CN112280405A - Water-based halogen-free intumescent flame-retardant coating adhesive, preparation method and flame-retardant fabric made of coating adhesive - Google Patents

Water-based halogen-free intumescent flame-retardant coating adhesive, preparation method and flame-retardant fabric made of coating adhesive Download PDF

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CN112280405A
CN112280405A CN202011241420.0A CN202011241420A CN112280405A CN 112280405 A CN112280405 A CN 112280405A CN 202011241420 A CN202011241420 A CN 202011241420A CN 112280405 A CN112280405 A CN 112280405A
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parts
flame
coating adhesive
water
retardant
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刘树骏
唐星三
崔剑光
钟世强
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SHANDONG OCEAN CHEMICAL INDUSTRY SCIENTIFIC RESEARCH INSTITUTE
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SHANDONG OCEAN CHEMICAL INDUSTRY SCIENTIFIC RESEARCH INSTITUTE
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D133/00Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0036Polyester fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0059Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06N3/042Acrylic polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a water-based halogen-free intumescent flame-retardant coating adhesive, which comprises the following raw materials in percentage by weight: 100 parts of water-based acrylic emulsion; 10-25 parts of a char-forming promoting agent; 10-25 parts of ammonium polyphosphate; 10-20 parts of a carbon forming agent; 5-10 parts of an inorganic flame-retardant synergist; 1-5 parts of an emulsifier; 1-5 parts of a thickening agent; 1-5 parts of a defoaming agent; 20-50 parts of softened water. The flame-retardant coating adhesive has good flame-retardant effect and excellent water resistance.

Description

Water-based halogen-free intumescent flame-retardant coating adhesive, preparation method and flame-retardant fabric made of coating adhesive
Technical Field
The invention relates to a water-based halogen-free intumescent flame-retardant coating adhesive, a preparation method and a flame-retardant fabric made of the coating adhesive.
Background
As a high polymer material, most of the fabric is easy to burn, and many domestic fire accidents are caused by textiles or indoor ornaments, so that the national field of fabric flame retardance is more and more emphasized. The terylene fabric widely applied to textiles and industrial products belongs to combustible fibers, is easy to burn through and curl during combustion, and can be melted and dripped to cause secondary ignition of other articles and secondary injury of personnel.
Flame-retardant finishing of polyester fabrics is the most common flame-retardant treatment process, flame-retardant coating glue is used in the flame-retardant finishing process of the fabrics, the flame-retardant performance of the flame-retardant finishing process directly determines the flame-retardant effect of the flame-retardant treated polyester fabrics, the most applications of the flame-retardant coating glue of bromine-antimony fabrics and the flame-retardant coating glue of halogen-containing fabrics are currently available in the market, for example, the Chinese patent CN200810104239.8 using the flame-retardant coating glue of halogen-containing fabrics can obtain good flame-retardant effect of the fabrics, but the flame-retardant coating glue contains halogen, toxic substances are easily generated during combustion, and the flame-retardant finishing process does not accord with the green and environment-friendly development direction of the flame retardant, so the application limit. The invention can prepare the water-based coating adhesive with excellent char forming performance, environmental protection and no toxicity by matching the halogen-free flame retardant, and has the characteristics of burning through resistance, self extinguishing after leaving fire, good water resistance and lower price after being applied to the secondary flame retardant finishing of polyester yarn release.
Disclosure of Invention
The invention aims to provide a water-based halogen-free intumescent flame-retardant coating adhesive, which comprises the following raw materials in percentage by weight:
100 parts of water-based acrylic emulsion; 10-25 parts of a char-forming promoting agent; 10-25 parts of ammonium polyphosphate; 10-20 parts of a carbon forming agent; 5-10 parts of an inorganic flame-retardant synergist; 1-5 parts of an emulsifier; 1-5 parts of a thickening agent; 1-5 parts of a defoaming agent; 20-50 parts of softened water.
The carbon forming agent is one or the combination of more than two of triazine Carbon Forming Agent (CFA), piperazine pyrophosphate, dipentaerythritol, urea-formaldehyde resin and phenolic resin.
The char-forming promoting agent is one or the combination of more than two of cyclic phosphate, cyclophosphamide, aluminum diethylphosphinate, pentaerythritol phosphate and bisphenol A bis (diphenyl phosphate) solid powder with the monomer content of more than 98%. Bisphenol a bis (diphenyl phosphate) is abbreviated as BDP, and bisphenol a bis (diphenyl phosphate) solid powder is abbreviated as BDP solid powder hereinafter.
The preparation method of the bisphenol A bis (diphenyl phosphate) solid powder comprises the following steps:
diphenyl chlorophosphate and bisphenol A are used as raw materials, triethylamine is used as a catalyst, and the material ratio (mol ratio) of diphenyl chlorophosphate, bisphenol A and triethylamine is 2.1: 1: 1.2. toluene is used as a reaction solvent, the dosage of the toluene is twice of the mass sum of diphenyl chlorophosphate and bisphenol A, and the reaction is carried out for 4 to 6 hours at the temperature of 100 to 120 ℃ to obtain bisphenol A bis (diphenyl phosphonate) reaction liquid; filtering triethylamine hydrochloride in the reaction liquid, removing the solvent in the reaction liquid, washing with water to remove residual triethylamine hydrochloride in the reaction liquid, standing for layering to obtain a product layer, and performing rotary evaporation to remove residual solvent and water in the product layer to obtain a crude product; and dissolving the crude product into absolute ethyl alcohol, crystallizing at a temperature of between 15 ℃ below zero and 18 ℃ below zero, performing suction filtration to obtain crystals, and drying the crystals to obtain bisphenol A bis (diphenyl phosphate) solid powder (BDP solid powder) with the monomer content of more than 98 percent.
The inorganic flame-retardant synergist is zinc borate, aluminum silicate or zirconium phosphate. Preferred are zinc borate and aluminum silicate.
The ammonium polyphosphate is modified by hydrophobization, and the polymerization degree of the ammonium polyphosphate is 1000-1400.
The emulsifier is desugarized sodium lignosulfonate.
The thickening agent is carboxymethyl cellulose.
The defoaming agent is a silicone defoaming agent, preferably RX-1210 defoaming agent, and the RX-1210 defoaming agent manufacturer is Dongguan Rong cooperative chemical materials Co.
The solid content of the water-based acrylic emulsion is 50 percent, and the pH value is 7.5-10.0.
The invention also aims to provide a preparation method of the water-based halogen-free intumescent flame-retardant coating adhesive, which comprises the following steps:
mixing a charring agent, a charring promoting agent, an inorganic synergist and ammonium polyphosphate, adding an emulsifier and part of softened water, and stirring at the rotating speed of 2000r/min-2500r/min for 10-12 minutes to prepare a flame retardant liquid; and mixing the flame retardant liquid with the water-based acrylate emulsion and the rest softened water, stirring for 10-15 minutes at the rotating speed of 2000r/min-2500r/min, then adding the thickening agent and the defoaming agent, and stirring for 10-15 minutes at the rotating speed of 2000r/min-2500r/min to obtain the water-based acrylic flame retardant coating adhesive.
The invention also aims to provide a flame-retardant fabric, which is prepared by using the aqueous halogen-free intumescent flame-retardant coating adhesive; coating the water-based halogen-free intumescent flame retardant coating adhesive on the back of the terylene sofa white cloth, drying and curing for 1-2 minutes at 150 ℃, then carrying out secondary frictioning coating on the back, drying and curing for 2-3 minutes at 170 ℃ to obtain the flame retardant fabric.
The invention uses the self-made solid bisphenol A bis (diphenyl phosphate), on one hand, the invention solves the problems that the liquid bisphenol A bis (diphenyl phosphate) is not easy to add when in use and is easy to solidify during storage and transportation, and simultaneously avoids the problem that the liquid bisphenol A bis (diphenyl phosphate) is easy to migrate and exude after being used. On the other hand, the flame retardant effect of the solid bisphenol A bis (diphenyl phosphate) on the polyester fabric is determined by comparing the flame retardant effect of the liquid bisphenol A bis (diphenyl phosphate) and the solid bisphenol A bis (diphenyl phosphate) on the fabric.
Compared with the halogen-containing aqueous flame-retardant coating adhesive, the aqueous acrylic flame-retardant coating adhesive has the advantages of environmental protection, no toxicity, excellent char forming performance, burn-through resistance and lower cost; compared with the common halogen-free water-based expansion flame-retardant coating adhesive, the coating adhesive has excellent carbon forming performance, is non-toxic and environment-friendly, has the performances of self-extinguishing when away from fire, small water bubble loss resistance and the like, and can pass the BS-5852 flame-retardant test. The flame retardant is dispersed in sections in the preparation stage, so that the flame retardant is dispersed more uniformly in the acrylic emulsion, and the water resistance of the flame-retardant coating on the fabric can be obviously improved by adopting the secondary frictioning and secondary curing processes for the flame-retardant fabric.
Drawings
FIG. 1 is a graph of the flame effect of the flame retardant fabric prepared in example 1;
FIG. 2 is a graph of the flame effect of the flame retardant fabric prepared in example 2;
FIG. 3 is a graph of the flame effect of the flame retardant fabric prepared in example 3;
FIG. 4 is a graph of the flame effect of the flame retardant fabric prepared in example 4;
fig. 5 is a graph of the flame effect of the flame retardant fabric prepared in example 5.
Detailed Description
The following examples are provided to illustrate the applicability of the present invention, and should not be construed as limiting the scope of the invention to the specific examples set forth below.
Example 1
1. Raw material composition of water-based acrylic acid flame-retardant coating adhesive
The raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion;
17 parts of a char-forming promoter (5 parts of BDP solid powder and 12 parts of cyclic phosphate);
10 parts of ammonium polyphosphate (MPP);
14 parts of a carbon forming agent (10 parts of a triazine carbon forming agent and 4 parts of urea-formaldehyde resin);
6 parts of inorganic flame-retardant synergist (aluminum silicate);
3 parts of an emulsifier (desugared sodium lignin sulfonate);
2 parts of a thickening agent (carboxymethyl cellulose);
3 parts of defoaming agent (RX-1210);
30 parts of softened water.
2. Preparation method of water-based acrylic acid flame-retardant coating adhesive
Taking the raw materials according to the proportion relation, adding a char forming agent, a char promoting agent, ammonium polyphosphate (MPP) and an inorganic flame retardant synergist into a disperser, then adding an emulsifier and 20 parts of softened water, opening the disperser, stirring at a high speed at a rotating speed of 2500r/min, and dispersing for 10 minutes to prepare a flame retardant liquid; and mixing the prepared flame retardant liquid with the water-based acrylate emulsion and the rest 10 parts of softened water, stirring at a high speed of 2500r/min again, dispersing for 10 minutes, adding a thickening agent and a defoaming agent, and continuously stirring at a high speed of 2500r/min, and dispersing for 15 minutes to obtain the water-based acrylic flame retardant coating adhesive.
3. Preparation of flame-retardant fabric
The back of the dacron sofa white cloth is subjected to glue scraping coating (the gram weight of the dacron fabric is 200g, namely the weight of each square meter of the cloth is 200g) by using the prepared water-based acrylic acid flame-retardant coating adhesive, the dacron sofa white cloth is dried and cured for 1 minute at the temperature of 150 ℃, the back of the dacron sofa white cloth is taken out and subjected to secondary glue scraping coating, the dacron sofa white cloth is dried and cured for 3 minutes at the temperature of 170 ℃, the net weight of the cured flame-retardant fabric is increased to 99.2g (the coating adhesive with the mass of 99.2g is coated on each square meter of.
Example 2
1. Raw material composition of water-based acrylic acid flame-retardant coating adhesive
The raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion;
15 parts of a char-forming promoter (12 parts of BDP solid powder and 3 parts of aluminum diethylphosphinate);
20 parts of ammonium polyphosphate (MPP);
15 parts of a carbon forming agent (10 parts of a triazine carbon forming agent and 5 parts of phenolic resin);
8 parts of inorganic flame-retardant synergist (zinc borate);
5 parts of an emulsifier (desugared sodium lignin sulfonate);
1 part of thickening agent (carboxymethyl cellulose);
2 parts of defoaming agent (RX-1210);
50 parts of softened water.
2. Preparation method of water-based acrylic acid flame-retardant coating adhesive
Referring to the preparation method of example 1, the preparation procedure was substantially the same as that of example 1 except that the amount of the softened water added was changed to 30 parts for the first time and 20 parts for the second time.
3. Preparation of flame-retardant fabric
The preparation steps are the same as those of the flame-retardant fabric prepared in example 1, and the net weight of the flame-retardant fabric prepared in this example after curing is 100.1g (namely, 100.1g of coating adhesive is coated on each square meter of fabric).
Example 3
1. Raw material composition of water-based acrylic acid flame-retardant coating adhesive
The raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion;
20 parts of a charring accelerator (12 parts of BDP solid powder and 8 parts of cyclophosphamide);
15 parts of ammonium polyphosphate (MPP);
17 parts of a carbon forming agent (12 parts of piperazine pyrophosphate and 5 parts of phenolic resin);
10 parts of inorganic flame-retardant synergist (zirconium phosphate);
3 parts of an emulsifier (desugared sodium lignin sulfonate);
2 parts of a thickening agent (carboxymethyl cellulose);
3 parts of defoaming agent (RX-1210);
40 parts of softened water.
2. Preparation method of water-based acrylic acid flame-retardant coating adhesive
Referring to the preparation method of example 1, the preparation procedure was substantially the same as that of example 1 except that the amount of the softened water added was changed to 20 parts for the first time and 20 parts for the second time.
3. Preparation of flame-retardant fabric
The preparation steps are the same as those of the flame-retardant fabric prepared in example 1, and the net weight of the flame-retardant fabric prepared in this example after curing is 98.9g (namely, 98.9g of coating adhesive is coated on each square meter of fabric).
Example 4
1. Raw material composition of water-based acrylic acid flame-retardant coating adhesive
The raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion;
15 parts of a char-forming promoter (8 parts of cyclic phosphate ester, 5 parts of BDP solid powder and 2 parts of aluminum diethylphosphinate);
10 parts of ammonium polyphosphate (MPP);
10 parts of a carbon forming agent (phenolic resin);
5 parts of inorganic flame-retardant synergist (aluminum silicate);
1 part of emulsifier (desugared sodium lignin sulfonate);
4 parts of a thickening agent (carboxymethyl cellulose);
2 parts of defoaming agent (RX-1210);
30 parts of softened water.
2. Preparation method of water-based acrylic acid flame-retardant coating adhesive
Referring to the preparation method of example 1, the preparation procedure was the same as in example 1.
3. Preparation of flame-retardant fabric
The preparation steps are the same as those of the flame-retardant fabric prepared in example 1, and the net weight of the flame-retardant fabric prepared in this example after curing is 96.5g (namely coating glue with the mass of 96.5g per square meter of the fabric).
Example 5
1. Raw material composition of water-based acrylic acid flame-retardant coating adhesive
The raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion;
15 parts of a char-forming promoting agent (10 parts of BDP solid powder and 5 parts of pentaerythritol phosphate);
15 parts of ammonium polyphosphate (MPP);
13 parts of a char forming agent (5 parts of dipentaerythritol and 8 parts of phenolic resin);
5 parts of inorganic flame-retardant synergist (aluminum silicate);
3 parts of an emulsifier (desugared sodium lignin sulfonate);
2 parts of a thickening agent (carboxymethyl cellulose);
2 parts of defoaming agent (RX-1210);
40 parts of softened water.
2. Preparation method of water-based acrylic acid flame-retardant coating adhesive
Referring to the preparation method of example 1, the preparation procedure was substantially the same as that of example 1 except that the amount of the softened water added was changed to 20 parts for the first time and 20 parts for the second time.
3. Preparation of flame-retardant fabric
The preparation steps are the same as those of the flame-retardant fabric prepared in example 1, and the net weight of the flame-retardant fabric prepared in this example after curing is 99.7g (namely, 99.7g of coating adhesive is coated on each square meter of fabric).
The flame retardant performance test refers to the BS5852 flame retardant test standard, the test samples are respectively covered on specified polyurethane sponge and placed under a specified combustor to be ignited, the butane flame height is 35mm, after the flame is stabilized for 30s, the test samples are continuously combusted by flame for 20s, and the flame retardant performance of the test samples is tested. The results of flame resistance measurements for the flame resistant fabrics prepared in examples 1-5 are shown in Table 1 and FIGS. 1-5.
The water resistance test takes 1 square meter of the flame-retardant fabric sample as m1The net weight gain (mass of coating gum per square meter of cloth) of the test specimen is m3Then soaked in water for 1 hour, taken out, dried and weighed as m2Mass loss of m1-m2By m1-m2And m3The percentage of the ratio represents the loss ratio, and the test results are shown in Table 2.
TABLE 1
Examples Net weight gain of fabric Carbon layer state of fabric Self-extinguishing time after leaving fire Ignition condition of sponge Conclusion
1 99.2g/m2 Compact with small broken holes 0s Not ignited By passing
2 100.1g/m2 Compact and non-damaged 2s Not ignited By passing
3 98.9g/m2 Compact with small broken holes 0s Not ignited By passing
4 96.5g/m2 Compact with small broken holes 3s Not ignited By passing
5 99.7g/m2 Compact and non-damaged 5s Not ignited By passing
TABLE 2
Examples Net weight gain of fabric Temperature of soaking water Time of soaking in water Loss of mass Loss ratio
1 99.2g/m2 40℃ 1h 10.7g/m2 10.8%
2 100.1g/m2 40℃ 1h 12g/m2 11.9%
3 98.9g/m2 40℃ 1h 9.1g/m2 9.2%
4 96.5g/m2 40℃ 1h 10.1g/m2 10.5%
5 99.7g/m2 40℃ 1h 9.8g/m2 9.83%
The test results show that the water-based acrylic flame-retardant coating adhesive has good flame-retardant effect and excellent water resistance.

Claims (12)

1. The water-based halogen-free intumescent flame-retardant coating adhesive is characterized in that: the raw materials comprise the following components in percentage by weight:
100 parts of water-based acrylic emulsion; 10-25 parts of a char-forming promoting agent; 10-25 parts of ammonium polyphosphate; 10-20 parts of a carbon forming agent; 5-10 parts of an inorganic flame-retardant synergist; 1-5 parts of an emulsifier; 1-5 parts of a thickening agent; 1-5 parts of a defoaming agent; 20-50 parts of softened water.
2. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the carbon forming agent is one or the combination of more than two of triazine carbon forming agent, piperazine pyrophosphate, dipentaerythritol, urea-formaldehyde resin and phenolic resin.
3. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the char-forming promoting agent is one or the combination of more than two of cyclic phosphate, cyclophosphamide, aluminum diethylphosphinate, pentaerythritol phosphate and bisphenol A bis (diphenyl phosphate) solid powder with the monomer content of more than 98%.
4. The aqueous halogen-free intumescent coating adhesive of claim 3, characterized in that: the preparation method of the bisphenol A bis (diphenyl phosphate) solid powder comprises the following steps:
diphenyl chlorophosphate and bisphenol A are used as raw materials, triethylamine is used as a catalyst, and the molar ratio of the diphenyl chlorophosphate to the bisphenol A to the triethylamine is 2.1: 1: 1.2; toluene is used as a reaction solvent, the dosage of the toluene is twice of the mass sum of diphenyl chlorophosphate and bisphenol A, and the reaction is carried out for 4 to 6 hours at the temperature of 100 to 120 ℃ to obtain bisphenol A bis (diphenyl phosphate) reaction liquid; filtering triethylamine hydrochloride in the reaction liquid, removing the solvent in the reaction liquid, washing with water to remove residual triethylamine hydrochloride in the reaction liquid, standing for layering to obtain a product layer, and performing rotary evaporation to remove residual solvent and water in the product layer to obtain a crude product; dissolving the crude product into absolute ethyl alcohol, crystallizing at-15 to-18 ℃, filtering to obtain crystals, and drying the crystals to obtain bisphenol A bis (diphenyl phosphate) solid powder with the monomer content of more than 98 percent.
5. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the inorganic flame-retardant synergist is zinc borate, aluminum silicate or zirconium phosphate.
6. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the ammonium polyphosphate is modified by hydrophobization, and the polymerization degree of the ammonium polyphosphate is 1000-1200.
7. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the emulsifier is desugarized sodium lignosulfonate.
8. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the thickening agent is carboxymethyl cellulose.
9. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the defoaming agent is an organic silicon defoaming agent.
10. The aqueous halogen-free intumescent coating adhesive of claim 1, characterized in that: the solid content of the water-based acrylic emulsion is 50 percent, and the pH value is 7.5-10.0.
11. A method for preparing the aqueous halogen-free intumescent flame retardant coating glue of any one of claims 1 to 10, characterized in that: the method comprises the following steps:
mixing a charring agent, a charring promoting agent, an inorganic synergist and ammonium polyphosphate, adding an emulsifier and part of softened water, and stirring at the rotating speed of 2000r/min-2500r/min for 10-12 minutes to prepare a flame retardant liquid; and mixing the flame retardant liquid with the water-based acrylate emulsion and the rest softened water, stirring for 10-15 minutes at the rotating speed of 2000r/min-2500r/min, then adding the thickening agent and the defoaming agent, and stirring for 10-15 minutes at the rotating speed of 2000r/min-2500r/min to obtain the water-based acrylic flame retardant coating adhesive.
12. A flame resistant fabric characterized by: the preparation method comprises the steps of preparing the aqueous halogen-free expansion flame-retardant coating adhesive according to any one of claims 1 to 11; coating the water-based halogen-free intumescent flame retardant coating adhesive on the back of the terylene sofa white cloth, drying and curing for 1-2 minutes at 150 ℃, then carrying out secondary frictioning coating on the back, drying and curing for 2-3 minutes at 170 ℃ to obtain the flame retardant fabric.
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CN113943512A (en) * 2021-11-12 2022-01-18 中车南京浦镇车辆有限公司 Efficient flame-retardant sprayable silicone-acrylic emulsion and preparation method thereof
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