CN113444424A - Preparation method of flame-retardant furniture composite coating - Google Patents
Preparation method of flame-retardant furniture composite coating Download PDFInfo
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- CN113444424A CN113444424A CN202110836726.9A CN202110836726A CN113444424A CN 113444424 A CN113444424 A CN 113444424A CN 202110836726 A CN202110836726 A CN 202110836726A CN 113444424 A CN113444424 A CN 113444424A
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- C—CHEMISTRY; METALLURGY
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- 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
- C09D5/185—Intumescent paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a preparation method of a flame-retardant furniture composite coating, which comprises the following steps: (1) preparing modified ammonium polyphosphate; (2) preparing hydrotalcite; (3) preparing zinc borate intercalated hydrotalcite; (4) and (3) mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after the grinding at a high speed is finished, and grinding at a low speed in the grinder to obtain the flame-retardant furniture composite coating. The invention has the advantages that the carbon layer formed by the prepared zinc borate additive type flame-retardant composite coating has better expansibility, the expansion height of the carbon layer is increased after the hydrotalcite is modified, and the formed carbon layer can well prevent flame and heat from spreading, thereby better protecting the organism from being damaged by the flame, enhancing the combustion effect and reducing the decomposition rate of the coating.
Description
Technical Field
The invention relates to the technical field of preparation of furniture flame-retardant coatings, in particular to a preparation method of a flame-retardant furniture composite coating.
Background
With the increasing use amount of wood materials for interior decoration year by year, the coating is more and more popular as an important raw and auxiliary material for wood material decoration and furniture. The furniture coating can make the wooden furniture bamboo ware more beautiful and beautiful, improve the rough hand feeling of the furniture, not only play a role in protecting and maintaining the wooden furniture bamboo ware, but also make the whole family life more comfortable. Currently, furniture coatings are mainly classified into three types: PU paint, UV paint and water paint.
In addition, fire hazards inevitably exist due to the flammability and flammability of the wood materials and some coatings themselves. In recent years, such a fire has been on the rise due to the use of a large amount of decorative materials. The preparation of novel non-combustible and non-combustible decorative materials is highly valued by relevant departments of China. Therefore, flame retardant coatings are hot points of research, and at present, almost all the surfaces of plates used in furniture are coated with coatings, the coatings can form films under certain conditions to protect the plates, and the flame retardant is the most basic requirement while the plates have a decoration function.
The furniture coating directly added with the flame retardant in the prior art can achieve the flame retardant effect, but the flame retardant has poor flame retardant effect, large using amount and poor compatibility with organic components.
Disclosure of Invention
The invention aims to provide a preparation method of a flame-retardant furniture composite coating.
The technical purpose of the invention is realized by the following technical scheme:
the preparation method of the flame-retardant furniture composite coating is characterized by comprising the following steps of:
(1) dropwise adding a silane coupling agent into an organic solvent, stirring uniformly, dropwise adding an acetic acid solution to adjust the pH of the solution, continuously stirring after dropwise adding, then adding ammonium polyphosphate and a proper amount of organic solvent, stirring and reacting under a water bath condition, centrifugally separating a product after reaction is finished, washing after separation, and drying in vacuum to obtain modified ammonium polyphosphate;
(2) respectively adding magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into deionized water, stirring uniformly, dropwise adding a NaOH solution to adjust the pH of the solution, stirring for reaction under a water bath condition, filtering a product after the reaction is finished, and then washing and drying to obtain hydrotalcite;
(3) adding zinc borate and the hydrotalcite prepared in the step (2) into an ethanol water solution, stirring and reacting under a water bath condition, filtering a product after the reaction is finished, and then washing and drying to obtain zinc borate intercalated hydrotalcite;
(4) and (3) mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after the grinding at a high speed is finished, and grinding at a low speed in the grinder to obtain the flame-retardant furniture composite coating.
Preferably, the organic solvent in (1) is selected from one of absolute ethyl alcohol, acetone, isopropanol or methanol.
Preferably, the pH of the solution in the step (1) is adjusted to 3.5-5 by an acetic acid solution.
Preferably, the temperature of the water bath in the step (1) is 75-85 ℃, and the stirring time is 2-5 h.
Preferably, the molar mass ratio of the magnesium nitrate hexahydrate to the aluminum nitrate nonahydrate in the step (2) is 3-4: 1.
Preferably, the pH of the NaOH solution in the step (2) is adjusted to 11-11.5, the water bath temperature is 60-70 ℃, and the stirring time is 2-5 h.
Preferably, the mass ratio of the zinc borate to the hydrotalcite in the step (3) is 1:5-7, the mass fraction of the ethanol aqueous solution is 50%, the water bath temperature is 75-85 ℃, and the stirring time is 2-5 h.
Preferably, the composite coupling agent in (4) is a mixture of gamma-isocyanatopropyl trimethoxy silane and methyl vinyl diethoxy silane, and the mass ratio of the gamma-isocyanatopropyl trimethoxy silane to the methyl vinyl diethoxy silane is 1: 2.
Preferably, the particle size of the solution in the step (4) after low-speed grinding is within 20 μm.
Preferably, the components in the step (4) are as follows by weight: 8-13 parts of modified ammonium polyphosphate, 15-23 parts of zinc borate intercalated hydrotalcite, 2-5 parts of pentaerythritol, 3-8 parts of melamine, 2-5 parts of a dispersing agent, 15-21 parts of an epoxy resin emulsion, 4-5 parts of a composite coupling agent and 2-3 parts of a defoaming agent.
In conclusion, the invention has the following beneficial effects: the carbon layer formed by the zinc borate additive type flame-retardant composite coating prepared by the invention has better expansibility, the expansion height of the carbon layer is increased after the hydrotalcite is modified, and the formed carbon layer can well prevent flame and heat from spreading, so that the body can be better protected from being damaged by flame, the combustion effect is enhanced, and the decomposition rate of the coating is reduced.
Detailed Description
The following further describes the embodiments of the present invention, which are not to be construed as limiting the invention.
Example 1
The preparation method of the flame-retardant furniture composite coating is characterized by comprising the following steps of:
(1) dropwise adding a silane coupling agent into absolute ethyl alcohol, stirring uniformly, dropwise adding an acetic acid solution to adjust the pH of the solution to 3.5, continuously stirring after dropwise adding is finished, then adding ammonium polyphosphate and a proper amount of organic solvent, stirring the reaction water bath at 75 ℃ under the water bath condition for 3 hours, centrifugally separating the reacted product after the reaction is finished, washing after the reaction is finished, and drying in vacuum to obtain the modified ammonium polyphosphate.
(2) Respectively adding magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into deionized water, wherein the molar mass ratio of the magnesium nitrate hexahydrate to the aluminum nitrate nonahydrate is 3:1, stirring uniformly, dropwise adding NaOH solution to adjust the pH of the solution to 11, stirring for reaction under the condition of a water bath, wherein the temperature of the water bath is 60 ℃, the stirring time is 2 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the hydrotalcite.
(3) Adding zinc borate and the hydrotalcite prepared in the step (2) into an ethanol water solution, wherein the mass ratio of the zinc borate to the hydrotalcite is 1:5, the mass fraction of the ethanol water solution is 50%, stirring and reacting under a water bath condition, the water bath temperature is 80 ℃, the stirring time is 2 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the zinc borate intercalated hydrotalcite.
(4) Mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, and adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after finishing the grinding at a high speed, wherein the components are as follows in parts by weight: 8 parts of modified ammonium polyphosphate, 15 parts of zinc borate intercalated hydrotalcite, 2 parts of pentaerythritol, 3 parts of melamine, 2 parts of a dispersing agent, 16 parts of an epoxy resin emulsion, 5 parts of a composite coupling agent and 3 parts of a defoaming agent, wherein the composite coupling agent is a mixture of gamma-isocyanatopropyl trimethoxy silane and methyl vinyl diethoxy silane, the mass ratio of the gamma-isocyanatopropyl trimethoxy silane to the methyl vinyl diethoxy silane is 1:2, then low-speed grinding is carried out in a grinder, and the granularity of the solution is within 20 mu m after the low-speed grinding, so that the flame-retardant furniture composite coating is obtained.
Example 2
The preparation method of the flame-retardant furniture composite coating is characterized by comprising the following steps of:
(1) dropwise adding a silane coupling agent into absolute ethyl alcohol, stirring uniformly, dropwise adding an acetic acid solution to adjust the pH value of the solution to 4, continuing stirring after dropwise adding is finished, adding ammonium polyphosphate and a proper amount of organic solvent, stirring and reacting under the water bath condition, wherein the water bath temperature is 80 ℃, the stirring time is 5 hours, centrifugally separating a product after reaction is finished, washing after separation, and drying in vacuum to obtain the modified ammonium polyphosphate.
(2) Respectively adding magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into deionized water, wherein the molar mass ratio of the magnesium nitrate hexahydrate to the aluminum nitrate nonahydrate is 4:1, stirring uniformly, dropwise adding NaOH solution to adjust the pH of the solution to 11.5, stirring for reacting under the condition of a water bath, wherein the temperature of the water bath is 65 ℃, the stirring time is 4 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the hydrotalcite.
(3) Adding zinc borate and the hydrotalcite prepared in the step (2) into an ethanol water solution, wherein the mass ratio of the zinc borate to the hydrotalcite is 1:6, the mass fraction of the ethanol water solution is 50%, stirring and reacting under a water bath condition, the water bath temperature is 75 ℃, the stirring time is 4 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the zinc borate intercalated hydrotalcite.
(4) Mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, and adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after finishing the grinding at a high speed, wherein the components are as follows in parts by weight: 8 parts of modified ammonium polyphosphate, 18 parts of zinc borate intercalated hydrotalcite, 4 parts of pentaerythritol, 5 parts of melamine, 3 parts of a dispersing agent, 19 parts of an epoxy resin emulsion, 4 parts of a composite coupling agent and 2 parts of a defoaming agent, wherein the composite coupling agent is a mixture of gamma-isocyanatopropyl trimethoxy silane and methyl vinyl diethoxy silane, the mass ratio of the gamma-isocyanatopropyl trimethoxy silane to the methyl vinyl diethoxy silane is 1:2, then low-speed grinding is carried out in a grinder, and the granularity of the solution is within 20 mu m after the low-speed grinding, so that the flame-retardant furniture composite coating is obtained.
Example 3
The preparation method of the flame-retardant furniture composite coating is characterized by comprising the following steps of:
(1) dropwise adding a silane coupling agent into absolute ethyl alcohol, stirring uniformly, dropwise adding an acetic acid solution to adjust the pH value of the solution to 5, continuing stirring after dropwise adding is finished, adding ammonium polyphosphate and a proper amount of organic solvent, stirring and reacting under the water bath condition, wherein the water bath temperature is 85 ℃, the stirring time is 3 hours, centrifugally separating a product after reaction is finished, washing after separation, and drying in vacuum to obtain the modified ammonium polyphosphate.
(2) Respectively adding magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into deionized water, wherein the molar mass ratio of the magnesium nitrate hexahydrate to the aluminum nitrate nonahydrate is 3:1, stirring uniformly, dropwise adding NaOH solution to adjust the pH of the solution to 11.5, stirring for reaction under the condition of water bath, wherein the temperature of the water bath is 70 ℃, the stirring time is 5 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the hydrotalcite.
(3) Adding zinc borate and the hydrotalcite prepared in the step (2) into an ethanol water solution, wherein the mass ratio of the zinc borate to the hydrotalcite is 1:7, the mass fraction of the ethanol water solution is 50%, stirring and reacting under a water bath condition, the water bath temperature is 75 ℃, the stirring time is 5 hours, filtering a product after the reaction is finished, and then washing and drying to obtain the zinc borate intercalated hydrotalcite.
(4) Mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, and adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after finishing the grinding at a high speed, wherein the components are as follows in parts by weight: 12 parts of modified ammonium polyphosphate, 22 parts of zinc borate intercalated hydrotalcite, 5 parts of pentaerythritol, 7 parts of melamine, 5 parts of a dispersing agent, 20 parts of an epoxy resin emulsion, 5 parts of a composite coupling agent and 3 parts of a defoaming agent, wherein the composite coupling agent is a mixture of gamma-isocyanatopropyl trimethoxy silane and methyl vinyl diethoxy silane, the mass ratio of the gamma-isocyanatopropyl trimethoxy silane to the methyl vinyl diethoxy silane is 1:2, then low-speed grinding is carried out in a grinder, and the granularity of the solution is within 20 mu m after the low-speed grinding, so that the flame-retardant furniture composite coating is obtained.
According to the invention, the addition of zinc borate can promote carbon formation, and the product generated by the dehydration reaction of zinc borate at high temperature and the acid source in the expansion type fireproof system have a synergistic effect, so that the material can generate a compact carbon layer under high-temperature radiation, air can be prevented from entering the material, and the effects of heat insulation, flame retardation and smoke suppression are achieved.
The formed carbon layer has better expansibility, the expansion height of the carbon layer is increased after the hydrotalcite is modified, and the formed carbon layer can well prevent flame and heat from spreading, so that a machine body can be better protected from being damaged by flame, the combustion effect is enhanced, and the decomposition rate of the coating is reduced.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation method of the flame-retardant furniture composite coating is characterized by comprising the following steps of:
dropwise adding a silane coupling agent into an organic solvent, stirring uniformly, dropwise adding an acetic acid solution to adjust the pH of the solution, continuously stirring after dropwise adding, then adding ammonium polyphosphate and a proper amount of organic solvent, stirring and reacting under a water bath condition, centrifugally separating a product after reaction is finished, washing after separation, and drying in vacuum to obtain modified ammonium polyphosphate;
respectively adding magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into deionized water, stirring uniformly, dropwise adding a NaOH solution to adjust the pH of the solution, stirring for reaction under a water bath condition, filtering a product after the reaction is finished, and then washing and drying to obtain hydrotalcite;
adding zinc borate and the hydrotalcite prepared in the step (2) into an ethanol water solution, stirring and reacting under a water bath condition, filtering a product after the reaction is finished, and then washing and drying to obtain zinc borate intercalated hydrotalcite;
and (3) mixing the products prepared in the steps (1) and (3) with pentaerythritol, melamine, a dispersing agent and deionized water, grinding at a high speed in a grinder, adding an epoxy resin emulsion, a composite coupling agent and a defoaming agent after the grinding at a high speed is finished, and grinding at a low speed in the grinder to obtain the flame-retardant furniture composite coating.
2. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the organic solvent in (1) is selected from one of absolute ethyl alcohol, acetone, isopropanol or methanol.
3. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: and (3) regulating the pH value of the solution to 3.5-5 by using an acetic acid solution in the step (1).
4. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the temperature of the water bath in the step (1) is 75-85 ℃, and the stirring time is 2-5 h.
5. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the molar mass ratio of the magnesium nitrate hexahydrate to the aluminum nitrate nonahydrate in the step (2) is 3-4: 1.
6. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: and (3) regulating the pH of the solution to 11-11.5 by using the NaOH solution in the step (2), controlling the water bath temperature to 60-70 ℃, and stirring for 2-5 h.
7. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the mass ratio of the zinc borate to the hydrotalcite in the step (3) is 1:5-7, the mass fraction of the ethanol aqueous solution is 50%, the water bath temperature is 75-85 ℃, and the stirring time is 2-5 h.
8. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the composite coupling agent in the step (4) is a mixture of gamma-isocyanatopropyl trimethoxy silane and methyl vinyl diethoxy silane, and the mass ratio of the gamma-isocyanatopropyl trimethoxy silane to the methyl vinyl diethoxy silane is 1: 2.
9. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: and (4) after low-speed grinding, the particle size of the solution is within 20 mu m.
10. The preparation method of the flame-retardant furniture composite coating according to claim 1, characterized by comprising the following steps: the components in the step (4) are as follows by weight: 8-13 parts of modified ammonium polyphosphate, 15-23 parts of zinc borate intercalated hydrotalcite, 2-5 parts of pentaerythritol, 3-8 parts of melamine, 2-5 parts of a dispersing agent, 15-21 parts of an epoxy resin emulsion, 4-5 parts of a composite coupling agent and 2-3 parts of a defoaming agent.
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Citations (7)
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CN1468913A (en) * | 2003-03-14 | 2004-01-21 | 北京化工大学 | Borate radical intercalated hydrotalcite and its prepn process and application as fire retardant |
CN101712840A (en) * | 2008-10-07 | 2010-05-26 | 北京理工大学 | Ultrathin water-based epoxy resin expandable fireproof paint and preparation method thereof |
CN102850905A (en) * | 2012-09-11 | 2013-01-02 | 安徽理工大学 | Aqueous expansion-type steel structure fireproof paint and preparation method thereof |
CN103224746A (en) * | 2013-04-17 | 2013-07-31 | 长安大学 | Anti-staining epoxy fire-retardant coating and preparation method thereof |
CN105384970A (en) * | 2015-12-28 | 2016-03-09 | 北京泰克来尔科技有限公司 | Low-smoke antimony-free composite flame retardant |
CN108485351A (en) * | 2018-04-23 | 2018-09-04 | 武汉工程大学 | A kind of aqueous suppression cigarette expanding fire-proof paint and preparation method thereof based on modified hydrotalcite |
CN108641559A (en) * | 2018-04-23 | 2018-10-12 | 太原理工大学 | A kind of expanding fire retardant and its preparation method and application |
-
2021
- 2021-07-23 CN CN202110836726.9A patent/CN113444424A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1468913A (en) * | 2003-03-14 | 2004-01-21 | 北京化工大学 | Borate radical intercalated hydrotalcite and its prepn process and application as fire retardant |
CN101712840A (en) * | 2008-10-07 | 2010-05-26 | 北京理工大学 | Ultrathin water-based epoxy resin expandable fireproof paint and preparation method thereof |
CN102850905A (en) * | 2012-09-11 | 2013-01-02 | 安徽理工大学 | Aqueous expansion-type steel structure fireproof paint and preparation method thereof |
CN103224746A (en) * | 2013-04-17 | 2013-07-31 | 长安大学 | Anti-staining epoxy fire-retardant coating and preparation method thereof |
CN105384970A (en) * | 2015-12-28 | 2016-03-09 | 北京泰克来尔科技有限公司 | Low-smoke antimony-free composite flame retardant |
CN108485351A (en) * | 2018-04-23 | 2018-09-04 | 武汉工程大学 | A kind of aqueous suppression cigarette expanding fire-proof paint and preparation method thereof based on modified hydrotalcite |
CN108641559A (en) * | 2018-04-23 | 2018-10-12 | 太原理工大学 | A kind of expanding fire retardant and its preparation method and application |
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