CN108314873A - Nano-silicon polymerize thermal insulation board - Google Patents
Nano-silicon polymerize thermal insulation board Download PDFInfo
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- CN108314873A CN108314873A CN201810125523.7A CN201810125523A CN108314873A CN 108314873 A CN108314873 A CN 108314873A CN 201810125523 A CN201810125523 A CN 201810125523A CN 108314873 A CN108314873 A CN 108314873A
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C08K7/10—Silicon-containing compounds
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- C08K9/10—Encapsulated ingredients
Abstract
The present invention provides a kind of nano-silicons to polymerize thermal insulation board, is related to building thermal insulation material technical field, solves the problems, such as that existing thermal insulation board flame retardant property is low.The nano-silicon polymerize thermal insulation board, is made up of following steps：Step 1：Hydrochloric acid and alundum (Al2O3) is soluble in water, and it is 50 70 DEG C to heat and keep temperature, and ethylenediamine tetra-acetic acid is added under stirring and continues to stir, and fully obtains the solution of organic ion containing aluminium after reaction；Step 2：Nano level silica dioxide granule is added in the solution of organic ion containing aluminium made from step 1, stirring is up to volatile dry at 90 110 DEG C, and is roasted at 550 650 DEG C, obtains the silica dioxide granule of cladding alundum (Al2O3)；Step 3：The silica dioxide granule that parts by weight are cladding alundum (Al2O3) made from 30 50 parts of melmac, 35 parts of curing agent, 69 parts of foaming agents and 40 70 parts of step 2 is mixed and is foamed at 50 100 DEG C, nano-silicon polymerization thermal insulation board is made.The present invention is used for building exterior wall heat preserving, has good flame retardant effect.
Description
Technical field
The invention belongs to building thermal insulation material technical fields, and in particular to a kind of nano-silicon polymerization thermal insulation board.
Background technology
On the basis of existing building, China can also increase a large amount of new building every year, and building energy consumption has accounted for national total
The significant proportion of energy consumption, Building Energy-saving have become the important link of China's sustainable development.It is arranged in external wall and keeps the temperature
Plate plays an important roll to reducing building energy consumption.The material of existing thermal insulation board can be divided into organic material and inorganic material；Its
In, extruded polystyrene board (XPS) or expansion polyphenyl plate (EPS) etc. are most common organic insulation materials, although organic material has
The advantages that thermal coefficient is low and density is small, but its combustibility also results in prodigious security risk；Inorganic heat insulation material has anti-
Fire is fire-retardant, deformation coefficient is small, anti-aging performance, while being combined with plinth course and float coat preferable, and safety and firmness is good, applies
Work difficulty is small, and engineering cost is relatively low, although inorganic heat insulation material has a variety of excellent properties, general density is larger, heat preservation
Effect is slightly worse, in order to improve the heat insulation effect of inorganic heat-insulation board, can increase the organic principle of some auxiliary, although improving heat preservation
The heat insulation effect of plate but reduces its anti-flammability.
Therefore, on the basis of ensureing heat insulation effect, how to further increase the flame retardant property of thermal insulation board is this field skill
Art personnel important technological problems to be solved.
Invention content
The purpose of the present invention is to provide a kind of nano-silicons to polymerize thermal insulation board, and it is relatively low to have solved existing thermal insulation board flame retardant property
The technical issues of.
To achieve the above object, nano-silicon of the invention polymerize thermal insulation board, is made up of following steps：
Step 1：Hydrochloric acid and alundum (Al2O3) is soluble in water, and it is 50-70 DEG C to heat and keep temperature, under stirring
Ethylenediamine tetra-acetic acid is added and continues to stir, fully obtains the solution of organic ion containing aluminium after reaction；
Step 2：Nano level silica dioxide granule is added in the solution of organic ion containing aluminium made from step 1, in
Stirring is up to volatile dry at 90-110 DEG C, and is roasted at 550-650 DEG C, obtains the silica of cladding alundum (Al2O3)
Grain；
Step 3：By parts by weight be 30-50 parts of melmac, 3-5 parts of curing agent, 6-9 parts of foaming agents and
The silica dioxide granule mixing of 40-70 parts of step 2 cladding alundum (Al2O3) obtained and the obtained nanometer that foams at 50-100 DEG C
Silicon polymerize thermal insulation board.
Wherein, alundum (Al2O3) is used as silicon source, and aluminium ion can be discharged under the action of hydrochloric acid；Ethylenediamine tetra-acetic acid
(EDTA) it is a polyacid, and is trilon；In the solution with H4Y、H3Y-、HY3-, Y4-Etc. forms exist, wherein Y4-
It can directly coordinate with aluminium ion and generate stable complex, match ratio 1：1.Pass through reactionThe solution of organic ion containing the aluminium i.e. cooperation of aluminium can be shaped
Object solution；Silica dioxide granule is added into the complex solution of aluminium again to be uniformly mixed, in the drying process, the cooperation of aluminium
Object can uniformly be attached to silica particles, and the complex of aluminium can three oxidation two of oxidation by air formation in roasting process
Aluminium, to which the silica dioxide granule with alundum (Al2O3) clad be made；Wherein hydrochloric acid is provided in initial reaction stage as main
A hydrionic side can speed up alundum (Al2O3) hydrolysis release aluminium ion, in the solution of organic ion containing aluminium of formation, hydrochloric acid
Also it can play the role of stabilizer；With the combination of aluminium ion and ethylenediamine tetra-acetic acid, the hydrogen ion of ethylenediamine tetra-acetic acid hydrolysis
It recombines with chlorion, is volatilized in the form of hydrogen chloride in heat drying process；Coat the silica of alundum (Al2O3)
Particle size determines by Primary silica granular size, and the thickness of alundum (Al2O3) clad is according to the complex and dioxy of aluminium
The molar ratio of silicon carbide particle is different and changes, and when silica dioxide granule large percentage, coating thickness is relatively thin；Work as dioxy
When silicon carbide particle ratio is smaller, coating thickness is thicker；Specific thickness can be adjusted according to actual needs.
The nano level silica dioxide granule of the present invention refers mainly to aerosil, has good heat-insulating property,
Civilian thermal insulation material is especially in terms of exterior-wall heat insulation, compared to traditional inorganic heat insulation material in building energy conservation heat insulation field and organic
Thermal insulation material；And the fusing point of alundum (Al2O3) is up to 2050 DEG C, compared to the silica that fusing point is 1650 DEG C with higher resistance to
Alundum (Al2O3) is coated on silica particles by fire, can improve the contact area between two kinds of substances, reduce at
Phase difficulty remains the good heat-insulating property of silica dioxide granule, and the characteristics of combine alundum (Al2O3) high fire-retardance, passes through
Thermal insulation board prepared by the silica dioxide granule of alundum (Al2O3) is coated, guarantor is further improved on the basis of ensureing heat insulation effect
The anti-flammability of warm plate meets the requirement of modern architecture exterior-wall heat insulation, while preparation method is simple by the present invention, mild condition,
Controllability is strong；And the raw material sources such as alundum (Al2O3), hydrochloric acid and ethylenediamine tetra-acetic acid used are at low cost extensively, convenient for big rule
Mould produces.
Preferably, it is additionally added sodium citrate in the step 1.Sodium citrate have it is preferable water-soluble, latent and
Stability can effectively inhibit ionic crystal, keep the solution system of organic ion containing aluminium made from step 1 more stable.
Preferably, the molar ratio of the alundum (Al2O3), ethylenediamine tetra-acetic acid, hydrochloric acid and silica dioxide granule is 1：
2~3：2~3：1-2.
Preferably, silica dioxide granule is aerosil in the step 2, and foaming agent is ten in the step 3
Sodium dialkyl sulfate.Aerosil have nanoporous and three-dimensional network skeleton structure, have density is small, aperture is small,
The advantages such as porosity height, large specific surface area, thermal coefficient be low；Lauryl sodium sulfate act not only as foaming agent also have go out
The property of fire, therefore help to improve the anti-flammability of thermal insulation board.
Preferably, in the step 3 curing agent be phosphoric acid and hexanedioic acid composite curing agent, and the phosphoric acid and hexanedioic acid
Weight ratio be 1：0.5-2.Curing agent uses organic cooperation of organic acid and inorganic acid, and solidification effect is more preferable, makes whole dosage
It reduces.
Preferably, alumina silicate fibre, and the melmac and the alumina silicate fibre are additionally added in the step 3
Weight ratio be 1：0.5-1.It is a kind of New type of light refractory material that alumina silicate fibre, which is called ceramic fibre, which, which has, holds
The advantages that heavy and light, high temperature resistant, thermal stability are good, and pyroconductivity is low, thermal capacitance is small, expanded by heating is small, heat-proof quality is good.
Preferably, phosphate ester glycine betaine, and the melmac and the phosphate ester sweet tea are additionally added in the step 3
The weight ratio of dish alkali is 1：0.1-0.2.Phosphate ester glycine betaine is made of phosphoric acid ester group (HPO4-) and quaternary ammonium group, there is both sexes table
The excellent solubilising of face activating agent, emulsifying dispersivity, antistatic property, thermal stability etc., and it is better than general anion surface active
Alkali resistance, electrolyte-resistant and the antistatic property advantage of agent, can be used in fire retardant, emulsifier, therefore phosphate ester glycine betaine
The uniformity consistency and anti-flammability of thermal insulation board can be improved by being added.
Preferably, the melmac is made by following steps：
Step A：At 80-90 DEG C, vinyl alcohol, melamine, formaldehyde are dissolved into water, sodium hydroxide is added and adjusts pH
It is reacted to 8.5-9.0, after reaction solution clarification, melamine methylol solution is made；
Step B：Phenol is modified to obtain blocking modification monomer by formaldehyde, sodium sulfite, reaction temperature is 50-55 DEG C,
Control ph is 6.5-7.5；
Step C：The blocking modification monomer that the melamine methylol solution that step A is obtained is obtained with step B is sealed
Polycondensation reaction, 60 DEG C of reaction temperature, control ph 7-8 is held to obtain melmac solution, be dried to obtain melamine tree
Fat.
The synthesis technology of traditional melmac is broadly divided into two steps：1, melamine is reacted with formaldehyde generates hydroxyl first
Base melamine；2, condensation reaction generation melmac occurs under certain condition for melamine methylol.And it is of the invention
The method for preparing melmac be that polyfunctional group Phenol Monomer is modified using formaldehyde and sodium sulfite, obtain having specific
Then the modified phenol monomer of degree of functionality is contained to close methylol with reaching reduction product free formaldehyde by modified phenol monomer
Amount, the process have good controllability, since monomer structure determines, can ensure there is spy by controlling feeding quantity to prepare
Determine the product of molecular structure.
Melmac prepared by the method for the present invention has lower free formaldehyde content, is used in the processing of thermal insulation board
The murder by poisoning to operating personnel can be effectively reduced in the process, while there is good select operator, mixed with other materials
Foaming can make thermal insulation board overall permanence evenly consistent when preparing thermal insulation board；Simultaneously using water as solvent, there is non-ignitable, peace
Entirely, the advantages of environmental protection, saving cost.
Preferably, melamine in the step A, vinyl alcohol, formaldehyde molar ratio be 1：2-3：1.5-2.5.
Preferably, in the step A phosphite ester is additionally added in melamine methylol solution obtained.Phosphite ester energy
The processing temperature for enough improving polymer is conducive to rapid reaction and stablizes progress, while can play the role of intercalating agent, makes finally to make
The melmac obtained is more stable.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, technical scheme of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.In case of no particular description, the material that the present invention uses
Or instrument is existing product.
Embodiment 1
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, is made up of following steps：
Step 1：A concentration of 2mol/L hydrochloric acid of 10L and 1020g alundum (Al2O3)s are dissolved in 10L water, temperature is heated and kept
Degree is 50 DEG C, and the ethylenediamine tetra-acetic acid of a concentration of 2mol/L of 10L is added under stirring and continues to stir, fully after reaction
To the solution of organic ion containing aluminium；
Step 2：600g aerosils are added in the solution of organic ion containing aluminium made from step 1, in 90
Stirring obtains the silica of cladding alundum (Al2O3) up to volatile dry, and in keeping roasting at 650 DEG C in crucible furnace at DEG C
Aeroge；
Step 3：It is 300g melmacs, 10g phosphoric acid, 20g hexanedioic acids, 60g dodecyl sulphates by parts by weight
The aerosil mixing of sodium and 700g steps 2 cladding alundum (Al2O3) obtained and the obtained nano-silicon that foams at 50 DEG C
It polymerize thermal insulation board.
Embodiment 2
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, is made up of following steps：
Step 1：A concentration of 3mol/L hydrochloric acid of 10L and 1020g alundum (Al2O3)s are dissolved in 10L water, temperature is heated and kept
Degree is 70 DEG C, and the ethylenediamine tetra-acetic acid of a concentration of 3mol/L of 10L is added under stirring and continues to stir, fully after reaction
To the solution of organic ion containing aluminium；
Step 2：1200g aerosils are added in the solution of organic ion containing aluminium made from step 1, in
Stirring obtains the dioxy of cladding alundum (Al2O3) up to volatile dry, and in keeping roasting at 550 DEG C in crucible furnace at 110 DEG C
SiClx aeroge；
Step 3：It is 500g melmacs, 25g phosphoric acid, 25g hexanedioic acids, 90g dodecyl sulphates by parts by weight
The aerosil mixing of sodium and 400g steps 2 cladding alundum (Al2O3) obtained and the obtained nano-silicon that foams at 50 DEG C
It polymerize thermal insulation board.
Embodiment 3
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, is made up of following steps：
Step 1：A concentration of 2.5mol/L hydrochloric acid of 10L and 1020g alundum (Al2O3)s are dissolved in 10L water, heated and kept
Temperature is 60 DEG C, and the ethylenediamine tetra-acetic acid of a concentration of 2.5mol/L of 10L is added under stirring and continues to stir, fully reacts
After obtain the solution of organic ion containing aluminium；
Step 2：900g aerosils are added in the solution of organic ion containing aluminium made from step 1, in 90
Stirring obtains the silica of cladding alundum (Al2O3) up to volatile dry, and in keeping roasting at 600 DEG C in crucible furnace at DEG C
Aeroge；
Step 3：Modified cyanurotriamide resin is prepared, at 80 DEG C, by 1260g melamines, 880g vinyl alcohols, 750g first
Aldehyde is dissolved into 10L water, and sodium hydroxide adjusting pH to 8.5-9.0 is added and is reacted, after reaction solution clarification, methylol is made
Melamine solution；940g phenol is modified to obtain blocking modification monomer, reaction temperature by 150g formaldehyde, 300g sodium sulfites
It is 60 DEG C, control ph 6.5；Melamine methylol solution and blocking modification monomer are subjected to sealing end polycondensation reaction, reacted
Temperature 60 C, control ph 7 obtain modified cyanurotriamide resin solution, modified cyanurotriamide resin are obtained after dry.
Step 4：By modified cyanurotriamide resin obtained, 26g phosphoric acid, 13g hexanedioic acids, 80g dodecanes in 400g steps 3
The aerosil mixing of base sodium sulphate and 550g steps 2 cladding alundum (Al2O3) obtained is simultaneously foamed obtained at 80 DEG C
Nano-silicon polymerize thermal insulation board.
Embodiment 4
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, difference lies in steps 3 with embodiment 3：It prepares and is modified
Melmac：At 90 DEG C, 1260g melamines, 1360g vinyl alcohols, 450g formaldehyde are dissolved into 10L water, are added
Sodium hydroxide adjusts pH to 8.5-9.0 and is reacted, and after reaction solution clarification, melamine methylol solution is made；By 940g
Phenol is modified to obtain blocking modification monomer by 150g formaldehyde, 300g sodium sulfites, and reaction temperature is 50 DEG C, and control ph is
7.5；Melamine methylol solution and blocking modification monomer are subjected to sealing end polycondensation reaction, 60 DEG C of reaction temperature, control ph
It is 8, obtains modified cyanurotriamide resin solution, modified cyanurotriamide resin is obtained after dry.
Embodiment 5
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, difference lies in steps 3 with embodiment 3：It prepares and is modified
Melmac：At 85 DEG C, 1260g melamines, 1110g vinyl alcohols, 600g formaldehyde are dissolved into 10L water, are added
Sodium hydroxide adjusts pH to 8.5-9.0 and is reacted, and after reaction solution clarification, 123.4g phosphite esters are added, are uniformly mixed system
Obtain melamine methylol solution；940g phenol is modified to obtain blocking modification monomer by 150g formaldehyde, 300g sodium sulfites,
Reaction temperature is 55 DEG C, control ph 7.5；It is anti-that melamine methylol solution and blocking modification monomer are subjected to sealing end polycondensation
It answers, 60 DEG C of reaction temperature, control ph 7.5, obtains modified cyanurotriamide resin solution, modified cyanurotriamide is obtained after dry
Resin.
Embodiment 6
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, difference lies in be additionally added in step 4 with embodiment 5
Alumina silicate fibre 400g and phosphate ester glycine betaine 60g.
Embodiment 7
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, difference lies in be additionally added in step 4 with embodiment 5
Alumina silicate fibre 200g and phosphate ester glycine betaine 40g.
Embodiment 8
A kind of nano-silicon polymerization thermal insulation board is present embodiments provided, difference lies in be additionally added in step 4 with embodiment 5
Alumina silicate fibre 300g and phosphate ester glycine betaine 80g.
Embodiment 9
The present embodiment is control experiment, provides control thermal insulation board, by 500g melmacs, 50g hexanedioic acids, 100g
Lauryl sodium sulfate, 315g alundum (Al2O3)s, the mixing of 185g aerosils and the obtained thermal insulation board that foams at 100 DEG C.
Wherein, melmac is commercial product, production method in embodiment 1, embodiment 2 and embodiment 9
It is reacted with formaldehyde for melamine and generates melamine methylol；Melamine is generated by melamine methylol condensation reaction again
Resin.
Flame retardant property detection is carried out to thermal insulation board made from 1-9 of the embodiment of the present invention, detection foundation is：GB8624-2012
《Construction material and product burns grading performance》, GB50222-95《Code for fire prevention design of interior decoration of buildings》, GB/T20284-
2006《The monomer combustion of construction material or product is tested》, GB/T8813-2008《Rigid foam compression performance measures》Deng.
Testing result is as shown in table 1, by testing result it is found that the nano-silicon polymerization thermal insulation board of the present invention has very high oxygen index (OI),
The preventive effect for avoiding flame from being formed can be played；And once flame is formed, in combustion process, fire growth rate and total heat are released
It is high-volume very low, it was demonstrated that the rate of fire travel is slow, and casualties is avoided convenient for control fire；While surplus of burning is more than
50%.The above Fire retardant test data is more than A2 grades of indexs of GB/T20284 standards.
Table 1：Embodiment 1-9 thermal insulation board flame retardant property testing results
Heat preservation and other performance detections, testing result such as 2 institute of table are carried out to thermal insulation board made from 1-9 of the embodiment of the present invention
Show, testing result shows that the thermal insulation board to the present invention maintains good mechanical property under the premise of with good flame-retardance energy
With lower thermal coefficient, heat insulation effect is good.
Table 2：Embodiment 1-9 thermal insulation boards are kept the temperature and other performance test results
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of nano-silicon polymerize thermal insulation board, which is characterized in that be made up of following steps：
Step 1：Hydrochloric acid and alundum (Al2O3) is soluble in water, and it is 50-70 DEG C to heat and keep temperature, is added under stirring
Ethylenediamine tetra-acetic acid simultaneously continues to stir, and fully obtains the solution of organic ion containing aluminium after reaction；
Step 2：Nano level silica dioxide granule is added in the solution of organic ion containing aluminium made from step 1, in 90-
Stirring is up to volatile dry at 110 DEG C, and is roasted at 550-650 DEG C, obtains the silica dioxide granule of cladding alundum (Al2O3)；
Step 3：It is 30-50 parts of melmac, 3-5 parts of curing agent, 6-9 parts of foaming agents and 40- by parts by weight
The silica dioxide granule of 70 parts of step 2 cladding alundum (Al2O3) obtained mixes and the obtained nano-silicon that foams at 50-100 DEG C is poly-
Close thermal insulation board.
2. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that be additionally added citric acid in the step 1
Sodium.
3. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that the alundum (Al2O3), ethylenediamine tetraacetic
The molar ratio of acetic acid, hydrochloric acid and silica dioxide granule is 1：2~3：2~3：1-2.
4. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that silica dioxide granule in the step 2
For silica aerogel particles, foaming agent is lauryl sodium sulfate in the step 3.
5. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that curing agent is phosphoric acid in the step 3
With the composite curing agent of hexanedioic acid, and the weight ratio of the phosphoric acid and hexanedioic acid be 1：0.5-2.
6. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that be additionally added alumina silicate in the step 3
Fiber, and the weight ratio of the melmac and the alumina silicate fibre is 1：0.5-1.
7. nano-silicon according to claim 1 polymerize thermal insulation board, which is characterized in that be additionally added phosphate ester in the step 3
Glycine betaine, and the weight ratio of the melmac and the phosphate ester glycine betaine is 1：0.1-0.2.
8. polymerizeing thermal insulation board according to any nano-silicons of claim 1-7, which is characterized in that the trimerization in the step 3
Melamine resin is made by following steps：
Step A：At 80-90 DEG C, vinyl alcohol, melamine, formaldehyde are dissolved into water, be added sodium hydroxide adjust pH to
8.5-9.0 is reacted, and after reaction solution clarification, melamine methylol solution is made；
Step B：Phenol is modified to obtain blocking modification monomer by formaldehyde, sodium sulfite, reaction temperature is 50-60 DEG C, control
PH value is 6.5-7.5；
Step C：The melamine methylol solution that step A is obtained is subjected to sealing end contracting with the obtained blocking modification monomers of step B
Poly- reaction, 60 DEG C of reaction temperature, control ph 7-8 obtain melmac solution, are dried to obtain melmac.
9. nano-silicon according to claim 8 polymerize thermal insulation board, which is characterized in that melamine, ethylene in the step A
Alcohol, formaldehyde molar ratio be 1：2-3：1.5-2.5.
10. nano-silicon according to claim 8 polymerize thermal insulation board, which is characterized in that methylol obtained in the step A
Phosphite ester is additionally added in melamine solution.
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| CN114044647A (en) * | 2021-10-30 | 2022-02-15 | 万华建筑科技有限公司 | Preparation process of A2-grade nano inorganic insulation board |
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Application publication date: 20180724 |