CN106947198A - A kind of aerogel material and preparation method thereof - Google Patents
A kind of aerogel material and preparation method thereof Download PDFInfo
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- CN106947198A CN106947198A CN201710248950.XA CN201710248950A CN106947198A CN 106947198 A CN106947198 A CN 106947198A CN 201710248950 A CN201710248950 A CN 201710248950A CN 106947198 A CN106947198 A CN 106947198A
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- C08L43/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium or a metal; Compositions of derivatives of such polymers
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J2343/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium or a metal; Derivatives of such polymers
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- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/02—Homopolymers or copolymers of hydrocarbons
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
Abstract
The invention discloses a kind of aerogel material and preparation method thereof, by the way that double bond containing polymer emulsion is well mixed with clay, freeze-drying post-crosslinking is formed, and obtains density for 0.05~0.5g/cm3Aerogel material；The double bond containing polymer emulsion includes one of which or several in polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion；The preparation method includes：(1), double bond containing polymer emulsion is well mixed with clay in proportion；(2), gained in (1) is freeze-dried；(3), gained in (2) is heated or cross-linking radiation, aerogel material is produced；The present invention is by selecting double bond containing polymer emulsion, and making the aerogel material of acquisition has excellent water resistance and mechanical property, while the size and stable appearance of product are good；Crosslink material process only needs to heat or irradiate, mild condition；Simple, low cost, easy processing with technological operation, it is easy to the characteristic such as popularization.
Description
Technical field
The present invention relates to aerogel material technical field, more particularly to a kind of aerogel material and preparation method thereof.
Background technology
Polymer/clay aeroge is a kind of new material that latest developments go out.The material has stratiform or netted sky
Between structure, porosity is high, density is low, the low feature of thermal conductivity factor, has in fields such as heat-insulation and heat-preservation, packaging protection, sorbing materials
Wide application prospect.
The preparation of polymer/clay aeroge is mainly carried out by way of freeze-drying to polymer/clay colloid
Processing, obtains aerogel material.Because the polymer of use is mainly water-soluble polymer, therefore resulting polymers water resistance is very
Difference, material easily absorbs water in atmosphere, causes thermal conductivity factor drastically to decline, and chance water then dissolves, and seriously restricts its application.
The mechanical property of polymer/clay aeroge is not ideal enough, it is necessary to change to it in the application in some fields
Property processing.Mechanical property to aeroge by way of the blended fiber of physics is improved to some extent, but effect is not
Significantly.The mechanical property that may be such that aeroge by the method for chemical crosslinking is effectively improved, such as old Chen etal. et al. are situated between
The method for adding divinyl sulfone in alkaline environment continued may be such that polyvinyl alcohol crosslinked so that Mechanical Properties of Aerogels is than uncrosslinked
When have the raising (Polymer, 2012,53,5825-5831) of the order of magnitude；The method for the crosslinking with radiation that CN103599734 is mentioned,
Can equally significantly improve the mechanical property of aeroge, but require that polymer is can be with the polymer of crosslinking with radiation.Chemical crosslinking
Although material mechanical performance can be effectively improved, needs first react generation gel in solution environmental, then are freezed.In freezing
When, ice crystal will be damaged to gel network structure, cause to produce stress in material, and equidimension is shunk after freezing
The phenomenon of change.
The content of the invention
For the drawbacks described above and problem of prior art, the purpose of the present invention is to be synthesized for airsetting collagen-based materials and modified
Demand provides a kind of aerogel material and preparation method thereof, by selecting double bond containing polymer, assigns material excellent water-fast
Performance and mechanical property, while assigning material good size and stable appearance.
In order to achieve the above object, the present invention provides following technical scheme：
A kind of aerogel material, by the way that polymer emulsion is well mixed with clay, freeze-drying post-crosslinking is formed.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：The gas
Gel rubber material is counted using polymer content as 100 parts, and the content of clay is 10 parts~500 parts.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：It is described glutinous
Soil includes montmorillonite, tired de- stone, kaolin, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxyapatite one of which or several
Kind；Using montmorillonite, the tired nano material for taking off stone, kaolin, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxy apatites,
It has it is cheap be easy to get, the characteristics of prepared aerogel material excellent in mechanical performance.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：It is described poly-
Compound emulsion is double bond containing polymer emulsion；The polymer emulsion of double bond is crosslinked under can heating or irradiate after freeze drying,
Aerogel structure is not had a negative impact, it is to avoid crosslinking before the freezing mentioned in reporting before this is so as to cause lyophilized rear material hair
The raw phenomenon shunk.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：It is described to contain
The polymer emulsion of double bond includes polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion one of which or several；
Such polymer emulsion is the material of building trade large-scale use, with cheap, it is easy to the spy of large-scale industrial production
Property.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：It is described to hand over
Connection uses heat cross-linking or cross-linking radiation；Double bond containing polymer emulsion heating or cross-linking radiation are without additionally addition chemical crosslinking
Agent, can greatly save time cost and financial cost in the industrial production.
Further is that aerogel material of the present invention is better achieved, especially using following set-up modes：The gas
The density of gel rubber material is 0.05~0.5g/cm3.
A kind of preparation method of aerogel material, for preparing described aerogel material, this method comprises the following steps：
(1), polymer emulsion is well mixed with clay in proportion；
(2), gained in (1) is freeze-dried；
(3) gained in (2), is subjected to heat cross-linking or cross-linking radiation, produced.
Further is the preparation method for being better achieved aerogel material of the present invention, especially uses following setting sides
Formula：The clay includes montmorillonite, tired de- stone, kaolin, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxyapatite wherein
It is one or more of.
Further is the preparation method for being better achieved aerogel material of the present invention, especially uses following setting sides
Formula：The aerogel material is counted using polymer content as 100 parts, and the content of clay is 10 parts~500 parts；The polymer emulsion
Including following double bond containing polymer emulsion one of which or several：Polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicon
Acrylic emulsion.
The present invention prepares aerogel material by the material for selecting nonessential use cross-linking radiation mode to be crosslinked,
Polymer emulsion and clay after being mainly well mixed using freeze-drying are frozen into ice, then gather heat cross-linking or spoke
Aerogel material is obtained according to crosslinking.Therefore, for person skilled in art, in the implementation process for carrying out freeze-drying,
Parameters in freezing dry process, including cryogenic temperature, polymer concentration etc. can be determined to material modification according to prior art
Gimmick, influences on the material morphology after freeze-drying, density formation.
For the best characteristic for reaching low-density of the present invention, finished product density of the present invention is controlled in 0.05~0.5g/cm3,
So that the present invention has lightweight nature, and in a preferred embodiment, the modulus of compressibility energy of 0.05g/cm3 density Example finished products
0.6MPa is reached, and thermal conductivity factor is only 0.028W/mK.
It is noted that for modifying agent and materials such as material modification addition surfactant, fire retardant, reinforcing fibers,
Material morphology, density, aperture are transformed, on the premise of present invention objective is met, the protection of the present invention is belonged to
Scope.
Except in embodiment or clearly state in addition, it will be understood that the weight used in specification and claims
Number numerical value can be changed according to term " about " in all cases.Therefore, unless indicated to the contrary, otherwise right will
Numerical parameter listed in book and the following description book is asked to be approximation, can be according to the performance that the present invention is gone for
Change.At least, rather than in order to limit the implementation of this principle equivalent to right, each numerical parameter at least should
When being explained according to effective digital and with common rounding-off method.
Although the number range and parameter of listing wide scope of the present invention are the numerical value listed in approximation, specific embodiment
Record as accurate as possible.But, any one numerical value natively has certain error.The error is its corresponding measurement side
The inevitable outcome of the standard deviation drawn in method.
A technical scheme in above-mentioned technical proposal has the advantages that：
1st, by selecting double bond containing polymer emulsion, make the aerogel material of acquisition with existing aeroge compared with excellent
Different water resistance and mechanical property, while the size and stable appearance of product are good；
2nd, technological operation is simple, low cost, easy processing, it is easy to promote.
Another technical scheme in above-mentioned technical proposal has the advantages that：
1st, by selecting double bond-contained polymer emulsion, making the aerogel material of acquisition has excellent water resistance and mechanics
Performance, while the size and stable appearance of product are good；
2nd, crosslink material process only needs to heat or irradiate, mild condition；
3rd, technological operation is simple, low cost, easy processing, it is easy to promote；And heat cross-linking is safer than cross-linking radiation,
Effectively, energy consumption is low, is easily realized without expensive device.
Embodiment
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described, it is clear that
Described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made is belonged to
The scope of protection of the invention.
Embodiment 1：
A kind of aerogel material, by the way that polymer emulsion is well mixed with clay, freeze-drying post-crosslinking is formed.
Embodiment 2：
The present embodiment is further optimized on the basis of above-described embodiment, further for institute of the present invention is better achieved
Aerogel material is stated, especially using following set-up modes：The aerogel material is counted using polymer content as 100 parts, clay
Content is 10 parts~500 parts.
Embodiment 3：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The bright aerogel material, especially using following set-up modes：The clay include montmorillonite, tired de- stone, kaolin, vermiculite,
One or more in sepiolite, hydrotalcite, diatomite, hydroxyapatite；Using montmorillonite, tired de- stone, kaolin, vermiculite,
Sepiolite, hydrotalcite, diatomite, the nano material of hydroxy apatites, its have it is cheap be easy to get, prepared aeroge
The characteristics of material mechanical performance is excellent.
Embodiment 4：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The bright aerogel material, especially using following set-up modes：The polymer emulsion is double bond containing polymer emulsion；Double bond
Polymer emulsion can heat or irradiate after freeze drying under crosslink, aerogel structure is not had a negative impact, it is to avoid this
Crosslinking before the freezing mentioned in preceding report is so as to cause the phenomenon of lyophilized rear material undergoing shrinkage.
Embodiment 5：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The bright aerogel material, especially using following set-up modes：The double bond containing polymer emulsion includes polyacrylate breast
One or more in liquid, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion；Such polymer emulsion is that building trade makes on a large scale
Material, with cheap, it is easy to the characteristic of large-scale industrial production.
Embodiment 6：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The bright aerogel material, especially using following set-up modes：The crosslinking uses heat cross-linking or cross-linking radiation；It is double bond containing
Polymer emulsion is heated or cross-linking radiation is without additionally adding chemical cross-linking agent, and time cost can be greatlyd save in the industrial production
And financial cost.
Embodiment 7：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The bright aerogel material, especially using following set-up modes：The density of the aerogel material is 0.05~0.5g/cm3.
Embodiment 8：
The present embodiment is further optimized on the basis of any of the above-described embodiment, a kind of preparation side of aerogel material
Method, for preparing described aerogel material, this method comprises the following steps：
(1), polymer emulsion is well mixed with clay in proportion；
(2), gained in (1) is freeze-dried；
(3) gained in (2), is subjected to heat cross-linking or cross-linking radiation, produced.
Embodiment 9：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The preparation method of the bright aerogel material, especially using following set-up modes：The clay includes montmorillonite, tired de- stone, height
Ridge soil, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxyapatite one of which or several.
Embodiment 10：
The present embodiment is further optimized on the basis of any of the above-described embodiment, and further is that this hair is better achieved
The preparation method of the bright aerogel material, especially using following set-up modes：The aerogel material using polymer content as
100 parts of meters, the content of clay is 10 parts~500 parts；The polymer emulsion is included in following double bond containing polymer emulsions
It is one or more of：Polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion.
Embodiment 11：
First 2g montmorillonites are added in 100mL polyacrylate dispersions (3wt%), high-speed stirred to homogeneous colloids, by institute
Obtain colloid complete to ice-crystal growth in -196 DEG C of snap frozens, be dried under vacuum to freeze completely at room temperature, 100 DEG C of heating are handed over
Connection.
Embodiment 12：
First 20g tired de- stone and 20g kaolin are added in 100mL styrene-acrylic emulsions (4wt%) and pure-acrylic emulsion (4wt%),
High-speed stirred is to homogeneous colloids, and obtained colloid is complete to ice-crystal growth in -196 DEG C of snap frozens, and vacuum is done at room temperature
It is dry to completely freeze, 30kGy cross-linking radiations.
Embodiment 13：
First 2g hydrotalcites, 2g diatomite and 6g hydroxyapatites are added in 100mL silicone acrylic emulsions (10wt%), high-speed stirring
Mix to homogeneous colloids, obtained colloid is complete to ice-crystal growth in -196 DEG C of snap frozens, it has been dried under vacuum at room temperature
It is complete lyophilized, 80 DEG C of heat cross-linkings.
Embodiment 14：
First 2g vermiculites and 3g sepiolites are added in 100mL pure-acrylic emulsions (5wt%), high-speed stirred to homogeneous colloids, will
Obtained colloid completely, is dried under vacuum to freezes completely at room temperature in -196 DEG C of snap frozens to ice-crystal growth, 110 DEG C of heating
Crosslinking.
Embodiment 15：
First 2g hydroxyapatites are added in 100mL styrene-acrylic emulsions (20wt%), high-speed stirred to homogeneous colloids will be obtained
Obtain colloid complete to ice-crystal growth in -196 DEG C of snap frozens, be dried under vacuum to freeze completely at room temperature, 10kGy irradiation is handed over
Connection.
Embodiment 16：
First the tired de- stones of 10g are added in 100mL polyacrylate dispersions (10wt%) and silicone acrylic emulsion (20wt%), at a high speed
Colloid is stirred until homogeneous, obtained colloid is complete to ice-crystal growth in -196 DEG C of snap frozens, it is dried under vacuum at room temperature
Freeze completely, 50kGy cross-linking radiations.
Embodiment 17：
First 7g hydrotalcites are added in 100mL silicone acrylic emulsions (3wt%), high-speed stirred to homogeneous colloids, by obtained glue
Body completely, is dried under vacuum to freezes completely at room temperature in -196 DEG C of snap frozens to ice-crystal growth, 20kGy cross-linking radiations.
Embodiment 18：
First 10g sepiolites, 15g hydroxyapatites are added in 100mL silicone acrylic emulsions (10wt%), high-speed stirred is to uniform
Colloid, obtained colloid is complete to ice-crystal growth in -196 DEG C of snap frozens, it is dried under vacuum to freeze completely at room temperature,
120 DEG C of heat cross-linkings.
Embodiment 19：
10g diatomite and 13g hydroxyapatites are first added into 100mL polyacrylate dispersions (10wt%) and styrene-acrylic emulsion
In (10wt%), high-speed stirred to homogeneous colloids is complete to ice-crystal growth in -196 DEG C of snap frozens by obtained colloid, in room
It is dried under vacuum to and freezes completely under temperature, 90 DEG C of heat cross-linkings.
Embodiment 20：
First 4g montmorillonites are added in 100mL pure-acrylic emulsions (10wt%), high-speed stirred to homogeneous colloids, by obtained glue
Body completely, is dried under vacuum to freezes completely at room temperature in -196 DEG C of snap frozens to ice-crystal growth, 40kGy cross-linking radiations.
Aerogel material performance obtained by above-described embodiment 11~20 see the table below.What deserves to be explained is, above-mentioned each implementation
In example performance, density is removed by the quality of material and obtained in terms of volume, and modulus of compressibility is by Instron5565 universal testing machines
Test, thermal conductivity factor is measured according to GB/T10801.1-2002, and oxygen index (OI) is measured according to ISO4589-1984
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention described should be defined by scope of the claims.
Claims (10)
1. a kind of aerogel material, it is characterised in that：By the way that polymer emulsion is well mixed with clay, post-crosslinking is freeze-dried
Form.
2. a kind of aerogel material according to claim 1, it is characterised in that：The aerogel material is with polymer content
For 100 parts of meters, the content of clay is 10 parts~500 parts.
3. a kind of aerogel material according to claim 1, it is characterised in that：The clay include montmorillonite, tired de- stone,
Kaolin, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxyapatite one of which or several.
4. a kind of aerogel material according to claim 1, it is characterised in that：The polymer emulsion is double bond containing poly-
Compound emulsion.
5. a kind of aerogel material according to claim 4, it is characterised in that：The double bond containing polymer emulsion includes
Polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion one of which or several.
6. a kind of aerogel material according to any one of Claims 1 to 5, it is characterised in that：The crosslinking is using heating
Crosslinking or cross-linking radiation.
7. a kind of aerogel material according to any one of Claims 1 to 5, it is characterised in that：The aerogel material
Density is 0.05~0.5g/cm3。
8. a kind of preparation method of aerogel material, for preparing the aerogel material as described in claim any one of 1-7, its
It is characterised by that this method comprises the following steps：
(1), polymer emulsion is well mixed with clay in proportion；
(2), gained in (1) is freeze-dried；
(3) gained in (2), is subjected to heat cross-linking or cross-linking radiation, produced.
9. a kind of preparation method of aerogel material according to claim 8, it is characterised in that：The clay includes covering de-
Soil, tired de- stone, kaolin, vermiculite, sepiolite, hydrotalcite, diatomite, hydroxyapatite one of which or several.
10. a kind of preparation method of aerogel material according to claim 8 or claim 9, it is characterised in that：The airsetting glue material
Material is counted using polymer content as 100 parts, and the content of clay is 10 parts~500 parts；The polymer emulsion includes following containing double bond
Polymer emulsion one of which or several：Polyacrylate dispersion, styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion.
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| CN107746481A (en) * | 2017-09-16 | 2018-03-02 | 南京工程学院 | A kind of NR latex/clay organic aerogel composite and preparation method thereof |
| CN108212089A (en) * | 2018-02-05 | 2018-06-29 | 江苏科技大学 | A kind of function bast-fibre biological matter carbon aerogels and preparation method and application |
| CN109897210A (en) * | 2019-01-16 | 2019-06-18 | 中国制浆造纸研究院有限公司 | A kind of preparation method of cellulose composite aerogel |
| CN112899804A (en) * | 2021-03-26 | 2021-06-04 | 江苏达胜伦比亚生物科技有限公司 | Novel vinylon preparation method |
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