CN109721319A - A kind of dry powder type wall heat-insulating material and preparation method thereof - Google Patents
A kind of dry powder type wall heat-insulating material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of dry powder type wall heat-insulating materials, belong to wall heat insulation material.It is poor that wall heat insulation material provided by the invention overcomes traditional plastic paint anticorrosive property, not environmentally the shortcomings that, it is prepared using perlite, cement, gypsum, methylcellulose, gel powder A, gel powder B, wherein, gel powder A is formed by resorcinol, formaldehyde, sodium carbonate, ethyl alcohol, pure water preparation；Gel powder B is formed by ammonium hydroxide, dimethylformamide, tetramethyl-orthosilicate, methanol, pure water preparation.Dry powder type wall heat-insulating material thermal insulation property with higher and lower heating conduction, good humidity resistance, use process provided by the invention are easy to operate.
Description
Technical field
The invention belongs to wall heat insulation material, especially a kind of dry powder type wall heat-insulating material and preparation method thereof.
Background technique
Heat preserving and insulating material be generally be lightweight, loose, porous, fibrous material.Organic material can be divided by its ingredient
With two kinds of inorganic material.Preferably compared with the latter, but the latter is good compared with the former durability for the former thermal and insulating performance.Thermal coefficient is weighing apparatus
Measure the main indicator of heat preserving and insulating material performance superiority and inferiority.Thermal coefficient is smaller, then the heat transmitted by material is smaller, thermal insulation separation
Hot property is better, and the thermal coefficient of material is decided by the ingredient of material, internal structure, bulk density etc., also determines putting down when heat transfer
The moisture content of equal temperature and material.Generally bulk density is lighter, and thermal coefficient is smaller.Wall heat insulation material (also known as inorganic active wall
Body heat preserving and insulating material) materials for wall can be largely saved, wall insulation performance is improved, economizes on resources, reduces environmental pollution, be special
It infuses in the new material for doing inside and outside wall thermal insulation.Wall energy-saving and heat-insulating material includes organic, inorganic and composite material class.
External-wall heat-insulation material needs to undertake the effect of the extraneous factors such as defence outdoor temperature, humidity variation, solar radiation.Mesh
The exterior wall protection materials that preceding comparison is popular are that certain heat insulation effect is played using materials such as thin web or plasterboards, but whole
Thickness is big, and heat insulation effect is general, and constructing operation is inconvenient, and poor for the adaptibility to response of humidity variation, and water suction is strong, while plate
Fire protecting performance is low.
Summary of the invention
Described above in order to overcome the shortcomings of, the present invention provides a kind of dry powder type wall heat-insulating materials, and the material is to wall
Body has excellent thermal insulation property.
Specifically, the present invention is achieved through the following technical solutions:
A kind of dry powder type wall heat-insulating material, by perlite, cement, gypsum, methylcellulose, gel powder A, gel powder
Last B is prepared.
The gel powder A includes that resorcinol, formaldehyde, sodium carbonate, ethyl alcohol, pure water preparation form, the gel powder B
It is prepared by ammonium hydroxide, dimethylformamide, tetramethyl-orthosilicate, methanol, water.
Preferably, the dry powder type wall heat-insulating material by by weight 15-25 part perlite, 15-25 parts of cement,
A, 10-30 parts of 20-30 parts of gypsum, 1-2 parts of methylcellulose, 20-40 parts of gel powders gel powder B are prepared.
Preferably, the gel powder A includes 1-5 part resorcinol, 1-5 parts of formaldehyde, 0.001-0.005 by weight
Part sodium carbonate, 80-100 parts of water are prepared；
Preferably, the gel powder B by by weight 0.1-1 part ammonium hydroxide, 5-10 parts of dimethylformamides,
100-200 parts of tetramethyl-orthosilicates, 350-400 parts of methanol, 100-200 parts of water are prepared.
Preferably, the gel powder A and gel powder B weight ratio are 2:1.
Preferably, gypsum, cement are added in agitator tank, is shut down after stirring 5-10min；It is separately added into perlite, first again
Base cellulose, gel powder A, in gel powder B to tank, dry powder type wall thermal insulating material that booting stirring 5-10min is mixed
Material, pack storage.
Preferably, the gel powder A's the preparation method is as follows:
(1) it forms powdered charcoal-aero gel: resorcinol is dissolved in pure water, add formaldehyde, stir 10-20min, be added
Sodium carbonate after stirring 10-20min, at 70-85 DEG C, stirs 60-80h with the speed of 300-400r/min, cleans 3- with ethyl alcohol
5 times, use supercritical CO2Dry, be then carbonized under 950-1000 DEG C, inert gas shielding 3-5h again, obtains powdered charcoal airsetting
Glue；
(2) chemical vapor deposition: gas-phase deposition system first is added in powdered charcoal-aero gel, then vacuumizes, is passed through mixed
Gas is closed, is reacted at 150-160 DEG C, subsequent device cooled to room temperature to be dried；
(3) it calcines: taking chemical vapor deposition obtained solid to calcine 2-4 hours at 500-600 DEG C in air, obtain gel powder
Last A；
The mixed gas is made of ethyl orthosilicate gas and ammonia.
Preferably, the flow velocity of mixed gas described in the preparation method of the gel powder A is 2mL/min.
Preferably, mixed gas described in the preparation method of the gel powder A is by ethyl orthosilicate gas and ammonia
It is formed by volume for 6:1.
Preferably, powdered charcoal-aero gel should disperse to spread out during the reaction, with a thickness of 2-5mm.
Preferably, powdered charcoal-aero gel and the mass volume ratio of ventilation are 1:10 (g/ml).
Preferably, chemical vapor deposition step cycle 3-5 times in the preparation method of the gel powder A.
Preferably, inert gas is nitrogen in the preparation method of the gel powder A.
Preferably, the gel powder B's the preparation method is as follows:
(1) tetramethyl-orthosilicate is dissolved in methanol, dimethylformamide is then added, ammonium hydroxide is then added
And deionized water, 100-200r/min are slowly stirred, and gel formation time is controlled in 40-80min；
(2) gel is immersed in 12-24h in the n-hexane containing hydrophobing agent, is submerged again after taking-up in ethanol, per for 24 hours
An ethyl alcohol is changed, continues 14-21 days；
(3) supercritical CO is used2It is dry, obtain gel powder B.
Preferably, the volume ratio of hydrophobing agent and n-hexane is 1:9 in the preparation method of the gel powder B.
Preferably, hydrophobing agent is trim,ethylchlorosilane in the preparation method of the gel powder B.
Thermal insulation material is added water and stirred into paste by the application method of dry powder type wall heat-insulating material, is coated with by engine request
Onto metope.
Preferably, thermal insulation material and water are 10:(3-5 by weight).
The invention has the beneficial effects that the present invention gel powder A and B used in thermal insulation material all have it is good
Thermal insulation property.Wherein, the nano tubular structure of gel powder A helps to enhance shortwave scattering, realizes visible light and near infrared light
High transmittance and low ultraviolet ray transmissivity, while there is good processability and ultralow hot transmitance.Gel powder B is having
While having good thermal insulation property, light transmittance with higher and good hydrophobic performance make thermal insulation material be coated on exterior wall
Meanwhile it being not easily susceptible to rain erosion, there is good humidity resistance, prolong the service life.
Specific embodiment
The present invention is further elaborated below with reference to embodiment, but following embodiments are only used to explain that the present invention cannot
For limiting the present invention.The number mentioned in following embodiments is except as otherwise pointing out that outer is parts by weight.
Specifically, the raw material used in following embodiments is as follows:
Resorcinol, No. CAS: 108-46-3.
Formaldehyde, No. CAS: 50-00-0.
Sodium carbonate, No. CAS: 497-19-8.
Ethyl alcohol, No. CAS: 64-17-5.
Ethyl orthosilicate, No. CAS: 78-10-4.
Ammonia, No. CAS: 7664-41-7.
Ammonium hydroxide, No. CAS: 1336-21-6.
Dimethylformamide, No. CAS: 68-12-2.
Methyl orthosilicate, No. CAS: 681-84-5.
Methanol, No. CAS: 67-56-1.
N-hexane, No. CAS: 110-54-3.
Trim,ethylchlorosilane, No. CAS: 75-77-4.
Ethyl orthosilicate, No. CAS: 78-10-4, it is purchased from Shenzhen Wang Dakang Science and Technology Ltd.
Perlite is purchased from Xinyang Pingqiao District great Fa pearlite insulation Building Materials Factory.
Cement is 42.5 portland cements, is purchased from Anhui Conch Cement limited liability company.
Gypsum is purchased from Chongqing Shuan Tian chemical industry Co., Ltd.
Methylcellulose is purchased from Zhejiang Hai Shen new material Co., Ltd.
CVD gas-phase deposition system, purchased from Zhengzhou at more scientific instrument Co., Ltd.
Embodiment 1
A kind of dry powder type wall heat-insulating material, by 15 parts of perlites by weight, 15 parts of cement, 30 parts of gypsum, 1 part of first
Base cellulose, 30 parts of gel powder A, 15 parts of gel powder B are prepared.
The preparation method of the gel powder A:
(1) it forms powdered charcoal-aero gel: 1 part of resorcinol is dissolved in pure water, add 1 part of formaldehyde, stir 10min,
0.001 part of sodium carbonate is added, after stirring 10min, at 85 DEG C, 60h is stirred with the speed of 300r/min, is cleaned 5 times with ethyl alcohol,
Use supercritical CO2Dry, be then carbonized under 1000 DEG C, nitrogen protection 3h again, obtains powdered charcoal-aero gel；(2) gas chemistry
Deposition: it takes powdered charcoal-aero gel that gas-phase deposition system is added, then vacuumizes, being passed through volume ratio with the flow velocity of 2mL/min is
The ethyl orthosilicate gas and ammonia of 6:1, ventilatory capacity are that 0.1g gel/mL reacts 3 hours at 160 DEG C, keep drier naturally cold
But it to room temperature, recycles 3 times；(3) it calcines 2 hours at 600 DEG C in air, obtains gel powder A.
The preparation method of the gel powder B:
(1) 100 parts of tetramethyl-orthosilicates are dissolved in 350 parts of methanol, 5 parts of dimethylformamides are then added, then
0.1 part of ammonium hydroxide and 100 parts of deionized waters is added, 100r/min is slowly stirred, and gel formation time is controlled in 40min；
(2) gel is immersed in 12h in the n-hexane containing 10vol% methylchlorosilane, is submerged again after taking-up in ethanol, per for 24 hours
An ethyl alcohol is changed, continues 21 days；(3) supercritical CO is used2It is dry, obtain gel powder B.
The preparation method of the dry powder type wall heat-insulating material:
30 parts of gypsum, 15 parts of cement are added in agitator tank, are shut down after stirring 5min；It is separately added into 15 parts of perlites, 1 again
Part methylcellulose, 30 parts of gel powder A, in 15 parts of gel powder B to tank, dry-powder-type wall that booting stirring 5min is mixed
Body thermal insulation material.
Embodiment 2
A kind of dry powder type wall heat-insulating material, by 25 parts of perlites by weight, 25 parts of cement, 30 parts of gypsum, 1 part of first
Base cellulose, 20 parts of gel powder A, 10 parts of gel powder B are prepared.
The preparation method of the gel powder A:
(1) it forms powdered charcoal-aero gel: 1 part of resorcinol is dissolved in pure water, add 1 part of formaldehyde, stir 10min,
0.001 part of sodium carbonate is added, after stirring 10min, at 85 DEG C, 60h is stirred with the speed of 300r/min, is cleaned 5 times with ethyl alcohol,
Use supercritical CO2Dry, be then carbonized under 1000 DEG C, nitrogen 3h again, obtains powdered charcoal-aero gel；(2) chemical vapor deposition:
Gas-phase deposition system first is added in powdered charcoal-aero gel, then vacuumizes, volume ratio is passed through as 6:1 with the flow velocity of 2mL/min
Ethyl orthosilicate gas and ammonia, ventilatory capacity be 0.1g gel/mL 160 DEG C react 3 hours, naturally cool to drier
Room temperature；(3) it calcines 2 hours at 600 DEG C in air, obtains gel powder A.
The preparation method of the gel powder B:
(1) 100 parts of tetramethyl-orthosilicates are dissolved in 350 parts of methanol, 5 parts of dimethylformamides are then added, then
0.1 part of ammonium hydroxide and 100 parts of deionized waters is added, 100r/min is slowly stirred, and gel formation time is controlled in 40min；
(2) gel is immersed in 12h in the n-hexane containing 10vol% trim,ethylchlorosilane, then submerged again in ethanol, per for 24 hours
An ethyl alcohol is changed, continues 21 days；(3) supercritical CO is used2It is dry, obtain gel powder B.
The preparation method of the dry powder type wall heat-insulating material:
30 parts of gypsum, 25 parts of cement are added in agitator tank, are shut down after stirring 5min；It is separately added into 25 parts of perlites, 1 again
Part methylcellulose, 20 parts of gel powder A, in 10 parts of gel powder B to tank, dry-powder-type wall that booting stirring 5min is mixed
Body thermal insulation material.
Embodiment 3
A kind of dry powder type wall heat-insulating material, by 25 parts of perlites by weight, 25 parts of cement, 30 parts of gypsum, 1 part of first
Base cellulose, 20 parts of gel powder A, 10 parts of gel powder B are prepared.
The preparation method of the gel powder A:
(1) it forms powdered charcoal-aero gel: 5 parts of resorcinols is dissolved in pure water, add 5 parts of formaldehyde, stir 10min,
0.005 part of sodium carbonate is added, after stirring 10min, at 85 DEG C, 60h is stirred with the speed of 400r/min, is cleaned 5 times with ethyl alcohol,
Use supercritical CO2Dry, be then carbonized under 1000 DEG C, nitrogen 5h again, obtains powdered charcoal-aero gel；(2) chemical vapor deposition:
Gas-phase deposition system first is added in powdered charcoal-aero gel, then vacuumizes, volume ratio is passed through as 6:1 with the flow velocity of 2mL/min
Ethyl orthosilicate gas and ammonia, ventilatory capacity be 0.1g gel/mL 160 DEG C react, be cooled to room temperature drier, so
Circulation 3 times；(3) it calcines 2 hours at 600 DEG C in air, obtains gel powder A.
The preparation method of the gel powder B:
(1) 200 parts of tetramethyl-orthosilicates are dissolved in 400 parts of methanol, 10 parts of dimethylformamides are then added, so
1 part of ammonium hydroxide is added afterwards and 100 parts of deionized waters, 100r/min are slowly stirred, gel formation time is controlled in 80min；
(2) gel is immersed in the n-hexane containing 10vol% trim,ethylchlorosilane for 24 hours, is then submerged again in ethanol, per for 24 hours
An ethyl alcohol is changed, continues 21 days；(3) supercritical CO is used2It is dry, obtain gel powder B.
The preparation method of the dry powder type wall heat-insulating material:
30 parts of gypsum, 25 parts of cement are added in agitator tank, are shut down after stirring 5min；It is separately added into 25 parts of perlites, 1 again
Part methylcellulose, 20 parts of gel powder A, in 10 parts of gel powder B to tank, booting stirring 5min obtains dry powder type wall heat preservation
Material.
Test case 1
Equivalent heat conductivity test
It is 500mm × 500mm in specification according to GB/T32981-2016 " materials for wall equivalent heat conductivity measuring method "
The thermal insulation material after 2mm is coated in the styrofoam of × 0.5mm, detection data is as shown in table 1:
The test of 1 equivalent heat conductivity of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Equivalent heat conductivity [W/ (m*K)] | 0.020 | 0.032 | 0.026 |
Test case 2
Humidity resistance test
In the thermal insulation material that specification is after being coated with 2mm in 500mm × 500mm × 0.5mm styrofoam, pressure testing machine is used
(middle wound, ZCYD-S100A) detects the unconfined compressive strength (F) under its drying condition, is immersed in 20 DEG C of water and takes out afterwards for 24 hours,
Swimming for surface is wiped out, its unconfined compressive strength (f) is surveyed, calculates its coefficient of softing K, as a result as shown in table 2 below.
K=f/F
The test of 2 humidity resistance of table
| Coefficient of softing | |
| Embodiment 1 | 0.91 |
| Embodiment 2 | 0.78 |
| Embodiment 3 | 0.87 |
Claims (10)
1. a kind of dry powder type wall heat-insulating material, which is characterized in that by perlite, cement, gypsum, methylcellulose, gel powder
Last A, gel powder B are prepared；
The gel powder A includes that resorcinol, formaldehyde, sodium carbonate, ethyl alcohol, water are prepared；
The gel powder B is prepared by ammonium hydroxide, dimethylformamide, tetramethyl-orthosilicate, methanol, water.
2. dry powder type wall heat-insulating material according to claim 1, which is characterized in that the dry powder type wall thermal insulating material
Material includes 15-25 part perlite, 15-25 parts of cement, 20-30 parts of gypsum, 1-2 parts of methylcellulose, 20-40 by weight
Part A, 10-30 parts of gel powder B of gel powder are prepared.
3. dry powder type wall heat-insulating material according to claim 1, which is characterized in that the gel powder A is by by weight
1-5 part resorcinol, 1-5 parts of formaldehyde, 0.001-0.005 parts of sodium carbonate, the 80-100 parts of water of part meter are prepared.
4. dry powder type wall heat-insulating material according to claim 1, which is characterized in that gel powder B is by by weight
0.1-1 part ammonium hydroxide, 5-10 parts of dimethylformamides, 100-200 parts of tetramethyl-orthosilicates, 350-400 parts of methanol,
100-200 parts of water are prepared.
5. dry powder type wall heat-insulating material according to claim 1, which is characterized in that the gel powder A and gel powder
Last B weight ratio is 2:1.
6. the method for preparing dry powder type wall heat-insulating material described in claim 1-5 any one, which is characterized in that stirring
Gypsum, cement are added in tank, is shut down after stirring 5-10min；It is separately added into perlite again, methylcellulose, gel powder A, coagulates
In the B to tank of rubber powder end, the dry powder type wall heat-insulating material that 5-10min is mixed is stirred in booting.
7. the method according to claim 6 for preparing dry powder type wall heat-insulating material, which is characterized in that the gel powder
A's the preparation method is as follows:
(1) it forms powdered charcoal-aero gel: resorcinol is dissolved in pure water, add formaldehyde, stir 10-20min, carbonic acid is added
Sodium after stirring 10-20min, at 70-85 DEG C, stirs 60-80h with the speed of 300-400r/min, is cleaned 3-5 times with ethyl alcohol,
Use supercritical CO2Dry, be then carbonized under 950-1000 DEG C, inert gas shielding 3-5h again, obtains powdered charcoal-aero gel；
(2) chemical vapor deposition: gas-phase deposition system first is added in powdered charcoal-aero gel, then vacuumizes, is passed through gaseous mixture
Body is reacted at 150-160 DEG C, subsequent device cooled to room temperature to be dried；
(3) it calcines: taking chemical vapor deposition obtained solid to calcine 2-4 hours at 500-600 DEG C in air, obtain gel powder A；
The mixed gas is made of ethyl orthosilicate gas and ammonia.
8. the method according to claim 6 for preparing dry powder type wall heat-insulating material, which is characterized in that the gel powder
B's the preparation method is as follows:
(1) tetramethyl-orthosilicate is dissolved in methanol, dimethylformamide is then added, ammonium hydroxide is then added and gone
Ionized water, 100-200r/min are slowly stirred, by gel formation time control between 40-80min；
(2) gel is immersed in 12-24h in the n-hexane containing hydrophobing agent, is submerged again after taking-up in ethanol, it is every to change one for 24 hours
Secondary ethyl alcohol continues 14-21 days；
(3) supercritical CO is used2It is dry, obtain gel powder B.
9. the application method of dry powder type wall heat-insulating material described in claim 1-5 any one, which is characterized in that will keep the temperature
Material adds water and stirs into paste, is applied on metope by engine request.
10. the application method of dry powder type wall heat-insulating material according to claim 9, which is characterized in that thermal insulation material with
Water is 10:(3-5 by weight).
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Application publication date: 20190507 |