A preparation method of cellulose flame-retardant modified composite phenolic foam

A technology of phenolic foam and cellulose, which is applied in the field of composite material preparation, can solve problems such as the difficulty of mixing cellulose evenly, and achieve the effects of promoting application, improving mechanical properties, and increasing the amount of addition

Inactive Publication Date: 2020-11-06
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Technical problem to be solved: The present invention provides a preparation method of cellulose flame-retardant modified composite phenolic foam, which aims to improve the interfacial compatibility between cellulose and phenolic resin matrix, and greatly increase the amount of cellulose added in the composite foam. Solve the problem that it is difficult to mix evenly when adding cellulose in the later foaming process, improve the mechanical properties of the phenolic foam composite material, reduce the pulverization rate of the phenolic foam composite material, and improve the composite material without reducing the flame retardancy of the phenolic foam composite material. Comprehensive properties of phenolic foam

Method used

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  • A preparation method of cellulose flame-retardant modified composite phenolic foam
  • A preparation method of cellulose flame-retardant modified composite phenolic foam

Examples

Experimental program
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Effect test

Embodiment 1

[0019] (1) Preparation of DOPO-g-ITA: Using xylene as solvent, under nitrogen protection, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Add oxide (DOPO) and itaconic acid (ITA) into the reactor, reflux at 120°C for 4 hours, cool to 110°C, filter with suction, wash with acetone several times, and dry to obtain DOPO-g-ITA solid White powder. (2) Preparation of DOPO-g-ITA flame retardant grafted ethyl cellulose: dissolve the dried ethyl cellulose (water content 2 CO 3 , react at 120°C for 8h, then filter with suction, wash and dry at 60°C to obtain DOPO-g-ITA flame retardant grafted ethyl cellulose.

[0020](3) Preparation of flame retardant grafted ethyl cellulose modified phenolic resin: according to the molar ratio of formaldehyde and phenol is 1.8:1, the molar ratio of 50wt.% NaOH and phenol is 0.15:1, add 1mol in the reaction vessel Phenol and DOPO-g-ITA modified ethyl cellulose, which accounted for 2% of the mass of phenol, were heated to 90-95°C for 30-40 minutes, and th...

Embodiment 2

[0023] (1) Preparation of DOPO-g-ITA: Using xylene as solvent, under nitrogen protection, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Add oxide (DOPO) and itaconic acid (ITA) into the reactor, reflux reaction at 125°C for 4.5h, cool to 110°C, wash with acetone several times after suction filtration, and obtain DOPO-g-ITA after drying Solid white powder.

[0024] (2) Preparation of DOPO-g-ITA flame retardant grafted ethyl cellulose: dissolve the dried ethyl cellulose (water content 2 CO 3 React at 125°C for 8.5h, then filter with suction, wash and dry at 65°C to obtain DOPO-g-ITA flame retardant grafted ethyl cellulose.

[0025] (3) Preparation of flame retardant grafted ethyl cellulose modified phenolic resin: according to the molar ratio of formaldehyde and phenol is 2.0:1, the molar ratio of 50wt.% NaOH and phenol is 0.16:1, add 1mol phenol and DOPO-g-ITA modified ethyl cellulose accounting for 10% of the mass of phenol, heated to 93°C for 35 minutes, then added 0.5mol p...

Embodiment 3

[0028] (1) Preparation of DOPO-g-ITA: Using xylene as solvent, under nitrogen protection, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Add oxide (DOPO) and itaconic acid (ITA) into the reactor, reflux at 130°C for 5 hours, cool to 110°C, filter with suction, wash with acetone several times, and dry to obtain DOPO-g-ITA solid White powder.

[0029] (2) Preparation of DOPO-g-ITA flame retardant grafted ethyl cellulose: dissolve the dried ethyl cellulose (water content 2 CO 3 React at 130°C for 9 hours, then filter with suction, wash and dry at 70°C to obtain DOPO-g-ITA flame-retardant grafted ethyl cellulose.

[0030] (3) Preparation of flame retardant grafted ethyl cellulose modified phenolic resin: according to the molar ratio of formaldehyde and phenol is 2.2:1, the molar ratio of 50wt.% NaOH and phenol is 0.17:1, add 1mol phenol and phenol DOPO-g-ITA modified ethyl cellulose with 20% mass was heated to 95°C for 40 minutes, then added 0.55mol paraformaldehyde, 1.56mol wate...

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Abstract

The invention discloses a preparation method of cellulose antiflaming modified compound phenolic foam. A fire retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and itaconic acid are adoptedto perform grafting reaction so as to prepare DOPO-g-ITA for modifying cellulose, then DOPO-g-ITA antiflaming grafting cellulose is prepared, then DOPO-g-ITA antiflaming grafting cellulose modified phenolic resin is prepared, and cellulose compound phenolic foam is prepared. The interfacial compatibility between the modified cellulose prepared by the method and a phenolic resin matrix is obviously improved, the additive amount of the cellulose in compound foam is substantially promoted, the prepared cellulose modified phenolic resin has moderate viscosity and strong fermentability, the mechanical property of the prepared cellulose compound phenolic foam is obviously promoted, the pulverulent ratio is obviously reduced, the flame retardance is slightly promoted, the production cost of compound foam is reduced, and the composite material of the phenolic foam is conducive to being popularized and applied.

Description

technical field [0001] The invention belongs to the field of preparation of composite materials, in particular to a method for preparing a flame-retardant modified composite phenolic foam of cellulose. Background technique [0002] Phenolic foam is a kind of thermosetting foam formed by blending various additives (including surfactants, foaming agents, curing agents, etc.) with phenolic resin and foaming and curing at a certain temperature. Compared with polyurethane and polystyrene foam, phenolic foam has the advantages of good fire resistance, heat resistance, self-extinguishing, resistance to flame penetration, less smoke and no dripping during fire. As thermal insulation materials, phenolic foam is widely used in places with high fire protection requirements such as large public buildings, special ships, aviation equipment, and oil pipelines. However, the defects of high brittleness and high pulverization rate of phenolic foam seriously limit its popularization and appl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/04C08G8/28
CPCC08G8/28C08J9/04C08J2361/14
Inventor 马玉峰徐明娟黄晶廖楚豪
Owner NANJING FORESTRY UNIV
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