CN109701494A - Aerogel composite and preparation method thereof - Google Patents
Aerogel composite and preparation method thereof Download PDFInfo
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- CN109701494A CN109701494A CN201811627832.0A CN201811627832A CN109701494A CN 109701494 A CN109701494 A CN 109701494A CN 201811627832 A CN201811627832 A CN 201811627832A CN 109701494 A CN109701494 A CN 109701494A
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- melamine
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Abstract
The present invention provides a kind of preparation methods of aerogel composite, the following steps are included: melamine and formaldehyde are mixed, aeroge is added under conditions of stirring the formaldehyde-melamine mixture, the formaldehyde-melamine-aeroge mixture is heated, melamine performed polymer is prepared;The melamine performed polymer is mixed with curing agent, foaming agent, deionized water, expanding foam solution is prepared;Expanding foam solution is foamed to obtain foaming body, and be will be cured and annealed, and the modified melamine foamed plastic of aeroge is prepared.The present invention also provides the aerogel composites that above-mentioned preparation method obtains.The embodiment of the present invention is carried out complementary using the feature that partial size is smaller and melamine is porous of aeroge, can be obviously improved thermal coefficient, while improve aeroge itself crisp, the frangible disadvantage of matter.
Description
Technical field
The present invention relates to thermal insulation material technical fields, are related to aerogel composite and preparation method thereof.
Background technique
Aeroge is referred to as most light by 10% solid and 90% gas composition as novel thermal insulation material
Thermal insulation material, and its special structure and thermal conduction mechanism, referred to as heat-insulation material of new generation.
Aeroge and silica solution are highly porous solid, because the major part of its volume is by Kong Zucheng.Aeroge can
Based on such as silicate but it may be based on plastics or carbon.The diameter of aerogel pores is in nanometer range.Due to their high pore volume,
Aeroge is particularly useful as the thermal insulation material for combining excellent thermal insulation property and low-density.Aeroge initially as
Grain exists, and can be used adhesive by moulding process for example by being pressed to form panel.
However aeroge has the shortcomings that matter is crisp, frangible, it is difficult to practical application;Aeroge is mainly and glass on the market at present
Compound form supply, such material preparation process are that addition glass is compound in aeroge sol-process or sprays aeroge
Be prepared to glass surface, such method there are the problem of be that the aeroge prepared is easy picking, thermal coefficient is higher
(20-22mk/mw), and the glass diameter and length that use are smaller, are easy to cause allergy etc. to react human body.
Also there is the composite material of some aeroges at present, as EP-A-1146070A2 and WO-A-2007/23118 is public
It has opened respectively with ammonium salt and sodium metasilicate impregnated melamine-formaldehyde foam;DE-A-102007009127A1, which is disclosed, to be based on having
The fiber enhanced foam of the melamine formaldehyde resin of 0.5-50 weight % fiber content;Long or staple fiber glass, carbon or three
Cymel is used as fiberfill;WO-A-2009/021963A1 discloses the side for producing a kind of abrasive foam
Method, the abrasive foam are calculated as 0.01-50 weight based on melamine-formaldehyde condensation product and containing the weight based on precondensate
Measure the inorganic nanoparticles of %.
The performance of well known materials is no longer complies with increased demand, especially with respect to thermal conductivity and intensity.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing aerogel composite;
Another object of the present invention is to provide the aerogel composites that the above method is prepared.
To achieve the above object, on the one hand, the embodiment of the invention discloses a kind of preparation method of aerogel composite,
The following steps are included:
S1, melamine and formaldehyde are mixed, obtains formaldehyde-melamine mixture;
S2, aeroge is added under conditions of stirring the formaldehyde-melamine mixture, obtains formaldehyde-melamine-
Aeroge mixture heats the formaldehyde-melamine-aeroge mixture under the conditions of 80-95 DEG C of temperature, is prepared three
Poly cyanamid performed polymer;
S3, the melamine performed polymer is mixed with curing agent, foaming agent, deionized water, expanding foam solution is prepared;
S4, the expanding foam solution are foamed to obtain foaming body at a temperature of microwave radiation forms 40-70 DEG C, and by the hair
Foam is solidified at a temperature of 80-120 DEG C, then anneals under the conditions of 120-260 DEG C of hot-air, melamine is prepared
Foam.
As the further improvement of embodiment of the present invention, the preparation method further includes three that step S4 is prepared
Poly cyanamid foam carries out hot compression processing.
As the further improvement of embodiment of the present invention, the formaldehyde-is being added in aeroge described in the step S2
Further include the steps that dissolving the formaldehyde-melamine mixture, the polarity with polar solvent before melamine mixture
Solvent is any in N,N-dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide, ethyl alcohol, acetone, ethyl acetate
It is a kind of.
As the further improvement of embodiment of the present invention, the molar ratio of melamine and the formaldehyde in the step S1
For 1:2-1:5.
As the further improvement of embodiment of the present invention, aeroge additional amount is melamine weight in the step S2
10-50%.
As the further improvement of embodiment of the present invention, the power of microwave radiation is 40-50KW in the step S4.
As the further improvement of embodiment of the present invention, the duration of the annealing operation is 25-60 minutes.
As the further improvement of embodiment of the present invention, the hot compression processing of melamine foamed plastic is specific in the S5
Mode are as follows: the modified melamine foamed plastic of the aeroge being prepared is warming up to 120-150 DEG C, then uses the pressure of 5-10MPa
Force contracting;
After being kept for described compressive state 1-2 hours, the melamine foamed plastic of hot compression is prepared.
As the further improvement of embodiment of the present invention, the aeroge is organic silica aerogel, the organosilicon gas
Gel is organosilane precursor by hydrolysis-sol-gel-drying process preparation;
The organosilane precursor is selected from least one of ethyl orthosilicate, silicon tetrachloride.
On the other hand, the embodiment of the invention discloses a kind of aerogel composites, are prepared by above-mentioned method.
The embodiment of the present invention has the following beneficial effects:
1, the embodiment of the present invention provides a kind of novel aerogel composite, and aeroge and porous nanometer material are passed through
The mode of interface cohesion is combined with each other, and 95% or more, aeroge is covered the percent opening of open-cell material by way of coating
It on open-cell material surface or infiltrates through in open-cell material gap, so that reduction is led by the air ' fixing ' in open-cell material
Hot coefficient;
2, it is the modified aperture melamine of aeroge that the embodiment of the present invention, which provides the novel aerogel composite of one kind,
Foam can be avoided the frangible feature of aeroge aeroge itself using open-cell material as matrix;
3. the present embodiments relate to modification aerogel composite preparation process relative ease it is easy, it is at low cost
It is honest and clean, there is great application prospect;
4. the modified aerogel composite of this programme is not easy to lose powder, using the partial size of aeroge is smaller and melamine
Porous feature carry out it is complementary, the shortcomings that thermal coefficient capable of being obviously improved, while improving aeroge itself.
Specific embodiment
To keep the purposes, technical schemes and advantages of the application clearer, below in conjunction with the application specific embodiment
Technical scheme is clearly and completely described.Obviously, described embodiment is only that the application a part is implemented
Mode, rather than whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not being made
Every other embodiment obtained, shall fall in the protection scope of this application under the premise of creative work.
The embodiment of the invention discloses a kind of preparation methods of aerogel composite, comprising the following steps:
S1, melamine and formaldehyde are mixed, obtains formaldehyde-melamine mixture;Wherein, melamine and formaldehyde
Molar ratio is 1:2-1:5.
S2, aeroge is added under conditions of stirring the formaldehyde-melamine mixture, obtains formaldehyde-melamine-
Aeroge mixture heats the formaldehyde-melamine-aeroge mixture under the conditions of 80-95 DEG C of temperature, is prepared three
Poly cyanamid performed polymer;Preferably, aeroge additional amount is the 10-50% of melamine weight.
S3, the melamine performed polymer is mixed with curing agent, foaming agent, deionized water, expanding foam solution is prepared;
S4, the expanding foam solution are foamed to obtain foaming body at a temperature of microwave radiation forms 40-70 DEG C, and by the hair
Foam is solidified at a temperature of 80-120 DEG C, is then annealed under the conditions of 120-260 DEG C of hot-air, annealing operation it is lasting when
Between be 25-60 minutes, melamine foamed plastic is prepared.Wherein, the power of microwave radiation is 40-50KW.
S5, the above-mentioned melamine foamed plastic being prepared is subjected to hot compression processing.
Wherein, aeroge described in step S2 further includes using polarity before the formaldehyde-melamine mixture is added
Solvent dissolves the formaldehyde-melamine mixture, and the preferred n,N-Dimethylformamide of polar solvent is implementable at other
Mode in, be also selected from N-Methyl pyrrolidone, dimethyl sulfoxide, ethyl alcohol, acetone, any one in ethyl acetate.
The concrete mode of the hot compression processing of melamine foamed plastic in the S5 are as follows: the aeroge being prepared is modified
Melamine foamed plastic is warming up to 120-150 DEG C, is then compressed with the pressure of 5-10MPa;
After being kept for described compressive state 1-2 hours, the melamine foamed plastic of hot compression is prepared.
In embodiments of the present invention, aeroge is organic silica aerogel, and organic silica aerogel is that organosilane precursor passes through
Hydrolysis-sol-gel-drying process preparation;Wherein, organosilane precursor in ethyl orthosilicate, silicon tetrachloride at least
It is a kind of.
On the other hand, the embodiment of the invention discloses a kind of aerogel composites, are prepared by above-mentioned method.
Wherein, organosilane precursor sol-gel process specifically includes the following steps:
Organosilane precursor is added in absolute alcohol, graphene oxide is then added and carries out ultrasonic disperse, acid is added, adjusts
PH value is saved to 1-3, promotes the hydrolysis of organosilane precursor;
Ammonium hydroxide is added, adjusts pH value to alkalinity to 10-12, carries out colloidal sol condensation course, be then allowed to stand and form gel overnight.
After gel process, aging can also be carried out to the gel of preparation, hydrophobic modifier is added and is blocked;Institute
The hydrophobic modifier of selection includes trim,ethylchlorosilane, hexamethyldisiloxane, methyltriethoxysilane and methyl trimethoxy oxygen
At least one of base silane.
In the present embodiment, aging is carried out to gel, aging temperature is controlled at 40-60 DEG C, aging a length of 48 hours;Add
It is 24 hours a length of when modified after entering hydrophobic modifier;At interval of 12 hours, it is molten that the replacement polarity was washed with nonpolar solvent
Agent repeats 5-8 times;Nonpolar solvent is preferably n-hexane in the present embodiment.
In embodiments of the present invention, the mode of the drying can be selected from as supercritical carbon dioxide drying, freeze-drying
Or soxhlet extraction.
Concrete example is prepared according to the method in above-described embodiment, and the heat preservation property of example in detail below is tested, is obtained
To following experimental result:
From the point of view of test result, the thermal coefficient of the sample prepared by the above method all decreases:
Test uses standard GB/T/T3399, and wherein cold plate temperature is 5 DEG C, and hot plate temperature is 20 DEG C;Comparative example is not
The melamine foamed plastic after the hot compression of aeroge modification.
In embodiments of the present invention, the calculating of the porosity of the modified melamine foamed plastic of the aeroge being related to is to pass through
The ratio of void volume and total measurement (volume) can be measured by nitrogen adsorption and desorption (<100nm) and mercury injection method (>100nm);And it relates to
And the nanoporous arrived, it is thus understood that mean aperture in the hole of the particle of 0.1-500nm, especially < 200nm, more preferably <
100nm (D50) and porosity in particular 50-99%, more specifically 70-99%, more preferable 80-99%.
In the present embodiment, preferred organic silicon sol refers to the two of the high temperature distillation obtained by hydrolysis of silicon tetrachloride
Silica and the primary particle diameter preferably with 5-50nm (D50);D50 value refer to the particle thinner than the value be 50% and more than it
Thick particle is 50%.
In embodiments of the present invention, melamine formaldehyde resin is expandable reaction resin, more preferably be can be processed into
The melamine formaldehyde resin of open celled foam, the open celled foam have the≤density of 25g/l, that is, 1.6-25g/l, preferably 2-
15g/l, more preferable 3-13g/l and more specifically 4-12g/l and/or aperture are between 10-1000 μm and preferably at 50-300 μm.
In embodiments of the present invention, in melamine resin foam the ratio of nanoporous particles preferably in 1-99 body
Product %, more preferably in 5-95 volume %, even more preferably 10-90 volume %.
Therefore, present invention is preferably related to foams of the invention, and wherein foam can also include nanoporous particles or it is mixed
Object is closed, wherein or mixtures thereof nanoporous particles are 1-99 volume %, preferably in 5-95 volume %, more preferably 10-90 body
Product %.
By the way that the above concrete example is compared with the aeroge comparative example do not modified and be modified, the embodiment of the present invention
It has the following beneficial effects:
1, the embodiment of the present invention provides a kind of novel aerogel composite, and aeroge and porous nanometer material are passed through
The mode of interface cohesion is combined with each other, and 95% or more, aeroge is covered the percent opening of open-cell material by way of coating
It on open-cell material surface or infiltrates through in open-cell material gap, so that reduction is led by the air ' fixing ' in open-cell material
Hot coefficient;
2, it is the modified aperture melamine of aeroge that the embodiment of the present invention, which provides the novel aerogel composite of one kind,
Foam can be avoided the frangible feature of aeroge aeroge itself using open-cell material as matrix;
3. the present embodiments relate to modification aerogel composite preparation process relative ease it is easy, it is at low cost
It is honest and clean, there is great application prospect;
4. the modified aerogel composite of this programme is not easy to lose powder, using the partial size of aeroge is smaller and melamine
Porous feature carry out it is complementary, the shortcomings that thermal coefficient capable of being obviously improved, while improving aeroge itself.
It should be appreciated that although this specification is described in terms of embodiments, but not each embodiment only includes one
A independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should will say
As a whole, the technical solution in each embodiment may also be suitably combined to form those skilled in the art can for bright book
With the other embodiments of understanding.
The series of detailed descriptions listed above only for feasible embodiment of the invention specifically
Protection scope that is bright, being not intended to limit the invention, it is all without departing from equivalent implementations made by technical spirit of the present invention or change
More it should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of aerogel composite, which is characterized in that the preparation method comprises the following steps:
S1, melamine and formaldehyde are mixed, obtains formaldehyde-melamine mixture;
S2, aeroge is added under conditions of stirring the formaldehyde-melamine mixture, obtains formaldehyde-melamine-airsetting
Glue mixture heats the formaldehyde-melamine-aeroge mixture under the conditions of 80-95 DEG C of temperature, melamine is prepared
Amine performed polymer;
S3, the melamine performed polymer is mixed with curing agent, foaming agent, deionized water, expanding foam solution is prepared;
S4, the expanding foam solution are foamed to obtain foaming body at a temperature of microwave radiation forms 40-70 DEG C, and by the foaming body
Solidified at a temperature of 80-120 DEG C, then annealed under the conditions of 120-260 DEG C of hot-air, melamine bubble is prepared
Foam.
2. the preparation method of aerogel composite according to claim 1, which is characterized in that the preparation method is also wrapped
It includes the melamine foamed plastic that step S4 is prepared and carries out hot compression processing.
3. the preparation method of aerogel composite according to claim 1, which is characterized in that described in the step S2
Aeroge further includes dissolving the formaldehyde-melamine with polar solvent before the formaldehyde-melamine mixture is added
The step of mixture, the polar solvent be selected from n,N-Dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide, ethyl alcohol,
Any one in acetone, ethyl acetate.
4. the preparation method of aerogel composite according to claim 1, which is characterized in that trimerization in the step S1
The molar ratio of cyanamide and the formaldehyde is 1:2-1:5.
5. the preparation method of aerogel composite according to claim 1, which is characterized in that airsetting in the step S2
Glue additional amount is the 10-50% of melamine weight.
6. the preparation method of aerogel composite according to claim 1, which is characterized in that microwave in the step S4
The power of radiation is 40-50KW.
7. the preparation method of aerogel composite according to claim 1, which is characterized in that the annealing operation is held
The continuous time is 25-60 minutes.
8. the preparation method of aerogel composite according to claim 1, which is characterized in that melamine in the S5
The concrete mode of the hot compression processing of foam are as follows: the modified melamine foamed plastic of the aeroge being prepared is warming up to 120-
It 150 DEG C, is then compressed with the pressure of 5-10MPa;
After being kept for described compressive state 1-2 hours, the melamine foamed plastic of hot compression is prepared.
9. the preparation method of aerogel composite according to claim 1, which is characterized in that the aeroge is organic
Silica aerogel, organic silica aerogel are organosilane precursors by hydrolysis-sol-gel-drying process preparation;
The organosilane precursor is selected from least one of ethyl orthosilicate, silicon tetrachloride.
10. a kind of aerogel composite, which is characterized in that the preparation of the method as described in -9 any one according to claim 1
It obtains.
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CN110183716A (en) * | 2019-05-13 | 2019-08-30 | 浙江工业大学 | A kind of preparation method of fire-retardant heat insulation fiber type element base aeroge |
CN112795048A (en) * | 2021-02-03 | 2021-05-14 | 峰特(浙江)新材料有限公司 | Mixed aerogel modified melamine foam and application thereof |
CN113150361A (en) * | 2021-02-03 | 2021-07-23 | 孚莱孚(上海)新材料有限公司 | Silica-starch aerogel modified melamine foam and application thereof |
CN115058049A (en) * | 2022-06-09 | 2022-09-16 | 西北工业大学深圳研究院 | Variable gradient structure flexible aerogel, preparation method thereof and flexible pressure sensor |
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CN113150361A (en) * | 2021-02-03 | 2021-07-23 | 孚莱孚(上海)新材料有限公司 | Silica-starch aerogel modified melamine foam and application thereof |
CN115058049A (en) * | 2022-06-09 | 2022-09-16 | 西北工业大学深圳研究院 | Variable gradient structure flexible aerogel, preparation method thereof and flexible pressure sensor |
CN115058049B (en) * | 2022-06-09 | 2023-05-05 | 西北工业大学深圳研究院 | Variable-gradient structure flexible aerogel, preparation method thereof and flexible pressure sensor |
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