CN108147829A - A kind of preparation method of novel heat-insulation nano material - Google Patents

A kind of preparation method of novel heat-insulation nano material Download PDF

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CN108147829A
CN108147829A CN201711455062.1A CN201711455062A CN108147829A CN 108147829 A CN108147829 A CN 108147829A CN 201711455062 A CN201711455062 A CN 201711455062A CN 108147829 A CN108147829 A CN 108147829A
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sio
nano material
btc
heat
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冯可
刘畅
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Xuzhou Creates Branch Intellectual Property Service Ltd Co
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Xuzhou Creates Branch Intellectual Property Service Ltd Co
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Abstract

The invention discloses a kind of preparation method of novel heat-insulation nanocomposite, Cu BTC SiO2Nano material, polyvinyl resin, makrolon, barium stearate, glass fibre, ethyl methacrylate and ethylene oxide are primary raw material, by by Cu BTC SiO2Nano material, polyvinyl resin, barium stearate, silica and glass fibre add in ethyl methacrylate at a certain temperature after mixing and ethylene oxide is reacted, carry out preliminary crosslinking, then aluminium oxide is added further to be reacted, so that condensate is equably penetrated into material at high temperature, improve the degree of cross linking of material, invention raw material sources are extensive, the low obtained nanometer heat insulation material intensity of production cost is high, bulk density is small low with thermal conductivity factor, has excellent heat insulation.

Description

A kind of preparation method of novel heat-insulation nano material
Technical field
Invention is related to a kind of preparation method of novel heat-insulation nanocomposite, belongs to heat proof material technology neck Domain.
Background technology
Heat-barrier material refers to the material or composite body that have heat-insulating property, shielding action can be played to hot-fluid, usually has There is the characteristics of light, loose, porous, thermal conductivity factor is small, being industrially widely used in prevents the heat of Thermal Equipment and pipeline to scatter and disappear, Or used in freezing and low temperature, thus heat-barrier material is also known as kept the temperature or cold insulation material.Currently used heat-barrier material type It is various, but generally as the heat-proof quality of the raising heat-barrier material of temperature reduces, especially many heat-barrier materials resistance in itself High temperatures poor, this just largely limits the application of heat-barrier material.
Invention content
The purpose of the present invention is to provide a kind of novel heat-insulation nano materials and preparation method thereof, are prepared by this method Material has excellent heat insulation.
A kind of preparation method of novel heat-insulation nano material, this method include the following steps：
Step 1, by 36 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；
Step 3, by the neat loading mold of blank of material made from above-mentioned steps, then mold is put into swaging machine and is carried out Disposal molding is suppressed, and is then carried out with cured, and solidification temperature room temperature is to 175 DEG C, 3 hours hardening times；
The above-mentioned intermediate products being cured are packed into high temperature sintering furnace by step 4, under the pressure of 15KPa, heated up with 75 DEG C/h To 1800 DEG C, 2200 DEG C so are warming up to 25 DEG C/h, keeps the temperature 2 hours, stops heating, comes out of the stove, obtain after Temperature fall to room temperature Heat insulation nano composite material.
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h, Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly, It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e., Nano material Cu-BTC-SiO2。
Advantageous effect：Novel heat-insulation nanocomposite prepared by the present invention, first by Cu-BTC-SiO2Nano material, Polyvinyl resin, barium stearate, silica and glass fibre add in methacrylic acid second at a certain temperature after mixing Ester and ethylene oxide are reacted, and carry out preliminary crosslinking, are then added aluminium oxide and are further reacted so that condensate It equably penetrates into material at high temperature, improves the degree of cross linking of material, and then reduce its thermal conductivity factor；In addition, Cu-MOF With porous silica Ceramic Composite, the porous silica ceramics of the high-strength high stable of one side play effectively a material Protective effect overcomes the low deficiency of the MOF strengths of materials, while realizes the supported of Cu-MOF so that the heat conduction system of material Number further reduces, so as to significantly improve the heat insulation after Material cladding.
Specific embodiment
Embodiment 1
A kind of preparation method of novel heat-insulation nano material, this method include the following steps：
Step 1, by 36 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；
Step 3, by the neat loading mold of blank of material made from above-mentioned steps, then mold is put into swaging machine and is carried out Disposal molding is suppressed, and is then carried out with cured, and solidification temperature room temperature is to 175 DEG C, 3 hours hardening times；
The above-mentioned intermediate products being cured are packed into high temperature sintering furnace by step 4, under the pressure of 15KPa, heated up with 75 DEG C/h To 1800 DEG C, 2200 DEG C so are warming up to 25 DEG C/h, keeps the temperature 2 hours, stops heating, comes out of the stove, obtain after Temperature fall to room temperature Heat insulation nano composite material.
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h, Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly, It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e., Nano material Cu-BTC-SiO2。
Embodiment 2
Step 1, by 26 parts of Cu-BTC-SiO2Nano material, 22 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 3
Step 1, by 19 parts of Cu-BTC-SiO2Nano material, 14 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 4
Step 1, by 14 parts of Cu-BTC-SiO2Nano material, 7 parts of polyvinyl resins, 4 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 5
Step 1, by 40 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 7 parts of makrolon, 4 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 6
Step 1, by 36 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 14 parts of methyl Ethyl acrylate and 9 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue 60 points of stirring Clock obtains blank of material after dry；Remaining is prepared and embodiment 1 is identical.
Embodiment 7
Step 1, by 16 parts of Cu-BTC-SiO2Nano material, 2 parts of polyvinyl resins, 8 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 8
Step 1, by 50 parts of Cu-BTC-SiO2Nano material, 34 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 8 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 9
Step 1, by 24 parts of Cu-BTC-SiO2Nano material, 9 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 26 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 10
Step 1, by 7 parts of Cu-BTC-SiO2Nano material, 14 parts of polyvinyl resins, 1 part of makrolon, 3 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
Embodiment 11
Step 1, by 36 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 6 parts of activated carbon fibers, 3 parts of makrolon, 6 parts of barium stearates and 5 parts of glass fibres stir evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl-props Olefin(e) acid ethyl ester and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue stirring 60 minutes, Blank of material is obtained after drying；Remaining is prepared and embodiment 1 is identical.
The activated carbon fiber preparation method is as follows：
Carbon fiber is placed in acetone soln and impregnates 12h, is filtered, deionized water is washed 3 times, dry in 120 DEG C of blast driers 4h, with 60% nitric acid reflux oxidation carbon fiber 7h, filtering, deionized water washing PH=6 are dried extremely in 120 DEG C of blast driers Constant weight；The carbon fiber of nitric acid oxidation is placed in polyvinylpyrrolidone, lauryl sodium sulfate and is equivalent to its total weight parts In the solution of 12 times of deionized water configuration, ultrasonic 50min, 60 DEG C of dryings obtain oxidation activity carbon fiber.
Reference examples 1
It is with 1 difference of embodiment：In the step 3 of heat insulation nano material preparation, mold is put into swaging machine and is carried out once Property molding compacting, then carry out with cured, solidification temperature room temperature is to 155 DEG C, 4 hours hardening times, remaining step is with implementing Example 1 is identical.
Reference examples 2
It is with 1 difference of embodiment：In the step 3 of heat insulation nano material preparation, mold is put into swaging machine and is carried out once Property molding compacting, then carry out with cured, solidification temperature room temperature is to 195 DEG C, 2 hours hardening times, remaining step is with implementing Example 1 is identical.
Reference examples 3
It is with 1 difference of embodiment：In the step 4 of heat insulation nano material preparation, under the pressure of 15KPa, with 55 DEG C/h liters Temperature is so warming up to 2200 DEG C to 1800 DEG C with 45 DEG C/h, keeps the temperature 2 hours, stops heating, comes out of the stove after Temperature fall to room temperature, Remaining step is identical with embodiment 1.
Reference examples 4
It is with 1 difference of embodiment：In the step 4 of heat insulation nano material preparation, under the pressure of 15KPa, with 95 DEG C/h liters Temperature is so warming up to 2000 DEG C to 1600 DEG C with 15 DEG C/h, keeps the temperature 1 hour, stops heating, comes out of the stove after Temperature fall to room temperature, Remaining step is identical with embodiment 1.
Reference examples 5
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 1 prepared by nano material, by 23 parts of silicon dioxide powders, 2.3 Part Sodium Polyacrylate, 17 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yttrium oxide mixing are put into flask, are uniformly stirred at 75 DEG C It mixes, obtains slurry, remaining step is identical with embodiment 1.
Reference examples 6
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 1 prepared by nano material, by 10 parts of silicon dioxide powders, 1.3 Part Sodium Polyacrylate, 10.4 parts of camphenes, 6.8 parts of tert-butyl alcohols and 3.7 parts of yttrium oxides mixing are put into flask, are uniformly stirred at 75 DEG C It mixes, obtains slurry, remaining step is identical with embodiment 1.
Reference examples 7
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 3 prepared by nano material, finally with the speed of 10 DEG C/min Heating carries out high temperature sintering, is warming up to 800 DEG C, keeps the temperature 3h, remaining step is identical with embodiment 1.
Reference examples 8
It is with 1 difference of embodiment：：Cu-BTC-SiO2In step 3 prepared by nano material, finally with the speed of 25 DEG C/min Degree heating carries out high temperature sintering, is warming up to 1500 DEG C, keeps the temperature 2h, remaining step is identical with embodiment 1.
Reference examples 9
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 4 prepared by nano material, 1.2 parts of nitrate trihydrate copper are added in, Remaining step is identical with embodiment 1.
Reference examples 10
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 4 prepared by nano material, 8.9 parts of nitrate trihydrate copper are added in, Remaining step is identical with embodiment 1.
It chooses the heat insulation nano composite material being prepared and carries out performance detection respectively,
Test result is as follows：
The experimental results showed that novel nanocomposite materials provided by the invention have good heat insulation, material is marked in country Under quasi- test condition, elongation at break is certain, and thermal conductivity factor is lower, illustrates good heat-insulation effect, conversely, effect is poorer；Embodiment 1 arrives embodiment 10, and thermal conductivity factor is below 1W/ (K.M), changes matching for each raw material composition in heat insulation nano composite material respectively Than having different degrees of influence to the heat-proof quality of material, in Cu-BTC-SiO2Nano material, polyvinyl resin quality are matched Than being 3：1, when other dispensing dosages are fixed, heat insulation is best；It is worth noting that embodiment 11 adds in activated carbon fiber, every Thermal effect significantly improves, and illustrates that modified carbon fiber has better optimization function to the heat-proof quality of MOF filling-material structures；Reference examples 1 Change the cured temperature and time of heat insulation nano material molds to reference examples 2, heat insulation is decreased obviously, illustrate solidification temperature and Time is synthetically produced great influence to material；Reference examples 3 and reference examples 4 change the heating rate and soaking time of green body, close Into material thermal conductivity it is still not low；Reference examples 5 change Cu-BTC-SiO to reference examples 82The dosage of nano material raw material and Proportioning, effect is also bad, illustrates that the dosage of silica, Sodium Polyacrylate and yttrium oxide plays an important role to material modification；It is right As usual 9 and example 10 change Cu-BTC-SiO2The dosage of nano material copper nitrate, heat insulation are substantially reduced, and illustrate three water nitre The excessive very few thermal conductivity on material of sour copper influences very big；Therefore the heat insulation type nanocomposite prepared using the present invention is had Good heat insulation.

Claims (2)

1. a kind of preparation method of novel heat-insulation nano material, it is characterised in that this method includes the following steps：
Step 1, by 36 parts of Cu-BTC-SiO2Nano material, 12 parts of polyvinyl resins, 3 parts of makrolon, 6 parts of barium stearates and 5 Part glass fibre stirs evenly to form mixed slurry in stirrer for mixing；
Above-mentioned slurry is transferred in reaction kettle by step 2, is heated to about 80 DEG C under conditions of argon gas protection, is added in 8 parts of methyl Ethyl acrylate and 3 parts of ethylene oxide stir 30min, then heat to 75 DEG C, add in 5 parts of aluminium oxide, continue 60 points of stirring Clock obtains blank of material after dry；
Step 3, by the neat loading mold of blank of material made from above-mentioned steps, then mold is put into swaging machine and is carried out Disposal molding is suppressed, and is then carried out with cured, and solidification temperature room temperature is to 175 DEG C, 3 hours hardening times；
The above-mentioned intermediate products being cured are packed into high temperature sintering furnace by step 4, under the pressure of 15KPa, heated up with 75 DEG C/h To 1800 DEG C, 2200 DEG C so are warming up to 25 DEG C/h, keeps the temperature 2 hours, stops heating, comes out of the stove, obtain after Temperature fall to room temperature Heat insulation nano composite material.
2. a kind of preparation method of novel heat-insulation nanocomposite according to claim 1, which is characterized in that
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h, Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly, It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e., Nano material Cu-BTC-SiO2。
CN201711455062.1A 2017-12-28 2017-12-28 A kind of preparation method of novel heat-insulation nano material Pending CN108147829A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113527928A (en) * 2021-08-10 2021-10-22 珠海海虹新材料有限公司 Glass heat-insulating coating with high visible light transmittance and high infrared barrier rate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113527928A (en) * 2021-08-10 2021-10-22 珠海海虹新材料有限公司 Glass heat-insulating coating with high visible light transmittance and high infrared barrier rate
CN113527928B (en) * 2021-08-10 2022-03-18 珠海海虹新材料有限公司 Glass heat-insulating coating with high visible light transmittance and high infrared barrier rate

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