Phosphorus-containing essence inflaming-retarding cellulose-based thermal insulation material and preparation method thereof

A technology for flame-retardant cellulose and heat-insulating material, which is applied to the field of phosphorus-containing intrinsic flame-retardant cellulose-based heat-insulating material and its preparation, can solve the problems of increased material density, difficulty in preparation, difficulty in dispersion and the like, and achieves thermal conductivity. Low coefficient and density, simple preparation process, and improved mechanical properties

Inactive Publication Date: 2019-06-28
应急管理部四川消防研究所
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  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the increasing depletion of petroleum resources, it has become an inevitable trend to look for environmentally friendly, green and renewable resources as alternative resources to develop new energy and new materials; cellulose is a renewable resource that exists widely in nature, with large reserves, It is easy to obtain materials and low in price, and is one of the most abundant biomass polymers on the earth; the development and use of new functional materials based on cellulose will produce good economic and ecological benefits; however, cellulose materials are extremely flammable and have low mechanical strength low, which hinders its further application in the field of thermal insulation; the existing cellulose flame-retardant technology has problems such as low flame-retardant efficiency, easy to produce toxic smoke when burning, and difficult to prepare; high-filling cellulose Inorganic micro / nano-particles can also easily lead to an increase in the density and thermal conductivity of thermal insulation materials; therefore, it is urgent to carry out more efficient environmental protection and flame-retardant modification of cellulose materials
[0003] At present, there are two commonly used methods for flame retardancy and reinforcement of cellulose-based thermal insulation materials, one is to add micro / nano particles with flame retardancy; the other is to add reactive phosphorus-containing flame retardants; add inorganic In the flame retardant system of flame retardants or nanoparticles with strong barrier properties, inorganic micro / nano particles generally need to be added to a higher content to obtain a satisfactory flame retardant effect; however, highly filled inorganic micro / nano particles are dispersed during the preparation process. It is difficult, and the addition of a large number of rigid particles will easily lead to an increase in the density and thermal conductivity of the material; adding reactive phosphorus-containing flame retardants cannot achieve material enhancement, and additional cross-linking agents need to be added to achieve enhancement; using essential The flame retardant method can avoid the collapse of the pore structure caused by the uneven distribution of inorganic micro / nano flame retardant particles, and can maintain the low density and low thermal conductivity of cellulose-based insulation materials; introduce phosphorus-containing flame retardant groups into fibers The element molecular chain is an effective way to achieve high-efficiency halogen-free intrinsic flame retardancy; however, traditional phosphorus-containing groups generally have a certain gas-phase flame-retardant effect, which increases the smoke release of materials during combustion, and many phosphorus-containing gases have certain Toxicity; fire statistics show that poisoning or suffocation by toxic fumes is the leading cause of casualties

Method used

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preparation example Construction

[0026] A method for preparing a phosphorus-containing intrinsic flame-retardant cellulose-based thermal insulation material, comprising the following steps:

[0027] Step 1: Repeatedly washing and treating the biomass raw material containing cellulose with deionized water to obtain a cellulose fiber suspension; adding urea and a phosphorylation modifier to the cellulose suspension of 1 wt% to 10 wt%, Under the condition of ~165°C, after stirring evenly and fully for reaction, the phosphorus-containing cellulose is obtained by washing; wherein the molar ratio of deoxyglucose unit, urea and phosphorylation modifier in the cellulose is 0.4-1.5:4-5:1.

[0028] The phosphorylation modifier is one of ammonium monohydrogen phosphate and ammonium dicyanide phosphate; the heat treatment time is 2-60 minutes, and the reaction time in step 2 is 1-2 hours.

[0029] Step 2: add the phosphorus-containing cellulose obtained in step 1 into deionized water to form a suspension of 0.5wt% to 2wt...

Embodiment 1

[0039] Step 1: Take 5 g of cellulose-containing wood pulp raw material (about 95% cellulose content), wash it repeatedly with deionized water, and configure it with deionized water to form a suspension with a cellulose mass concentration of 1 wt%; Add 4.9g of diamine hydrogen phosphate and 8.9g of urea, stir evenly; dry at 70°C to remove most of the water, then treat at 150°C for 10min, and wash repeatedly with deionized water to obtain phosphorus-containing cellulose fibers;

[0040] Step 2: Prepare the phosphorus-containing cellulose fiber into a 2wt% suspension with deionized water, add sodium hydroxide to adjust the pH to 9.5 under high-speed stirring, and react for 1 hour; continue ultrasonic treatment for 2 hours, wash with deionized water to remove excess sodium hydroxide , the mechanical fibrillation treatment makes phosphorus-containing cellulose nanofibers with a phosphorus content of 0.5%;

[0041]Step 3: Stir the 1 wt% suspension of phosphorus-containing cellulose ...

Embodiment 2

[0043] Step 1: Take 5 g of cellulose-containing wood pulp raw material (about 95% cellulose content), wash it repeatedly with deionized water, and configure it with deionized water to form a suspension with a cellulose mass concentration of 1 wt%; Add 4.9g of diamine hydrogen phosphate and 8.9g of urea, stir evenly; dry at 70°C to remove most of the water, then treat at 150°C for 60min, and wash repeatedly with deionized water to obtain phosphorus-containing cellulose fibers;

[0044] Step 2: Prepare the phosphorus-containing cellulose fiber into a 2wt% suspension with deionized water, add sodium hydroxide to adjust the pH to 9.5 under high-speed stirring, and react for 1 hour; continue ultrasonic treatment for 2 hours, wash with deionized water to remove excess sodium hydroxide , the mechanical fibrillation treatment makes phosphorus-containing cellulose nanofibers with a phosphorus content of 0.7%;

[0045] Step 3: Stir the 0.50wt% suspension of phosphorus-containing cellulo...

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Abstract

The invention discloses a phosphorus-containing essence inflaming-retarding cellulose-based thermal insulation material and a preparation method thereof. The preparation method comprises the followingsteps that 1, urea and a phosphorylation modifier are added to a cellulose suspension solution with the concentration of 1-10wt%, and at 150-165 DEG C, after even stirring and a sufficient reaction,through washing, phosphorus-containing cellulose is obtained; 2, the phosphorus-containing cellulose is prepared into a suspension solution with the concentration of 0.5-2wt%, the pH of the suspensionsolution is adjusted to be 9.5-12, and under the stirring condition, after a sufficient reaction, through washing and fiber separation, phosphorus-containing cellulose nanofibers are obtained; 3, phosphorus-containing groups in the phosphorus-containing cellulose nanofibers are subjected to ionization modification through an in-situ formation method or an after-treatment crosslinking method for obtaining the phosphorus-containing essence inflaming-retarding cellulose-based thermal insulation material. The preparation technology is simple, the raw material source is wide, the cost is low, theenvironment protection is achieved, and the obtained thermal insulation material is low in heat conductivity coefficient and density and good in flame retardant property.

Description

technical field [0001] The invention relates to the technical field of biomass thermal insulation materials, in particular to a phosphorus-containing intrinsic flame-retardant cellulose-based thermal insulation material and a preparation method thereof. Background technique [0002] With the increasing depletion of petroleum resources, it has become an inevitable trend to look for environmentally friendly, green and renewable resources as alternative resources to develop new energy and new materials; cellulose is a renewable resource that exists widely in nature, with large reserves, It is easy to obtain materials and low in price, and is one of the most abundant biomass polymers on the earth; the development and use of new functional materials based on cellulose will produce good economic and ecological benefits; however, cellulose materials are extremely flammable and have low mechanical strength low, which hinders its further application in the field of thermal insulation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J9/40C08B15/00C08B15/05C08L1/08C08K3/16C08K3/22
Inventor 张怡葛欣国卢国建赵长征
Owner 应急管理部四川消防研究所
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