CN114195951A - Modified water-based acrylic flame-retardant resin with good wettability and preparation method thereof - Google Patents

Modified water-based acrylic flame-retardant resin with good wettability and preparation method thereof Download PDF

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Publication number
CN114195951A
CN114195951A CN202111538468.2A CN202111538468A CN114195951A CN 114195951 A CN114195951 A CN 114195951A CN 202111538468 A CN202111538468 A CN 202111538468A CN 114195951 A CN114195951 A CN 114195951A
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parts
retardant resin
mixed solution
good wettability
polyoxyethylene ether
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CN202111538468.2A
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Chinese (zh)
Inventor
张武
康伦国
姚东生
陈有权
阳京辉
徐景华
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Shaoguan Union Chemical Co Ltd
Union Foshan Chemical Co Ltd
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Shaoguan Union Chemical Co Ltd
Union Foshan Chemical Co Ltd
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Priority to CN202111538468.2A priority Critical patent/CN114195951A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • 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
    • 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
    • C09D151/08Coating 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 otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • 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

Abstract

The invention relates to a modified water-based acrylic flame-retardant resin with good wettability and a preparation method thereof, wherein the modified water-based acrylic flame-retardant resin comprises the following components in parts by weight: 10.0-18.0 parts of allyl polyoxyethylene ether phosphate, 3.5-6.0 parts of acrylic acid and N- (hydroxyl)2.5-5.0 parts of methyl) acrylamide, 0.3-1.0 part of benzoyl peroxide, 15.0-35.0 parts of hard acrylate monomer, 30.0-70.0 parts of soft acrylate monomer, 35.0-75.0 parts of butyl cellosolve, 2.5-8.0 parts of neutralizer and 100.0-220.0 parts of deionized water; the allyl polyoxyethylene ether phosphate is prepared from allyl polyoxyethylene ether and P2O5Is prepared by reaction; the modified water-based acrylic flame-retardant resin with good wettability prepared by the invention has good wettability, adhesive force and flexibility, and when the modified water-based acrylic flame-retardant resin is prepared into a coating, a flame retardant and a wetting agent are not required to be added, so that the modified water-based acrylic flame-retardant resin has good flame retardance and wetting performance.

Description

Modified water-based acrylic flame-retardant resin with good wettability and preparation method thereof
Technical Field
The invention relates to a modified water-based acrylic resin, in particular to a modified water-based acrylic flame-retardant resin with good wettability and a preparation method thereof, belonging to the technical field of synthetic water-based resins.
Background
Acrylate resins are a general class of synthetic polymers that, due to their unique advantages: the acrylic resin has good weather resistance, solvent depolymerization resistance, electrical insulation performance and the like, and has the advantages of various raw materials, high selectivity, relatively low price and good flexibility in synthesis, and can be modified by adopting certain special functional groups, so that the material can be widely applied to the fields of materials, coatings, adhesives, printing ink and the like. However, the acrylate polymer has the disadvantages of poor thermal stability, poor adhesion, poor wettability, flammability, etc., so that it is limited in the use process.
Chinese patent CN111675785A discloses a ferrocene-organophosphorus reactive flame retardant modified acrylic resin, wherein a unique cavity structure of beta-cyclodextrin has good inclusion effect on 1,1 '-ferrocene diformyl chloride, an acyl chloride group of the 1, 1' -ferrocene diformyl chloride reacts with an active phenolic hydroxyl group of 10- (2, 5-dihydroxyphenyl) -9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to obtain the beta-cyclodextrin coated ferrocene-organophosphorus composite flame retardant, ammonium ceric nitrate is used as an initiator to initiate in-situ polymerization of beta-cyclodextrin components and monomers such as methyl methacrylate and the like, so that beta-cyclodextrin-coated ferrocene-organophosphorus is used as a reactive flame retardant and added into a molecular chain of acrylic resin; chinese patent CN111909302A discloses a phosphorus/silicon-containing flame-retardant transparent acrylic resin and a preparation method thereof, and the flame retardant property of the acrylic resin reaches UL94-V0 grade through the synergistic effect of phosphorus/silicon. The acrylic resin is prepared by methyl methacrylate and a phosphorus/silicon reactive flame retardant in the presence of an initiator through prepolymerization, low-temperature polymerization in a mold, high-temperature post-treatment and demolding; chinese patent CN101775101A discloses an organosilicon/hydroxyl phosphate composite modified water emulsion acrylic resin and a preparation method and application thereof, wherein the acrylic resin is modified by copolymerization of synthesized hydroxyl phosphate and organosiloxane, the weight percentage of resin solids is 45-55%, and the balance is deionized water; the components for forming the acrylic resin and the using amount thereof are as follows: 35-60% of acrylate monomer, 3-10% of organosilicon monomer, 5-10% of hydroxyl phosphate monomer, 1.5-4.0% of composite emulsifier, 0.5-1% of pH regulator and 0.5-1.5% of initiator based on the acrylate monomer, wherein after the resin is prepared into a single-component anticorrosive coating, the anticorrosive performance of a paint film of the single-component anticorrosive coating is superior to that of the single-component anticorrosive coating prepared from the existing water-dispersible acrylic resin; chinese patent CN110818828A discloses a self-retardant fuel alcohol polyether-2 phosphate modified waterborne acrylic acid anticorrosive resin and a preparation method thereof, wherein the self-retardant fuel alcohol polyether-2 phosphate modified waterborne acrylic acid anticorrosive resin comprises the following components in parts by weight: 6.0-15.0 parts of oleyl polyether-2 phosphate, 5.0-9.0 parts of crosslinking monomer, 0.6-2.0 parts of benzoyl peroxide, 6.0-12.0 parts of propyl polyoxyethylene epoxy ether, 4.0-7.0 parts of acrylic acid, 65.0-130.0 parts of acrylate hard monomer, 10.0-30.0 parts of acrylate soft monomer, 2.0-5.0 parts of silane coupling agent, 3.0-8.0 parts of allyl glycidyl ether, 30.0-50.0 parts of cosolvent, 4.0-12.0 parts of neutralizer and 100.0-200.0 parts of deionized water; said invention possesses fire-resisting property, but its wettability for base material is not enough, and when it is made into coating material, the wetting agent must be added.
Therefore, how to solve the problem of poor wettability of the existing water-based acrylic resin meets the requirement of social development on better product.
Disclosure of Invention
In order to solve the technical problems, the invention adopts allyl polyoxyethylene ether phosphate to modify the water-based acrylic resin, the allyl polyoxyethylene ether phosphate is connected with the water-based acrylic resin through chemical bonds, the performance is stable and durable, and no wetting agent is required to be added when the coating is prepared.
The invention aims to provide a modified water-based acrylic flame-retardant resin with good wettability.
The invention also aims to provide a preparation method of the modified waterborne acrylic flame retardant resin with good wettability.
The invention relates to a modified water-based acrylic flame-retardant resin with good wettability, which adopts the following technical scheme: the composition comprises the following components in parts by weight: 10.0-18.0 parts of allyl polyoxyethylene ether phosphate, 3.5-6.0 parts of acrylic acid, 2.5-5.0 parts of N- (hydroxymethyl) acrylamide, 0.3-1.0 part of benzoyl peroxide, 15.0-35.0 parts of an acrylate hard monomer, 30.0-70.0 parts of an acrylate soft monomer, 35.0-75.0 parts of ethylene glycol butyl ether, 2.5-8.0 parts of a neutralizer and 100.0-220.0 parts of deionized water; the allyl polyoxyethylene ether phosphate is prepared from allyl polyoxyethylene ether and P2O5Is prepared through reaction.
The allyl polyoxyethylene ether phosphate is prepared by the following method:
in the invention, allyl polyoxyethylene ether and P are selected2O5The amount ratio of the substances of (a) to (b) is 2.5: 1; adding weighed allyl polyoxyethylene ether into a three-neck flask provided with a thermometer, a temperature control device and a stirrer, and slowly adding P under the condition of high-speed stirring2O5Controlling the temperature below 50 ℃ in the feeding process, and finishing the feeding of P2O5Then slowly raising the temperature to 70 ℃, keeping the temperature and continuously reacting for 4 hours, adding quantitative water for hydrolysis for 2 hours to complete the synthesis of the phosphate, sampling and measuring the acid value. Cooling to below 50 ℃, neutralizing with 20% sodium hydroxide solution according to the measured acid value result until the PH value is 6-8, keeping the temperature for reaction for a period of time to obtain a crude product, and purifying to obtain the allyl polyoxyethylene ether phosphate。
The acrylate hard monomer is one or a combination of methyl acrylate, methyl methacrylate, isobornyl acrylate and cyclohexyl methacrylate.
The acrylate soft monomer is one or a combination of butyl methacrylate, isooctyl methacrylate, lauryl methacrylate, tridecyl methacrylate, glycidyl methacrylate and stearyl methacrylate.
The neutralizing agent is one or a combination of more of triethylamine, ammonia water and dimethylethanolamine.
The invention provides a preparation method of modified water-based acrylic flame-retardant resin with good wettability, which comprises the following steps:
a. uniformly stirring an acrylate hard monomer, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, according to the weight part of the formula, uniformly stirring allyl polyoxyethylene ether phosphate, an acrylate soft monomer and 1/4 ethylene glycol butyl ether to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 3.5-4.0 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating partial solvent under reduced pressure, cooling, adding a neutralizing agent, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the modified water-based acrylic flame-retardant resin with good wettability.
The modified water-based acrylic flame-retardant resin with good wettability prepared by the invention has good wettability, adhesive force and flexibility, and when the modified water-based acrylic flame-retardant resin is prepared into a coating, a flame retardant and a wetting agent are not required to be added, so that the modified water-based acrylic flame-retardant resin has good flame retardance and wetting performance.
Detailed Description
The modified aqueous acrylic flame retardant resin with good wettability of the present invention will be further described with reference to the following examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention.
The following are specific examples of the present invention, and raw materials, equipments and the like used in the following examples can be obtained by purchasing them unless otherwise specified.
Example 1
A modified water-based acrylic flame-retardant resin with good wettability comprises the following components in parts by weight: 16.0 parts of allyl polyoxyethylene ether phosphate, 5.0 parts of acrylic acid, 4.0 parts of N- (hydroxymethyl) acrylamide, 0.8 part of benzoyl peroxide, 26.0 parts of methyl methacrylate, 25.0 parts of butyl methacrylate, 25.0 parts of isooctyl methacrylate, 60.0 parts of ethylene glycol butyl ether, 6.0 parts of triethylamine and 170.0 parts of deionized water.
The preparation method of the modified water-based acrylic flame-retardant resin with good wettability in the embodiment comprises the following steps:
a. uniformly stirring methyl methacrylate, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, according to the weight part of the formula, uniformly stirring allyl polyoxyethylene ether phosphate, butyl methacrylate, isooctyl methacrylate and 1/4 ethylene glycol butyl ether to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 4.0 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating partial solvent under reduced pressure, cooling, adding triethylamine, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the modified aqueous acrylic flame-retardant resin with good wettability.
Example 2
A modified water-based acrylic flame-retardant resin with good wettability comprises the following components in parts by weight: 14.0 parts of allyl polyoxyethylene ether phosphate, 4.0 parts of acrylic acid, 5.0 parts of N- (hydroxymethyl) acrylamide, 0.7 part of benzoyl peroxide, 20.0 parts of isobornyl acrylate, 20.0 parts of tridecyl methacrylate, 25.0 parts of glycidyl methacrylate, 55.0 parts of ethylene glycol butyl ether, 4.5 parts of ammonia and 150.0 parts of deionized water.
The preparation method of the modified water-based acrylic flame-retardant resin with good wettability in the embodiment comprises the following steps:
a. uniformly stirring isobornyl acrylate, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, according to the weight part of the formula, uniformly stirring allyl polyoxyethylene ether phosphate, tridecyl methacrylate, glycidyl methacrylate and 1/4 ethylene glycol butyl ether to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 3.5 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating part of the solvent under reduced pressure, cooling, adding ammonia water, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the modified aqueous acrylic flame-retardant resin with good wettability.
Example 3
A modified water-based acrylic flame-retardant resin with good wettability comprises the following components in parts by weight: 12.0 parts of allyl polyoxyethylene ether phosphate, 5.0 parts of acrylic acid, 2.5 parts of N- (hydroxymethyl) acrylamide, 0.6 part of benzoyl peroxide, 10.0 parts of methyl methacrylate, 10.0 parts of cyclohexyl methacrylate, 15.0 parts of isooctyl methacrylate, 25.0 parts of lauryl methacrylate, 50.0 parts of ethylene glycol butyl ether, 7.5 parts of dimethylethanolamine and 140.0 parts of deionized water.
The preparation method of the modified water-based acrylic flame-retardant resin with good wettability in the embodiment comprises the following steps:
a. uniformly stirring methyl methacrylate, cyclohexyl methacrylate, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, according to the weight part of the formula, uniformly stirring allyl polyoxyethylene ether phosphate, isooctyl methacrylate, lauryl methacrylate and 1/4 ethylene glycol butyl ether to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 3.5 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating part of the solvent under reduced pressure, cooling, adding dimethylethanolamine, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the modified water-based acrylic flame-retardant resin with good wettability.
Comparative example 1
A conventional modified water-based acrylic resin comprises the following components in parts by weight: 4.0 parts of acrylic acid, 4.0 parts of N- (hydroxymethyl) acrylamide, 0.6 part of benzoyl peroxide, 20.0 parts of methyl acrylate, 20.0 parts of butyl methacrylate, 20.0 parts of isooctyl methacrylate, 45.0 parts of butyl cellosolve, 5.0 parts of triethylamine and 130.0 parts of deionized water.
The preparation method of the conventional modified waterborne acrylic resin in the embodiment comprises the following steps:
a. uniformly stirring methyl acrylate, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, uniformly stirring butyl methacrylate, isooctyl methacrylate and 1/4 ethylene glycol butyl ether according to the weight part of the formula to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 3.5 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating partial solvent under reduced pressure, cooling, adding triethylamine, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the conventional modified water-based acrylic resin.
And (3) testing performance indexes: the samples of the above examples 1, 2, 3 and 1 were prepared into paints according to the raw material formulas of table 1, and the corresponding paint samples were respectively designated as paint 1, paint 2, paint 3 and paint 4; and tested for performance separately.
Table 1: coating formulation
Name of raw materials Specification of Amount/% of
Water (W) Deionized water 4.5
Film forming aid Twelve alcohol ester 5.0
Aqueous resin Sample aqueous resin 90.0
Leveling agent BYK-333 0.5
The prepared coating is tested for performance indexes according to relevant standards, and the test results are shown in table 2.
Wherein, the adhesive force is as follows: testing was carried out as specified in GB/T1720-1988;
impact resistance: detecting according to the GB/T1732-2020;
flame-retardant time: detecting according to the regulation of GB 12441-2005;
flexibility: detection is carried out according to the specification of GB/T1731-1993;
salt spray resistance: the assay was carried out as specified in GB/T1771-1991.
Table 2: performance specification of coating
Detecting items Coating 1 Paint 2 Coating 3 Coating 4
Adhesion force Level 0 Level 0 Level 0 Stage 2
Water resistance/240 h Normal paint film Normal paint film Normal paint film Slight blistering of the paint film
Salt spray resistance/480 h Normal paint film Normal paint film Normal paint film Discoloration of paint film
Impact resistance Normal paint film Normal paint film Normal paint film Cracking of paint film
Flame resistance time/min 26 28 25 11
Flexibility/mm 1 1 1 2
Wettability (visual inspection) Good effect Good effect Good effect In general
As can be seen from Table 2, the adhesion, wettability, impact resistance and flame retardant time of the coatings 1, 2 and 3 of the invention are much better than those of the comparative example 1 (conventional modified waterborne acrylic resin), that is, the adhesion, wettability, impact resistance and flame retardant time of the examples 1, 2 and 3 are better than those of the conventional modified waterborne acrylic resin of the comparative example 1, which shows that the modified waterborne acrylic flame retardant resin with good wettability prepared by the invention has good adhesion, wettability, impact resistance and flame retardant properties.
The foregoing description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed; it will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.

Claims (5)

1. A modified water-based acrylic flame-retardant resin with good wettability is characterized in that: a modified water-based acrylic flame-retardant resin with good wettability comprises the following components in parts by weight: 10.0-1 parts of allyl polyoxyethylene ether phosphate8.0 parts, 3.5-6.0 parts of acrylic acid, 2.5-5.0 parts of N- (hydroxymethyl) acrylamide, 0.3-1.0 part of benzoyl peroxide, 15.0-35.0 parts of acrylate hard monomer, 30.0-70.0 parts of acrylate soft monomer, 35.0-75.0 parts of ethylene glycol butyl ether, 2.5-8.0 parts of neutralizer and 100.0-220.0 parts of deionized water; the allyl polyoxyethylene ether phosphate is prepared from allyl polyoxyethylene ether and P2O5Is prepared by reaction; the allyl polyoxyethylene ether phosphate is prepared by the following method: in the invention, allyl polyoxyethylene ether and P are selected2O5The amount ratio of the substances of (a) to (b) is 2.5: 1; adding weighed allyl polyoxyethylene ether into a three-neck flask provided with a thermometer, a temperature control device and a stirrer, and slowly adding P under the condition of high-speed stirring2O5Controlling the temperature below 50 ℃ in the feeding process, and finishing the feeding of P2O5Then slowly raising the temperature to 70 ℃, keeping the temperature and continuously reacting for 4 hours, adding quantitative water for hydrolysis for 2 hours to complete the synthesis of the phosphate, sampling and measuring the acid value. And (3) cooling to below 50 ℃, neutralizing with 20% sodium hydroxide solution according to the measured acid value result until the PH value is 6-8, keeping the temperature for reaction for a period of time to obtain a crude product, and purifying to obtain the allyl polyoxyethylene ether phosphate.
2. The modified aqueous acrylic flame retardant resin with good wettability as claimed in claim 1, wherein: the acrylate hard monomer is one or a combination of methyl acrylate, methyl methacrylate, isobornyl acrylate and cyclohexyl methacrylate.
3. The modified aqueous acrylic flame retardant resin with good wettability as claimed in claim 1, wherein: the acrylate soft monomer is one or a combination of butyl methacrylate, isooctyl methacrylate, lauryl methacrylate, tridecyl methacrylate, glycidyl methacrylate and stearyl methacrylate.
4. The modified aqueous acrylic flame retardant resin with good wettability as claimed in claim 1, wherein: the neutralizing agent is one or a combination of more of triethylamine, ammonia water and dimethylethanolamine.
5. The modified aqueous acrylic flame retardant resin with good wettability as claimed in claim 1, wherein: the preparation method of the modified water-based acrylic flame-retardant resin with good wettability comprises the following steps:
a. uniformly stirring an acrylate hard monomer, N- (hydroxymethyl) acrylamide, 2/3 benzoyl peroxide and acrylic acid in parts by weight of a formula in a titration tank to obtain a mixed solution I;
b. in a titration tank, according to the weight part of the formula, uniformly stirring allyl polyoxyethylene ether phosphate, an acrylate soft monomer and 1/4 ethylene glycol butyl ether to obtain a mixed solution II;
c. adding 3/4 ethylene glycol monobutyl ether and 1/3 benzoyl peroxide into a multifunctional reaction kettle, heating to 78-82 ℃, uniformly stirring, and then simultaneously dropwise adding the mixed solution I and the mixed solution II for 3.5-4.0 hours;
d. respectively controlling the dropping speed, heating the mixed solution I and the mixed solution II to 86-88 ℃ after the mixed solution I and the mixed solution II are simultaneously dropped, and stirring for reacting for 1.5 hours;
e. and (3) evaporating partial solvent under reduced pressure, cooling, adding a neutralizing agent, stirring and dispersing under high-speed shearing force, adding a proper amount of deionized water until the specified solid content is achieved, and filtering to obtain the modified water-based acrylic flame-retardant resin with good wettability.
CN202111538468.2A 2021-12-15 2021-12-15 Modified water-based acrylic flame-retardant resin with good wettability and preparation method thereof Withdrawn CN114195951A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110818828A (en) * 2019-12-07 2020-02-21 合众(佛山)化工有限公司 Self-retardant fuel alcohol polyether-2 phosphate modified waterborne acrylic acid anticorrosive resin and preparation method thereof
CN110819193A (en) * 2019-12-07 2020-02-21 合众(佛山)化工有限公司 Self-flame-retardant acrylic resin water-based anticorrosive 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
CN110894285A (en) * 2019-12-07 2020-03-20 合众(佛山)化工有限公司 Oleyl polyether-2 phosphate modified waterborne alkyd flame-retardant resin and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110818828A (en) * 2019-12-07 2020-02-21 合众(佛山)化工有限公司 Self-retardant fuel alcohol polyether-2 phosphate modified waterborne acrylic acid anticorrosive resin and preparation method thereof
CN110819193A (en) * 2019-12-07 2020-02-21 合众(佛山)化工有限公司 Self-flame-retardant acrylic resin water-based anticorrosive 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
CN110894285A (en) * 2019-12-07 2020-03-20 合众(佛山)化工有限公司 Oleyl polyether-2 phosphate modified waterborne alkyd flame-retardant resin and preparation method thereof

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