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Phosphated lignin-based flame-retardant and reinforced rigid polyurethane foam and preparation method thereof

A polyurethane rigid foam, lignin-based technology, applied in the field of foam materials, can solve the problems of polyurethane foam not having flame retardant properties, low reactivity of flame retardants, easy migration, etc., to reduce the heat release rate and enhance the mechanical properties. , Improve the effect of flame retardant performance

Active Publication Date: 2014-07-09
HEFEI GENIUS NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent CN101696261A uses separated lignin to modify epoxides to increase the reactivity of lignin, but the modified reaction temperature is high, the conditions are harsh, and the process is complicated
The foam material has excellent mechanical properties and high lignin utilization rate, but the polyurethane foam prepared by the above-mentioned patented method has poor flame retardancy and is flammable in the air, which limits its application range
Although the prior art has disclosed some polyurethane foams prepared by using additive flame retardants, these flame retardants have low reactivity in the polyurethane foam matrix and cannot be polymerized with polyurethane during the foaming process, and are easy to migrate. So that polyurethane foam can not have long-term effective flame retardant properties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Raw material preparation:

[0045] Preparation of anhydrous phosphoric acid solution: mix 50% phosphorus pentoxide, 30% phosphoric acid and 20% hexanol by mass percentage to prepare anhydrous phosphoric acid solution;

[0046] Preparation of degradable liquefaction agent: Mix 20 parts of degradable polyol and 10 parts of glycerol prepared by polyethylene glycol and polycaprolactone at a mass ratio of 1:3;

[0047] (2) Preparation of Phosphated Lignin:

[0048] Add 10 parts of alkali lignin into 100ml of formaldehyde alkaline solution, heat up and react for 3 hours, then adjust the pH value to acidic with acid, then add 50ml of anhydrous phosphoric acid solution, stir for 60 hours, and dry to obtain phosphide; then the phosphide is stirred Add it into 30 parts of degradable liquefaction agent, heat and react for 0.5h in the presence of a catalyst, adjust the pH value of the solution to neutral with alkali, and obtain the phosphated lignin liquefaction product;

[0...

Embodiment 2

[0053] (1) Raw material preparation:

[0054] Preparation of anhydrous phosphoric acid solution: mix 60% phosphorus pentoxide, 20% phosphoric acid and 20% hexanol by mass percentage to prepare anhydrous phosphoric acid solution;

[0055] Preparation of degradable liquefaction agent: Mix 20 parts of degradable polyol and 10 parts of glycerol prepared by polyethylene glycol and polycaprolactone at a mass ratio of 1:3;

[0056] (2) Preparation of Phosphated Lignin:

[0057] Add 20 parts of alkali lignin into 120ml of formaldehyde alkaline solution, heat up and react for 3 hours, then adjust the pH value to acidic with acid, then add 50ml of anhydrous phosphoric acid solution, stir for 60 hours, and dry to obtain phosphide; then the phosphide is stirred Add it to 30 parts of degradable liquefaction agent, heat and react for 1 hour in the presence of a catalyst, adjust the pH value of the solution to neutral with alkali, and obtain phosphated lignin liquefaction;

[0058] (3) Pre...

Embodiment 3

[0062] (1) Raw material preparation:

[0063] Preparation of anhydrous phosphoric acid solution: mix 60% phosphorus pentoxide, 25% phosphoric acid and 15% hexanol by mass percentage to prepare anhydrous phosphoric acid solution;

[0064] Preparation of degradable liquefaction agent: Mix 25 parts of degradable polyol and 10 parts of glycerol prepared by polyethylene glycol and polycaprolactone at a mass ratio of 1:3;

[0065] (2) Preparation of Phosphated Lignin:

[0066] Add 30 parts of calcium lignosulfonate to 120ml of formaldehyde alkaline solution, heat up and react for 4 hours, then adjust the pH value to acidic with acid, then add 80ml of anhydrous phosphoric acid solution, stir for 70 hours, and dry to obtain phosphide; then the phosphide Add it into 35 parts of degradable liquefaction agent under stirring, heat and react for 1 hour in the presence of a catalyst, adjust the pH value of the solution to neutral with alkali, and obtain the phosphated lignin liquefaction p...

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Abstract

The invention discloses phosphated lignin-based flame-retardant and reinforced rigid polyurethane foam and a preparation method thereof. The polyurethane foamed plastic is prepared by mixing, pouring and foaming 50-90 parts of bio-based polyhydric alcohols, 10-50 parts of phosphated lignin, 1-3 parts of amine catalyst, 0.05-0.2 part of tin catalyst, 0.5-2 parts of foam stabilizer, 100-140 parts of isocyanate and 4-7 parts of water. The activity of the lignin is improved through phosphorization modification, and formation of a crosslinking network of the polyurethane foam system is promoted, so that the mechanical property of the foam is improved, the utilization rate of the lignin in the polyurethane foam is increased, and the production cost of the polyurethane foam is reduced. In addition, an anhydrous phosphate solution in modified liquid directly serves as a flame retardant component and is uniformly dispersed in the polyurethane foam, and the heat release rate of the polyurethane foam is reduced, so that the polyurethane foam has high flame-retardant property.

Description

[0001] technical field [0002] The invention belongs to the technical field of foaming materials, and in particular relates to a phosphating lignin-based flame-retardant reinforced polyurethane rigid foam and a preparation method thereof Background technique [0003] With the decrease of non-renewable resources and the continuous deepening of environmental protection problems, the application of natural resources such as plants and natural polymer materials as new chemical raw materials has been paid more and more attention. Lignin is a rich and renewable resource. The industrial lignin produced in the process of pulping and papermaking and plant hydrolysis is discharged as waste, which not only causes a great waste of resources, but also seriously pollutes the environment. [0004] At present, the preparation of polyurethane foam from renewable plant resources has attracted attention. There are a large number of active functional groups such as alcoholic hydroxyl groups, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/67C08G18/64C08G18/48C08H7/00C08J9/08C08G101/00
CPCC08G18/165C08G18/4081C08G18/6492C08G18/6547C08G18/6696C08G2230/00C08H6/00C08G2110/0025C08G2110/0083
Inventor 杨桂生袁海霞
Owner HEFEI GENIUS NEW MATERIALS
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