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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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Publication number
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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cross
linking
drying
natural
natural polymer
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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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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • 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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    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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)

1.一种天然高分子基气凝胶，其特征在于，其原料按照质量份计，由如下组分构成：1. a natural macromolecular-based aerogel, is characterized in that, its raw material is made up of following components according to mass parts: 天然大分子及其衍生物0.1～10份0.1-10 parts of natural macromolecules and their derivatives 富氮分子0.05～5份Nitrogen-rich molecules 0.05 to 5 copies 富磷分子0.005～3份Phosphorus-rich molecules 0.005 to 3 copies 交联剂0～15份。0-15 parts of cross-linking agent. 2.根据权利要求1所述的天然高分子基气凝胶，其特征在于，其原料按照质量份计，由如下组分构成：2. natural macromolecular-based aerogel according to claim 1, is characterized in that, its raw material is made up of following components according to mass parts: 天然大分子及其衍生物0.5～10份0.5-10 parts of natural macromolecules and their derivatives 富氮分子0.05～4份Nitrogen-rich molecules 0.05 to 4 copies 富磷分子0.01～2份Phosphorus-rich molecules 0.01 to 2 copies 交联剂0～15份。0-15 parts of cross-linking agent. 3.根据权利要求1所述的天然高分子基气凝胶，其特征在于，所述的天然大分子及其衍生物包括甲基纤维素、羟乙基纤维素、羟乙基甲基纤维素、羟乙基甲基羧甲基纤维素、羟丙基纤维素、羟丙基甲基纤维素、羟乙基磺乙基纤维素、壳聚糖、明胶、海藻酸钠中的至少一种。3. The natural polymer-based aerogel according to claim 1, wherein the natural macromolecules and derivatives thereof include methyl cellulose, hydroxyethyl cellulose, and hydroxyethyl methyl cellulose , at least one of hydroxyethyl methyl carboxymethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl sulfoethyl cellulose, chitosan, gelatin, and sodium alginate. 4.根据权利要求1所述的天然高分子基气凝胶，其特征在于，所述天然大分子及其衍生物为羟乙基纤维素、羟丙基纤维素、羟乙基磺乙基纤维素、淀粉、壳聚糖、明胶、海藻酸钠中的至少一种。4. The natural polymer-based aerogel according to claim 1, wherein the natural macromolecules and derivatives thereof are hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxyethyl sulfoethyl cellulose At least one of vegan, starch, chitosan, gelatin, and sodium alginate. 5.根据权利要求1所述的天然高分子基气凝胶，其特征在于，所述富氮分子为脲醛树脂、双氰胺、聚丙烯胺、聚烯丙基胺盐酸盐、聚乙烯亚胺、支化聚乙烯亚胺、四乙烯五胺、三聚氰胺、三聚氰胺-甲醛树脂中的至少一种。5. The natural polymer-based aerogel according to claim 1, wherein the nitrogen-rich molecule is urea-formaldehyde resin, dicyandiamide, polyacrylamine, polyallylamine hydrochloride, polyethylene At least one of amine, branched polyethyleneimine, tetraethylenepentamine, melamine, and melamine-formaldehyde resin. 6.根据权利要求1所述的天然高分子基气凝胶，其特征在于，所述富磷分子为磷酸、磷酸盐、聚磷酸、聚磷酸盐、聚磷酸衍生物、植酸中的至少一种。6. The natural polymer-based aerogel according to claim 1, wherein the phosphorus-rich molecule is at least one of phosphoric acid, phosphate, polyphosphoric acid, polyphosphate, polyphosphoric acid derivatives, and phytic acid kind. 7.根据权利要求1所述的天然高分子基气凝胶，其特征在于，所述交联剂为二乙烯基砜、环氧氯丙烷、柠檬酸、硼酸、硼酸盐、甲醛、乙二醛、戊二醛、1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐(EDC)、1-乙基-3-(3-二甲基氨基丙基)碳二亚胺中的至少一种。7. The natural polymer-based aerogel according to claim 1, wherein the cross-linking agent is divinyl sulfone, epichlorohydrin, citric acid, boric acid, borate, formaldehyde, ethylene glycol Aldehyde, glutaraldehyde, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC), 1-ethyl-3-(3-dimethylaminopropyl) at least one of carbodiimides. 8.一种如权利要求1所述天然高分子基气凝胶的制备方法，其特征在于，包括如下步骤：8. a preparation method of natural polymer-based aerogel as claimed in claim 1, is characterized in that, comprises the steps: (1)按所述重量份数，将所述天然大分子、富氮分子、富磷分子、交联剂分散在溶剂中；所述溶剂为水、甲醇、乙醇、丙醇、异丙醇、叔丁醇、丙酮和二甲基亚砜的一种或多种的组合；(1) according to the parts by weight, the natural macromolecules, nitrogen-rich molecules, phosphorus-rich molecules, and cross-linking agents are dispersed in a solvent; the solvent is water, methanol, ethanol, propanol, isopropanol, a combination of one or more of tert-butanol, acetone, and dimethyl sulfoxide; (2)将上述分散液制成固态；其中固态处理的方式包括：陈化处理、冷冻处理、溶胶化处理中的一种或多种的组合；(2) above-mentioned dispersion liquid is made into solid state; Wherein the mode of solid state treatment comprises: one or more combinations in aging treatment, freezing treatment, sol treatment; (3)将该固态进行干燥；所述干燥的方式包括：超临界干燥、冷冻干燥、真空干燥、喷雾干燥、微波干燥和红外干燥中的一种或多种的组合进行干燥；(3) drying the solid state; the drying method includes: drying by one or more combinations of supercritical drying, freeze drying, vacuum drying, spray drying, microwave drying and infrared drying; (4)将干燥后的固态进行交联稳定；所述交联稳定的方式包括：热交联、超声交联、微波辐照交联、红外线辐照交联、紫外线辐照交联、电子束辐照交联、等离子体辐照交联、伽马射线辐照交联和X射线辐照交联中的一种或多种的组合。(4) cross-linking and stabilizing the dried solid state; the methods for cross-linking stabilization include: thermal cross-linking, ultrasonic cross-linking, microwave irradiation cross-linking, infrared irradiation cross-linking, ultraviolet irradiation cross-linking, electron beam cross-linking A combination of one or more of radiation crosslinking, plasma radiation crosslinking, gamma radiation crosslinking, and X-ray radiation crosslinking. 9.权利要求1～7任一项所述天然高分子基气凝胶在柔性保温材料和二氧化碳捕捉领域的应用。9. Application of the natural polymer-based aerogel according to any one of claims 1 to 7 in the fields of flexible thermal insulation materials and carbon dioxide capture.
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CN111592680A (en) * 2020-06-15 2020-08-28 齐鲁工业大学 A kind of super absorbent aerogel packaging material prepared by using reed waste residue and preparation method thereof
CN113683811A (en) * 2021-06-30 2021-11-23 青岛科技大学 Efficient flame-retardant phosphorylated chitosan aerogel and preparation method thereof
CN114181422A (en) * 2021-11-15 2022-03-15 安徽工程大学 A kind of microfiber reinforced cellulose composite aerogel and its preparation method and application
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CN116751404A (en) * 2023-06-14 2023-09-15 大连工业大学 Anisotropic heat-insulating and flame-retardant guar gum aerogel and preparation method thereof
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