CN111334152B - Water-based flame-retardant gloss oil and preparation method thereof - Google Patents

Water-based flame-retardant gloss oil and preparation method thereof Download PDF

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CN111334152B
CN111334152B CN202010302879.0A CN202010302879A CN111334152B CN 111334152 B CN111334152 B CN 111334152B CN 202010302879 A CN202010302879 A CN 202010302879A CN 111334152 B CN111334152 B CN 111334152B
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retardant
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aqueous solution
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CN111334152A (en
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许华君
许少宏
罗英武
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Hangzhou Hiwetech Chemical Technology Co ltd
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    • 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
    • C09D151/00Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
    • C09D151/003Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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    • 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
    • C09D127/00Coating 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 a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02Coating 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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/04Coating 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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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    • 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
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
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Abstract

The invention provides water-based flame-retardant gloss oil and a preparation method thereof, wherein the water-based flame-retardant gloss oil is prepared from the following raw materials in parts by weight: 10-15 parts of flame retardant, 3-5 parts of dispersant, 10-20 parts of silicon dioxide dispersion liquid, 10-20 parts of vinyl chloride-ethylene copolymer resin, 10-20 parts of modified high-silicon resin, 1-3 parts of wetting agent, 0.8-1.2 parts of thickening agent, 0.1-0.6 part of defoaming agent and 24.1-41.2 parts of deionized water; the invention adopts a water-based system, is green and environment-friendly, and has a storage period of more than one year; the glossiness of the product after film forming is high, and the display effect of the printed patterns of the film is not influenced; after the gloss oil is dried into a film, the water resistance is good, the adhesive force is strong, and the alcohol rub resistance is excellent; after the product is coated on plastic films such as PVC furniture films/floor films, PET plastic films, PP decorative films and the like, the plastic films can realize the flame-retardant function of self-extinguishing after leaving fire.

Description

Water-based flame-retardant gloss oil and preparation method thereof
Technical Field
The invention relates to water-based gloss oil and a preparation method thereof, in particular to water-based flame-retardant gloss oil applied to a plastic film and a preparation method thereof.
Background
With the improvement of living standard of people, the requirement of interior decoration is higher and higher, and besides the requirement of decoration, the requirements of environmental protection, safety and the like are considered. Plastic film type laminated boards, such as PVC furniture film boards, PVC floor film boards, etc., are increasingly receiving attention from modern interior decoration industry due to their characteristics of easy processing, convenient molding, etc. As interior materials, environmental protection and safety have been the focus of social attention.
Traditional plastic film printing ink and gloss oil are solvent-based systems, and the solvent-based ink and gloss oil contain a large amount (generally accounting for more than 60% of the ink composition) of volatile organic solvents (VOC), such as toluene, xylene, ethyl acetate, butanone and the like. When printing ink and gloss oil are printed and dried, a large amount of organic solvent is released, and the printing ink is flammable and explosive, and causes great damage and pollution to printing workers and the environment. Moreover, after the furniture board attached with the oily printing film enters the home decoration market, VOC can be released slowly, which undoubtedly causes long-term damage to the home health of consumers. The water-based ink and the gloss oil are transferred to a printing stock by taking water as a main dispersion medium, and then dried to form a film along with the volatilization of water into the environment or the permeation into the printing stock, so that the water-based ink and the gloss oil have the characteristics of no toxicity, no harm, environmental protection, safety and the like. Therefore, water-based inks and gloss oils are becoming more and more popular with government and industry, and are becoming a trend of development of the industry.
On the other hand, the cost is high because a large amount of flame-retardant filler is adopted in part of plastic films, especially PVC base films. In practical application, if the surface of the film has flame retardant property, the dosage of the flame retardant additive of the base material can be reduced, thereby greatly reducing the product cost. Moreover, the flame-retardant protective layer is expanded from the inner layer to the surface layer, so that the flame-retardant protective layer is safer and more reliable.
Disclosure of Invention
The invention aims to provide water-based flame-retardant gloss oil applicable to plastic films and a preparation method thereof.
The technical scheme of the invention is as follows:
the water-based flame-retardant gloss oil is prepared from the following raw materials in parts by weight:
10-15 parts of flame retardant, 3-5 parts of dispersant, 10-20 parts of silicon dioxide dispersion liquid, 10-20 parts of vinyl chloride-ethylene copolymer resin, 10-20 parts of modified high-silicon resin, 1-3 parts of wetting agent, 0.8-1.2 parts of thickening agent, 0.1-0.6 part of defoaming agent and 24.1-41.2 parts of deionized water.
Further:
the flame retardant is preferably an inorganic flame retardant, particularly preferably magnesium hydroxide.
The dispersant may be a modified polyether dispersant (e.g., a polyether dispersant)
Figure BDA0002454671430000011
653, EVONIK corporation;
Figure BDA0002454671430000012
655,EVONIK Corp.) or polyacrylate-type dispersants (e.g., sodium polyacrylate, and sodium polyacrylate
Figure BDA0002454671430000013
715W, EVONIK corporation) in any ratio, and particularly preferably a polyacrylate dispersant
Figure BDA0002454671430000014
715W (EVONIK, Inc.).
The silica dispersion preferably has a solids content of 30% to 50% and a particle size of 100nm or less (e.g.R301, Akzo noble; R302, Akzo noble; R303, Akzo noble; R402, Akzo noble; R1050, Akzo noble; R1020, Akzo noble; R1010, Akzo noble; R900, Akzo noble; WV33, Akzo noble; XP4080, Akzo noble), particularly preferably WV33(Akzo noble).
The wetting agent is a (modified) polyalkyl oxide wetting agent, specifically is one or a mixture of more than two of Levaslip W-461(Elementis company), Levelol W-469(Elementis company) and DW-390 (Shanghai silicon material technology company) in any proportion, and Levaslip W-469(Elementis company) is particularly preferred.
The thickener is cellulose thickener (such as NATROSOL HE 3KB, ASHLAND-AQUALON, NATROSOL HE 10K, ASHLAND-AQUALON, WALOCEL)TMXM 20000PV, dow chemical; WALOCELTMXM 6000PV, Dow chemical company), polyurethane-based thickeners (e.g.
Figure BDA0002454671430000021
510, tequila;
Figure BDA0002454671430000022
644, tequila;
Figure BDA0002454671430000023
655, texie corporation;
Figure BDA0002454671430000024
666, Germany Corp.), polyacrylic thickeners (e.g. as
Figure BDA0002454671430000025
125, tequila;
Figure BDA0002454671430000026
420, tequila;
Figure BDA0002454671430000027
425, tequila;
Figure BDA0002454671430000028
450, deutsche), polyacrylate thickeners (e.g. thickener D-11, ohmingme aviation assistant ltd; latex D, BASF) in any ratio, preferably a cellulosic thickener, and particularly preferably NATROSOL HE 10K (ASHLAND-AQUALON).
The defoaming agent can be silicone defoaming agent (such as Drewplus T-4201, ASHLAND-AQUALON Co., Drewplus TS-4481, ASHLAND-AQUALON Co., Ltd.), lower alcohol defoaming agent (such as Drewplus T-4201, ASHLAND-AQUALON Co., Ltd.), or lower alcohol defoaming agent (such as
Figure BDA0002454671430000029
DF 1760, demote corporation;
Figure BDA00024546714300000210
DF 3163, courtesy corporation), preferably silicone-based antifoaming agents, and particularly preferably Drewplus TS-4201 (ASHLAND-AQUALON).
The vinyl chloride-ethylene copolymer resin is particularly preferably
Figure BDA00024546714300000211
Vinyl chloride CEN8752(WACKER Co.).
The modified high-silicon resin is prepared by modifying organic silicon modified poly (methyl) acrylate emulsion (disclosed and named in patent name of the invention: an anti-fouling and waterproof silicone-acrylate emulsion and a preparation method thereof, application number: 201810271472.9) prepared by the company. Specifically, the preparation method of the modified high-silicon resin comprises the following steps:
(1) preparing a shell layer monomer dropwise-adding phase:
stirring and dissolving 4 parts by weight of methyl acrylate monomer (Shanghai and Chuang chemical technology Co., Ltd.), 5 parts by weight of N-butyl acrylate monomer (Guangzhou, China, Industrial chemical Co., Ltd.), 25 parts by weight of AC-76 (Canoe (Buddha) chemical materials Co., Ltd.), 10 parts by weight of methyl methacrylate monomer (Guangzhou, China, Industrial chemical Co., Ltd.), 0.8 part by weight of cumene hydroperoxide (SIGMA-ALDRICH Co., Ltd.), 0.6 part by weight of N, N-dimethyl toluidine (Tianjin, Kaita chemical Co., Ltd.) and 2 parts by weight of NE-10(ADEKA Co., Ltd.) at 250rpm to obtain a shell layer monomer dropping phase;
(2) preparation of seed phase:
adding 5 parts by weight of SE-1025A (ADEKA), 1.5 parts by weight of NE-10 (ADEKA) and 5 parts by weight of n-butyl acrylate monomer into 102 parts by weight of deionized water, stirring at 750rpm, raising the temperature, adjusting the stirring speed to 250rpm when the temperature is raised to 88 ℃, and adding 4.3 parts by weight of sodium persulfate aqueous solution;
the sodium persulfate aqueous solution is obtained by dissolving 0.3 weight part of sodium persulfate in 4 weight parts of deionized water;
(3) preparation of self-crosslinking core phase:
after the reaction system has obvious blue light, dropwise adding 62 parts by weight of n-butyl acrylate monomer within 7 hours, dropwise adding 12 parts by weight of sodium persulfate aqueous solution while dropwise adding the n-butyl acrylate monomer, and keeping the sodium persulfate aqueous solution and the n-butyl acrylate monomer dropwise added simultaneously;
the sodium persulfate aqueous solution is obtained by dissolving 2 parts by weight of sodium persulfate in 10 parts by weight of deionized water;
(4) preparing an organic silicon shell layer:
reducing the temperature of the system to 63 ℃, adding 1.5 parts by weight of isopropanol, dropwise adding a shell monomer dropwise adding phase within 2 hours, dropwise adding 6.4 parts by weight of sodium bicarbonate aqueous solution while dropwise adding the shell monomer dropwise adding phase, measuring the pH value of the reaction system every 20 minutes, and adjusting the dropwise adding speed of the sodium bicarbonate aqueous solution according to the test result to maintain the pH value of the reaction system between 5.5 and 7.5;
the sodium bicarbonate aqueous solution is obtained by dissolving 0.4 weight part of sodium bicarbonate in 6 weight parts of deionized water;
(5) removing the residual sheets:
after all monomers and the pH buffer solution are dripped, stirring the reaction system for 1.5 hours under heat preservation, adding 2.08 parts by weight of tert-butyl hydrogen peroxide aqueous solution, stirring for 10 minutes under heat preservation, adding 2.08 parts by weight of rongalite aqueous solution, and stirring for 10 minutes under heat preservation; cooling to room temperature and discharging to obtain the modified high-silicon resin;
the tert-butyl hydroperoxide aqueous solution is obtained by dissolving 0.08g of tert-butyl hydroperoxide in 2g of deionized water;
the rongalite aqueous solution is obtained by dissolving 0.08g of rongalite in 2g of deionized water.
The invention also provides a preparation method of the water-based flame-retardant gloss oil, which comprises the following steps of (in parts by weight):
at room temperature (20-30 ℃), sequentially adding 18-22 parts of deionized water, 3-5 parts of dispersing agent, 10-20 parts of silicon dioxide dispersion liquid and 0.06-0.4 part of defoaming agent into a dispersion kettle, stirring and mixing uniformly at the speed of 100 plus materials and 200rpm, then adding 10-15 parts of flame retardant, stirring and mixing uniformly at the speed of 200 plus materials and 300rpm, transferring to a horizontal sand mill for grinding for 5-8 times until the particle size reaches below 250nm, and then filtering (using a 200-mesh nylon filter bag) for discharging to obtain aqueous flame retardant slurry; then adding 10-20 parts of vinyl chloride-ethylene copolymer, 10-20 parts of modified silicone-acrylic emulsion, 6.1-19.2 parts of deionized water, the obtained water-based flame-retardant slurry, 1-3 parts of wetting agent, 0.8-1.2 parts of thickening agent and 0.04-0.2 part of defoaming agent into a dispersion cylinder in sequence, stirring at the speed of 200-250rpm for 0.5-1h, filtering (using a 200-mesh nylon filter bag), and discharging to obtain the water-based flame-retardant gloss oil.
Compared with the prior art, the invention has the beneficial effects that:
1. an aqueous system is adopted, so that the environment is protected;
2. the stable dispersion of the inorganic flame retardant is realized through the optimized design of the formula, and the storage period of the system is as long as more than one year;
3. through strict process control, the particle size of the inorganic flame retardant is below 250nm, the glossiness of the product after film forming is high, the display effect of a film printing pattern is not influenced, and the defect of low glossiness of common surface printing flame-retardant coatings, printing ink and gloss oil is overcome;
4. after the gloss oil is dried into a film, the water resistance is good, the adhesive force is strong, the alcohol wiping resistance is excellent, and the functional requirement of serving as a surface protective coating is met;
5. after the product is coated on plastic films such as PVC furniture films/floor films, PET plastic films, PP decorative films and the like, the plastic films can realize the flame-retardant function of self-extinguishing after leaving fire.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Particle size and particle size distribution testing of the aqueous flame retardant slurry was performed on a Malvern ZETASIZER 3000 HAS particle sizer at a test temperature of 25 ℃.
The storage stability of the water-based flame-retardant gloss oil means that the gloss oil stands still for 18 days at the temperature of 60 ℃, and the storage stability of the gloss oil is more than 12 months without precipitation and delamination.
The water resistance of the gloss oil coating is determined to be qualified according to GB1733-1993, and the water resistance is determined to be qualified when the sample is soaked for 100 hours without phenomena of fading, reduction of glossiness, foaming, falling off and the like, and the longer the soaking time is, the better the water resistance is without the change.
The adhesion test of the gloss oil coating is carried out according to GB/T13217.7-2009, and the adhesion fastness of the resin is considered to be excellent when the adhesion fastness is more than or equal to 95%.
The alcohol-resistant wiping performance test of the gloss oil coating film is carried out according to GB/T23989-2009, wherein the organic solvent for wiping is changed into alcohol, the coating is wiped repeatedly 10 without breakage, and the alcohol-resistant wiping performance of the coating is qualified, and the performance is proved to be better as the wiping times are more.
The gloss of the gloss oil coating was measured by a 60 ° gloss meter.
The flame retardant performance of the gloss oil is carried out according to GB 8624-. Wherein the burning class a represents a noncombustible material (article), the burning class B1 represents a nonflammable material (article), the burning class B2 represents a combustible material (article), and the burning class B3 represents a combustible material (article). The A and B1 grades can achieve self-extinguishing of the burning product when the burning product is away from the fire, and can delay or prevent the fire from spreading in the actual fire.
Example 1:
22kg of deionized water and 3kg of deionized water were mixed at room temperature
Figure BDA0002454671430000031
715W (EVONIK), 10kg of WV33(Akzo noble company) and 0.4kg of Drewplus TS-4201(ASHLAND-AQUALON company) are sequentially added into a dispersion kettle, and after being uniformly stirred and mixed at the speed of 100rpm, 10kg of magnesium hydroxide (Hongtai flame retardant materials Co., Ltd. of Dongguan city) is added, and after being uniformly stirred and mixed at the speed of 200rpm, the mixture is transferred into a horizontal sand mill (TBM-50, Taiyao (Shanghai) practice Co., Ltd.) to be ground for 5 times until the particle size reaches below 250nm, and then a 200-mesh nylon filter bag is used for filtering and discharging to obtain the water-based flame retardant slurry; then sequentially adding 10kg of
Figure BDA0002454671430000032
Vinyl chloride CEN8752(WACKER Co.), 20kg of modified high-silicon resin, 19.2kg of deionized water, 45.4kg of the above aqueous flame retardant slurry, 3kg of Levaslip W-469(ELEMENTIS Co.), 1.2kg of NATROSOL HE 10K (ASHLAND-AQUALON Co.), and 0.2kg of Drewplus TS-4201(ASHLAND-AQUALON Co.) were charged into a dispersion cylinder, stirred at 200rpm for 1 hour, and the discharge was filtered with a 200 mesh nylon filter bag to obtain the aqueous flame retardant gloss oil.
Example 2:
19kg of deionized water and 3kg of deionized water were mixed at room temperature
Figure BDA0002454671430000041
715W (EVONIK), 15kg of WV33(Akzo noble company) and 0.2kg of Drewplus TS-4201(ASHLAND-AQUALON company) are sequentially added into a dispersion kettle, and after being uniformly stirred and mixed at the speed of 150rpm, 12kg of magnesium hydroxide (Hongtai flame retardant materials Co., Ltd., Togao) is added, and after being uniformly stirred and mixed at the speed of 250rpm, the mixture is transferred into a horizontal sand mill (TBM-50, Tai (Shanghai) practice Co., Ltd.) to be ground for 6 times until the particle size reaches below 250nm, and then a 200-mesh nylon filter bag is used for filtering and discharging to obtain the water-based flame retardant slurry; then sequentially adding 15kg of
Figure BDA0002454671430000042
Vinyl chloride CEN8752(WACKER Co.), 19kg of modified high-silicon resin, 11.7kg of deionized water, 49.2kg of the above aqueous flame retardant slurry, 2kg of Levaslip W-469(ELEMENTIS Co.), 1kg of NATROSOL HE 10K (ASHLAND-AQUALON Co.), and 0.1kg of Drewplus TS-4201(ASHLAND-AQUALON Co.) were charged into a dispersion tank, stirred at 250rpm for 0.5h, and the discharge was filtered through a 200 mesh nylon filter bag to obtain the aqueous flame retardant gloss oil.
Example 3:
20kg of deionized water and 4kg of deionized water were mixed at room temperature
Figure BDA0002454671430000043
715W (EVONIK), 18kg of WV33(Akzo noble company) and 0.2kg of Drewplus TS-4201(ASHLAND-AQUALON company) are sequentially added into a dispersion kettle, and after being uniformly stirred and mixed at the speed of 200rpm, 14kg of magnesium hydroxide (Hongtai flame retardant materials Co., Ltd. of Dongguan) is added, and after being uniformly stirred and mixed at the speed of 250rpm, the mixture is transferred into a horizontal sand mill (TBM-50, Tai (Shanghai) practice Co., Ltd.) to be ground for 7 times until the particle size reaches below 250nm, and then a 200-mesh nylon filter bag is used for filtering and discharging to obtain the water-based flame retardant slurry; then sequentially adding 16kg of
Figure BDA0002454671430000044
Vinyl chloride CEN8752(WACKER Co.), 13kg of modified high silicone resin, and 8.7kg of deionized waterThe aqueous flame-retardant gloss oil was obtained by adding brine, 56.2kg of the aqueous flame-retardant slurry, 2kg of Levaslip W-469(Elementis Co.), 1kg of NATROSOL HE 10K (ASHLAND-AQUALON Co.), and 0.1kg of Drewplus TS-4201(ASHLAND-AQUALON Co.) to a dispersion tank, stirring at 250rpm for 0.5 hour, and filtering the discharged material with a 200 mesh nylon filter bag.
Example 4:
18kg of deionized water and 5kg of deionized water were mixed at room temperature
Figure BDA0002454671430000045
715W (EVONIK), 20kg of WV33(Akzo noble company) and 0.06kg of Drewplus TS-4201(ASHLAND-AQUALON company) are sequentially added into a dispersion kettle, stirred and mixed uniformly at the speed of 150rpm, then 15kg of magnesium hydroxide (Hongtai flame retardant materials Co., Togao) is added, stirred and mixed uniformly at the speed of 300rpm, and then transferred into a horizontal sand mill (TBM-50, Tai (Shanghai) practice Co., Ltd.) to be ground for 8 times until the particle size reaches below 250nm, and then a 200-mesh nylon filter bag is used for filtering and discharging to obtain the water-based flame retardant slurry; then sequentially adding 20kg of
Figure BDA0002454671430000046
Vinyl chloride CEN8752(WACKER Co.), 10kg of modified high-silicon resin, 6.1kg of deionized water, 58.06kg of the above aqueous flame retardant slurry, 1kg of Levaslip W-469(ELEMENTIS Co.), 0.8kg of NATROSOL HE 10K (ASHLAND-AQUALON Co.), and 0.04kg of Drewplus TS-4201(ASHLAND-AQUALON Co.) were put into a dispersion tank, stirred at 250rpm for 0.5h and then the discharge was filtered with a 200 mesh nylon filter bag to obtain the aqueous flame retardant gloss oil.
TABLE 1 results of the experiments in the examples section
Figure BDA0002454671430000047
TABLE 2 Experimental results on PVC furniture films
Figure BDA0002454671430000051
TABLE 3 Experimental results on PVC floor films of examples
Figure BDA0002454671430000052
TABLE 4 Experimental results on PET Plastic films for examples
Figure BDA0002454671430000053
TABLE 5 Experimental results on PP decorative films of examples
Figure BDA0002454671430000054
The above-described embodiments are intended to illustrate rather than to limit the invention, and any modifications and variations of the present invention are within the spirit of the invention and the scope of the claims.

Claims (8)

1. The water-based flame-retardant gloss oil is characterized by comprising the following raw materials in parts by weight:
10-15 parts of flame retardant, 3-5 parts of dispersant, 10-20 parts of silicon dioxide dispersion liquid, 10-20 parts of vinyl chloride-ethylene copolymer resin, 10-20 parts of modified high-silicon resin, 1-3 parts of wetting agent, 0.8-1.2 parts of thickening agent, 0.1-0.6 part of defoaming agent and 24.1-41.2 parts of deionized water;
the preparation method of the modified high-silicon resin comprises the following steps:
(1) preparing a shell layer monomer dropwise-adding phase:
stirring and dissolving 4 parts by weight of methyl acrylate monomer, 5 parts by weight of N-butyl acrylate monomer, 25 parts by weight of AC-76, 10 parts by weight of methyl methacrylate monomer, 0.8 part by weight of cumene hydroperoxide, 0.6 part by weight of N, N-dimethyl toluidine and 2 parts by weight of NE-10 at 250rpm to obtain a shell monomer dropwise adding phase;
(2) preparation of seed phase:
adding 5 parts by weight of SE-1025A, 1.5 parts by weight of NE-10 and 5 parts by weight of n-butyl acrylate monomer into 102 parts by weight of deionized water, stirring at 750rpm, starting to heat up, adjusting the stirring speed to 250rpm when the temperature is raised to 88 ℃, and adding 4.3 parts by weight of sodium persulfate aqueous solution;
the sodium persulfate aqueous solution is obtained by dissolving 0.3 weight part of sodium persulfate in 4 weight parts of deionized water;
(3) preparation of self-crosslinking core phase:
after the reaction system has obvious blue light, dropwise adding 62 parts by weight of n-butyl acrylate monomer within 7 hours, dropwise adding 12 parts by weight of sodium persulfate aqueous solution while dropwise adding the n-butyl acrylate monomer, and keeping the sodium persulfate aqueous solution and the n-butyl acrylate monomer dropwise added simultaneously;
the sodium persulfate aqueous solution is obtained by dissolving 2 parts by weight of sodium persulfate in 10 parts by weight of deionized water;
(4) preparing an organic silicon shell layer:
reducing the temperature of the system to 63 ℃, adding 1.5 parts by weight of isopropanol, dropwise adding a shell monomer dropwise adding phase within 2 hours, dropwise adding 6.4 parts by weight of sodium bicarbonate aqueous solution while dropwise adding the shell monomer dropwise adding phase, measuring the pH value of the reaction system every 20 minutes, and adjusting the dropwise adding speed of the sodium bicarbonate aqueous solution according to the test result to maintain the pH value of the reaction system between 5.5 and 7.5;
the sodium bicarbonate aqueous solution is obtained by dissolving 0.4 weight part of sodium bicarbonate in 6 weight parts of deionized water;
(5) removing the residual sheets:
after all monomers and the pH buffer solution are dripped, stirring the reaction system for 1.5 hours under heat preservation, adding 2.08 parts by weight of tert-butyl hydrogen peroxide aqueous solution, stirring for 10 minutes under heat preservation, adding 2.08 parts by weight of rongalite aqueous solution, and stirring for 10 minutes under heat preservation; cooling to room temperature and discharging to obtain the modified high-silicon resin;
the tert-butyl hydroperoxide aqueous solution is obtained by dissolving 0.08 weight part of tert-butyl hydroperoxide in 2 weight parts of deionized water;
the rongalite aqueous solution is prepared by dissolving 0.08 weight part of rongalite in 2 weight parts of deionized water.
2. The aqueous flame retardant gloss oil of claim 1, wherein the flame retardant is magnesium hydroxide.
3. The aqueous flame-retardant gloss oil of claim 1, wherein the dispersant is one or a mixture of two or more of modified polyether dispersants or polyacrylate dispersants in any proportion.
4. The aqueous flame-retardant gloss oil of claim 1, wherein the silica dispersion has a solid content of 30-50% and a particle size of 100nm or less.
5. The aqueous flame retardant gloss oil of claim 1, wherein the wetting agent is a modified polyalkylsiloxane wetting agent.
6. The aqueous flame retardant gloss oil of claim 1, wherein the thickener is one or a mixture of two or more of cellulose thickener, polyurethane thickener, polyacrylic thickener and polyacrylate thickener.
7. The aqueous flame-retardant gloss oil according to claim 1, wherein the defoaming agent is one or a mixture of two or more of a silicone defoaming agent and a lower alcohol defoaming agent in any proportion.
8. The preparation method of the water-based flame-retardant gloss oil as claimed in claim 1, which is characterized by comprising the following steps:
at room temperature, sequentially adding 18-22 parts of deionized water, 3-5 parts of a dispersing agent, 10-20 parts of a silicon dioxide dispersion liquid and 0.06-0.4 part of a defoaming agent into a dispersion kettle, stirring and mixing uniformly at the speed of 100 plus of 200rpm, then adding 10-15 parts of a flame retardant, stirring and mixing uniformly at the speed of 200 plus of 300rpm, transferring to a horizontal sand mill for grinding for 5-8 times until the particle size of particles reaches below 250nm, and then filtering and discharging to obtain aqueous flame retardant slurry; then adding 10-20 parts of vinyl chloride-ethylene copolymer, 10-20 parts of modified high-silicon resin, 6.1-19.2 parts of deionized water, the obtained water-based flame-retardant slurry, 1-3 parts of wetting agent, 0.8-1.2 parts of thickening agent and 0.04-0.2 part of defoaming agent into a dispersion cylinder in sequence, stirring at the speed of 200-250rpm for 0.5-1h, and filtering and discharging to obtain the water-based flame-retardant gloss oil.
CN202010302879.0A 2020-04-17 2020-04-17 Water-based flame-retardant gloss oil and preparation method thereof Active CN111334152B (en)

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