CN103599734A - Aerogel material and preparation method thereof - Google Patents
Aerogel material and preparation method thereof Download PDFInfo
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- CN103599734A CN103599734A CN201310590267.6A CN201310590267A CN103599734A CN 103599734 A CN103599734 A CN 103599734A CN 201310590267 A CN201310590267 A CN 201310590267A CN 103599734 A CN103599734 A CN 103599734A
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Abstract
The invention provides an aerogel material and a preparation method thereof. The material is prepared from a polymer and clay by the steps of aqueous solution blending, irradiation crosslinking and freeze drying, wherein the polymer accounts for 5-95% of the aerogel weight, the clay accounts for 95-5% of the aerogel weight, and the aerogel density is 0.03-0.20g/cm<3>. The preparation method of the aerogel material provided by the invention sequentially comprises the following steps: (a) dissolving the polymer in deionized water, adding the clay and stirring to obtain turbid liquid in uniform distribution; (b) performing irradiation crosslinking of the turbid liquid obtained by the step (a) under high-energy rays, wherein the irradiation dosage of the high-energy rays is 1-200kGy; and (c) freezing the irradiation product obtained by the step (b), and drying to obtain the aerogel material. Since water is used as a solvent only in the preparation process and a chemical crosslinking agent is not required by the irradiation crosslinking, the crosslinking is efficient and controllable, the crosslinking density is uniform, the preparation process is green and environment-friendly, and the production efficiency is high.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of aerogel material and preparation method thereof.
Background technology
Aeroge claims again xerogel, and its preparation is to replace the liquid in gel with gas, and gel network structure substantially remains unchanged and forms.Traditional silicon dioxide aeroge is invented by Kistler in nineteen thirty at first, there is very high porosity, very high specific area, very low apparent density and refractive index, have application prospect in fields such as light laser research target material, heat-barrier material, energy storage material, catalysis material, sorbing material, Qie Lunkefu threshold values detectors.The preparation of tradition aeroge be take silanol salt as raw material, and its preparation process is divided into gelation, ageing and dry three steps.Because cost of material is high, preparation process is complicated, and need to use a large amount of solvents, causes the production of traditional aeroge to be difficult to scale, expensive; And the common lacking toughness of inorganic material, in use easily fracture.
The Schiraldi of U.S. CWRU teach problem group has made Novel air gel rubber material by cheap polyalcohol/clay soil (often selecting imvite) colloid by cryogenic freezing, rapid freeze-drying technology.This material has stratiform or netted space structure, and porosity is high, density is low, thermal conductivity factor is low, in fields such as heat-insulation and heat-preservation, packing protection, sorbing materials, has broad prospect of application.
Yet the mechanical property of polyalcohol/clay soil aerogel material is mainly subject to type of polymer and content influence, not ideal enough while using in some field, need to strengthen modification to it.Schiraldi seminar adopts the method for blend string to improve the mechanical property of aeroge, and gained Mechanical Properties of Aerogels improves, but effect is not remarkable, and especially, when polymer content is lower, the humidification of this method is also not obvious.The inventor once, by add the method for chemical cross-linking agent at alkaline environment, prepared cross-linked type polyethylene alcohol/imvite aeroge, and the mechanical property of this aeroge has very obviously the even order of magnitude to improve when uncrosslinked.But also there is distinct disadvantage in the method, such as crosslinked required alkaline environment can promote polymer degraded in use, residual poisonous crosslinking agent can bring environment and personal security problem, crosslinking agent water solution system normal and that material preparation adopts is incompatible, under high viscosity systems, crosslinking agent is difficult to mix with polyalcohol/clay soil material, causes that material property is inhomogeneous, preparation efficiency is low.
Summary of the invention
The object of this invention is to provide a kind of aerogel material.
Another object of the present invention is to provide a kind of preparation method of aerogel material.
Aerogel material of the present invention, be characterized in: described material is prepared from through aqueous solution blend, cross-linking radiation, freeze drying by polymer and clay, wherein polymer is counted 5-95% with aeroge weight, clay is counted 95-5% with aeroge weight, and aeroge density is between 0.03-0.20 g/cm3.
Described polymer is at least one in polyvinyl alcohol, polyethylene glycol oxide, natural rubber, polyacrylic acid, PVP, methylol chitin, carboxymethyl chitosan, hydroxymethyl starch, CMC, carragheen.
Described clay is one or more in imvite, tired de-stone, LAPONITE, synthetic mica, kaolin, vermiculite, sepiolite, concave convex rod, galapectite, layered double-hydroxide, diatomite, wollastonite, hydroxyapatite.
Described cross-linking radiation adopts high-energy ray, and high-energy ray type is one or more in gamma ray, electron beam, ion beam.
The preparation method of aerogel material of the present invention, in turn includes the following steps:
A. by polymer dissolution in deionized water, add clay, stir, until equally distributed suspension;
B. the suspension of step a) gained is carried out under high-energy ray to cross-linking radiation, the irradiation dose of high-energy ray is 1 kGy-200 kGy;
C. by the freezing rear freeze-drying of the irradiation product of step b) gained, form required aerogel material.
Compared with prior art, tool has the following advantages in the present invention:
1, due to aerogel material provided by the invention, to take polymer and clay be raw material, and preparation process only adopts water as solvent, adopts cryodesiccated method, makes preparation process environmental protection, and production efficiency is high.
2, because aerogel material provided by the invention adopts radiation mode cross-linking modified, do not need chemical cross-linking agent, thereby avoid the residual safety problem of bringing of crosslinking agent; Cross-linking radiation is efficiently controlled, and crosslink density is even, easily the product of large-scale production large scale stable performance; Cross-linking radiation reacts owing to easily occurring at boundary, thereby strengthens the adhesion strength between polymer and clay, contributes to improve the mechanical property of material; Cross-linking radiation mode is selectively low, and most of crosslinked polymer is had to universality.
3, technological operation of the present invention is simple, and cost is low, is easy to promote.
The specific embodiment
Embodiment given below is so that the invention will be further described.Be necessary to be pointed out that at this following examples can not be interpreted as limiting the scope of the invention; if the person skilled in the art in this field makes some nonessential improvement and adjustment according to the invention described above content to the present invention, still belong to protection domain of the present invention.
Prepared aerogel material performance sees attached list.What deserves to be explained is, in following embodiment performance, density is obtained divided by density calculation by the quality of material, modulus of compressibility is tested by Instron5565 universal testing machine, thermal conductivity factor records according to GB/T10801.1-2002, oxygen index (OI) records according to ISO4589-1984, and peak heat rate of release records (heat radiation power 50 kW/m by FTT taper calorimeter
2).
Embodiment 1
First by 0.8 g polyvinyl alcohol, (Mw 31,000 ~ 50,000, alcoholysis degree 99%) heating is dissolved in 100 mL deionized waters, after adding 15 g imvites, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 1 kGy, the ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 2
First 1 g imvite is added in 100 mL deionized waters, high-speed stirred is to even suspension, by 20 g polyvinyl alcohol, (Mw 31 again, 000 ~ 50,000, alcoholysis degree 99%) heating is dissolved in above-mentioned suspension, carries out the cross-linking radiation of accumulated dose 200 kGy under gamma ray, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 3
First by 10 g polyvinyl alcohol, (Mw 31,000 ~ 50,000, alcoholysis degree 99%) heating is dissolved in 100 mL deionized waters, add extremely evenly colloid of the rear high-speed stirred of the tired de-soil of 5 g, under gamma ray, carry out the cross-linking radiation of accumulated dose 100 kGy, the ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 4
First by 2 g polyvinyl alcohol (Mw31,000 ~ 50,000, alcoholysis degree 78%) heating is dissolved in 100 mL deionized waters, after adding 1 g LAPONITE, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 50 kGy, by product at-196 ° of C(liquid nitrogen baths) snap frozen is complete to ice-crystal growth, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 5
First by 3 g polyvinyl alcohol, (Mw 31,000 ~ 50,000 alcoholysis degree 99%) heating is dissolved in 100 mL deionized waters, after adding 4 g imvites, 4 g synthetic micas and 5 g fire retardant aluminium hydroxides, high-speed stirred is to even colloid, under electron beam, carry out the cross-linking radiation of accumulated dose 20 kGy, by product at-196 ° of C(liquid nitrogen baths) snap frozen is complete to ice-crystal growth, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 6
First by 5 g polyvinyl alcohol, (Mw 31,000 ~ 50,000 alcoholysis degree 99%) heating is dissolved in 100 mL deionized waters, after adding 9 g kaolin, high-speed stirred is to even colloid, under electron beam, carry out the cross-linking radiation of accumulated dose 10 kGy, by product at-196 ° of C(liquid nitrogen baths) snap frozen is complete to ice-crystal growth, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 7
First 5 g polyethylene glycol oxide heating are dissolved in 100 mL deionized waters, after adding 5 g vermiculites and 3 g fire retardant aluminium hydroxides, high-speed stirred is to even colloid, under electron beam, carry out the cross-linking radiation of accumulated dose 150 kGy, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 8
First 2 g natural rubbers are dissolved in 100 mL deionized waters, after adding 10 g sepiolites and 3 g lead powder, high-speed stirred is to even colloid, under ion beam, carry out the cross-linking radiation of accumulated dose 10 kGy, by product at-10 ° of C(refrigerators) to be refrigerated to ice-crystal growth complete, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 9
First 3 g polyacrylic acid are dissolved in 100 mL deionized waters, after adding 4 g imvites, 4 g concave convex rods and 4 g galapectites, high-speed stirred is to even colloid, under ion beam, carry out the cross-linking radiation of accumulated dose 5 kGy, by product at-10 ° of C(refrigerators) to be refrigerated to ice-crystal growth complete, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 10
First 2 g polyvinyl alcohol and 2 g carragheens are dissolved in 100 mL deionized waters, after adding 1 g galapectite and 10 g fire retardant magnesium hydroxides, high-speed stirred is to even colloid, under ion beam, carry out the cross-linking radiation of accumulated dose 5 kGy, by product at-30 ° of C(refrigerators) to be refrigerated to ice-crystal growth complete, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 11
First 3 g nature rubber latexes are scattered in 100 mL deionized waters, after adding 5 g layered double-hydroxides, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 10 kGy, by product at-30 ° of C(refrigerators) to be refrigerated to ice-crystal growth complete, at room temperature vacuum freeze-drying is to bone dry.
Embodiment 12
First 10 g polyvinyl alcohol and 5 g polyethylene glycol oxides are dissolved in 100 mL deionized waters, after adding 3 g diatomite, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 40 kGy, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 13
First 4 g carboxymethyl chitosans, 4 g hydroxymethyl starches and 4 g CMCs are dissolved in 100 mL deionized waters, after adding 2 g wollastonites, high-speed stirred is to even suspension, under gamma ray, carry out the cross-linking radiation of dosage 10 kGy, adopt again electron beam to carry out the cross-linking radiation of 10 kGy, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 14
First 2 g methylol chitins are dissolved in 100 mL deionized waters, after adding 8 g hydroxyapatites and 3 g aluminium hydroxides, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 60 kGy, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum freeze-drying is to bone dry.
Embodiment 15
First 2 g PVPs are dissolved in 100 mL deionized waters, after adding 8 g hydroxyapatites and 3 g lead powder, high-speed stirred is to even colloid, under gamma ray, carry out the cross-linking radiation of accumulated dose 30 kGy, ethanol bath by product at-78 ° of C(dry ice) snap frozen is complete to ice-crystal growth, and at room temperature vacuum drying is to freeze-drying completely.
Embodiment 16
Other conditions of the present embodiment are with embodiment 1, slightly.Difference is that the polyvinyl alcohol adding is 6 g, and imvite is 4 g.
Embodiment 17
Other conditions of the present embodiment are with embodiment 1, slightly.Difference is that the polyvinyl alcohol adding is 2 g, and imvite is 8 g.
Subordinate list:
A, B is comparative example.A is with embodiment 16, not cross-linking radiation; B is embodiment 17, not cross-linking radiation.
Claims (8)
1. an aerogel material, it is characterized in that: described material is prepared from through aqueous solution blend, cross-linking radiation, freeze drying by polymer and clay, wherein polymer is counted 5-95% with aeroge weight, and clay is counted 95-5% with aeroge weight, and aeroge density is between 0.03-0.20 g/cm
3.
2. aerogel material according to claim 1, is characterized in that: described polymer is at least one in polyvinyl alcohol, polyethylene glycol oxide, natural rubber, polyacrylic acid, PVP, methylol chitin, carboxymethyl chitosan, hydroxymethyl starch, CMC, carragheen.
3. aerogel material according to claim 1, is characterized in that: described clay is one or more in imvite, tired de-stone, LAPONITE, synthetic mica, kaolin, vermiculite, sepiolite, concave convex rod, galapectite, layered double-hydroxide, diatomite, wollastonite, hydroxyapatite.
4. aerogel material according to claim 1, is characterized in that: described cross-linking radiation adopts high-energy ray, and high-energy ray type is one or more in gamma ray, electron beam, ion beam.
5. a preparation method for aerogel material claimed in claim 1, is characterized in that: described preparation method in turn includes the following steps:
A. by polymer dissolution in deionized water, add clay, stir, until equally distributed suspension;
B. the suspension of step a) gained is carried out under high-energy ray to cross-linking radiation, the irradiation dose of high-energy ray is 1 kGy-200 kGy;
C. by the freezing rear freeze-drying of the irradiation product of step b) gained, form required aerogel material.
6. the preparation method of aerogel material according to claim 5, is characterized in that: described polymer is one or more in polyvinyl alcohol, polyethylene glycol oxide, natural rubber, polyacrylic acid, PVP, methylol chitin, carboxymethyl chitosan, hydroxymethyl starch, CMC, carragheen.
7. the preparation method of aerogel material according to claim 5, is characterized in that: described clay is one or more in imvite, tired de-stone, LAPONITE, synthetic mica, kaolin, vermiculite, sepiolite, concave convex rod, galapectite, layered double-hydroxide, diatomite, wollastonite, hydroxyapatite.
8. the preparation method of aerogel material according to claim 5, is characterized in that: described cross-linking radiation adopts high-energy ray, and high-energy ray type is one or more in gamma ray, electron beam, ion beam.
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