discloses a preparation method of plant-oil-based polyurethane composites modified by dual-layer cage type silsesquioxane, and belongs to the technical field of polymer composites. Plant-oil-based polyurethane is synthesized with plant-oil-based polyhydric alcohol and isophorone diisocyanate (IPDI) as the raw materials, and a series of plant-oil-based polyurethane composites are synthesized with organic-inorganic hybrid material dual-layer cage type silsesquioxane (DDSQ) as the modifier. Environment-friendly renewable plant-oil-based polyhydric alcohol serves as the raw material, the composites are chemically modified by dual-layer silsesquioxane of a regular cage type structure for overcoming the defects of plant-oil-based polyurethane, and the thermal performance, mechanical performance and water resistance of the modified composites are improved to different extents. Compared with ordinary plant-oil-based polyurethane, the initial decomposition temperature of the composites is increased by 31 DEG C, and the tensile strength is improved by nearly four times.

Description

technical field [0001] The invention relates to a preparation method of a double-layer cage-type silsesquioxane modified vegetable oil-based polyurethane composite material, which belongs to the technical field of polymer composite materials. Background technique [0002] As one of the six major synthetic materials in the world today, polyurethane has good physical and chemical properties, making it widely used in the preparation of soft and hard foams, coatings, adhesives, sealants, elastomers, leather and fibers. However, the synthetic raw materials of traditional polyurethane come from petrochemical products, which will inevitably bring about some environmental and product safety problems in the production process, such as toxicity and refractory biodegradation. In contrast, vegetable oil is recognized as the best substitute for petroleum raw materials because of its cheapness, availability, renewability and biodegradability. At the same time, the proposal of a variety o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/75C08G18/61C08G18/36C08G18/32C08G77/04
CPCC08G18/10C08G18/36C08G18/755C08G77/045C08G18/61C08G18/3206
Inventor 蒋平平黄杰闻月
Owner JIANGNAN UNIV
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