CN109575512A - A kind of natural polymer subbase aeroge and preparation method thereof, application - Google Patents

A kind of natural polymer subbase aeroge and preparation method thereof, application Download PDF

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CN109575512A
CN109575512A CN201811490343.5A CN201811490343A CN109575512A CN 109575512 A CN109575512 A CN 109575512A CN 201811490343 A CN201811490343 A CN 201811490343A CN 109575512 A CN109575512 A CN 109575512A
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aeroge
natural polymer
drying
cellulose
polymer subbase
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廖望
廖敏惠
张文静
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Xihua University
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Xihua University
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    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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Abstract

The present invention provides a kind of natural polymer subbase aeroge and preparation method thereof, application, which is made of according to mass parts meter following component: natural macromolecular and its 0.1~10 part of derivative；0.05~5 part of rich nitrogen molecular；0.005~3 part of rich phosphorus molecule；0~15 part of crosslinking agent.Have many advantages, such as high flame retardant, low thermal conductivity, low-density, high tenacity using natural polymer subbase aeroge prepared by the method for the present invention.

Description

A kind of natural polymer subbase aeroge and preparation method thereof, application
Technical field
The present invention relates to field of material technology more particularly to a kind of natural polymer subbase aeroge and preparation method thereof, answer With.
Background technique
Aeroge is a kind of mutually to coalesce high dispersive solid-state constitute and using air as decentralized medium by ultramicro powder Material has extremely-low density, superhigh specific surface area (600~1200m2/ g) and the characteristics such as superelevation porosity (> 90%), it is current World's upper density is minimum, the smallest solid material of thermal conductivity.SiO is made by hydrolysis sodium metasilicate in typical aerogel material2Colloidal sol, SiO is obtained through aging again2Gel.In the drying process, in order to guarantee that fragile gel skeleton is not destroyed by capillary tension, It generallys use solvent displacement and supercritical drying method is dried.However, this aerogel-like intensity is low, poor toughness, nanometer The disadvantages of pore structure is easily destroyed under external force significantly limits its practical application.
The flexibility that aeroge can be obviously improved aeroge is prepared using high molecular material.Wang et al. reports one kind The polymer aerogel made of hydrophobically modified gelatin is simultaneously adsorbed for greasy dirt, due to its good flexibility, can be pressed repeatedly Contracting uses up to 5000 times.[J.Wang et al., J.Mater.Chem.A, 2016,4,9381-9389.] Takeshita and Yoda formaldehyde crosslinking chitosan, then passes through supercritical CO2A kind of transparent, with high flexibility aeroge has been made in drying Material, elasticity modulus can be up to 38.9MPa.[S.Takeshita*and S.Yoda,Chem.Mater.,2015,27, 7569-7572.] Chinese invention patent CN 1032050125 A disclose and a kind of prepare flexible aeroge with regenerated cellulose Method.
However, common high molecular material belongs to combustible material more, there is fire risk in use process.Aeroge is come It says, due to its high specific surface area, it is easier to detonation occur.
Summary of the invention
It is an object of the invention to solve the problems of the above-mentioned prior art, a kind of natural polymer subbase aeroge is provided And preparation method thereof, application.
A kind of natural polymer subbase aeroge, raw material are made of according to mass parts meter following component:
Natural macromolecular and its 0.1~10 part of derivative
0.05~5 part of rich nitrogen molecular
0.005~3 part of rich phosphorus molecule
0~15 part of crosslinking agent.
Further, natural polymer subbase aeroge as described above, raw material is according to mass parts meter, by following component structure At:
Natural macromolecular and its 0.5~10 part of derivative
0.05~4 part of rich nitrogen molecular
0.01~2 part of rich phosphorus molecule
0~15 part of crosslinking agent.
Further, natural polymer subbase aeroge as described above, the natural macromolecular and its derivative include Methylcellulose, hydroxyethyl cellulose, hydroxyethylmethylcellulose, hydroxyethyl methyl carboxymethyl cellulose, hydroxypropyl cellulose, At least one of hydroxypropyl methyl cellulose, ethoxy SE-cellulose, chitosan, gelatin, sodium alginate.
Further, natural polymer subbase aeroge as described above, the natural macromolecular and its derivative are hydroxyl second Base cellulose, hydroxypropyl cellulose, ethoxy SE-cellulose, starch, chitosan, gelatin, at least one in sodium alginate Kind.
Further, natural polymer subbase aeroge as described above, it is described richness nitrogen molecular be Lauxite, dicyandiamide, Polypropylene amine, polyallylamine hydrochloride, polyethyleneimine, branched polyethylene imine, tetraethylenepentamine, melamine, trimerization At least one of cyanogen amine-formaldehyde resin.
Further, natural polymer subbase aeroge as described above, the richness phosphorus molecule is phosphoric acid, phosphate, poly- phosphorus At least one of acid, Quadrafos, poly-phosphate derivative, phytic acid.
Further, natural polymer subbase aeroge as described above, the crosslinking agent are divinylsulfone, epoxy chloropropionate Alkane, citric acid, boric acid, borate, formaldehyde, glyoxal, glutaraldehyde, 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide salt At least one of hydrochlorate (EDC), 1- ethyl -3- (3- dimethylaminopropyl) carbodiimide.
A kind of preparation method of natural polymer subbase aeroge as described above, includes the following steps:
(1) parts by weight are pressed, the natural macromolecular, rich nitrogen molecular, rich phosphorus molecule, crosslinking agent are dispersed in solvent In；The solvent is one or more groups of water, methanol, ethyl alcohol, propyl alcohol, isopropanol, the tert-butyl alcohol, acetone and dimethyl sulfoxide It closes；
(2) solid-state is made in above-mentioned dispersion liquid；Wherein the mode of solid-state processing includes: ripening, freezing processing, colloidal sol One of change processing or a variety of combinations；
(3) solid-state is dried；The mode of the drying include: supercritical drying, freeze-drying, vacuum drying, One of spray drying, microwave drying and infra-red drying or a variety of combinations are dried；
(4) solid-state after drying is subjected to cross-linked stable；The mode of the cross-linked stable include: heat cross-linking, ultrasound crosslinking, Microwave irradiation crosslinking, infrared irridiation crosslinked, ultraviolet irradiation crosslinking, electron beam irradiation crosslinking, plasma radiation crosslinking, gal One of the crosslinking of horse x ray irradiation x and x-ray irradiation crosslinking or a variety of combinations.
According to the natural polymer subbase aeroge any one of as above in flexibly thermal insulation material and carbon dioxide capture field Application.
The utility model has the advantages that
Using the method for the present invention preparation natural polymer subbase aeroge have high flame retardant, low thermal conductivity, low-density, The advantages that high tenacity.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
The present invention provides a kind of natural polymer subbase aeroge, and the material is in parts by weight, constituted by the following substances, 0.1~10 part of soluble natural macromolecular, 0.05~5 part of rich nitrogen molecular, 0.005~3 part of rich phosphorus molecule, crosslinking agent 0.01~15 Part, 100 parts of water.The density of material is 10~50kg/m3,20~60kPa of tensile strength, 0.010~0.030W/ of thermal coefficient (mK), limit oxygen index is higher than 50%, porosity 80~95%, 60~150m2/g of specific surface area, in 0.1MPa, 273K ring In border, carbon dioxide adsorption capacity is 5~20% quality of materials.The material can be used for flexibly thermal insulation material and carbon dioxide is inhaled It is attached.
The present invention also provides a kind of preparation methods of natural polymer subbase aeroge, include the following steps:
(1) parts by weight are pressed, the natural macromolecular, rich nitrogen molecular, rich phosphorus molecule, crosslinking agent are dispersed in solvent In；The solvent is one or more groups of water, methanol, ethyl alcohol, propyl alcohol, isopropanol, the tert-butyl alcohol, acetone and dimethyl sulfoxide It closes；
(2) solid-state is made in above-mentioned dispersion liquid；Wherein the mode of solid-state processing includes: ripening, freezing processing, colloidal sol One of change processing or a variety of combinations；
(3) solid-state is dried；The mode of the drying include: supercritical drying, freeze-drying, vacuum drying, One of spray drying, microwave drying and infra-red drying or a variety of combinations are dried；
(4) solid-state after drying is subjected to cross-linked stable；The mode of the cross-linked stable include: heat cross-linking, ultrasound crosslinking, Microwave irradiation crosslinking, infrared irridiation crosslinked, ultraviolet irradiation crosslinking, electron beam irradiation crosslinking, plasma radiation crosslinking, gal One of the crosslinking of horse x ray irradiation x and x-ray irradiation crosslinking or a variety of combinations.
It should be understood that when the component of crosslinking agent is 0, the cross-linked stable means of step 4 use in the preparation method Using cross-linking radiation.
Embodiment:
Referring in particular to Tables 1 and 2.
1. formula table of table
2. performance parameter table of table
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features； And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and Range.

Claims (9)

1. a kind of natural polymer subbase aeroge, which is characterized in that its raw material is made of according to mass parts meter following component:
Natural macromolecular and its 0.1~10 part of derivative
0.05~5 part of rich nitrogen molecular
0.005~3 part of rich phosphorus molecule
0~15 part of crosslinking agent.
2. natural polymer subbase aeroge according to claim 1, which is characterized in that its raw material according to mass parts meter, by Following component is constituted:
Natural macromolecular and its 0.5~10 part of derivative
0.05~4 part of rich nitrogen molecular
0.01~2 part of rich phosphorus molecule
0~15 part of crosslinking agent.
3. natural polymer subbase aeroge according to claim 1, which is characterized in that the natural macromolecular and its spread out Biology includes methylcellulose, hydroxyethyl cellulose, hydroxyethylmethylcellulose, hydroxyethyl methyl carboxymethyl cellulose, hydroxypropyl Base cellulose, hydroxypropyl methyl cellulose, ethoxy SE-cellulose, chitosan, gelatin, at least one in sodium alginate Kind.
4. natural polymer subbase aeroge according to claim 1, which is characterized in that the natural macromolecular and its derivative Object is hydroxyethyl cellulose, in hydroxypropyl cellulose, ethoxy SE-cellulose, starch, chitosan, gelatin, sodium alginate At least one.
5. natural polymer subbase aeroge according to claim 1, which is characterized in that the richness nitrogen molecular is ureaformaldehyde tree Rouge, dicyandiamide, polypropylene amine, polyallylamine hydrochloride, polyethyleneimine, branched polyethylene imine, tetraethylenepentamine, trimerization At least one of cyanamide, melamine formaldehyde resin.
6. natural polymer subbase aeroge according to claim 1, which is characterized in that the richness phosphorus molecule is phosphoric acid, phosphorus At least one of hydrochlorate, polyphosphoric acid, Quadrafos, poly-phosphate derivative, phytic acid.
7. natural polymer subbase aeroge according to claim 1, which is characterized in that the crosslinking agent is divinyl Sulfone, epoxychloropropane, citric acid, boric acid, borate, formaldehyde, glyoxal, glutaraldehyde, 1- (3- dimethylamino-propyl) -3- ethyl At least one of carbodiimide hydrochloride (EDC), 1- ethyl -3- (3- dimethylaminopropyl) carbodiimide.
8. a kind of preparation method of natural polymer subbase aeroge as described in claim 1, which is characterized in that including walking as follows It is rapid:
(1) parts by weight are pressed, in a solvent by the natural macromolecular, rich nitrogen molecular, rich phosphorus molecule, crosslinking agent dispersion； The solvent is one or more combinations of water, methanol, ethyl alcohol, propyl alcohol, isopropanol, the tert-butyl alcohol, acetone and dimethyl sulfoxide；
(2) solid-state is made in above-mentioned dispersion liquid；Wherein the mode of solid-state processing includes: ripening, freezing processing, at solation One of reason or a variety of combinations；
(3) solid-state is dried；The mode of the drying includes: supercritical drying, freeze-drying, vacuum drying, is sprayed One of dry, microwave drying and infra-red drying or a variety of combinations are dried；
(4) solid-state after drying is subjected to cross-linked stable；The mode of the cross-linked stable includes: heat cross-linking, ultrasound crosslinking, microwave Cross-linking radiation, infrared irridiation crosslinked, ultraviolet irradiation crosslinking, electron beam irradiation crosslinking, plasma radiation crosslinking, gamma are penetrated One of line cross-linking radiation and x-ray irradiation crosslinking or a variety of combinations.
9. any one of the claim 1~7 natural polymer subbase aeroge is led in flexibly thermal insulation material and carbon dioxide capture The application in domain.
CN201811490343.5A 2018-12-06 2018-12-06 A kind of natural polymer subbase aeroge and preparation method thereof, application Pending CN109575512A (en)

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CN110669262A (en) * 2019-10-09 2020-01-10 西华大学 Foam material and preparation method and application thereof
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CN110204796A (en) * 2019-06-10 2019-09-06 四川师范大学 Fire-retardant aeroge with self-healing properties and preparation method thereof
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CN114181422A (en) * 2021-11-15 2022-03-15 安徽工程大学 Micron fiber reinforced cellulose composite aerogel and preparation method and application thereof
CN114832741A (en) * 2022-05-05 2022-08-02 彗晶新材料科技(杭州)有限公司 Preparation method of heat-conducting wave-absorbing composite aerogel and heat-conducting wave-absorbing composite aerogel
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CN116284961A (en) * 2022-12-22 2023-06-23 华南理工大学 Preparation of pure biomass high-flame-retardance aerogel through two-step crosslinking

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