CN109554056B - Functional self-flame-retardant coating - Google Patents
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Abstract
The invention relates to a functional self-flame-retardant coating, which consists of waterborne alkyd self-flame-retardant resin, pigment, filler, auxiliary agent and deionized water; the waterborne alkyd self-flame-retardant resin is prepared by reacting drying oil, organic acid anhydride, polybasic acid, polyalcohol, octadecanol, benzoic acid, melamine derivative, acrylic monomer, dimethylolpropionic acid and a neutralizing agent; the functional self-flame-retardant coating prepared by the invention does not precipitate during storage; the leveling property of the coating film is good in the film forming process, sagging is not generated, and a flame retardant is not required to be added; the coating film has good adhesive force, fullness, durability, chemical resistance, flame retardant property and low price; widely used for surface protection and decoration of furniture, musical instruments, metal, concrete and the like.
Description
Technical Field
The invention relates to an environment-friendly coating, in particular to a functional self-flame-retardant coating, and belongs to the technical field of water-based functional coatings.
Background
With the development of society and the improvement of living standard, the global environment is worsened day by day, and then people's environmental protection and health consciousness are strengthened gradually, and the comfort level and the security requirement to the living environment are higher and higher. In the living environment of people, the use of the coating is indispensable, and the performance of the coating plays a crucial role in the living environment, so that the requirement on the coating is higher and higher, and particularly, a functional coating with multiple performances is expected to be obtained.
The flame-retardant coating is a special coating which is used for the surface of a flammable base material, can reduce the flammability of the surface of a coated object, retards the rapid spread of fire and is used for improving the fire endurance of the coated object. Along with the rapid development of economy in recent years, the fire-fighting concept is gradually improved, the selection of fireproof building materials is particularly important besides the effective escape space planning of buildings, the existing fireproof coating can generate the phenomena of melting, dripping or cracking and peeling off and the like when being baked at high temperature, the effective fireproof capability cannot be provided, and the existing flame-retardant coating is often high in production cost and is not environment-friendly.
Chinese patent CN103484005A discloses a novel flame-retardant coating, which is composed of the following components in parts by weight: 60-70 parts of waterborne polyurethane, 3-8 parts of barite powder, 5-10 parts of magnesium hydroxide, 1-5 parts of vinyl acetate, 1-2 parts of potassium chloride, 5-10 parts of bentonite and 5-10 parts of styrene-acrylic emulsion. Chinese patent CN103589216A discloses a flame-retardant coating, which is composed of common coating and components, and is characterized in that: 2-8 parts of water-soluble ammonium polyphosphate, 3-6 parts of anhydrous magnesium chloride, 2-6 parts of melamine and 5-10 parts of a solidification accelerator are also added; the flame retardant coating of the invention can realize the flame retardant performance only by adding a flame retardant, and the added flame retardant is easy to pulverize and is not durable.
Chinese patent CN104087101A discloses an antifreezing flame-retardant coating, which comprises 900-1100 parts of acrylic acid-ethylene copolymer, 10-30 parts of carbon black, 90-110 parts of bismaleimide triazine resin, 90-110 parts of organic solvent, 900-1100 parts of magnesium hydroxide and 1-3 parts of antioxidant, so that the coating has the characteristics of freezing resistance, flame retardance and fire resistance; the invention contains more organic solvents and is harmful to the environment and human body.
Therefore, the development of an environment-friendly water-based paint with good flame retardant property without adding a flame retardant is a problem to be solved.
Disclosure of Invention
The invention aims to provide a functional self-flame-retardant coating and a preparation method thereof.
The functional self-flame-retardant coating does not need to be added with a flame retardant, and thoroughly solves the problems that the flame retardant is not uniformly dispersed in the coating and is easy to settle, and the influence of over-high or over-low pH value of part of the flame retardant on the performance of the coating.
In order to solve the problems, the invention adopts the flame-retardant resin with the self-flame-retardant function as a film-forming substance, and the melamine chemical bond with the flame-retardant function is bonded on the molecular structure of the water-based alkyd resin through a chemical reaction.
The invention relates to a functional self-flame-retardant coating, which comprises the following basic formula in parts by weight: 50.0-70.0 parts of water-based alkyd self-flame-retardant resin, 10-30.0 parts of pigment and filler, 3.0-10.0 parts of auxiliary agent and 10.0-20.0 parts of deionized water.
The pigment and filler is one or a combination of more of mica powder, talcum powder, barium sulfate, bentonite, kaolin, zinc phosphate, aluminum zinc phosphate, calcium carbonate, bentonite, titanium dioxide and water-based color paste.
The auxiliary agent at least comprises a wetting agent, a dispersing agent, a bactericide, a defoaming agent, a flatting agent, a thickening agent, a pH regulator, an antifreezing agent, a film-forming auxiliary agent and a combination of four or more of nano auxiliary agents.
The preparation process of the waterborne alkyd self-flame-retardant resin comprises the following steps:
a) sequentially adding dry vegetable oil, organic acid anhydride, polyol, dimethylolpropionic acid and polybasic acid into a four-port reactor provided with a thermometer, a condenser pipe, a water separator and a stirrer according to the weight part of the formula, starting heating, and introducing N into the reactor after the materials in the reactor are completely melted2Stirring and heating to 165-180 ℃, adding benzoic acid, octadecanol and a reflux solvent xylene, carrying out heat preservation reaction for 2-3 h, removing water brought out by the reflux reaction, and circulating the cooled reflux solvent in a reaction kettle;
b) when the separated water is little or basically no water, heating to 190 ℃, preserving heat, reacting for 1-1.5 h, heating to 200 ℃, preserving heat, reacting for 1-1.5 h, and heating to 210-220 ℃, preserving heat, and reacting for 2-4 h;
c) sampling, and stopping introducing N after the sample is qualified by inspection2Cooling, removing reflux solvent, cooling to below 50 deg.C, adding neutralizer, stirring and dispersing for 10-20 min, adding appropriate amount of deionized water, stirring and dispersing for 0.5h, and filtering to obtain a water-based alkyd resin prepolymer;
d) adding a prepared 5% ammonium persulfate aqueous solution, adding a 20% ammonium persulfate aqueous solution and part of acrylic acid monomer into the prepolymer, heating to 80 ℃, and stirring for 0.5 h; then dropwise adding the rest acrylic monomer, melamine derivative and ammonium persulfate aqueous solution, and controlling the dropwise adding time to be 3-4 h; and then heating to 85 ℃, carrying out heat preservation reaction for 1-1.5 h, adding water to reach the specified solid content, cooling to 40 ℃, and filtering to obtain the water-based alkyd self-flame-retardant resin.
The invention discloses a waterborne alkyd self-flame-retardant resin, which is based on the applied invention patent 'a waterborne alkyd self-flame-retardant resin and a preparation method thereof', and is described in detail.
The functional self-flame-retardant coating prepared by the invention does not precipitate during storage; the leveling property of the coating film is good in the film forming process, sagging is not generated, and a flame retardant is not required to be added; the coating film has good adhesive force, fullness, durability, chemical resistance, flame retardant property and low price; widely used for surface protection and decoration of furniture, musical instruments, metal, concrete and the like.
Detailed Description
The present invention is further described with reference to the following examples of a functional self-flame retardant coating. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention.
Example 1
A water-based alkyd self-flame-retardant resin A is prepared by the following steps:
a) sequentially adding 6.5 parts of linseed oil, 6.5 parts of phthalic anhydride, 3.5 parts of propylene glycol, 6.3 parts of pentaerythritol, 2.0 parts of dimethylolpropionic acid and m-xylene in parts by weight of the formula into a four-port reactor provided with a thermometer, a condenser pipe, a water separator and a stirrer2.6 portions of formic acid, heating, and introducing N after the materials in the kettle are completely melted2Stirring and heating to 165-180 ℃, adding 2.0 parts of benzoic acid, 1.8 parts of octadecanol and 10.0 parts of reflux solvent xylene, reacting for 2-3 hours under heat preservation, removing water brought out by the reflux reaction, and circulating the cooled reflux solvent in a reaction kettle;
b) when the separated water is little or basically no water, heating to 190 ℃, preserving heat, reacting for 1-1.5 h, heating to 200 ℃, preserving heat, reacting for 1-1.5 h, and heating to 210-220 ℃, preserving heat, and reacting for 2-4 h;
c) sampling, and stopping introducing N after the sample is qualified by inspection2Cooling, removing reflux solvent, cooling to below 50 ℃, adding 1.5 parts of triethylamine, stirring and dispersing for 10-20 min, adding a proper amount of deionized water, continuing stirring and dispersing for 0.5h, and filtering to obtain the waterborne alkyd resin prepolymer.
d) Adding 1.5 parts of a pre-prepared 5% ammonium persulfate aqueous solution, 0.3 part of ammonium persulfate aqueous solution, 1.2 parts of methyl methacrylate and 0.8 part of butyl methacrylate into the prepolymer, heating to 80 ℃, and stirring for 0.5 h; then dropwise adding the remaining 2.5 parts of methyl methacrylate, 1.5 parts of butyl methacrylate, 4.2 parts of melamine derivative and 1.2 parts of ammonium persulfate aqueous solution, and controlling the dropwise adding time to be 3-4 h; and then heating to 85 ℃, carrying out heat preservation reaction for 1-1.5 h, adding deionized water to reach the specified solid content, cooling to 40 ℃, and filtering to obtain the water-based alkyd self-flame-retardant resin A.
Example 2
A water-based alkyd self-flame-retardant resin B is prepared by the following steps:
a) sequentially adding 7.0 parts of tung oil, 5.5 parts of acetic anhydride, 3.0 parts of neopentyl glycol, 6.5 parts of trimethylolpropane, 2.0 parts of dimethylolpropionic acid and 3.0 parts of adipic acid according to the weight parts of the formula into a four-port reactor provided with a thermometer, a condenser pipe, a water separator and a stirrer, starting heating, and introducing N into the reactor after materials in the reactor are completely melted2Stirring and heating to 165-180 ℃, adding 1.5 parts of benzoic acid, 1.2 parts of octadecanol and 10.0 parts of reflux solvent xylene, reacting for 2-3 hours under heat preservation, removing reflux reaction and taking outThe cooled reflux solvent is circulated in the reaction kettle;
b) when the separated water is little or basically no water, heating to 190 ℃, preserving heat, reacting for 1-1.5 h, heating to 200 ℃, preserving heat, reacting for 1-1.5 h, and heating to 210-220 ℃, preserving heat, and reacting for 2-4 h;
c) sampling, and stopping introducing N after the sample is qualified by inspection2Cooling, removing reflux solvent, cooling to below 50 ℃, adding 1.5 parts of triethylamine, stirring and dispersing for 10-20 min, adding a proper amount of deionized water, continuing stirring and dispersing for 0.5h, and filtering to obtain the waterborne alkyd resin prepolymer.
d) Adding 1.5 parts of a pre-prepared 5% ammonium persulfate aqueous solution, 0.3 part of ammonium persulfate aqueous solution, 1.0 part of methyl acrylate and 0.6 part of lauryl acrylate into the prepolymer, heating to 80 ℃, and stirring for 0.5 h; then dropwise adding 2.0 parts of the remaining methyl acrylate, 2.2 parts of lauryl acrylate, 3.8 parts of melamine derivative and 1.2 parts of ammonium persulfate aqueous solution, and controlling the dropwise adding time to be 3-4 h; and then heating to 85 ℃, carrying out heat preservation reaction for 1-1.5 h, adding deionized water to reach the specified solid content, cooling to 40 ℃, and filtering to obtain the water-based alkyd self-flame-retardant resin B.
Example 3
Putting 16.2 parts of deionized water, 0.3 part of wetting agent, 0.8 part of dispersing agent and 0.2 part of defoaming agent into a stirring barrel according to the weight ratio of the formula, and uniformly stirring; adding 4.5 parts of mica powder, 8.0 parts of titanium dioxide, 6.0 parts of barium sulfate and 0.2 part of pH regulator under high-speed dispersion, then slowly adding 60.0 parts of waterborne alkyd self-flame-retardant resin A under low-speed stirring, stirring for 20-25 min, then adding 3.0 parts of alcohol ester, 0.2 part of thickener, 0.1 part of defoamer, 0.3 part of flatting agent and 0.2 part of bactericide, stirring for 10-15 min, filtering and packaging.
Example 4
Adding 11.2 parts of deionized water, 3.5 parts of ethylene glycol, 0.3 part of wetting agent, 0.5 part of dispersing agent and 0.1 part of defoaming agent into a stirring barrel according to the weight ratio of the formula, and uniformly stirring; 3.0 parts of bentonite, 9.0 parts of titanium dioxide, 3.0 parts of calcium carbonate and 0.2 part of pH regulator are added under high-speed dispersion, then 65.0 parts of waterborne alkyd self-flame-retardant resin B is slowly added under low-speed stirring, the mixture is stirred for 20-25 min, then 3.5 parts of alcohol ester, 0.1 part of thickener, 0.1 part of defoamer, 0.3 part of flatting agent and 0.2 part of bactericide are added, the mixture is stirred for 10-15 min, and the mixture is filtered and packaged.
The performance of the examples of the invention and the commercially available flame retardant coatings was tested according to the relevant standards, and the performance indexes are shown in table 1.
Table 1: performance indexes tested by the embodiment and the comparative example of the invention
| Detecting items | Example 3 | Example 4 | Comparative example |
| Hardness of pencil | H | H | HB |
| Adhesion (cross-hatch method)/grade | 0 | 0 | 1 |
| Bending test/mm | 1 | 1 | 1 |
| Impact resistance/50 cm | Normal paint film | Normal paint film | Discoloration of paint film |
| Sag resistance | Without sagging | Without sagging | Little sagging |
| Water resistance | 20d | 20d | 5d |
| Alkali resistance (50 g/L NaOH) | 10d | 10d | 3d |
| Acid resistance (50 g/L H2SO 4) | 10d | 10d | 3d |
| Resistance to artificial aging | 960h | 960h | 240h |
| Flame retardant properties | V-0 | V-0 | V-1 |
| Burning time | 21min 40s | 23min 20s | 17min 40s |
| Ratio of flame propagation | 17.5 | 16.7 | 21.4 |
| Carbonization volume/cm3 | 18.2 | 17.1 | 21.9 |
| Mass loss per g | 3.1 | 3 | 4.7 |
Although the present invention has been described in detail and with reference to exemplary embodiments thereof, it will be apparent to one skilled in the art that various changes, modifications and variations can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (3)
1. A functional self-flame-retardant coating is characterized in that: the functional self-flame-retardant coating comprises the following components in parts by weight: 50.0-70.0 parts of waterborne alkyd flame-retardant resin, 10.0-30.0 parts of pigment and filler, 3.0-10.0 parts of auxiliary agent and 10.0-20.0 parts of deionized water, wherein the preparation process of the waterborne alkyd flame-retardant resin comprises the following steps:
A. sequentially adding dry vegetable oil, organic acid anhydride, polyalcohol, dimethylolpropionic acid and polybasic acid into a four-port reactor provided with a thermometer, a condenser pipe, a water separator and a stirrer according to the weight part of the formula, starting heating, and introducing N after the materials in the reactor are completely melted2Stirring and heating to 165-180 ℃, and adding benzoic acidReacting octadecanol and a reflux solvent xylene for 2-3 h under the condition of heat preservation, removing moisture brought out by the reflux reaction, and circulating the cooled reflux solvent in a reaction kettle;
B. when the separated water is little or basically no water, heating to 190 ℃, preserving heat, reacting for 1-1.5 h, heating to 200 ℃, preserving heat, reacting for 1-1.5 h, and heating to 210-220 ℃, preserving heat, reacting for 2-4 h;
C. sampling, and stopping introducing N after the sample is qualified by inspection2Cooling, removing reflux solvent, cooling to below 50 deg.C, adding neutralizer, stirring and dispersing for 10-20 min, adding appropriate amount of deionized water, stirring and dispersing for 0.5h, and filtering to obtain a water-based alkyd resin prepolymer;
D. preparing a 5% ammonium persulfate aqueous solution in advance, adding a 20% ammonium persulfate aqueous solution and part of acrylic acid monomer into the prepolymer, heating to 80 ℃, and stirring for 0.5 h; then dropwise adding the rest acrylic monomer, melamine derivative and ammonium persulfate aqueous solution, and controlling the dropwise adding time to be 3-4 h; then heating to 85 ℃, carrying out heat preservation reaction for 1-1.5 h, adding water to reach the specified solid content, cooling to 40 ℃, and filtering to obtain the water-based alkyd self-flame-retardant resin;
wherein, the synthetic molecular structural formula of the melamine derivative is shown as follows:
2. the functional self-flame retardant coating of claim 1, wherein: the pigment and filler is one or a combination of more of mica powder, talcum powder, barium sulfate, bentonite, kaolin, zinc phosphate, aluminum zinc phosphate, calcium carbonate, titanium dioxide and water-based color paste.
3. The functional self-flame retardant coating of claim 1, wherein: the auxiliary agent at least comprises the combination of four or more than four of wetting agent, dispersant, bactericide, defoaming agent, flatting agent, thickening agent, pH regulator, antifreezing agent, film-forming auxiliary agent and nano auxiliary agent.
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| CN110591432A (en) * | 2019-09-01 | 2019-12-20 | 合众（佛山）化工有限公司 | Self-flame-retardant antibacterial multifunctional water-based paint and preparation method thereof |
| CN110577790A (en) * | 2019-09-01 | 2019-12-17 | 合众（佛山）化工有限公司 | Premixed flame-retardant antibacterial radiation-proof multifunctional water-based paint |
| CN110894395A (en) * | 2019-12-07 | 2020-03-20 | 合众（佛山）化工有限公司 | Oleyl polyether-2 phosphate modified alkyd resin water-based paint |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788304A (en) * | 2014-01-09 | 2014-05-14 | 抚顺市久丰合成树脂制造有限公司 | Amino resin-grafted modified water-based acrylic resin and preparation method thereof |
| WO2016100163A1 (en) * | 2014-12-15 | 2016-06-23 | Ppg Industries Ohio, Inc. | Coating compositions, coatings and methods for sound and vibration damping and water resistance |
| CN107936819A (en) * | 2017-12-15 | 2018-04-20 | 合众（佛山）化工有限公司 | A kind of inflaming-retarding antifouling antibiotic water paint |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788304A (en) * | 2014-01-09 | 2014-05-14 | 抚顺市久丰合成树脂制造有限公司 | Amino resin-grafted modified water-based acrylic resin and preparation method thereof |
| WO2016100163A1 (en) * | 2014-12-15 | 2016-06-23 | Ppg Industries Ohio, Inc. | Coating compositions, coatings and methods for sound and vibration damping and water resistance |
| CN107936819A (en) * | 2017-12-15 | 2018-04-20 | 合众（佛山）化工有限公司 | A kind of inflaming-retarding antifouling antibiotic water paint |
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Denomination of invention: A functional self flame retardant coating Effective date of registration: 20230607 Granted publication date: 20210608 Pledgee: Agricultural Bank of China Limited Shaoguan Wujiang Sub branch Pledgor: SHAOGUAN UNION CHEMICAL Co.,Ltd.|UNION (FOSHAN) CHEMICAL Co.,Ltd. Registration number: Y2023980043074 |
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