Preparation method and applications of synergic oligomeric phosphate ester polyol

A technology of oligomeric phosphate and polyols, which is applied in the field of preparation of synergistic oligomeric phosphate polyols, can solve the problems that the flame retardant ability cannot meet the use requirements, etc., and achieves easy industrial production, low-cost and easy-to-obtain raw materials, Practical effect

Inactive Publication Date: 2016-01-20
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The flame retardant ability of polyurethane foam insulation materials prepared by a single flame re...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1 A kind of preparation method of synergistic oligomeric phosphate polyol

[0034] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 3.0g of water in 5min, heat to 50°C for 40min; add 70g of epichlorohydrin in 5min, and then add 0.25g of catalyst IV Ethyl ammonium bromide; heated to 130°C for 3 hours to obtain phosphate-based polyols;

[0035] 2) Cool to 50°C, add 20g of phosphorus pentoxide, and react for 20min to dissolve completely;

[0036] 3) Add 100g of epichlorohydrin, add 0.8g of catalyst tetraethylammonium bromide, raise the temperature to 115°C, react for 1h, add 40g of tetrabromophthalic anhydride, react for 3h, cool, and discharge to obtain synergistic oligomerization Phosphate polyol; it is a light yellow transparent liquid with an acid value of 11.5mgKOH / g and a viscosity of 9686mPa.s.

Embodiment 2

[0037] Embodiment 2 A kind of preparation method of synergistic oligomeric phosphate polyol

[0038] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 3.5g of water in 12min, heat to 65°C for 50min; add 90g of epichlorohydrin in 7.5min, and then add 0.35g of catalyst Benzyltriethylammonium chloride; heated to 135°C for 3 hours to obtain phosphate-based polyols;

[0039] 2) Cool to 65°C, add 25g of phosphorus pentoxide, and react for 40min to dissolve completely;

[0040] 3) Add 120g of epichlorohydrin, add 0.8-1.3 parts by mass of benzyltriethylammonium chloride, raise the temperature to 120°C, react for 1h, add 50g of tetrabromophthalic anhydride, react for 3h, cool, and discharge to obtain Synergistic oligomeric phosphate polyol; the synergistic oligomeric phosphate polyol is a light yellow transparent liquid with an acid value of 11.6 mgKOH / g and a viscosity of 9201 mPa.s.

Embodiment 3

[0041] Embodiment 3 A kind of preparation method of synergistic oligomeric phosphate polyol

[0042] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 4.0g of water in 10min, heat to 80°C and react for 60min; add 110 mass parts of epichlorohydrin in 10min, and then add 0.45g of Catalyst benzyltriethylammonium chloride; heated to 140°C for 3 hours to obtain phosphate-based polyols;

[0043] 2) Cool to -80°C, add 30 parts by mass of phosphorus pentoxide, and react for 40 minutes to completely dissolve;

[0044] 3) Add 140g of epichlorohydrin, add 1.3g of catalyst, raise the temperature to 125°C, react for 1h, add tetrabromophthalic anhydride-60g, react for 3h, cool, and discharge to prepare synergistic oligophosphate polyol; It is a light yellow transparent liquid with an acid value of 10.4mgKOH / g and a viscosity of 8974mPa.s.

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Abstract

The invention discloses a preparation method and applications of synergic oligomeric phosphate ester polyol, and belongs to the high-molecular material, reaction-type flame retardant, energy saving and protection, environment friendly new technology and building insulation material technology fields. The synergic oligomeric phosphate ester polyol is prepared from phosphorus pentoxide, water, alkylene oxide and tetrabromophthalic anhydride as raw materials through a catalytic reaction. The raw materials are cheap and easily available, the reaction is mild, the technology is simple, operation is easy, and industrial production is easy. The product is used for preparation of flame retardation polyurethane foam materials.

Description

technical field [0001] The present invention relates to a preparation method and application of a synergistic oligomeric phosphate polyol, in particular to a preparation method of a synergistic oligomeric phosphate polyol used for preparing flame-retardant polyurethane foam, which belongs to polymer materials, reaction Type flame retardants, energy conservation and protection, environmentally friendly new technology and building insulation materials technology. Background technique [0002] Polyurethane foam is a low-density microporous urethane polymer material produced by the reaction of polyester or polyether polyols with isocyanate. It has light weight, low water absorption, good heat insulation, strong weather resistance, and low thermal conductivity. And good mechanical properties and chemical corrosion resistance, and has a strong bond strength with a variety of materials, is widely used as thermal insulation materials for petrochemical pipelines, refrigeration equipm...

Claims

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Application Information

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IPC IPC(8): C08G65/26C08G18/50C08G18/76C08G18/18C08G101/00
Inventor 王志玲崔玉匡轩郑鲁沂张书香
Owner UNIV OF JINAN
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