CN110144095A - A kind of Organic-inorganic composite nano heat-insulating film - Google Patents
A kind of Organic-inorganic composite nano heat-insulating film Download PDFInfo
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- CN110144095A CN110144095A CN201910416479.XA CN201910416479A CN110144095A CN 110144095 A CN110144095 A CN 110144095A CN 201910416479 A CN201910416479 A CN 201910416479A CN 110144095 A CN110144095 A CN 110144095A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K2003/0812—Aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses a kind of Organic-inorganic composite nano heat-insulating films, belong to technical field of composite materials.The Organic-inorganic composite nano heat-insulating film that the present invention develops includes functional stuffing, ultraviolet absorber, ethyl acetate, coupling agent, adhesive, wherein functional stuffing is to make compound functional stuffing by oneself, in functional stuffing preparation, it first disperses nano graphene oxide in oleic acid, adds dehydrated alcohol, esters of silicon acis and organo-aluminium, primary cladding microballoon is made in heating stirring reaction；It is restored again with the ethanol solution of hydrazine hydrate, primary cladding microballoon must be restored；The primary cladding microballoon of reduction and dopamine-gelatin dispersion liquid are stirred, secondary cladding microballoon is made；After itself and silver nitrate solution are mixed dispersion again, precipitating reagent is added dropwise, is made and coats microballoon three times；After its slowly heating charing, sintering is further heated up, sintering feed is obtained；After gained sintering feed is impregnated with sodium hydroxide solution again, filtering, washing and drying are to get the compound functional stuffing of self-control.
Description
Technical field
The invention discloses a kind of Organic-inorganic composite nano heat-insulating films, belong to technical field of composite materials.
Background technique
Thermal isolation film has high visible light transmissivity, low ultraviolet transmission rate, Gao Hong as the energy-efficient means of simple glass are improved
The characteristics of outer rejection rate.Very, but thermal and insulating performance is very poor for traditional glass energy light transmission, and because glass breaking
Caused by security risk be also extremely serious.Currently, glass is widely used on the building doors and windows of various regions with pad pasting,
Or it is using low emissivity glass or using vacuum interlayer glass come heat-insulated, or pastes thermal isolation film on glass and reduce heat
The transmission of radiation, or use antisolar glass.Wherein, glass heat-proof pad pasting is a kind of common effectively barrier solar radiation
Film also improves the safety of glass simultaneously, when glass is broken by external force, can reduce splashing.Building
In energy conservation, the light transmission of glass and it is heat-insulated be a very crucial problem, in the building using large area exterior window and transparent ceiling
The heat radiation of the occasions such as object, automotive window, sunlight will lead to the increase of air conditioning energy consumption, cause very big energy waste.To change
It is apt to this phenomenon, people take using the products such as metal coating heat-reflecting glass and various heat reflection pad pastings, to reflect too
Portion of energy in sunlight, to achieve the purpose that heat insulation and heat control.But the heat insulation that these products have is bad, some light transmissions
Rate is lower, and some then needs expensive equipment, and the control of process conditions is also very complicated, is unfavorable for being widely applied to market, because
This researchs and develops a kind of material for having good light permeability and heat-proof quality concurrently, has for solving the problems, such as glass heat-proof not only important
Theory significance, and have vast market prospect.Nano antimony tin oxide (ATO) can both allow visible light-transmissive well, simultaneously
Most infrared-ray can be obstructed again, is a kind of excellent light transmission heat-barrier material.The partial size of nanoparticle is small, specific surface area
Greatly, surface free energy is high, easily reunites between particle, therefore the preparation of nano paint cannot be filled out as traditional coating by face
Simple mixture between material and base-material obtains.
Thermal isolation film, also referred to as " solar film ", come across the seventies of eighties of last century, have transparent heat-insulated, uvioresistant, beauty
Many advantages, such as sight.Heat-insulation and heat-preservation with curtain etc. is not light-blocking but heat-insulated compares, thermal isolation film can be effectively absorbed and be reflected infrared
Line, it is effectively heat-insulated.And in winter, additionally it is possible to reflect back into room the thermal energy of 20-30% again.Reduce because glass and
The heat of loss, to keep the temperature.Glass after having pasted thermal isolation film can obstruct 90% ultraviolet light, can largely extend house
Has the service life used；When glass is broken up by external force, the glass fragment of splashing is easy to hurt sb.'s feelings.And because thermal isolation film is sticked to glass
Adhesive used in upper remains to be sticked in thermal isolation film after enabling to glass breaking, and which reduces glass fragments everywhere
It splashes, substantially increases the safety coefficient of glass.Thermal isolation film has 80% or more visible light transmittance substantially, to the vision of people
Do not have too much influence.
And the introducing of inorganic functional form filler used causes because filler self performance is insufficient in Conventional nano thermal isolation film
The heat-proof quality of thermal isolation film is bad, and that there are compatibilities between inorganic functional fillers and organic bond is poor, and the two has been difficult to
Effect combines, and the drawbacks of causing heat-proof quality and mechanical property not to be promoted further is for the promotion for obtaining more high combination property
It is promoted and is applied to broader field, and industrial production demand urgent problem to be solved is met.
Summary of the invention
The present invention solves the technical problem of: for inorganic functional form filler used in Conventional nano thermal isolation film
Introduce, because filler self performance is insufficient, cause the heat-proof quality of thermal isolation film bad, and inorganic functional fillers and organic bond it
Between that there are compatibilities is poor, the two is difficult to effectively combine, the drawbacks of causing heat-proof quality and mechanical property not to be promoted further,
And the drawbacks of adverse effect is caused to the long-term heat-proof quality of product, provide a kind of Organic-inorganic composite nano heat-insulating film.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of Organic-inorganic composite nano heat-insulating film, the raw material including following parts by weight: 8~10 parts of functional stuffings, 4~8 parts
Ultraviolet absorber, 10~20 parts of ethyl acetate, 2~4 parts of coupling agents, 100~120 parts of acrylate adhesives, the function are filled out
Material is the compound functional stuffing of self-control；
The specific preparation step of the compound functional stuffing of self-control are as follows:
(1) according to parts by weight, 80~100 parts of oleic acid, 30~50 parts of dehydrated alcohols, 10~20 parts of nano oxidized graphite are successively taken
Alkene, 10~20 parts of esters of silicon acis, 8~10 parts of organo-aluminiums first disperse nano graphene oxide in oleic acid, add anhydrous second
Alcohol, esters of silicon acis and organo-aluminium, after heating stirring reaction, filtering washs and dry, obtains and once coat microballoon；
(2) the ethanol solution reduction that gained is once coated to microballoon hydrazine hydrate must restore primary cladding microballoon；
It (3) is in mass ratio mistake after 1:8~1:10 is stirred by the primary cladding microballoon of reduction and dopamine-gelatin dispersion liquid
Filter, it is dry, obtain secondary cladding microballoon；
It (4) is in mass ratio that after 1:10~1:20 mixes dispersion, precipitating is slowly added dropwise by secondary cladding microballoon and silver nitrate solution
Agent, after being stirred to react, filtering washs and dry, obtains and coat microballoon three times；
(5) microballoon will be coated three times under inert gas shielding state, slowly after heating charing, further heat up to 1500~
1800 DEG C, heat preservation sintering is cooling, obtains sintering feed；
(6) after impregnating gained sintering feed with sodium hydroxide solution, filtering, washing and drying are filled out to get compound function is made by oneself
Material.
The ultraviolet absorber is benzophenone type ultraviolet absorbent, benzotriazole ultraviolet absorber, poplar esters of gallic acid purple
Any one in outer absorbent, triazines ultraviolet absorber.
The coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560, appointing in Silane coupling reagent KH-570
It anticipates one kind.
Step (1) esters of silicon acis is methyl orthosilicate, ethyl orthosilicate, any one in positive silicic acid propyl ester.
Step (1) organo-aluminium is aluminium isopropoxide, any one in aluminium ethylate.
It is that 1:1~1:3 is prepared that the ethanol solution of step (2) described hydrazine hydrate is by hydrazine hydrate and dehydrated alcohol in mass ratio
It forms.
It is 1:10 that step (3) dopamine-gelatin dispersion liquid is by dopamine, gelatin and deionized water in mass ratio:
80 are formulated；It is 6.0~6.2 gelatin that the gelatin, which selects isoelectric point,.
Step (4) described precipitating reagent be mass fraction be 8~10% ammonium hydroxide, mass fraction be 8~10% urea, quality
Any one in the ammonium carbonate that ammonium hydrogen carbonate that score is 8~10%, mass fraction are 8~10%.
Step (5) inert gas is nitrogen, helium, any one in argon gas.
The beneficial effects of the present invention are:
(1) technical solution of the present invention first with nano graphene oxide as inner core, using ultrasonication by its interlayer
After structure removing, make that dehydrating condensation occurs before oleic acid and dehydrated alcohol, the moisture of generation keeps esters of silicon acis and organo-aluminium slowly equal
Even to hydrolyze, part is effectively embedded into graphene oxide interlayer in hydrolysis final product (nano aluminium oxide and nano silica)
In structure, partial adsorbates are in surface of graphene oxide, during hydrazine hydrate reduction, partial oxidation of graphite alkene and partial oxidation aluminium
It is restored, recycles dopamine and gelatin as modifying agent, re-form new clad, by the aluminium of reduction and remaining
Aluminium oxide and coated with silica make the absorption of inorganic interface surface while avoiding newly-generated aluminium simple substance from being reoxidized
Property can be promoted, thus effectively adsorption precipitation generate silver oxide, partial oxidation silver, can be by dopamine in precipitation process
Reduction, as in subsequent heating carbonization process, the organic layer charing of dopamine and gelatin composition in internal layer forms carbonaceous bone
Frame, and due to the difference of the coefficient of expansion between multilayer inorganic-organic structure, cause in slow temperature-rise period core-shell structure it
Between different degrees of contraction occurs, so that filler is formed multilayered fold structure, it is intermediate in addition, during subsequent further heat up
The carbonaceous skeleton of layer can form carbon-chemistry of silicones between the silica in kernel and be bonded, to effectively improve between layers
Interaction force, avoid in the process of processing and using filler itself it is peeling-off between layers and filler is caused to fail,
Furthermore in high-temperature sintering process, pure aluminum can restore silver oxide to obtain elemental silver, and dissolve and impregnate in final sodium hydroxide
In the process, so that the silica for remaining nano rank and aluminium oxide is removed, and form nanometer inside functional stuffing
The hole of size；
(2) the present invention is based on the realizations of foregoing invention design, firstly, originally by nanometer between graphene oxide layer and layer works
The aluminium oxide and silica of grade occupy, and widen its interlayer structure, and go in the aluminium oxide and silica for finally making interlayer
It removes, to form hollow structure, hollow structure itself just has lower thermal coefficient and lesser bulk density, makes
With hot-fluid in the process, can be made to occur various shuntings in conduction, and due to the presence of pleated structure, make heat conduction path more
It complicates, the heating conduction of material is further decreased, at the same time, due to the aluminium oxide of Nano grade and disappearing for silica
Lose, inside system formed Nano grade hole, thus make the air molecule among hole be adsorbed on completely hole inner wall it
On, can not free movement, that is, make hole be in similar to vacuum state, further improve the heat-proof quality of product；
In addition, the formation of pleated structure, the macromolecular chain that can be conducive to organic bond is formed in the protrusion of pleated structure and edges and corners
It physical entanglement and is affiliated to, to make to form effective mechanical snap between the two, effectively prevents product and storing and using
The sedimentation of functional stuffing in journey mutually separates, and makes to form firm connection between inorganic functional stuffing and organic bond, makes product
While mechanical property is effectively promoted, ensure that heat-proof quality is able to long-acting holding to product in the long-term use；
(3) technical solution of the present invention forms silvering in the outer surface of pleated structure, makes product not by reasonable technological means
Only it is indoor temperature increasing using extraneous solar radiation, while the radiation loss that indoor airflow gives out can be effectively reduced, plays
Good heat insulation effect, and the coating is to react generation under the high temperature conditions by metallic aluminium simple substance and silver oxide, can be conducive to silver
Metallurgical bonding is formed between coating and filler matrix, is effectively prevented the removing of silvering in the process of processing and using, is made to produce
The heat insulation effect of product is able to long-acting holding.
Specific embodiment
According to parts by weight, 80~100 parts of oleic acid, 30~50 parts of dehydrated alcohols, 10~20 parts of nano oxygen fossils are successively taken
Nano graphene oxide and oleic acid are first mixed and are poured into three-necked flask by black alkene, 10~20 parts of esters of silicon acis, 8~10 parts of organo-aluminiums,
And by three-necked flask move into ultrasonic disperse instrument in, in temperature be 45~55 DEG C, supersonic frequency be 45~55kHz under the conditions of, ultrasound
After dispersing 15~20min, dehydrated alcohol, esters of silicon acis and organo-aluminium are added, after continuing 10~20min of ultrasonic disperse, Jiang Sankou
Flask moves to digital display and tests the speed constant temperature blender with magnetic force, is 85~90 DEG C in temperature, under the conditions of revolving speed is 300~500r/min, adds
After 2~3h is reacted in thermal agitation, filtering obtains filter residue, and washed filter residue 3~5 times with dehydrated alcohol, then the filter residue after washing is transferred to
In vacuum oven, it is 95~105 DEG C in temperature, under the conditions of pressure is 60~80Pa, is dried under vacuum to constant weight, obtains and once coat
Microballoon；The ethanol solution that gained is once coated to microballoon and hydrazine hydrate is after 1:3~1:5 is mixed in mass ratio, and stirring reduction is anti-
After answering 20~30min, lower sediment thing is collected in centrifuge separation, and by gained lower sediment thing vacuum freeze drying, obtains reduction one
Secondary cladding microballoon；Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:8~1:10 mixes in mass ratio
Enter in beaker, after being stirred 10~20min with glass bar, filtering obtains No. 1 filter cake, and No. 1 filter cake vacuum refrigeration of gained is done
It is dry, obtain secondary cladding microballoon；By it is secondary cladding microballoon and mass fraction be 5~8% silver nitrate solution be in mass ratio 1:10~
1:20 mixing is poured into reaction kettle, under the conditions of supersonic frequency is 55~60kHz, after 10~20min of ultrasonic disperse, is in temperature
It is 55~60 DEG C, slow into reaction kettle with 3~5mL/min rate in constant temperature stirring under the conditions of revolving speed is 400~500r/min
Precipitating reagent is added dropwise, to be precipitated dose is added dropwise, and after continuation constant temperature is stirred to react 35~55min, filtering obtains No. 2 filter cakes, and spend
No. 2 filter cake 3~5 times obtained by ion water washing, then by No. 2 filter cake vacuum freeze dryings after washing, obtain and coat microballoon three times；It will
Gained coats microballoon three times and is transferred in sintering furnace, inert gas is passed through into furnace with 600~800mL/min rate, in indifferent gas
Under body guard mode, with the slow temperature programming of 1.5~2.0 DEG C/min rate to 550~600 DEG C, after 2~3h of heat preservation charing, after
It is continuous to be warming up to 1500~1800 DEG C with 10~15 DEG C/min rate program, after 3~5h of heat preservation sintering, cool to room temperature with the furnace, out
Material, obtains sintering feed；It is in mass ratio that 1:5~1:10 is mixed by the sodium hydroxide solution that gained sintering feed and mass fraction are 8~15%
Close dipping 25~30min after, filtering, obtain No. 3 filter cakes, and be washed with deionized No. 3 filter cakes until cleaning solution be in neutrality, then will
No. 3 filter cake vacuum freeze dryings after washing derive from and make compound functional stuffing；According to parts by weight, successively take 8~10 parts from
Make compound functional stuffing, 4~8 parts of ultraviolet absorbers, 10~20 parts of ethyl acetate, 2~4 parts of coupling agents, 100~120 part third
Ethyl acetate and acrylate adhesive are first stirred with blender with 600~800r/min revolving speed by olefin(e) acid ester adhesive
After 20~30min, the compound functional stuffing of self-control, ultraviolet absorber and coupling agent are added, continues to be stirred 30~60min
Afterwards, discharge, obtain into film liquid, then by gained at film liquid in film on substrate, controlling coating thickness is 20~40 μm, film-forming,
Up to Organic-inorganic composite nano heat-insulating film.The ultraviolet absorber is benzophenone type ultraviolet absorbent, benzotriazole purple
Outer absorbent, poplar esters of gallic acid ultraviolet absorber, any one in triazines ultraviolet absorber.The coupling agent is silane coupled
Agent KH-550, silane coupling agent KH-560, any one in Silane coupling reagent KH-570.The esters of silicon acis is positive silicic acid first
Ester, ethyl orthosilicate, any one in positive silicic acid propyl ester.The organo-aluminium is aluminium isopropoxide, any one in aluminium ethylate.
It is that 1:1~1:3 is formulated that the ethanol solution of the hydrazine hydrate is by hydrazine hydrate and dehydrated alcohol in mass ratio.The DOPA
Amine-gelatin dispersion liquid is formulated in mass ratio for 1:10:80 by dopamine, gelatin and deionized water；The gelatin is selected
The gelatin that isoelectric point is 6.0~6.2.The precipitating reagent be mass fraction be 8~10% ammonium hydroxide, mass fraction be 8~10%
Any one in the ammonium carbonate that ammonium hydrogen carbonate that urea, mass fraction are 8~10%, mass fraction are 8~10%.The inertia
Gas is nitrogen, helium, any one in argon gas.
Example 1
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 20 parts of esters of silicon acis,
Nano graphene oxide and oleic acid are first mixed and are poured into three-necked flask, and three-necked flask is moved into ultrasound point by 10 parts of organo-aluminiums
It dissipates in instrument, is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol, silicic acid
Three-necked flask after continuing ultrasonic disperse 20min, is moved to digital display and tested the speed constant temperature blender with magnetic force, be in temperature by ester and organo-aluminium
90 DEG C, under the conditions of revolving speed is 500r/min, after heating stirring reacts 3h, filtering obtains filter residue, and wash filter residue 5 with dehydrated alcohol
It is secondary, then the filter residue after washing is transferred in vacuum oven, it is 105 DEG C in temperature, under the conditions of pressure is 80Pa, is dried under vacuum to
Constant weight obtains and once coats microballoon；Gained is once coated microballoon and hydrazine hydrate ethanol solution be in mass ratio 1:5 mixing after,
After stirring reduction reaction 30min, lower sediment thing is collected in centrifuge separation, and by gained lower sediment thing vacuum freeze drying, is obtained
The primary cladding microballoon of reduction；Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:10 is mixed in mass ratio
It pours into beaker, after being stirred 20min with glass bar, filtering obtains No. 1 filter cake, and No. 1 filter cake vacuum refrigeration of gained is done
It is dry, obtain secondary cladding microballoon；It is in mass ratio that 1:20 is mixed by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%
Pour into reaction kettle, in supersonic frequency be 60kHz under the conditions of, after ultrasonic disperse 20min, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate in constant temperature stirring, to be precipitated dose is added dropwise,
Continue after constant temperature is stirred to react 55min, filtering obtains No. 2 filter cakes, and is washed with deionized gained 2 filter cake 5 times, then will wash
No. 2 filter cake vacuum freeze dryings after washing, obtain and coat microballoon three times；Gained is coated to microballoon three times to be transferred in sintering furnace, with
800mL/min rate is passed through inert gas into furnace, under inert gas shielding state, with the slow program of 2.0 DEG C/min rate
It is warming up to 600 DEG C, after heat preservation charing 3h, continues to be warming up to 1800 DEG C with 15 DEG C/min rate program, after heat preservation sintering 5h, with furnace
It is cooled to room temperature, discharges, obtain sintering feed；It is in mass ratio by the sodium hydroxide solution that gained sintering feed and mass fraction are 15%
1:10 be mixed with dipping 30min after, filtering, obtain No. 3 filter cakes, and be washed with deionized No. 3 filter cakes until cleaning solution be in neutrality, then
By No. 3 filter cake vacuum freeze dryings after washing, derives from and make compound functional stuffing；According to parts by weight, successively take 10 parts from
Make compound functional stuffing, 8 parts of ultraviolet absorbers, 20 parts of ethyl acetate, 4 parts of coupling agents, 120 parts of acrylate adhesives, elder generation
After ethyl acetate and acrylate adhesive are stirred 30min with blender with 800r/min revolving speed, it is multiple to add self-control
Mould assembly functional stuffing, ultraviolet absorber and coupling agent continue after being stirred 60min, and discharging obtains into film liquid, then by gained at
Film liquid is in film on substrate, and controlling coating thickness is 40 μm, and film-forming is to get Organic-inorganic composite nano heat-insulating film.It is described
Ultraviolet absorber is benzophenone type ultraviolet absorbent.The coupling agent is silane resin acceptor kh-550.The esters of silicon acis is positive
Methyl silicate.The organo-aluminium is aluminium isopropoxide.The ethanol solution of the hydrazine hydrate is by hydrazine hydrate and dehydrated alcohol by quality
Than being formulated for 1:3.The dopamine-gelatin dispersion liquid be by dopamine, isoelectric point be 6.0 gelatin and deionized water by
Mass ratio is formulated for 1:10:80.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
Example 2
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 10 parts of organo-aluminiums,
First nano graphene oxide and oleic acid are mixed and poured into three-necked flask, and three-necked flask is moved into ultrasonic disperse instrument, Yu Wen
Degree is 55 DEG C, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol and organo-aluminium, continues to surpass
After sound disperses 20min, three-necked flask is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 90 DEG C, revolving speed 500r/
Under the conditions of min, after heating stirring reacts 3h, filtering obtains filter residue, and washed filter residue 5 times with dehydrated alcohol, then by the filter after washing
Slag is transferred in vacuum oven, in temperature be 105 DEG C, pressure be 80Pa under the conditions of, be dried under vacuum to constant weight, obtain once coat it is micro-
Ball；The ethanol solution that gained is once coated to microballoon and hydrazine hydrate is stirring reduction reaction 30min after 1:5 mixing in mass ratio
Afterwards, it is centrifugated, collects lower sediment thing, and by gained lower sediment thing vacuum freeze drying, primary cladding microballoon must be restored；
Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:10 mixing is poured into beaker in mass ratio, uses glass
After stick is stirred 20min, filtering obtains No. 1 filter cake, and by No. 1 filter cake vacuum freeze drying of gained, obtain secondary cladding microballoon；
It is in mass ratio that 1:20 mixing is poured into reaction kettle by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%, Yu Chaosheng
It is 60 DEG C in temperature, under the conditions of revolving speed is 500r/min, Bian Hengwen is stirred after ultrasonic disperse 20min under the conditions of frequency is 60kHz
It mixes side and precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate, to be precipitated dose is added dropwise, and continues constant temperature and is stirred to react
After 55min, filtering obtains No. 2 filter cakes, and is washed with deionized gained 2 filter cake 5 times, then by No. 2 filter cake vacuum after washing
Freeze-drying, obtains and coats microballoon three times；Gained is coated to microballoon three times to be transferred in sintering furnace, with 800mL/min rate into furnace
It is passed through inert gas, under inert gas shielding state, with the slow temperature programming of 2.0 DEG C/min rate to 600 DEG C, heat preservation charing
After 3h, continues to be warming up to 1800 DEG C with 15 DEG C/min rate program, after heat preservation sintering 5h, cool to room temperature with the furnace, discharge, must burn
Ramming material；By the sodium hydroxide solution that gained sintering feed and mass fraction are 15% be in mass ratio 1:10 be mixed with dipping 30min after,
Filtering, obtains No. 3 filter cakes, and No. 3 filter cakes is washed with deionized until cleaning solution is in neutrality, then No. 3 filter cakes after washing are true
Vacuum freecing-dry derives from and makes compound functional stuffing；According to parts by weight, 10 parts of compound functional stuffings of self-control are successively taken, 8 parts
Ultraviolet absorber, 20 parts of ethyl acetate, 4 parts of coupling agents, 120 parts of acrylate adhesives, first by ethyl acetate and acrylate
After adhesive is stirred 30min with blender with 800r/min revolving speed, the compound functional stuffing of self-control, UV absorption are added
Agent and coupling agent continue after being stirred 60min, and discharging obtains into film liquid, then by gained at film liquid in film on substrate, control
Coating thickness is 40 μm, and film-forming is to get Organic-inorganic composite nano heat-insulating film.The ultraviolet absorber is benzophenone
Class ultraviolet absorber.The coupling agent is silane resin acceptor kh-550.The organo-aluminium is aluminium isopropoxide.The second of the hydrazine hydrate
Alcoholic solution is formulated in mass ratio for 1:3 by hydrazine hydrate and dehydrated alcohol.The dopamine-gelatin dispersion liquid is by DOPA
The gelatin and deionized water that amine, isoelectric point are 6.0 are that 1:10:80 is formulated in mass ratio.The precipitating reagent is mass fraction
For 10% ammonium hydroxide.The inert gas is nitrogen.
Example 3
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 20 parts of esters of silicon acis,
First nano graphene oxide and oleic acid are mixed and poured into three-necked flask, and three-necked flask is moved into ultrasonic disperse instrument, Yu Wen
Degree is 55 DEG C, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol, esters of silicon acis, continues ultrasound
After dispersing 20min, three-necked flask is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 90 DEG C, revolving speed 500r/min
Under the conditions of, after heating stirring reacts 3h, filtering obtains filter residue, and washed filter residue 5 times with dehydrated alcohol, then by the filter residue after washing
Be transferred in vacuum oven, in temperature be 105 DEG C, pressure be 80Pa under the conditions of, be dried under vacuum to constant weight, obtain once coat it is micro-
Ball；The ethanol solution that gained is once coated to microballoon and hydrazine hydrate is stirring reduction reaction 30min after 1:5 mixing in mass ratio
Afterwards, it is centrifugated, collects lower sediment thing, and by gained lower sediment thing vacuum freeze drying, primary cladding microballoon must be restored；
Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:10 mixing is poured into beaker in mass ratio, uses glass
After stick is stirred 20min, filtering obtains No. 1 filter cake, and by No. 1 filter cake vacuum freeze drying of gained, obtain secondary cladding microballoon；
It is in mass ratio that 1:20 mixing is poured into reaction kettle by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%, Yu Chaosheng
It is 60 DEG C in temperature, under the conditions of revolving speed is 500r/min, Bian Hengwen is stirred after ultrasonic disperse 20min under the conditions of frequency is 60kHz
It mixes side and precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate, to be precipitated dose is added dropwise, and continues constant temperature and is stirred to react
After 55min, filtering obtains No. 2 filter cakes, and is washed with deionized gained 2 filter cake 5 times, then by No. 2 filter cake vacuum after washing
Freeze-drying, obtains and coats microballoon three times；Gained is coated to microballoon three times to be transferred in sintering furnace, with 800mL/min rate into furnace
It is passed through inert gas, under inert gas shielding state, with the slow temperature programming of 2.0 DEG C/min rate to 600 DEG C, heat preservation charing
After 3h, continues to be warming up to 1800 DEG C with 15 DEG C/min rate program, after heat preservation sintering 5h, cool to room temperature with the furnace, discharge, must burn
Ramming material；By the sodium hydroxide solution that gained sintering feed and mass fraction are 15% be in mass ratio 1:10 be mixed with dipping 30min after,
Filtering, obtains No. 3 filter cakes, and No. 3 filter cakes is washed with deionized until cleaning solution is in neutrality, then No. 3 filter cakes after washing are true
Vacuum freecing-dry derives from and makes compound functional stuffing；According to parts by weight, 10 parts of compound functional stuffings of self-control are successively taken, 8 parts
Ultraviolet absorber, 20 parts of ethyl acetate, 4 parts of coupling agents, 120 parts of acrylate adhesives, first by ethyl acetate and acrylate
After adhesive is stirred 30min with blender with 800r/min revolving speed, the compound functional stuffing of self-control, UV absorption are added
Agent and coupling agent continue after being stirred 60min, and discharging obtains into film liquid, then by gained at film liquid in film on substrate, control
Coating thickness is 40 μm, and film-forming is to get Organic-inorganic composite nano heat-insulating film.The ultraviolet absorber is benzophenone
Class ultraviolet absorber.The coupling agent is silane resin acceptor kh-550.The esters of silicon acis is methyl orthosilicate.The hydrazine hydrate
Ethanol solution is formulated in mass ratio for 1:3 by hydrazine hydrate and dehydrated alcohol.The dopamine-gelatin dispersion liquid is by more
Bar amine, the gelatin of isoelectric point 6.0 and deionized water are formulated in mass ratio for 1:10:80.The precipitating reagent is mass fraction
For 10% ammonium hydroxide.The inert gas is nitrogen.
Example 4
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 20 parts of esters of silicon acis,
Nano graphene oxide and oleic acid are first mixed and are poured into three-necked flask, and three-necked flask is moved into ultrasound point by 10 parts of organo-aluminiums
It dissipates in instrument, is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol, silicic acid
Three-necked flask after continuing ultrasonic disperse 20min, is moved to digital display and tested the speed constant temperature blender with magnetic force, be in temperature by ester and organo-aluminium
90 DEG C, under the conditions of revolving speed is 500r/min, after heating stirring reacts 3h, filtering obtains filter residue, and wash filter residue 5 with dehydrated alcohol
It is secondary, then the filter residue after washing is transferred in vacuum oven, it is 105 DEG C in temperature, under the conditions of pressure is 80Pa, is dried under vacuum to
Constant weight obtains and once coats microballoon；Gained is once coated to microballoon and dopamine-gelatin dispersion liquid is that 1:10 mixing is fallen in mass ratio
Enter in beaker, after being stirred 20min with glass bar, filtering obtains No. 1 filter cake, and by No. 1 filter cake vacuum freeze drying of gained,
Obtain secondary cladding microballoon；It is in mass ratio that 1:20 mixing is poured by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%
In reaction kettle, in supersonic frequency be 60kHz under the conditions of, after ultrasonic disperse 20min, in temperature be 60 DEG C, revolving speed 500r/min
Under the conditions of, precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate in constant temperature stirring, to be precipitated dose is added dropwise, after
After continuous constant temperature is stirred to react 55min, filtering, obtain No. 2 filter cakes, and be washed with deionized gained No. 2 filter cake 5 times, then will washing
No. 2 filter cake vacuum freeze dryings afterwards, obtain and coat microballoon three times；Gained is coated to microballoon three times to be transferred in sintering furnace, with
800mL/min rate is passed through inert gas into furnace, under inert gas shielding state, with the slow program of 2.0 DEG C/min rate
It is warming up to 600 DEG C, after heat preservation charing 3h, continues to be warming up to 1800 DEG C with 15 DEG C/min rate program, after heat preservation sintering 5h, with furnace
It is cooled to room temperature, discharges, obtain sintering feed；It is in mass ratio by the sodium hydroxide solution that gained sintering feed and mass fraction are 15%
1:10 be mixed with dipping 30min after, filtering, obtain No. 3 filter cakes, and be washed with deionized No. 3 filter cakes until cleaning solution be in neutrality, then
By No. 3 filter cake vacuum freeze dryings after washing, derives from and make compound functional stuffing；According to parts by weight, successively take 10 parts from
Make compound functional stuffing, 8 parts of ultraviolet absorbers, 20 parts of ethyl acetate, 4 parts of coupling agents, 120 parts of acrylate adhesives, elder generation
After ethyl acetate and acrylate adhesive are stirred 30min with blender with 800r/min revolving speed, it is multiple to add self-control
Mould assembly functional stuffing, ultraviolet absorber and coupling agent continue after being stirred 60min, and discharging obtains into film liquid, then by gained at
Film liquid is in film on substrate, and controlling coating thickness is 40 μm, and film-forming is to get Organic-inorganic composite nano heat-insulating film.It is described
Ultraviolet absorber is benzophenone type ultraviolet absorbent.The coupling agent is silane resin acceptor kh-550.The esters of silicon acis is positive
Methyl silicate.The organo-aluminium is aluminium isopropoxide.The dopamine-gelatin dispersion liquid is by the gelatin of dopamine, isoelectric point 6.0
It is formulated in mass ratio for 1:10:80 with deionized water.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inertia
Gas is nitrogen.
Example 5
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 20 parts of esters of silicon acis,
Nano graphene oxide and oleic acid are first mixed and are poured into three-necked flask, and three-necked flask is moved into ultrasound point by 10 parts of organo-aluminiums
It dissipates in instrument, is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol, silicic acid
Three-necked flask after continuing ultrasonic disperse 20min, is moved to digital display and tested the speed constant temperature blender with magnetic force, be in temperature by ester and organo-aluminium
90 DEG C, under the conditions of revolving speed is 500r/min, after heating stirring reacts 3h, filtering obtains filter residue, and wash filter residue 5 with dehydrated alcohol
It is secondary, then the filter residue after washing is transferred in vacuum oven, it is 105 DEG C in temperature, under the conditions of pressure is 80Pa, is dried under vacuum to
Constant weight obtains and once coats microballoon；Gained is once coated microballoon and hydrazine hydrate ethanol solution be in mass ratio 1:5 mixing after,
After stirring reduction reaction 30min, lower sediment thing is collected in centrifuge separation, and by gained lower sediment thing vacuum freeze drying, is obtained
The primary cladding microballoon of reduction；Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:10 is mixed in mass ratio
It pours into beaker, after being stirred 20min with glass bar, filtering obtains No. 1 filter cake, and No. 1 filter cake vacuum refrigeration of gained is done
It is dry, obtain secondary cladding microballoon；It is in mass ratio that 1:20 is mixed by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%
Pour into reaction kettle, in supersonic frequency be 60kHz under the conditions of, after ultrasonic disperse 20min, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate in constant temperature stirring, to be precipitated dose is added dropwise,
Continue after constant temperature is stirred to react 55min, filtering obtains No. 2 filter cakes, and is washed with deionized gained 2 filter cake 5 times, then will wash
No. 2 filter cake vacuum freeze dryings after washing, obtain and coat microballoon three times；Gained is coated to microballoon three times and mass fraction is 15%
Sodium hydroxide solution is after 1:10 is mixed with dipping 30min in mass ratio, and filtering obtains No. 3 filter cakes, and be washed with deionized No. 3
Filter cake is until cleaning solution is in neutrality, then by No. 3 filter cake vacuum freeze dryings after washing, is derived from and made compound functional stuffing；It presses
Parts by weight meter, successively takes 10 parts of compound functional stuffings of self-control, 8 parts of ultraviolet absorbers, 20 parts of ethyl acetate, 4 parts of coupling agents,
120 parts of acrylate adhesives are first stirred ethyl acetate and acrylate adhesive blender with 800r/min revolving speed mixed
After closing 30min, the compound functional stuffing of self-control, ultraviolet absorber and coupling agent are added, is continued after being stirred 60min, out
Material, obtains into film liquid, then by gained at film liquid in film on substrate, controlling coating thickness is 40 μm, film-forming to get it is organic-
Inorganic composite nano thermal isolation film.The ultraviolet absorber is benzophenone type ultraviolet absorbent.The coupling agent is silane coupled
Agent KH-550.The esters of silicon acis is methyl orthosilicate.The organo-aluminium is aluminium isopropoxide.The ethanol solution of the hydrazine hydrate be by
Hydrazine hydrate and dehydrated alcohol are formulated in mass ratio for 1:3.The dopamine-gelatin dispersion liquid is by dopamine, isoelectric point
6.0 gelatin and deionized water is formulated in mass ratio for 1:10:80.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.
Example 6
According to parts by weight, 100 parts of oleic acid are successively taken, 50 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 20 parts of esters of silicon acis,
Nano graphene oxide and oleic acid are first mixed and are poured into three-necked flask, and three-necked flask is moved into ultrasound point by 10 parts of organo-aluminiums
It dissipates in instrument, is 55 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 20min, adds dehydrated alcohol, silicic acid
Three-necked flask after continuing ultrasonic disperse 20min, is moved to digital display and tested the speed constant temperature blender with magnetic force, be in temperature by ester and organo-aluminium
90 DEG C, under the conditions of revolving speed is 500r/min, after heating stirring reacts 3h, filtering obtains filter residue, and wash filter residue 5 with dehydrated alcohol
It is secondary, then the filter residue after washing is transferred in vacuum oven, it is 105 DEG C in temperature, under the conditions of pressure is 80Pa, is dried under vacuum to
Constant weight obtains and once coats microballoon；Gained is once coated microballoon and hydrazine hydrate ethanol solution be in mass ratio 1:5 mixing after,
After stirring reduction reaction 30min, lower sediment thing is collected in centrifuge separation, and by gained lower sediment thing vacuum freeze drying, is obtained
The primary cladding microballoon of reduction；Gained is restored into primary cladding microballoon and dopamine-gelatin dispersion liquid is that 1:10 is mixed in mass ratio
It pours into beaker, after being stirred 20min with glass bar, filtering obtains No. 1 filter cake, and No. 1 filter cake vacuum refrigeration of gained is done
It is dry, obtain secondary cladding microballoon；It is in mass ratio that 1:20 is mixed by the silver nitrate solution that secondary cladding microballoon and mass fraction are 8%
Pour into reaction kettle, in supersonic frequency be 60kHz under the conditions of, after ultrasonic disperse 20min, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, precipitating reagent is slowly added dropwise into reaction kettle with 5mL/min rate in constant temperature stirring, to be precipitated dose is added dropwise,
Continue after constant temperature is stirred to react 55min, filtering obtains No. 2 filter cakes, and is washed with deionized gained 2 filter cake 5 times, then will wash
No. 2 filter cake vacuum freeze dryings after washing, obtain and coat microballoon three times；Gained is coated to microballoon three times to be transferred in sintering furnace, with
800mL/min rate is passed through inert gas into furnace, under inert gas shielding state, with the slow program of 2.0 DEG C/min rate
It is warming up to 600 DEG C, after heat preservation charing 3h, continues to be warming up to 1800 DEG C with 15 DEG C/min rate program, after heat preservation sintering 5h, with furnace
It is cooled to room temperature, discharges, obtain sintering feed to get compound functional stuffing is made by oneself；According to parts by weight, successively take 10 parts of self-controls multiple
Mould assembly functional stuffing, 8 parts of ultraviolet absorbers, 20 parts of ethyl acetate, 4 parts of coupling agents, 120 parts of acrylate adhesives, first by second
After acetoacetic ester and acrylate adhesive are stirred 30min with blender with 800r/min revolving speed, it is compound to add self-control
Functional stuffing, ultraviolet absorber and coupling agent continue after being stirred 60min, and discharging obtains into film liquid, then by gained at film liquid
In film on substrate, controlling coating thickness is 40 μm, and film-forming is to get Organic-inorganic composite nano heat-insulating film.It is described ultraviolet
Absorbent is benzophenone type ultraviolet absorbent.The coupling agent is silane resin acceptor kh-550.The esters of silicon acis is positive silicic acid
Methyl esters.The organo-aluminium is aluminium isopropoxide.The ethanol solution of the hydrazine hydrate is to be in mass ratio by hydrazine hydrate and dehydrated alcohol
1:3 is formulated.The dopamine-gelatin dispersion liquid be by dopamine, the gelatin of isoelectric point 6.0 and deionized water in mass ratio
It is formulated for 1:10:80.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
Comparative example: the Organic-inorganic composite nano heat-insulating film of Wuxi new material Co., Ltd production.
Example 1 to the resulting Organic-inorganic composite nano heat-insulating film of example 6 and comparative example product are subjected to performance detection,
The specific detection method is as follows:
Mercurial thermometer is inserted into from body side, cabinet center is placed in, tests test specimen adiabatic temperature, template is placed in cabinet
Top makes heat source just vertical irradiation template.Before opening power supply, reads case body temperature and record.Power on, from photograph
It penetrates and initially plays timing and reading, record a case body temperature every 5min, and it is heat-insulated to calculate the intracorporal differential thermal calculation of 1h rear cabinet
Rate, and calculate using the heat-insulated rate after 90 days.Using tensile testing machine (CMT-6203), pass through three-point bending resistance intensity (GB1965)
Measure its bending strength.
Specific testing result is as shown in table 1:
The 1 specific testing result of Organic-inorganic composite nano heat-insulating film of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example |
| Heat-insulated rate/% | 92 | 83 | 76 | 53 | 68 | 52 | 46 |
| Heat-insulated rate/% after 90 days | 87 | 75 | 61 | 49 | 53 | 42 | 37 |
| Bending strength/MPa | 87 | 63 | 72 | 74 | 65 | 57 | 42 |
By 1 testing result of table it is found that the Organic-inorganic composite nano heat-insulating film of technical solution of the present invention preparation has heat-proof quality
With the feature of excellent in mechanical performance and length of heat-insulated time limit, have broad prospects in the development of composite technology industry.
Claims (9)
1. a kind of Organic-inorganic composite nano heat-insulating film, the raw material including following parts by weight: 8~10 parts of functional stuffings, 4~8
Part ultraviolet absorber, 10~20 parts of ethyl acetate, 2~4 parts of coupling agents, 100~120 parts of acrylate adhesives, feature exist
It is to make compound functional stuffing by oneself in the functional stuffing；
The specific preparation step of the compound functional stuffing of self-control are as follows:
(1) according to parts by weight, 80~100 parts of oleic acid, 30~50 parts of dehydrated alcohols, 10~20 parts of nano oxidized graphite are successively taken
Alkene, 10~20 parts of esters of silicon acis, 8~10 parts of organo-aluminiums first disperse nano graphene oxide in oleic acid, add anhydrous second
Alcohol, esters of silicon acis and organo-aluminium, after heating stirring reaction, filtering washs and dry, obtains and once coat microballoon；
(2) the ethanol solution reduction that gained is once coated to microballoon hydrazine hydrate must restore primary cladding microballoon；
It (3) is in mass ratio mistake after 1:8~1:10 is stirred by the primary cladding microballoon of reduction and dopamine-gelatin dispersion liquid
Filter, it is dry, obtain secondary cladding microballoon；
It (4) is in mass ratio that after 1:10~1:20 mixes dispersion, precipitating is slowly added dropwise by secondary cladding microballoon and silver nitrate solution
Agent, after being stirred to react, filtering washs and dry, obtains and coat microballoon three times；
(5) microballoon will be coated three times under inert gas shielding state, slowly after heating charing, further heat up to 1500~
1800 DEG C, heat preservation sintering is cooling, obtains sintering feed；
(6) after impregnating gained sintering feed with sodium hydroxide solution, filtering, washing and drying are filled out to get compound function is made by oneself
Material.
2. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that the UV absorption
Agent is benzophenone type ultraviolet absorbent, benzotriazole ultraviolet absorber, poplar esters of gallic acid ultraviolet absorber, the ultraviolet suction of triazines
Receive any one in agent.
3. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that the coupling agent is
Silane resin acceptor kh-550, silane coupling agent KH-560, any one in Silane coupling reagent KH-570.
4. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (1) described silicon
Acid esters is methyl orthosilicate, ethyl orthosilicate, any one in positive silicic acid propyl ester.
5. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (1) is described to be had
Machine aluminium is aluminium isopropoxide, any one in aluminium ethylate.
6. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (2) described water
It is that 1:1~1:3 is formulated that the ethanol solution for closing hydrazine is by hydrazine hydrate and dehydrated alcohol in mass ratio.
7. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (3) is described more
Bar amine-gelatin dispersion liquid is formulated in mass ratio for 1:10:80 by dopamine, gelatin and deionized water；The gelatin choosing
The gelatin for being 6.0~6.2 with isoelectric point.
8. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (4) is described heavy
Shallow lake agent be mass fraction be 8~10% ammonium hydroxide, mass fraction be 8~10% urea, mass fraction be 8~10% bicarbonate
Ammonium, mass fraction are any one in 8~10% ammonium carbonate.
9. a kind of Organic-inorganic composite nano heat-insulating film according to claim 1, which is characterized in that step (5) is described lazy
Property gas be nitrogen, helium, any one in argon gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112225456A (en) * | 2020-10-22 | 2021-01-15 | 林玉婷 | Antibacterial and mildewproof ceramic glaze as well as preparation method and application thereof |
| CN112939459A (en) * | 2021-02-21 | 2021-06-11 | 林玉婷 | Wear-resistant corrosion-resistant ceramic glaze as well as preparation method and application thereof |
| CN114634675A (en) * | 2022-03-24 | 2022-06-17 | 西北工业大学 | Method for preparing heat-insulating material by using polydopamine-modified carbon nano tube |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106183148A (en) * | 2016-08-30 | 2016-12-07 | 常州山由帝杉防护材料制造有限公司 | Nano ceramics heat-insulation and heat-preservation fenestrated membrane |
-
2019
- 2019-05-20 CN CN201910416479.XA patent/CN110144095A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106183148A (en) * | 2016-08-30 | 2016-12-07 | 常州山由帝杉防护材料制造有限公司 | Nano ceramics heat-insulation and heat-preservation fenestrated membrane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225456A (en) * | 2020-10-22 | 2021-01-15 | 林玉婷 | Antibacterial and mildewproof ceramic glaze as well as preparation method and application thereof |
| CN112939459A (en) * | 2021-02-21 | 2021-06-11 | 林玉婷 | Wear-resistant corrosion-resistant ceramic glaze as well as preparation method and application thereof |
| CN114634675A (en) * | 2022-03-24 | 2022-06-17 | 西北工业大学 | Method for preparing heat-insulating material by using polydopamine-modified carbon nano tube |
| CN114634675B (en) * | 2022-03-24 | 2023-09-26 | 西北工业大学 | Method for preparing heat insulation material by using polydopamine modified carbon nano tube |
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