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Method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof

A polyester polyol, castor oil-based technology, applied in the preparation of structural flame-retardant castor oil-based polyester polyol and its application field, can solve the difficulties in the synthesis of tribromostyrene, harsh reaction conditions, and corrosion of foaming equipment In order to achieve the effects of low cost, low smoke density and improved flame retardant performance

Inactive Publication Date: 2012-05-02
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the homopolymer and the copolymer of polyethylene, vinylidene chloride are unstable, emit poisonous HCl gas in foaming process, have corrosivity to foaming equipment; Acrylonitrile mixed monomers are copolymerized to prepare flame-retardant polyols. The polyurethane foams produced by it have certain flame retardancy, but the synthesis of tribromostyrene is difficult and expensive
Patent 200910024675.9 discloses a structural flame-retardant castor oil-based polyol; however, its preparation process requires a bromination reaction, which requires relatively harsh reaction conditions

Method used

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  • Method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof
  • Method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof
  • Method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: put 100g castor oil into the reactor, carry out alcoholysis reaction with 20g glycerol, catalyst calcium hydroxide 1g, reaction temperature is 200 ℃, keep warm for 1h, heat up to 220 ℃ keep warm for 2 hours. Gradually lower the temperature to 150°C, add 70g of tetrabromophthalic anhydride and 0.5g of tetrabutyl titanate, control the outlet water temperature to less than 100°C, slowly continue to heat up to 220°C, and then continue to react at 220-240°C for 4 hours. When the temperature is about 10 mg / g, cool down to 180°C, vacuumize, gradually increase the vacuum degree to 95 kPa, and vacuumize for about 1 h to end the reaction. The acid value of the obtained product was 1.0 mg / g KOH, the hydroxyl value was 340 mgKOH / g, the content of bromine in the product was 25 wt%, and the appearance of the product was a viscous brown-yellow liquid. Then obtain the combined polyol according to the preparation formula of rigid polyurethane foam in Table 1, stir at high ...

Embodiment 2

[0043] Example 2: Put 100g of castor oil into a reactor, carry out alcoholysis reaction with 35g of pentaerythritol, catalyst sodium methoxide 1g, reaction temperature is 180°C, keep warm for 1h, heat up to 230°C and keep warm for 2 hours. Gradually lower the temperature to 160°C, add 50g of tetrabromophthalic anhydride and 0.6g of tetraisopropyl titanate, control the outlet water temperature to less than 100°C, slowly continue to heat up to 220°C, and then continue to react at 220-240°C for 5 hours, when the acid value When the temperature is about 10 mg / g, cool down to 180°C, vacuumize, gradually increase the vacuum degree to 95 kPa, and vacuumize for about 2 h to end the reaction. The acid value of the obtained product is 0.8mg / g KOH, the hydroxyl value is 420mgKOH / g, the content of bromine in the product is 20wt%, and the appearance of the product is viscous brown-yellow liquid. Then obtain the combined polyol according to the preparation formula of rigid polyurethane foam...

Embodiment 3

[0044] Example 3: Put 100g castor oil into the reactor, carry out alcoholysis reaction with 50g trimethylolpropane, catalyst zinc oxide 2g, reaction temperature is 210°C, keep warm for 4h, heat up to 240°C and keep warm for 2 hours. Gradually lower the temperature to 170°C, add 90g of tetrabromophthalic anhydride and 1.0 g of p-toluenesulfonic acid, control the outlet water temperature to less than 100°C, slowly continue to heat up to 220°C, and then continue to react at 220-240°C for 5 hours, when the acid value is 10 When the concentration is about mg / g, cool down to 180°C, vacuumize, gradually increase the vacuum to 95 kPa, and vacuumize for about 1 h to end the reaction. The acid value of the obtained product was 1.2mg / g KOH, the hydroxyl value was 230mgKOH / g, the content of bromine in the product was 28wt%, and the appearance of the product was viscous brown-yellow liquid. Then obtain the combined polyol according to the preparation formula of rigid polyurethane foam in T...

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Abstract

The invention relates to a method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof. The method comprises the following steps: castor oil and small-molecular alcohol generate alcoholysis reaction under the existence of an alkali catalyst, and then generate esterification reaction with tetrabromophthalic anhydride under the existence of an esterification catalyst, and the flame-retardant castor-oil-based polyester polyol is obtained, wherein the hydroxyl value is 100-450mg / gKOH, the acid value is less than or equal to 1.5mg / gKOH and the content of bromine is 5-30wt%. In the method, the middle process does not need to be separated, the cost is low and the process is simple, and the flame retardance of the prepared polyurethane foam is obviously improved. The prepared polyurethane foam has the advantages of no liquid drop of a product in burning, shape maintenance, less smoke density and the like and can be used for buildings, insulation and certain special fields.

Description

technical field [0001] The invention relates to the preparation of a structural flame-retardant castor oil-based polyester polyol and its application in polyurethane foam, mainly relating to the preparation of a flame-retardant castor oil-based polyester polyol and its use as a polyol component in polyurethane Application in foam. [0002] Background technique [0003] Polyurethane is a kind of high polymer containing carbamate group (-NHCOO-) in its molecular chain. With the different raw materials, additives and process conditions during synthesis, products with different properties can be synthesized, such as foam plastics, rubber, coatings, adhesives, elastic fibers, etc. Polyurethane foam is currently the best thermal insulation material in the world. Because developed countries such as Europe and the United States attach great importance to building energy conservation, polyurethane rigid foam has been widely used in roofs, walls, ceilings, floors, doors and windows ...

Claims

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Application Information

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IPC IPC(8): C08G63/49C08G63/672C08G18/68C08G101/00
Inventor 周永红张猛杨晓慧谢友利
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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