CN108003694B - Halogen-free intumescent flame retardant for water-based acrylic coating and preparation method thereof - Google Patents
Halogen-free intumescent flame retardant for water-based acrylic coating and preparation method thereof Download PDFInfo
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- CN108003694B CN108003694B CN201711443215.0A CN201711443215A CN108003694B CN 108003694 B CN108003694 B CN 108003694B CN 201711443215 A CN201711443215 A CN 201711443215A CN 108003694 B CN108003694 B CN 108003694B
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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
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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
- C09D133/00—Coating 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
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- 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
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- 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
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- 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
- C08K2003/327—Aluminium phosphate
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- Wood Science & Technology (AREA)
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Abstract
The invention discloses a composition of a halogen-free intumescent flame retardant for water-based acrylic paint and a preparation method thereof, wherein the flame retardant comprises the following components; 10-80% of ammonium polyphosphate, 10-80% of char forming agent, 10-30% of emulsifier, 1-40% of thickener, 1-45% of deflocculant and 1-20% of carbon layer reinforcing agent, wherein the thickener comprises; sodium bentonite, attapulgite, molecular sieve, silica gel, diatomite and fumed silica, wherein the deflocculant comprises; sodium citrate, sodium tartrate, phosphate and magnesium succinate, wherein the carbon layer enhancer comprises; dicyclic phosphate, aluminum dihydrogen phosphate and sodium aluminum acid phosphate. The method has the advantages of simplicity and strong practicability.
Description
Technical Field
The invention relates to the halogen-free related field for water-based acrylic facing paint prepared by triazine charring agent, in particular to a halogen-free intumescent flame retardant for water-based acrylic paint and a preparation method thereof.
Background
Along with the development of society, people are rich in life, and the floors of the commodity new-type houses are higher and higher. The large population gathering building facilities are more and more, and the requirement on the appearance is higher and higher. Wall decoration becomes a basic requirement of people for improving house beauty. The building safety is also paid unprecedented attention. The catastrophic consequences of a fire are exacerbated. Therefore, people can greatly solve the fire hazard of buildings by using the flame retardant material in the building materials. At present, most of coatings with major veneering surfaces are halogen flame-retardant composite flame-retardant coatings. It is known that halogen flame retardants have high flame retardant efficiency and stable properties and are favored by many paint manufacturers, but they produce dense black smoke when burned or subjected to high temperatures, and such dense smoke contains a large amount of heavy particles, and toxic substances such as halogen compound gas and dioxin pollute the environment and air greatly, have a great influence on the respiratory system of people in fire, and even kill many people in smoke. At present, part of manufacturers for producing halogen-free flame-retardant decorative coatings exist in the market, and the manufacturers also use the intumescent flame retardant as the flame-retardant material. However, most of the concrete has the characteristics of poor anti-settling effect, large influence on flame retardance due to aggregate addition, difficulty in long-term storage and the like, can be used only in a specific construction state, and is difficult to popularize in a large area.
Disclosure of Invention
The invention aims to solve the problems and designs a halogen-free intumescent flame retardant for water-based acrylic paint and a preparation method thereof.
The technical scheme of the invention for realizing the aim is that the flame retardant comprises the following components; 10-80% of ammonium polyphosphate, 10-80% of charring agent, 10-30% of emulsifier, 1-40% of thickener, 1-45% of deflocculant and 1-20% of carbon layer reinforcing agent.
The flame retardant comprises the following components in a preferential component ratio; 34% of ammonium polyphosphate, 28% of charring agent, 11% of emulsifier, 3% of bentonite, 3% of anhydrous sodium pyrophosphate, 3.5% of sodium citrate, 7% of dicyclic phosphate and 10.5% of aluminum dihydrogen phosphate.
The thickening agent comprises; one or more of sodium bentonite, attapulgite, molecular sieve, silica gel, diatomite and fumed silica, wherein the sodium bentonite and the diatomite are preferred.
The deflocculant comprises; one or more of sodium citrate, sodium tartrate, phosphate and magnesium succinate, preferably phosphate and sodium citrate.
The carbon layer enhancer comprises; one or more of dicyclic phosphate, aluminum dihydrogen phosphate, sodium aluminum acid phosphate and the like, wherein the dicyclic phosphate and the aluminum dihydrogen phosphate are preferred.
The emulsifier comprises; tween-80, span-60, polyethylene glycol-200, sodium polyacrylate, polyacrylamide, carboxymethyl cellulose, and sodium desugarized lignin sulfonate, preferably tween-80 and span-60.
The preparation method of the flame retardant comprises the following steps;
step one, adding 51g of cyanuric chloride and 300ml of acetone into a reactor provided with a stirrer, a thermometer and a dropping funnel, and fully stirring until the cyanuric chloride is dissolved for later use;
step two, adding 45g of p-phenylenediamine and 17.5g of sodium carbonate into 100ml of deionized water for later use;
thirdly, placing the reactor in a water bath, dropwise adding the prepared p-phenylenediamine and sodium carbonate solution into the cyanuric chloride acetone solution through a constant-pressure dropping funnel, continuously reacting for 7 hours, and then performing suction filtration, washing, drying and crushing to obtain the triazine charring agent for later use;
and step four, adding ammonium polyphosphate, a char forming agent, bentonite, anhydrous sodium pyrophosphate, sodium citrate, dicyclic phosphate and aluminum dihydrogen phosphate in a preferable formula into a high-speed cylinder according to a proper proportion, stirring at a high speed, discharging, adding the stirred material into a kneading machine, continuously kneading, slowly adding span-60 and tween-80 into the kneading machine according to the proportion in the formula, kneading, and discharging when the flame retardant material becomes a viscous dough after half an hour to obtain a flame retardant finished product.
The water bath temperature of the water bath kettle is controlled within 15 ℃.
The stirring time of the high-speed cylinder is 10 minutes.
The temperature of the deionized water was 80 ℃.
The components of the halogen-free intumescent flame retardant for the water-based acrylic coating and the preparation method thereof, which are manufactured by the technical scheme of the invention, have the advantages of high carbon forming speed, good heat insulation effect, less smoke generation and high flame retardant efficiency.
Detailed Description
The present invention will be described in detail below with reference to examples, as shown in examples 1 to 5.
Example 1
The first ratio target product is prepared according to the preferred ratio in claim 2 and the preparation method of step four, 32 g of the target product is added into 78 g of base paint containing 50 g of acrylic acid glue, 8 g of water and 20 g of rutile titanium dioxide. Mixing, and grinding in a three-roll grinder to obtain coating slurry. The coating is subjected to a combustion detection experiment according to the detection experiment method specified in GB 12441-2005. The detection results are as follows:
example 2
30% of ammonium polyphosphate, 25% of charring agent, 6% of sodium polyacrylate, 5% of polyethylene glycol, 3% of bentonite, 3% of sodium tartrate, 3.5% of phosphate and 17.5% of aluminum dihydrogen phosphate. Adding ammonium polyphosphate, a charring agent, bentonite, sodium tartrate, sodium polyacrylate, phosphate and aluminum dihydrogen phosphate in a formula according to a proper proportion into a high-speed cylinder, stirring at a high speed for 10 minutes, and discharging. And adding the stirred materials into a kneader, continuously kneading, and slowly adding polyethylene glycol into the kneader according to the proportion in the formula for kneading. After half an hour, the flame retardant material becomes adhesive, and when the flame retardant material is crystalline, the material can be discharged, and the finished flame retardant product is obtained. 32 g of the target product is taken and added into 78 basic coatings containing 55 g of acrylic acid glue, 8 g of water and 15 g of rutile titanium dioxide. Mixing, and grinding in a three-roll grinder to obtain coating slurry. The coating is subjected to a combustion detection experiment according to the detection experiment method specified in GB 12441-2005. The detection results are as follows:
embodiment 3
The first ratio target product is prepared according to the preferred proportion in the claim 2 and the preparation method of the step four, 32 g of the target product is added into 80 g of base paint containing 45g of acrylic acid glue, 10 g of water and 25 g of rutile titanium dioxide. Mixing, and grinding in a three-roll grinder to obtain coating slurry. The coating is subjected to a combustion detection experiment according to the detection experiment method specified in GB 12441-2005. The detection results are as follows:
example 4
Taking 35% of ammonium polyphosphate, 25% of charring agent, 806% of tween-tween, 5% of polyethylene glycol, 3% of bentonite, 3% of sodium tartrate, 3.5% of phosphate, 10% of cyclic phosphate and 5.5% of aluminum dihydrogen phosphate. Adding ammonium polyphosphate, a charring agent, bentonite, sodium tartrate, cyclic phosphate, phosphate and aluminum dihydrogen phosphate in a formula according to a proper proportion into a high-speed cylinder, stirring at a high speed for 10 minutes, and discharging. And adding the stirred materials into a kneader, continuously kneading, and slowly adding polyethylene glycol and tween-80 into the kneader according to the proportion in the formula for kneading. After half an hour, the flame retardant material becomes adhesive, and when the flame retardant material is in a conglomerate shape, the material can be discharged, and the finished flame retardant product is obtained. 32 g of the target product is taken and added into 78 basic coatings containing 55 g of acrylic acid glue, 8 g of water and 15 g of rutile titanium dioxide. Mixing, and grinding in a three-roll grinder to obtain coating slurry. The coating is subjected to a combustion detection experiment according to the detection experiment method specified in GB 12441-2005. The detection results are as follows:
example 5
Taking 35% of ammonium polyphosphate, 25% of charring agent, 806% of tween-tween, 5% of polyethylene glycol, 3% of silica gel, 3% of magnesium succinate, 3.5% of phosphate and 17.5% of cyclic phosphate. Adding ammonium polyphosphate, a carbonizing agent, silica gel, magnesium succinate, cyclic phosphate and phosphate in a formula according to a proper proportion into a high-speed cylinder, stirring at a high speed for 15 minutes, and discharging. And adding the stirred materials into a kneader, continuously kneading, and slowly adding polyethylene glycol and tween-80 into the kneader according to the proportion in the formula for kneading. After half an hour, the flame retardant material becomes adhesive, and when the flame retardant material is in a conglomerate shape, the material can be discharged, and the finished flame retardant product is obtained. 30 g of the target product is taken and added into 63 basic coatings containing 45g of acrylic acid glue, 8 g of water and 10 g of rutile titanium dioxide. Mixing, and grinding in a three-roll grinder to obtain coating slurry. The coating is subjected to a combustion detection experiment according to the detection experiment method specified in GB 12441-2005. The detection results are as follows:
the embodiment has the characteristics that the intumescent flame retardant contains a carbon source, an acid source and a gas source, and after the char formation layer reinforcing agent is added, the intumescent flame retardant can be free from sedimentation for a long time through special surface particle coupling treatment, and the aggregate has small influence on the flame retardance. And phosphine, formaldehyde, polycyclic aromatic hydrocarbon and other harmful gases are hardly generated. In addition, the flame-retardant material has the advantages of high carbon forming speed, good heat insulation effect, less smoke generation and high flame-retardant efficiency, and is an ideal flame-retardant material for replacing halogen-containing flame retardants.
In this embodiment, cyanuric chloride (51 g) and acetone (300 ml) were charged into a reactor equipped with a stirrer, a thermometer and a dropping funnel, and sufficiently stirred until it was dissolved, to be used. 45g of p-phenylenediamine and 17.5g of sodium carbonate are added to 100ml of deionized water at 80 ℃ for further use. The reactor is placed in a water bath kettle, and the water bath temperature is controlled within 15 ℃. And dropwise adding the prepared p-phenylenediamine and sodium carbonate solution into the cyanuric chloride acetone solution through a constant-pressure dropping funnel, continuously reacting for 7 hours, then performing suction filtration, washing, drying and crushing to obtain the triazine charring agent for later use. The preferred proportions of the use components set forth in the corresponding claim 2 are: 34% of ammonium polyphosphate, 28% of charring agent, 806% of tween-tween, 605% of span, 3% of bentonite, 3% of anhydrous sodium pyrophosphate, 3.5% of sodium citrate, 7% of dicyclic phosphate and 10.5% of aluminum dihydrogen phosphate. Ammonium polyphosphate, a charring agent, bentonite, anhydrous sodium pyrophosphate, sodium citrate, dicyclic phosphate and aluminum dihydrogen phosphate in a preferable formula are added into a high-speed cylinder according to a proper proportion, stirred at a high speed for 10 minutes and then discharged. And adding the stirred materials into a kneader, continuously kneading, and slowly adding span-60 and tween-80 into the kneader according to the proportion in the formula for kneading. And after half an hour, the flame retardant material becomes viscous and can be discharged when being agglomerated, and a finished flame retardant product is obtained.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (5)
1. A halogen-free intumescent flame retardant for water-based acrylic paint is characterized in that the flame retardant comprises the following components; 10-80% of ammonium polyphosphate, 10-80% of charring agent, 10-30% of emulsifier, 1-40% of thickener, 1-45% of deflocculant and 1-20% of carbon layer reinforcing agent;
the thickening agent comprises; sodium bentonite, attapulgite, molecular sieve, silica gel, diatomite and fumed silica;
the deflocculant comprises; sodium citrate, sodium tartrate, phosphate, magnesium succinate;
the carbon layer enhancer comprises; dicyclic phosphate, aluminum dihydrogen phosphate and sodium aluminum acid phosphate;
the emulsifier comprises; tween-80, span-60, polyethylene glycol-200, sodium polyacrylate, polyacrylamide, carboxymethyl cellulose and sodium desugarized lignin sulfonate;
the charring agent is triazine charring agent.
2. The halogen-free intumescent flame retardant for the water-based acrylic paint as claimed in claim 1, wherein the flame retardant comprises the following components in proportion; 34% of ammonium polyphosphate, 28% of charring agent, 11% of emulsifier, 3% of thickening agent, 6.5% of deflocculant and 17.5% of carbon layer reinforcing agent.
3. The halogen-free intumescent flame retardant for the water-based acrylic paint as claimed in claim 1, wherein the preparation method of the triazine char forming agent comprises the following steps;
step one, adding 51g of cyanuric chloride and 300ml of acetone into a reactor provided with a stirrer, a thermometer and a dropping funnel, and fully stirring until the cyanuric chloride is dissolved for later use;
step two, adding 45g of p-phenylenediamine and 17.5g of sodium carbonate into 100ml of deionized water for later use;
and step three, placing the reactor in a water bath kettle, dropwise adding the prepared p-phenylenediamine and sodium carbonate solution into the cyanuric chloride acetone solution through a constant-pressure dropping funnel, continuously reacting for 7 hours, and then performing suction filtration, washing, drying and crushing to obtain the triazine charring agent.
4. The halogen-free intumescent flame retardant for water-based acrylic paint as claimed in claim 3, wherein the temperature of the water bath is controlled within 15 ℃.
5. The halogen-free intumescent flame retardant for water-based acrylic paint as claimed in claim 3, wherein the temperature of the deionized water is 80 ℃.
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| CN108841230A (en) * | 2018-07-18 | 2018-11-20 | 合肥欧仕嘉机电设备有限公司 | A kind of New Building Materials fireproof coating and preparation method thereof |
| CN110229551A (en) * | 2019-07-12 | 2019-09-13 | 顺德职业技术学院 | A kind of aqueous UV anti-flaming dope and preparation method thereof |
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| CN106377863B (en) * | 2016-10-14 | 2019-12-06 | 浙江环亚消防新材料股份有限公司 | Water-based extinguishing agent and preparation method thereof |
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