CN115849796B - Waterproof thermal insulation mortar and preparation process thereof - Google Patents
Waterproof thermal insulation mortar and preparation process thereof Download PDFInfo
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- CN115849796B CN115849796B CN202211622439.9A CN202211622439A CN115849796B CN 115849796 B CN115849796 B CN 115849796B CN 202211622439 A CN202211622439 A CN 202211622439A CN 115849796 B CN115849796 B CN 115849796B
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- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 54
- 238000009413 insulation Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000003822 epoxy resin Substances 0.000 claims abstract description 133
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 133
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 23
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 93
- 238000003756 stirring Methods 0.000 claims description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 69
- 239000012782 phase change material Substances 0.000 claims description 65
- 238000001723 curing Methods 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 48
- 239000002041 carbon nanotube Substances 0.000 claims description 45
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 45
- 239000008367 deionised water Substances 0.000 claims description 41
- 229910021641 deionized water Inorganic materials 0.000 claims description 41
- 239000003795 chemical substances by application Substances 0.000 claims description 35
- 239000002131 composite material Substances 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 30
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 19
- 239000003638 chemical reducing agent Substances 0.000 claims description 19
- 239000004952 Polyamide Substances 0.000 claims description 18
- 239000006004 Quartz sand Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 150000001412 amines Chemical class 0.000 claims description 18
- 239000002518 antifoaming agent Substances 0.000 claims description 18
- 239000004568 cement Substances 0.000 claims description 18
- 239000013530 defoamer Substances 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 239000003995 emulsifying agent Substances 0.000 claims description 18
- 229920002647 polyamide Polymers 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- CUXYLFPMQMFGPL-UHFFFAOYSA-N (9Z,11E,13E)-9,11,13-Octadecatrienoic acid Natural products CCCCC=CC=CC=CCCCCCCCC(O)=O CUXYLFPMQMFGPL-UHFFFAOYSA-N 0.000 claims description 15
- CUXYLFPMQMFGPL-SUTYWZMXSA-N all-trans-octadeca-9,11,13-trienoic acid Chemical compound CCCC\C=C\C=C\C=C\CCCCCCCC(O)=O CUXYLFPMQMFGPL-SUTYWZMXSA-N 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 239000012188 paraffin wax Substances 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000013329 compounding Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000002209 hydrophobic effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- 239000011083 cement mortar Substances 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 239000011257 shell material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical group NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
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- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
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- Epoxy Resins (AREA)
Abstract
The application discloses a waterproof thermal insulation mortar and a preparation process thereof, wherein the thermal insulation mortar adopts epoxy resin and modified epoxy resin as mortar doping materials, the modified epoxy resin is prepared by reacting allyl epoxy resin, octadecanethiol and a photoinitiator, the allyl epoxy resin and the octadecanethiol are adopted as raw materials, and the hydrophobic modified epoxy resin is prepared by click chemistry.
Description
Technical Field
The application relates to the technical field of thermal insulation mortar, in particular to waterproof thermal insulation mortar and a preparation process thereof.
Background
The phase-change temperature-regulating building material is a building material prepared by using a phase-change energy storage material as a raw material. The phase change materials in practical application comprise solid-fixed phase change materials, solid-liquid microcapsule phase change materials and organic-inorganic phase change composite materials taking porous materials as carriers, and have important significance for building energy conservation and changing the comfort level of indoor environment.
In the prior art, a phase-change material is generally added into the cement mortar, the thermal insulation performance of the cement mortar is realized through phase-change temperature adjustment, the phase-change material is coated to prepare a phase-change capsule by a microcapsule method, but the compatibility between the phase-change capsule and the cement mortar can influence the mechanical performance of the cement mortar.
Aiming at the problem, we disclose a waterproof thermal insulation mortar and a preparation process thereof, so as to ensure the phase-change temperature-regulating effect and mechanical property of the cement mortar.
Disclosure of Invention
The application aims to provide waterproof thermal insulation mortar and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the application provides the following technical scheme:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material;
mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 20-30min, and then placing the mixture at 80-85 ℃ for stirring reaction, wherein the reaction is under the condition of UV illumination to obtain modified epoxy resin;
taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1-2h, adding phase change material, mixing, placing in water bath at 40-45 ℃, stirring for 30-40min, heating for solidification, and cooling to room temperature to obtain composite phase change material;
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 20-30min, adding an organic amine curing agent, and continuously stirring for 20-30min to obtain a component A;
mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifying agent and deionized water for 30-40min to obtain a component B;
mixing cement, quartz sand, a water reducing agent and a defoaming agent, and stirring for 20-30min to obtain a component C;
mixing the component A and the component B, stirring to uniformity, adding the component C, and continuously stirring to uniformity to obtain a finished product.
In the more optimized scheme, in the step (1), the preparation steps of the modified carbon nano tube are as follows:
taking a carbon nano tube, and performing plasma surface modification treatment by taking oxygen as a plasma source to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 1-2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 1-2 hours, placing the carbon nano tube at 60-65 ℃ for reaction for 4-5 hours, heating the carbon nano tube to 70-80 ℃ for reaction for 2-2.2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube.
In the more optimized scheme, the treatment power is 120-150W and the treatment time is 10-15min during the plasma surface modification treatment.
In the more optimized scheme, in the step (2), the raw materials of each component of the thermal insulation mortar comprise: 10-12 parts of component A, 10-14 parts of component B and 90-110 parts of component C by weight.
And according to a more optimized scheme, the raw materials of the component A comprise the following components in percentage by mass: 8-10wt% of composite phase change material, 20-30wt% of organic amine curing agent, 2-3wt% of defoamer, 3-5wt% of dispersing agent and the balance of deionized water;
the raw materials of the component B comprise: 15-20wt% of modified epoxy resin, 15-20wt% of epoxy resin, 2-4wt% of emulsifier, 10-15wt% of silane coupling agent and the balance deionized water;
the raw materials of the component C comprise: 40-45wt% of quartz sand, 1-2wt% of water reducer, 1-2wt% of defoamer and the balance of cement.
In the optimized scheme, in the step (1), the temperature is raised to 50-55 ℃ for curing for 12-14 hours, then raised to 70-75 ℃ for curing for 10-12 hours, and cooled to room temperature.
In the more optimized scheme, the reaction time is 3-4 hours when the modified epoxy resin is prepared.
According to an optimized scheme, the waterproof thermal insulation mortar is prepared according to the preparation process of the waterproof thermal insulation mortar.
Compared with the prior art, the application has the following beneficial effects:
the application discloses waterproof thermal insulation mortar and a preparation process thereof, wherein the waterproof thermal insulation mortar comprises the following raw materials in parts by weight: 10-12 parts of component A, 10-14 parts of component B and 90-110 parts of component C; the component A comprises a composite phase change material, deionized water, a defoaming agent, a dispersing agent, an organic amine curing agent and the like, the component B comprises an epoxy resin, a modified epoxy resin, a silane coupling agent, an emulsifying agent, deionized water and the like, and the component C comprises cement, quartz sand, a water reducing agent, a defoaming agent and the like; according to the heat-insulating mortar, epoxy resin and modified epoxy resin are selected as mortar doping materials, the modified epoxy resin is prepared by reacting allyl epoxy resin, octadecanethiol and a photoinitiator, the allyl epoxy resin and the octadecanethiol are adopted as raw materials, and the hydrophobic modified epoxy resin is prepared through click chemistry, so that the epoxy resin has excellent hydrophobic performance, and the modified epoxy resin, the epoxy resin and a silane coupling agent are mutually doped for crosslinking and curing, so that the crosslinking density of the whole system can be improved, the mechanical property of the heat-insulating mortar can be improved, the waterproof and dampproof properties of the heat-insulating mortar can be improved, and the service life of the mortar can be prolonged.
The application also adds composite phase change material, which is mainly prepared by the reaction of phase change material, epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube; in order to avoid the condition of flowing leakage when the phase change material is converted into a liquid state in the processing process, the application selects the epoxy resin to be solidified and sealed into a three-dimensional network structure through the cooperation of the epoxy resin, the modified epoxy resin and the polyamide curing agent, and the phase change material is coated and packaged, so that the leakage of the phase change material is greatly reduced through the operation.
Because the main components of the mortar are epoxy resin and modified epoxy resin, when the composite phase-change material is prepared, the shell material is selected to be doped with the epoxy resin and the modified epoxy resin, so that the compatibility of the composite phase-change material in the epoxy mortar is improved, the composite phase-change material can be uniformly dispersed in a mortar system, and the phase-change performance of the mortar is ensured. And mechanical properties, so that the mortar has excellent heat preservation performance.
However, the heat-conducting property of the epoxy resin is poor, and the epoxy resin and the modified epoxy resin are doped as the shell material, so that the heat-conducting property of the composite phase-change material can be greatly reduced; therefore, the modified carbon nano tube is added in the process, and has ultrahigh heat conductivity, so that the heat transfer performance of the whole composite phase change material can be improved.
In order to avoid agglomeration of the carbon nano tube and improve the compatibility of the carbon nano tube in epoxy resin/modified epoxy resin, the surface plasma modification is firstly carried out on the carbon nano tube, oxygen is used as a plasma source, the oxygen-containing functional groups on the surface of the obtained pretreated carbon nano tube are greatly improved, and the surface contains a large number of hydroxyl groups and carboxyl groups; then, the surface of the carbon nanotube is grafted with the eleostearic acid, the eleostearic acid contains long-chain alkyl, hydroxyl and carboxyl, the hydroxyl and the carboxyl can react with the carboxyl and the hydroxyl on the surface of the carbon nanotube, so that the long-chain alkyl is introduced, and the dispersion performance of the carbon nanotube can be effectively improved by introducing the long-chain alkyl; meanwhile, the surfaces of the modified epoxy resin and the modified carbon nano tube are both provided with hydrophobic long-chain alkyl groups, so that the modified carbon nano tube can be uniformly dispersed in the epoxy resin/modified epoxy resin, and the heat transfer performance of the whole composite phase change material is ensured.
The application discloses waterproof thermal insulation mortar and a preparation process thereof, which are reasonable in process design and simple in operation, the prepared thermal insulation mortar not only has excellent waterproof and moistureproof performances, but also can realize phase change temperature adjustment, improves the thermal insulation performance of the mortar, and meanwhile, the mechanical property of the thermal insulation mortar is enhanced, so that the thermal insulation mortar can be widely applied to various fields and has higher practicability.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
In this example, the carbon nanotubes have a diameter of 50-90 nm and a length of 5-10 μm, and are available from Suzhou first element nanotechnology Co., ltd; the polyamide curing agent is polyamide 650, purchased from the company of new material stock, brother of the company of the Hunan province; the organic amine curing agent is diethylenetriamine; the defoamer is a Mingliu 158 defoamer; the dispersing agent is hydroxyethyl cellulose; the emulsifier is OP-10; the silane coupling agent is prepared by mixing KH-550 and KH-560 with the mass ratio of 1:2. the water reducer is a megabetter 8040 polycarboxylate water reducer. The cement is 42.5 ordinary Portland cement. Quartz sand with fineness modulus of 2.7.
The preparation method of the allyl epoxy resin comprises the following steps: 314g of epichlorohydrin and 208g of 2,2' -diallyl bisphenol are mixed, stirred for 30min, 54g of sodium hydroxide is added, then a catalyst of tetramethyl ammonium bromide is added, the temperature is raised to 65 ℃ under the nitrogen environment, the reaction is carried out for 2.5h in a collective way, and the allyl epoxy resin is obtained after filtration, washing and purification and reduced pressure distillation. The catalyst was used in an amount of 1% by weight of 4, 4-diallyl bisphenol.
Example 1:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 20min, and then placing the mixture at 80 ℃ for stirring reaction for 4h under the UV illumination condition (365 nm) to obtain modified epoxy resin; the photoinitiator is photoinitiator 1173. The mass ratio of the allyl epoxy resin to the octadecyl mercaptan is 4:1, wherein the dosage of the photoinitiator is 1.5wt% of that of the allyl epoxy resin.
Taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1h, adding phase change material, mixing, placing in a water bath at 40 ℃, stirring for 40min, heating to cure, firstly heating to 50 ℃, curing for 14h, heating to 70 ℃ again, curing for 12h, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin to the modified epoxy resin to the polyamide curing agent is 1:1:2; the dosage of the modified carbon nano tube is 6wt% of the total amount of the epoxy resin and the modified epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin and the modified epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 20min, adding an organic amine curing agent, and continuing stirring for 20min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifier and deionized water for 30min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 20wt% of modified epoxy resin, 20wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 20min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
taking a carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 2 hours, placing the carbon nano tube at 65 ℃ for reaction for 4 hours, heating to 75 ℃ for reaction for 2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube. The mass ratio of the pretreated carbon nano tube to the eleostearic acid is 1:10.
example 2:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 25min, and then placing the mixture at 85 ℃ for stirring reaction for 3.5h under the condition of UV illumination (365 nm) to obtain modified epoxy resin; the photoinitiator is photoinitiator 1173. The mass ratio of the allyl epoxy resin to the octadecyl mercaptan is 4:1, wherein the dosage of the photoinitiator is 1.5wt% of that of the allyl epoxy resin.
Taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1.5 hours, adding phase change material, mixing, placing in a water bath at 45 ℃, stirring for 35 minutes, heating to cure, firstly heating to 55 ℃, curing for 13 hours, heating to 75 ℃, curing for 11 hours, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin to the modified epoxy resin to the polyamide curing agent is 1:1:2; the dosage of the modified carbon nano tube is 6wt% of the total amount of the epoxy resin and the modified epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin and the modified epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 25min, adding an organic amine curing agent, and continuing stirring for 25min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifier and deionized water for 35min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 20wt% of modified epoxy resin, 20wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 25min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
taking a carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 2 hours, placing the carbon nano tube at 65 ℃ for reaction for 4 hours, heating to 75 ℃ for reaction for 2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube. The mass ratio of the pretreated carbon nano tube to the eleostearic acid is 1:10.
example 3:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 30min, and then placing the mixture at 85 ℃ for stirring reaction for 3h under the UV illumination condition (365 nm) to obtain modified epoxy resin; the photoinitiator is photoinitiator 1173. The mass ratio of the allyl epoxy resin to the octadecyl mercaptan is 4:1, wherein the dosage of the photoinitiator is 1.5wt% of that of the allyl epoxy resin.
Taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 2 hours, adding phase change material, mixing, placing in a water bath at 45 ℃, stirring for 30 minutes, heating to cure, firstly heating to 55 ℃, curing for 12 hours, heating to 75 ℃, curing for 10 hours, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin to the modified epoxy resin to the polyamide curing agent is 1:1:2; the dosage of the modified carbon nano tube is 6wt% of the total amount of the epoxy resin and the modified epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin and the modified epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 30min, adding an organic amine curing agent, and continuously stirring for 30min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifier and deionized water for 40min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 20wt% of modified epoxy resin, 20wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 30min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
taking a carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 2 hours, placing the carbon nano tube at 65 ℃ for reaction for 4 hours, heating to 75 ℃ for reaction for 2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube. The mass ratio of the pretreated carbon nano tube to the eleostearic acid is 1:10.
comparative example 1:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 25min, and then placing the mixture at 85 ℃ for stirring reaction for 3.5h under the condition of UV illumination (365 nm) to obtain modified epoxy resin; the photoinitiator is photoinitiator 1173. The mass ratio of the allyl epoxy resin to the octadecyl mercaptan is 4:1, wherein the dosage of the photoinitiator is 1.5wt% of that of the allyl epoxy resin.
Taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1.5 hours, adding phase change material, mixing, placing in a water bath at 45 ℃, stirring for 35 minutes, heating to cure, firstly heating to 55 ℃, curing for 13 hours, heating to 75 ℃, curing for 11 hours, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin to the modified epoxy resin to the polyamide curing agent is 1:1:2; the dosage of the modified carbon nano tube is 6wt% of the total amount of the epoxy resin and the modified epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin and the modified epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 25min, adding an organic amine curing agent, and continuing stirring for 25min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifier and deionized water for 35min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 20wt% of modified epoxy resin, 20wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 25min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
and taking the carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain the modified carbon nano tube.
Comparative example 1 a control experiment was performed on the basis of example 2, in which carbon nanotubes were not modified by graft of eleostearic acid, and the remaining process and step parameters were identical to those of example 2.
Comparative example 2:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 25min, and then placing the mixture at 85 ℃ for stirring reaction for 3.5h under the condition of UV illumination (365 nm) to obtain modified epoxy resin; the photoinitiator is photoinitiator 1173. The mass ratio of the allyl epoxy resin to the octadecyl mercaptan is 4:1, wherein the dosage of the photoinitiator is 1.5wt% of that of the allyl epoxy resin.
Taking epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1.5 hours, adding phase change material, mixing, placing in a water bath at 45 ℃, stirring for 35 minutes, heating and curing, heating to 55 ℃, curing for 13 hours, heating to 75 ℃ again, curing for 11 hours, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin to the polyamide curing agent is 1:1, a step of; the dosage of the modified carbon nano tube is 6wt% of the total epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 25min, adding an organic amine curing agent, and continuing stirring for 25min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifier and deionized water for 35min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 20wt% of modified epoxy resin, 20wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 25min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
taking a carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 2 hours, placing the carbon nano tube at 65 ℃ for reaction for 4 hours, heating to 75 ℃ for reaction for 2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube. The mass ratio of the pretreated carbon nano tube to the eleostearic acid is 1:10.
comparative example 2 a control experiment was performed on the basis of example 2, in which comparative example 2 the modified epoxy resin was not doped in the composite phase change material, and the remaining process and step parameters were identical to those of example 2.
Comparative example 3:
a preparation process of waterproof thermal insulation mortar comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material; the mass ratio of the expanded graphite to the paraffin is 1.5:8.5. vacuum adsorption is carried out, vacuum is pumped to-0.1 MPa, and the vacuum adsorption is maintained for 20min.
Taking epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1.5 hours, adding phase change material, mixing, placing in a water bath at 45 ℃, stirring for 35 minutes, heating and curing, heating to 55 ℃, curing for 13 hours, heating to 75 ℃ again, curing for 11 hours, and cooling to room temperature to obtain the composite phase change material. The mass ratio of the epoxy resin polyamide curing agent is 1:1, a step of; the dosage of the modified carbon nano tube is 6wt% of the total epoxy resin; the amount of the phase change material is 75wt% of the total amount of the epoxy resin.
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 25min, adding an organic amine curing agent, and continuing stirring for 25min to obtain a component A; the A component comprises the following raw materials in percentage by mass: 10wt% of composite phase change material, 25wt% of organic amine curing agent, 3wt% of defoamer, 4wt% of dispersant and the balance of deionized water.
Mixing and stirring epoxy resin, a silane coupling agent, an emulsifier and deionized water for 35min to obtain a component B; the component B comprises the following raw materials in percentage by mass: 40wt% of epoxy resin, 3wt% of emulsifier, 14wt% of silane coupling agent and the balance of deionized water.
Mixing and stirring cement, quartz sand, a water reducing agent and a defoaming agent for 25min to obtain a component C; the C component comprises the following raw materials in percentage by mass: 45wt% of quartz sand, 2wt% of water reducer, 2wt% of defoamer and the balance of cement.
Taking 10 parts of the component A and 10 parts of the component B by mass, mixing and stirring until uniform, adding 90 parts of the component C, and continuously stirring until uniform to obtain a finished product.
Wherein: the preparation method of the modified carbon nano tube comprises the following steps:
taking a carbon nano tube, taking oxygen as a plasma source, performing plasma surface modification treatment with the treatment power of 120W and the treatment time of 15min, and introducing air pressure of 10Pa at the oxygen flow rate of 20ml/min to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 2 hours, placing the carbon nano tube at 65 ℃ for reaction for 4 hours, heating to 75 ℃ for reaction for 2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube. The mass ratio of the pretreated carbon nano tube to the eleostearic acid is 1:10.
comparative example 3 a control test was carried out on the basis of example 2, in which comparative example 3 the modified epoxy resin was not doped in the composite phase change material and the modified epoxy resin was not doped in the thermal insulation mortar, the remaining process and step parameters being identical to example 2.
And (3) testing:
1. the compressive strength and the flexural strength of the mortar were tested according to the technical procedure of epoxy resin mortar DL/T5193-2004 and the reinforcing design Specification for concrete construction GB/T50367-2006.
2. Pouring mortar building blocks with side length of 30cm and thickness of 5cm, inserting a temperature sensor into the center of each building block, and recording the temperature change of the center of each building block in real time; the mortar blocks are respectively put into an incubator, heated to a heating temperature of 20 ℃ to 60 ℃ for 40min, then stopped heating for 140min, and the temperature difference is recorded.
| Project | Compressive Strength/MPa | Flexural Strength/MPa | Water absorption percentage% | Heating stage | Cooling stage |
| Example 1 | 98 | 23 | 2.1 | 42.1℃ | 33.2℃ |
| Example 2 | 100 | 25 | 2.0 | 41.7℃ | 34.6℃ |
| Example 3 | 99 | 23 | 2.1 | 42.1℃ | 33.8℃ |
| Comparative example 1 | 96 | 21 | 2.3 | 44.3℃ | 30.5℃ |
| Comparative example 2 | 95 | 20 | 2.7 | 43.9℃ | 31.2℃ |
| Comparative example 3 | 89 | 17 | 3.1 | 46.3℃ | 28.7℃ |
Conclusion: the application discloses waterproof thermal insulation mortar and a preparation process thereof, which are reasonable in process design and simple in operation, the prepared thermal insulation mortar not only has excellent waterproof and moistureproof performances, but also can realize phase change temperature adjustment, improves the thermal insulation performance of the mortar, and meanwhile, the mechanical property of the thermal insulation mortar is enhanced, so that the thermal insulation mortar can be widely applied to various fields and has higher practicability.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (6)
1. A preparation process of waterproof thermal insulation mortar is characterized by comprising the following steps: the method comprises the following steps:
(1) Taking expanded graphite and paraffin wax, and carrying out vacuum adsorption compounding to obtain a phase change material;
mixing allyl epoxy resin, stearyl mercaptan and a photoinitiator, stirring for 20-30min, and then placing the mixture at 80-85 ℃ for stirring reaction, wherein the reaction is under the condition of UV illumination to obtain modified epoxy resin;
taking epoxy resin, modified epoxy resin, polyamide curing agent and modified carbon nano tube, performing ultrasonic dispersion for 1-2h, adding phase change material, mixing, placing in water bath at 40-45 ℃, stirring for 30-40min, heating for solidification, and cooling to room temperature to obtain composite phase change material;
(2) Mixing and stirring the composite phase change material, deionized water, a defoaming agent and a dispersing agent for 20-30min, adding an organic amine curing agent, and continuously stirring for 20-30min to obtain a component A;
mixing and stirring modified epoxy resin, a silane coupling agent, an emulsifying agent and deionized water for 30-40min to obtain a component B;
mixing cement, quartz sand, a water reducing agent and a defoaming agent, and stirring for 20-30min to obtain a component C;
mixing and stirring the component A and the component B until the components are uniform, adding the component C, and continuously stirring until the components are uniform to obtain a finished product; the thermal insulation mortar comprises the following raw materials in parts by weight: 10-12 parts of component A, 10-14 parts of component B and 90-110 parts of component C by weight;
in the step (1), the preparation steps of the modified carbon nano tube are as follows:
taking a carbon nano tube, and performing plasma surface modification treatment by taking oxygen as a plasma source to obtain a pretreated carbon nano tube; and (3) placing the pretreated carbon nano tube in a dimethylformamide solution, performing ultrasonic dispersion for 1-2 hours, adding eleostearic acid, continuing ultrasonic dispersion for 1-2 hours, placing the carbon nano tube at 60-65 ℃ for reaction for 4-5 hours, heating the carbon nano tube to 70-80 ℃ for reaction for 2-2.2 hours, washing with deionized water after the reaction is finished, and performing freeze drying to obtain the modified carbon nano tube.
2. The process for preparing the waterproof thermal insulation mortar as claimed in claim 1, wherein: during the plasma surface modification treatment, the treatment power is 120-150W, and the treatment time is 10-15min.
3. The process for preparing the waterproof thermal insulation mortar as claimed in claim 1, wherein: the A component comprises the following raw materials in percentage by mass: 8-10wt% of composite phase change material, 20-30wt% of organic amine curing agent, 2-3wt% of defoamer, 3-5wt% of dispersing agent and the balance of deionized water;
the raw materials of the component B comprise: 15-20wt% of modified epoxy resin, 15-20wt% of epoxy resin, 2-4wt% of emulsifier, 10-15wt% of silane coupling agent and the balance deionized water;
the raw materials of the component C comprise: 40-45wt% of quartz sand, 1-2wt% of water reducer, 1-2wt% of defoamer and the balance of cement.
4. The process for preparing the waterproof thermal insulation mortar as claimed in claim 1, wherein: in the step (1), the temperature is raised to 50-55 ℃ for curing for 12-14 hours, then to 70-75 ℃ for curing for 10-12 hours, and then cooled to room temperature.
5. The process for preparing the waterproof thermal insulation mortar as claimed in claim 1, wherein: in the step (1), the reaction time is 3-4h when the modified epoxy resin is prepared.
6. The heat-insulating mortar prepared by the preparation process of the waterproof heat-insulating mortar according to any one of claims 1-5.
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