CN112876742A - Flame-retardant material and preparation method and application thereof - Google Patents
Flame-retardant material and preparation method and application thereof Download PDFInfo
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant material, a preparation method and application thereof, wherein the flame-retardant material is prepared according to the following method: (1) preparation of Al (OH)3Alcohol solution of KH-570; (2) preparation of KH-570-Al (OH)3(ii) a (3) Adopts a direct hydration method to prepare OH-KH-570-Al (OH)3(ii) a (4) Mixing OH-KH-570-Al (OH)3And reacting with water-based acrylic resin to obtain the flame-retardant material. According to the invention, the acrylic resin is modified, so that the flame retardant property of the acrylic resin is improved, the service life of the acrylic resin is prolonged, and the flame retardant material with excellent flame retardant property and stability is prepared.
Description
Technical Field
The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant material and a preparation method and application thereof.
Background
The flame retardant is a functional additive for endowing the polymer material with flame retardancy, and can be divided into an additive flame retardant and a reactive flame retardant, wherein the additive flame retardant is filled into the polymer material by a physical and mechanical mixing method, and mostly influences the mechanical property and the like of the material, the reactive flame retardant is used as a polymerization reaction monomer and is added into a polymer molecular chain by a chemical covalent bond grafting method, and the reactive flame retardant has the advantages of less influence on the mechanical property and the service performance of the material and lasting flame retardancy.
Compared with the traditional solvent-based coating, the water-based coating has the advantages of low price, safe use, resource and energy conservation, environmental pollution and public nuisance reduction, and the like, thereby becoming the main development direction of the current coating. The water-based acrylic resin coating is pollution-free coating which is the fastest developed and most diversified in water-based coatings, the acrylic resin is thermoplastic or thermosetting resin prepared by taking styrene, acrylic ester and derivatives thereof as polymerization monomers, and the acrylic resin is widely applied to the fields of automobiles, electrical appliances, machinery, buildings and the like. However, the traditional acrylic resin has poor flame retardant property and is easy to burn, and practical application of the acrylic resin is limited, so that the acrylic resin with high thermal stability and excellent flame retardancy prepared by modifying the acrylic resin becomes a research hotspot.
At present, the acrylic resin flame-retardant mode mainly adopts an additive flame-retardant method, a reactive flame-retardant method, an impregnation method and the like, wherein the additive flame-retardant method is most widely applied, and the method adds a solid or liquid flame retardant in the process of processing acrylic resin so as to play a flame-retardant role, has the advantages of wide selection range, convenient use, small reaction influence on the generation of paint, economy and practicability and simple process; the disadvantages are poor stability and easy degradation in the environment, which in turn leads to the decrease of flame retardancy with the increase of time, and flame retardant materials with long-term stable flame retardant effect and excellent flame retardant property can not be obtained.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a flame retardant material, a preparation method and application thereof, the invention modifies acrylic resin and realizes a flame retardant Al (OH) through a KH-570 coupling agent3And the flame retardant material with excellent flame retardant property and stability is prepared by stable connection with the water-based acrylic resin.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a flame retardant material comprises the following steps:
(1) preparation of Al (OH)3An alcohol solution;
(2) dripping 0.05% by mass of KH-570 alcohol solution of silane coupling agent into the Al (OH) solution in the step (1)3In alcoholic solution, in N2Stirring at 60-90 deg.C for 12-18h under atmosphere, filtering, washing, and vacuum drying to obtain KH-570-Al (OH)3；
Wherein, the silane coupling agent KH-570 and Al (OH)3The mass ratio of the nano powder material is 1: 1.1-1.2;
(3) KH-570-Al (OH) from step (2)3Placing in deionized water, and preparing by direct hydration method to obtain OH-KH-570-Al (OH)3；
(4) Uniformly mixing the water-based acrylic resin and the surfactant, and adding the OH-KH-570-Al (OH) obtained in the step (3)3Carrying out esterification reaction for 3-5h at the temperature of 100-;
wherein, OH-KH-570-Al (OH)3The mass ratio of the acrylic resin to the water-based acrylic resin is 1-1.2: 1.
Preferably, Al (OH) in the step (1)3The preparation method of the alcoholic solution comprises the following steps: drying Al (OH)3Ultrasonically dispersing the nano powder in an alcohol solvent to obtain Al (OH)3An alcoholic solution.
Preferably, the alcohol solvent is absolute ethyl alcohol, absolute propyl alcohol or absolute n-amyl alcohol.
Preferably, the direct hydration in step (3) is performed by: reacting for 6-12h under the catalysis of molybdophosphoric acid at the temperature of 200-3；
Wherein, the molybdophosphoric acid is mixed with KH-570-Al (OH)3The mass ratio of (A) to (B) is 0.05-0.1: 1.
Preferably, said KH-570-Al (OH)3The ratio of the mass of the (B) to the volume of the deionized water is 1mg:10-20 mL.
Preferably, the surfactant of step (4) comprises Tween 80 and n-pentanol, wherein the volume of the n-pentanol is equal to OH-KH-570-Al (OH)3The mass ratio of (1-2 mL) of the mixture is 1mg of tween 80 and OH-KH-570-Al (OH)3The mass ratio of (A) to (B) is 0.04-0.06: 1.
The invention also provides the flame-retardant material prepared by the preparation method of the flame-retardant material.
The invention also protects the application of the flame-retardant material in preparing the flame-retardant building coating.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention firstly dries Al (OH)3Ultrasonically dispersing the nano powder in an alcohol solvent to obtain Al (OH)3An alcohol solution; hydroxyl exists on the surface of the silane coupling agent KH-570, and the alcoholic solution of the silane coupling agent KH-570 is mixed with Al (OH)3Are blended and reacted such that Al (OH)3The nano powder is stably coated in the silane coupling agent KH-570, and double bonds of the silane coupling agent KH-570 are exposed outside;
mixing KH-570-Al (OH)3The double bond at the end position of KH-570 reacts with water by adopting a direct hydration method in water through addition reaction, and the double bond at the end position is changed into hydroxyl after the addition reaction, thus obtaining OH-KH-570-Al (OH)3A material;
mixing OH-KH-570-Al (OH)3Reacting with aqueous acrylic resin through the carboxyl of the aqueous acrylic resin and OH-KH-570-Al (OH)3The terminal hydroxyl group is subjected to esterification reaction, so that the acrylic resin is stably grafted on OH-KH-570-Al (OH)3A surface.
2. The application adopts a solid flame retardant Al (OH)3The silane coupling agent KH-570 and the water-based acrylic resin, and the hydroxyl and double bonds carried on the KH-570 coupling agent realize the effect of adding Al (OH) into the solid flame retardant3The coating and the grafting of the water-based acrylic resin form a flame-retardant material with stable structure, and compared with the addition type flame-retardant method in the prior art, the flame-retardant material prepared by the method is prepared in the way that Al (OH)3Under the combined action of the flame retardant and the water-based acrylic resin, the flame retardant has excellent flame retardant property, maintains long-term stable structure in the environment, and prolongs the service life.
3. The flame retardant principle of the invention is as follows: the aluminum hydroxide is also called as Alumina Trihydrate (ATH), is a safe and sanitary inorganic flame retardant with the largest dosage, and the ATH is used within the range of 245-320 ℃, has lower effective use temperature range, and is suitable for acrylic resin flame-retardant materials with lower processing temperature. In addition, on one hand, the thermal decomposition process of the aluminum hydroxide is an endothermic reaction (the endothermic amount is about 2kJ/g), a large amount of heat generated by combustion can be taken away, the temperature of a combustion interface is reduced, and in addition, one of decomposition products of the aluminum hydroxide is water vapor, and the effects of reducing the temperature and diluting the concentration of oxygen and combustible gas can be achieved; on the other hand, the alumina of the aluminum hydroxide decomposition product is compact inorganic oxide powder, can cover the surface of the water-based acrylic resin coating to form a protective carbon layer with heat insulation and oxygen isolation effects, and has a smoke suppression effect, so that the aluminum hydroxide nano-particles are coated by the silane coupling agent KH-570, the flame retardant effect is improved, and the long-term structural stability of the aluminum hydroxide in the environment is realized.
KH-570 is a silane coupling agent with double bonds and hydroxyl at the terminal position, the hydroxyl is used for combining with and coating aluminum hydroxide, the double bonds can be added with water by a direct hydration method, so that the terminal position carries the hydroxyl, and the grafting with the flame-retardant material is convenient; after the acrylic emulsion is grafted, the flame retardant property of the material is improved through the flame retardant property of the polypropylene.
Drawings
FIG. 1 is a thermogravimetric analysis comparison graph of the flame retardant materials obtained in example 2 of the present invention and comparative example 1, wherein a is a thermogravimetric analysis graph of the flame retardant material obtained in example 2, and b is a thermogravimetric analysis graph of the flame retardant material obtained in comparative example 1;
FIG. 2 is a graph showing the thermal deformation properties of the flame retardant materials obtained in example 2 of the present invention and comparative example 1, wherein a is a graph showing the thermal deformation properties of the flame retardant material obtained in example 2, and b is a graph showing the thermal deformation properties of the flame retardant material obtained in comparative example 1;
FIG. 3 is a thermogravimetric analysis comparison graph of a flame retardant material prepared by comparative example 1 of the present invention at different aging times, wherein a is a thermogravimetric analysis graph of aging for 0h, b is a thermogravimetric analysis graph of aging for 6 months, and c is a thermogravimetric analysis graph of aging for 12 months;
FIG. 4 is a thermogravimetric analysis comparison graph of a flame retardant material prepared in example 2 of the present invention at different aging times, wherein a is a 0h thermogravimetric analysis graph, b is a 6 months thermogravimetric analysis graph, and c is a 12 months thermogravimetric analysis graph.
Detailed Description
The following description of the preferred embodiments and the accompanying drawings are incorporated in and constitute a part of this specification.
Example 1
A preparation method of a flame retardant material comprises the following steps:
(1) preparation of Al (OH)3An alcohol solution; drying Al (OH)3The nano powder is ultrasonically dispersed in absolute ethyl alcohol to obtain Al (OH)3An alcohol solution;
(2) dripping 0.05% by mass of KH-570 alcohol solution of silane coupling agent into the Al (OH) solution in the step (1)3In alcoholic solution, silane coupling agent KH-570 and Al (OH)3The mass ratio of the nano powder material is 1:1.1 in N2Stirring at 60 deg.C for 18h under atmosphere, filtering, washing, and vacuum drying to obtain KH-570-Al (OH)3；
(3) KH-570-Al (OH) from step (2)3Placing in deionized water, KH-570-Al (OH)3The mass to volume ratio of deionized water of1mg of 10mL, reacting the mixture for 6h at 230 ℃ under the catalytic action of molybdophosphoric acid and under the condition of 19MPa, wherein the molybdophosphoric acid and KH-570-Al (OH)3The mass ratio of the (B) is 0.05:1, and OH-KH-570-Al (OH) is prepared by adopting a direct hydration method3；
(4) Mixing the water-based acrylic resin and surfactant uniformly, wherein the surfactant comprises Tween 80 and n-amyl alcohol, and the volume of the n-amyl alcohol is equal to that of OH-KH-570-Al (OH)3The mass ratio of (1 mL) to (1 mg) of Tween 80 to OH-KH-570-Al (OH)3The mass ratio of (3) is 0.06:1, and OH-KH-570-Al (OH) is added3Performing esterification reaction, OH-KH-570-Al (OH)3The mass ratio of the flame retardant to the water-based acrylic resin is 1:1, and the flame retardant material is obtained after reaction for 5 hours at 100 ℃.
Example 2
A preparation method of a flame retardant material comprises the following steps:
(1) preparation of Al (OH)3An alcohol solution; drying Al (OH)3The nano powder is ultrasonically dispersed in absolute propanol to obtain Al (OH)3An alcohol solution;
(2) dripping 0.05% by mass of KH-570 alcohol solution of silane coupling agent into the Al (OH) solution in the step (1)3In alcoholic solution, silane coupling agent KH-570 and Al (OH)3The ratio of the nano powder material to the N is 1:1.152Stirring at 75 deg.C for 15h under atmosphere, filtering, washing, and vacuum drying to obtain KH-570-Al (OH)3；
(3) KH-570-Al (OH) from step (2)3Placing in deionized water, KH-570-Al (OH)3The mass ratio of the molybdenum phosphate to the deionized water is 1mg:15mL, the reaction is carried out for 10h under the catalysis of the molybdenum phosphate at 220 ℃ and under the condition of 19MPa, and the molybdenum phosphate and KH-570-Al (OH)3The mass ratio of the components is 0.075:1, and OH-KH-570-Al (OH) is prepared by a direct hydration method3；
(4) Mixing the water-based acrylic resin and surfactant uniformly, wherein the surfactant comprises Tween 80 and n-amyl alcohol, and the volume of the n-amyl alcohol is equal to OH-KH-570-Al (OH)3In a mass ratio of
1.5mL of 1mg, Tween 80 and OH-KH-570-Al (O)H)3The mass ratio of (3) is 0.05:1, and OH-KH-570-Al (OH) is added3Performing esterification reaction, OH-KH-570-Al (OH)3The mass ratio of the flame retardant to the water-based acrylic resin is 1.1:1, and the flame retardant material is obtained after reaction at 120 ℃ for 4 hours.
Example 3
A preparation method of a flame retardant material comprises the following steps:
(1) preparation of Al (OH)3An alcohol solution; drying Al (OH)3The nano powder is dispersed in anhydrous n-amyl alcohol by ultrasonic to obtain Al (OH)3An alcohol solution;
(2) dripping 0.05% by mass of KH-570 alcohol solution of silane coupling agent into the Al (OH) solution in the step (1)3In alcoholic solution, silane coupling agent KH-570 and Al (OH)3The ratio of the nano powder material to the N is 1:1.22Stirring at 90 deg.C for 12h under atmosphere, filtering, washing, and vacuum drying to obtain KH-570-Al (OH)3；
(3) KH-570-Al (OH) from step (2)3Placing in deionized water, KH-570-Al (OH)3The mass ratio of the molybdenum phosphate to the deionized water is 1mg:20mL, the reaction is carried out for 12h under the catalysis of the molybdenum phosphate at 200 ℃ and under the condition of 19MPa, and the molybdenum phosphate and KH-570-Al (OH)3The mass ratio of the components is 0.1:1, and OH-KH-570-Al (OH) is prepared by adopting a direct hydration method3；
(4) Mixing the water-based acrylic resin and surfactant uniformly, wherein the surfactant comprises Tween 80 and n-amyl alcohol, and the volume of the n-amyl alcohol is equal to OH-KH-570-Al (OH)3The mass ratio of (1 mg) to (2 mL) of Tween 80 to OH-KH-570-Al (OH)3The mass ratio of (3) is 0.04:1, and OH-KH-570-Al (OH) is added3Performing esterification reaction, OH-KH-570-Al (OH)3The mass ratio of the flame retardant to the water-based acrylic resin is 1.2:1, and the flame retardant material is obtained after reaction at 130 ℃ for 3 hours.
Comparative example 1
Adopting an additive flame-retardant method, adding Al (OH)3Mixing the nanometer powder with water-based acrylic resin uniformly to obtain a flame retardant material Al (OH)3Amount of nanopowder and aqueous acrylic resinIn an amount equivalent to that of example 2.
The flame retardant materials with excellent flame retardant property are prepared in the embodiments 1 to 3 of the invention, and the effects are parallel, the following comparative study on flame retardant property is carried out by taking the embodiment 2 as an example, and the specific study method and results are as follows:
(1) thermogravimetric analysis
The flame retardant materials prepared in example 2 and comparative example 1 were pulverized, respectively, and the weight loss by heat was measured by a thermogravimetric analyzer (usa. pe. co) in a nitrogen atmosphere, with a sample weight of 4mg, a temperature rise rate of 20 ℃/min, and a test temperature range of 50 to 600 ℃, and the results are shown in fig. 1.
(2) Test of thermal deformation Property
The cured flame retardant materials of example 2 and comparative example 1 were processed into specimens having a thickness of 3. + -. 0.5mm, a width of 60. + -. 0.5mm, and a length of 30. + -. 0.5mm, respectively, and placed in a J-1 type high polymer deformation-temperature measuring apparatus, and a deformation-temperature curve was measured at a temperature rise rate of 12 ℃/min within a test temperature range of 30 to 150 ℃ to determine the deformation temperature of the sample, and the expansion coefficient was calculated, the results are shown in FIG. 2.
As shown in FIG. 1, a is a thermal deformation performance diagram of the flame retardant material prepared in example 2, b is a thermal deformation performance diagram of the flame retardant material prepared in comparative example 1, and in comparison, both are thermally decomposed at the temperature of 150 ℃ and 200 ℃, and the decomposed raw materials are small molecular substances such as adsorbed water molecules in a sample; after 200 ℃, the flame retardant material prepared in comparative example 1 linearly decreases with the increase of temperature, which shows that the aluminum hydroxide and the water-based acrylic resin are combusted together and completely decomposed at 550 ℃; the flame retardant material prepared in example 2 has 2 weight loss regions after 200 ℃, the first weight loss region is about 300 ℃, aluminum hydroxide is partially decomposed, the second weight loss region is mainly decomposed by the water-based acrylic resin at the temperature of 400-.
The thermal deformation condition of the material can reflect the heat-resistant stability of the material to different degrees, and for better comparison and research on the flame retardant properties of the flame retardant materials in the example 2 and the comparative example 1, the thermal deformation research is carried out on the flame retardant materials, and the specific research results are as follows:
as shown in FIG. 2, FIG. 2 is a graph showing the thermal deformation properties of the flame retardant materials of example 2 of the present invention and comparative example 1, wherein a is a graph showing the thermal deformation properties of the flame retardant material of example 2, and b is a graph showing the thermal deformation properties of the flame retardant material of comparative example 1, and it can be seen from FIG. 2 that the thermal deformation temperature of example 2 of the present invention is between about 90 ℃ and about 100 ℃, and the thermal deformation temperature of comparative example 1 is between about 80 ℃ and about 90 ℃, which shows that the thermal deformation properties of example 2 of the present invention are better, and the heat resistance stability of the flame retardant material of example 2 is better.
The acrylic resin coating is degraded due to chemical and physical changes such as the breakage of a high molecular main chain and a side chain under the action of ultraviolet rays and heat, and radicals are generated, so that oxygen and moisture promote oxidation, and simultaneously, pigments and residual initiators catalyze photo-oxidation, so that the performance of a coating is reduced, and the environmental stability of the flame retardant materials of the embodiment 2 and the comparative example 1 is researched, wherein the specific research method comprises the following steps:
the same mass of the flame retardant materials prepared in example 2 and comparative example 1 were aged in a thermostat for 6 months and 12 months under the humid heat condition of 80 ℃ and 90% humidity, respectively, and the influence of the aging time on the thermal stability of the flame retardant material is shown in fig. 3 and fig. 4:
FIG. 3 is a thermogravimetric analysis comparison graph of a flame retardant material prepared by comparative example 1 of the present invention at different aging times, wherein a is a thermogravimetric analysis graph of aging for 0h, b is a thermogravimetric analysis graph of aging for 6 months, and c is a thermogravimetric analysis graph of aging for 12 months; as seen from FIG. 3, the thermal stability of the flame retardant material is greatly affected as the damp-heat time is prolonged, and when the aging time reaches 12 months, the complete decomposition temperature is reduced from 550 ℃ to 500 ℃, which indicates that the environment has a great influence on the flame retardant material of comparative example 1.
Fig. 4 is a thermogravimetric analysis comparison graph of the flame retardant material prepared in example 2 of the invention under different aging times, wherein a is a thermogravimetric analysis graph of aging for 0h, b is a thermogravimetric analysis graph of aging for 6 months, and c is a thermogravimetric analysis graph of aging for 12 months, and compared with the graph, as the comparison shows, there is a certain influence on the thermal stability of the material with the time being prolonged, but the thermal performance is slower, and the decomposition temperature is not changed, which shows that the change of the material itself is very small, then comparative example 1 has more excellent environmental aging resistance compared with example 2.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. The preparation method of the flame retardant material is characterized by comprising the following steps of:
(1) preparation of Al (OH)3An alcohol solution;
(2) dripping 0.05% by mass of KH-570 alcohol solution of silane coupling agent into the Al (OH) solution in the step (1)3In alcoholic solution, in N2Stirring at 60-90 deg.C for 12-18h under atmosphere, filtering, washing, and vacuum drying to obtain KH-570-Al (OH)3；
Wherein, the silane coupling agent KH-570 and Al (OH)3The mass ratio of the nano powder material is 1: 1.1-1.2;
(3) KH-570-Al (OH) from step (2)3Placing in deionized water, and preparing by direct hydration method to obtain OH-KH-570-Al (OH)3；
(4) Uniformly mixing the water-based acrylic resin and the surfactant, and adding the OH-KH-570-Al (OH) obtained in the step (3)3Carrying out esterification reaction for 3-5h at the temperature of 100-;
wherein, OH-KH-570-Al (OH)3The mass ratio of the acrylic resin to the water-based acrylic resin is 1-1.2: 1.
2. The method for preparing a fire retardant material according to claim 1, wherein Al (OH) in the step (1)3The preparation method of the alcoholic solution comprises the following steps: drying Al (OH)3Ultrasonically dispersing the nano powder in an alcohol solvent to obtain Al (OH)3An alcoholic solution.
3. The method for preparing a flame retardant material according to claim 2, wherein the alcohol solvent is absolute ethyl alcohol, absolute propyl alcohol or absolute n-amyl alcohol.
4. The method for preparing a fire retardant material according to claim 1, wherein the step (3) of direct hydration is performed by: reacting for 6-12h under the catalysis of molybdophosphoric acid at the temperature of 200-3；
Wherein, the molybdophosphoric acid is mixed with KH-570-Al (OH)3The mass ratio of (A) to (B) is 0.05-0.1: 1.
5. The method for preparing a fire retardant material according to claim 4, wherein said KH-570-Al (OH)3The ratio of the mass of the (B) to the volume of the deionized water is 1mg:10-20 mL.
6. The method of claim 1, wherein the surfactant of step (4) comprises Tween 80 and n-pentanol, wherein the volume of n-pentanol is equal to OH-KH-570-Al (OH)3The mass ratio of (1-2 mL) of the mixture is 1mg of tween 80 and OH-KH-570-Al (OH)3The mass ratio of (A) to (B) is 0.04-0.06: 1.
7. The flame retardant material prepared by the method for preparing the flame retardant material according to claim 1.
8. Use of the flame retardant material according to claim 7 for the preparation of flame retardant coatings for construction.
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| CN108841043A (en) * | 2018-07-13 | 2018-11-20 | 广州广化塑料管道有限公司 | Pvc material nanosizing coating modification composite flame-retardant agent and preparation method thereof |
| CN109135478A (en) * | 2018-08-17 | 2019-01-04 | 盛世瑶兰（深圳）科技有限公司 | A kind of environmentally friendly fire prevention composite coating |
| CN109810216A (en) * | 2018-12-25 | 2019-05-28 | 昆明理工大学 | A kind of flame-retardant aqueous acrylic resin and preparation method thereof |
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Application publication date: 20210601 |