CN114525092A - High-thixotropic flame-retardant water-based transparent nail-free adhesive and preparation method thereof - Google Patents
High-thixotropic flame-retardant water-based transparent nail-free adhesive and preparation method thereof Download PDFInfo
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- CN114525092A CN114525092A CN202210257079.0A CN202210257079A CN114525092A CN 114525092 A CN114525092 A CN 114525092A CN 202210257079 A CN202210257079 A CN 202210257079A CN 114525092 A CN114525092 A CN 114525092A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 84
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000003063 flame retardant Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 239000000853 adhesive Substances 0.000 title claims abstract description 32
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 32
- 239000003292 glue Substances 0.000 claims abstract description 68
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001509 sodium citrate Substances 0.000 claims abstract description 13
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 13
- 230000009974 thixotropic effect Effects 0.000 claims abstract description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 10
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 9
- 239000003899 bactericide agent Substances 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 239000000839 emulsion Substances 0.000 claims description 76
- 239000007864 aqueous solution Substances 0.000 claims description 46
- 239000003999 initiator Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 25
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 11
- POLZHVHESHDZRD-UHFFFAOYSA-N 2-hydroxyethyl 2-methylprop-2-enoate;phosphoric acid Chemical group OP(O)(O)=O.CC(=C)C(=O)OCCO POLZHVHESHDZRD-UHFFFAOYSA-N 0.000 claims description 10
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical group OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 claims description 10
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 8
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical group CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000003242 anti bacterial agent Substances 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 26
- 239000002585 base Substances 0.000 description 24
- 239000002904 solvent Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 6
- 238000007711 solidification Methods 0.000 description 6
- 230000008023 solidification Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 230000008719 thickening Effects 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000002313 adhesive film Substances 0.000 description 3
- 239000000440 bentonite Substances 0.000 description 3
- 229910000278 bentonite Inorganic materials 0.000 description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000013008 moisture curing Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000013008 thixotropic agent Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012780 transparent material Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 241000195649 Chlorella <Chlorellales> Species 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives 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; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
Abstract
The invention provides a high-thixotropy flame-retardant water-based transparent nail-free adhesive which comprises the following components in percentage by mass: 40 to 45 percent of reaction monomer; 2% -4% of functional monomer; 4% -6% of a flame-retardant monomer; 1.0 to 3.0 percent of composite emulsifier; 40% -45% of deionized water; 0.2 to 0.3 percent of ammonium persulfate; 0.2 to 0.3 percent of sodium citrate; 1.0 to 2.0 percent of pH regulator; 0.1 to 0.2 percent of bactericide; 2.5 to 4.0 percent of silica sol. The invention also provides a preparation method of the high-thixotropy flame-retardant water-based transparent nail-free adhesive. The nail-free glue has excellent thixotropic capability, can be constructed on a vertical surface, and simultaneously, the glue solution has flame retardant capability due to the introduction of a flame retardant monomer for copolymerization. The nail-free glue is in a transparent state after being cured, and can realize traceless bonding on materials.
Description
Technical Field
The invention belongs to the field of environment-friendly adhesives, and particularly relates to a high-thixotropy flame-retardant water-based transparent nail-free adhesive and a preparation method thereof.
Background
The nail-free glue is also called a liquid nail, is a multifunctional decorative adhesive with strong adhesive force, can replace a nail, and realizes the non-nail hole adhesion. The nail-free glue has the characteristics of high curing speed, high bonding strength, wide application range, convenience in use and the like, and is widely applied to industries of decoration, furniture manufacture, artware manufacture and the like.
The nail-free glue can be divided into solvent volatile type, moisture curing type and water-based type according to the composition. Solvent type nail-free glue, moisture curing type nail-free glue and water-based nail-free glue usually contain a large amount of organic high molecular compounds, which are flammable, and after the glue solution is cured, the danger of possible fire hazard exists. Meanwhile, the cured adhesive film can generate smoke and toxic gas during combustion, which can harm the environment and the health of people.
In addition, the nail-free glue products sold in the market at present mainly take non-transparent products, the transparent nail-free glue is rare and is both solvent volatile type and moisture curing type, and the environmental protection level of the products is low. The water-based transparent nail-free glue is not reported. Because the glue body of the nail-free glue is not transparent, the non-trace bonding can not be realized when the nail-free glue is used for bonding transparent materials such as glass, acrylic sheets, PVC sheets and the like, and the appearance is influenced.
In summary, these adverse factors affect the use and deployment of nail-free adhesives. Therefore, it is necessary to develop a flame-retardant water-based transparent nail-free adhesive which can meet the use requirements of customers, provide reliable safety and realize 'traceless' bonding.
Disclosure of Invention
The invention provides a high-thixotropy flame-retardant water-based transparent nail-free adhesive and a preparation method thereof, and the specific technical scheme is as follows:
the high-thixotropy flame-retardant water-based transparent nail-free glue comprises the following components in percentage by mass:
preferably, the reaction monomer is a mixture of styrene, butyl acrylate and acrylic acid, wherein the mass percentage ratio of the styrene to the butyl acrylate to the acrylic acid is 34-40: 50-61: 2-5.5.
Preferably, the functional monomer is 4-hydroxybutylacrylate.
Preferably, the flame retardant monomer is hydroxyethyl methacrylate phosphate.
Preferably, the composite emulsifier is a mixture of SR-10 and ER-10, and the mass fraction ratio of SR-10 to ER-10 is 1-4: 1.
Wherein SR-10 is an anionic emulsifier and is Idiaceae brand; ER-10 is a nonionic emulsifier and is made by Ediko brand.
Preferably, the pH adjusting agent is 2-amino-2-methyl-1-propanol.
Preferably, the antimicrobial agent is CN-46.
The antibacterial agent used in the invention is a hoffman Defros CN-46 tank preservative.
Preferably, the silica sol is a dispersion liquid with the mass fraction of silica being 28-32%, the pH value of the silica sol is 9.0-11.0, and the average particle size of the silica in the silica sol is 3-5 nm.
The silica sol used in the present invention was HS-530K, and the manufacturer was Linyi Kohn silicon products, Inc.
The invention also aims to provide a preparation method of the high-thixotropy flame-retardant water-based transparent nail-free glue, which comprises the following specific steps:
preparation of pre-emulsion:
adding a composite emulsifier and deionized water into an emulsifying machine, and stirring for 1h until the mixture is dispersed to prepare an emulsifier aqueous solution with the mass percentage concentration of 5-16%; dropwise adding a reaction monomer, a functional monomer and a flame-retardant monomer into the emulsifier aqueous solution, and stirring for 1h until the mixture is uniformly dispersed to obtain a pre-emulsion;
preparing a seed emulsion:
dissolving ammonium persulfate in deionized water to prepare an initiator aqueous solution with the mass percentage concentration of 12-17%; according to the weight ratio of sodium citrate: pre-emulsion: emulsifier: deionized water is 1.4-2: 20: 1: 181-200, stirring and heating to 78 ℃; adding an aqueous initiator solution to the reaction kettle when the temperature rises to 78 ℃, wherein the ratio of the aqueous initiator solution: the mass ratio of the sodium citrate is 3.3: 1.3-2.1; reacting for 1h at the temperature of 79 +/-1 ℃ to obtain seed emulsion;
preparing the water-based base material:
at the temperature of 79 +/-1 ℃, dropwise adding the pre-emulsion and the initiator aqueous solution into the seed emulsion again, wherein the dropwise adding of the pre-emulsion and the initiator aqueous solution is carried out simultaneously, wherein the initiator aqueous solution: pre-emulsion: the mass ratio of the sodium citrate is 8.0-9.0: 446-450: 1.3-2.1, wherein the dripping time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 1-2 h at the temperature of 83 +/-2 ℃ to obtain a water-based base material;
fourthly, preparing glue:
and (3) putting the water-based base material into a high-speed dispersion power mixer, sequentially adding the pH regulator, the bactericide and the silica sol at the rotating speed of 600 +/-30 r/min, and stirring for 15 +/-2 min until the materials are uniformly dispersed to prepare the high-thixotropy flame-retardant water-based transparent nail-free adhesive.
In the step of preparing the pre-emulsion, a part of emulsifier is added to prepare emulsifier aqueous solution; in the preparation step of the seed emulsion, a part of emulsifier is added into the reaction kettle, and the sum of the two parts is the total amount of the whole emulsifier.
In the step of preparing the pre-emulsion, mixed monomers (reaction monomers, functional monomers and flame-retardant monomers) are added dropwise into an emulsifier aqueous solution to prepare the pre-emulsion, wherein the pre-emulsion is the amount of the whole pre-emulsion, part of the pre-emulsion is added into a reaction kettle in the process of preparing the seed emulsion, and the rest of the pre-emulsion is added in the process of preparing the aqueous base material.
In the preparation process of the seed emulsion, ammonium persulfate is dissolved in deionized water to prepare an initiator aqueous solution with the mass percentage concentration of 12-17%, wherein the initiator aqueous solution is the whole initiator aqueous solution. And c, adding a part of initiator aqueous solution into the reaction kettle in the preparation process of the seed emulsion, and dropwise adding the rest of initiator aqueous solution into the seed emulsion in the preparation process of the water-based base material, wherein the sum of the part of initiator aqueous solution and the rest of initiator aqueous solution is the amount of the whole initiator aqueous solution.
Compared with the prior art, the invention has the following characteristics:
the invention uses deionized water as a dispersion medium, does not add any organic solvent, tackifying emulsion, chelating tin and other metal catalysts, is environment-friendly and harmless to human bodies, and ensures that the product really has good environmental protection;
styrene, butyl acrylate and acrylic acid are used as reaction monomers, 4-hydroxybutyl acrylate is used as a functional monomer for polymerization, the obtained polymer has a large number of hydroxyl structures and can form strong hydrogen bonds with silicon dioxide particles in alkaline silica sol, so that silicon dioxide aggregates dispersed in the system are connected into a complete silicon dioxide network to fill the whole system, the viscosity of the system is increased, and the thickening effect is achieved; in addition, carboxyl on the obtained polymer can be neutralized into salt by alkali, electrostatic repulsion and hydration are generated in molecules, a macromolecular structure is gradually stretched from a curling state, a large amount of water molecules around the macromolecular structure are adsorbed, free water is reduced, the consistency of the system is further greatly improved, the glue solution can obtain high thixotropy, and the vertical face construction can be realized;
the traditional thickening thixotropic agent such as fumed silica, precipitated silica, modified polyamide wax powder, modified castor oil, organic bentonite, inorganic bentonite and the like is not used, so that the adverse effect of the thickening thixotropic agent on the transparency is avoided, and the excellent transparency of the glue solution is ensured;
the invention adopts hydroxyethyl methacrylate phosphate as a reactive phosphorus-containing flame retardant, and introduces phosphate groups with flame retardant function to the polymer through copolymerization, so that the polymer has certain flame retardant capability, thereby realizing flame retardance of the adhesive film;
the invention uses the anionic reactive emulsifier SR-10 and the nonionic reactive emulsifier ER-10 to compound as the compound emulsifier. The reactive emulsifier can copolymerize with monomers, so that the polymer molecular chain is grafted with a long chain with a surface active structure, and the long chain structure has both hydrophobic groups and hydrophilic groups, so that the polymer molecular chain also has surface activity. They can form a large micelle structure in water, and are mutually adsorbed and associated in molecules or among molecules, so that the consistency of the emulsion is further increased. Meanwhile, the stability of the aqueous base material is greatly improved;
sixthly, the water-based transparent nail-free glue provided by the invention has the advantages that the glue film is milky when in use, and is in a completely transparent state after the glue film is completely cured. The adhesive film has good transparency, the light transmission capability is better than that of a shoulder solvent type nail-free adhesive, the seamless adhesion can be realized on transparent materials such as glass, acrylic and the like, and the application range is wider;
the invention has the curing speed and the super strong bonding ability which are comparable to those of solvent type transparent nail-free glue.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The high-thixotropy flame-retardant water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
preparation of a Pre-emulsion
Adding 105g of deionized water, 3.0gSR-10 and 3.0gER-10 emulsifiers into an emulsifying machine in sequence, and stirring for 1h until the mixture is uniformly dispersed to obtain an emulsifier aqueous solution; the mixed monomers (110g of styrene, 189g of butyl acrylate, 16g of acrylic acid, 14g of 4-hydroxybutyl acrylate and 28g of hydroxyethyl methacrylate phosphate) were added dropwise to the aqueous emulsifier solution, and the mixture was stirred for 1 hour until the dispersion was uniform, thereby obtaining 468g of a pre-emulsion.
② preparation of seed emulsion
a. Dissolving 1.4g of ammonium persulfate in 10g of deionized water to prepare 11.4g of initiator aqueous solution;
b. adding 200g of deionized water, 1.4g of sodium citrate, 20g of pre-emulsion, 0.5g of SR-10 and 0.5g of ER-10 emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1h at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dropwise adding 448g of the residual whole pre-emulsion and 8.1g of the residual initiator aqueous solution into the seed emulsion at the temperature of 79 +/-1 ℃, wherein the dropwise adding time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, glue preparation
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring, sequentially adding 7.0g of 2-amino-2-methyl-1-propanol, 0.7g of bactericide CN-46 and 17.5g of silica sol HS-530K at the rotating speed of 600 +/-30 r/min, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to prepare the high-thixotropy flame-retardant water-based transparent nail-free adhesive.
The nail-free glue prepared by the ingredients and the method is white before solidification, has excellent thixotropy, does not flow when standing upside down, and is transparent after solidification.
Example 2
The high-thixotropy flame-retardant water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
preparation of a Pre-emulsion
Adding 105g of deionized water, 10gSR-10 and 3gER-10 emulsifier in sequence into an emulsifying machine, and stirring for 1h until the mixture is uniformly dispersed; mixed monomers (98g of styrene, 168g of butyl acrylate, 14g of acrylic acid, 28g of 4-hydroxybutyl acrylate and 42g of hydroxyethyl methacrylate phosphate) are added dropwise into the emulsifier aqueous solution, and the mixture is stirred for 1 hour until the mixture is uniformly dispersed, so that 468g of pre-emulsion is prepared.
② preparation of seed emulsion
a. 2.0g of ammonium persulfate is dissolved in 10g of deionized water to prepare 12g of initiator aqueous solution;
b. adding 181.3g of deionized water, 2.0g of sodium citrate, 20g of pre-emulsion, 0.5gSR-10 and 0.5gER-10 of emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1h at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dropwise adding 448g of the rest of all pre-emulsion and 8.7g of initiator aqueous solution into the seed emulsion at the temperature of 79 +/-1 ℃, wherein the dropwise adding time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, glue preparation
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring at 600 +/-30 r/min, sequentially adding 7.0g of 2-amino-2-methyl-1-propanol, 0.7g of bactericide CN-46 and 28g of HS-530K, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to obtain the high-thixotropy flame-retardant water-based transparent nail-free adhesive.
The nail-free glue prepared by the ingredients and the method is white before solidification, has excellent thixotropy, does not flow when standing upside down, and is transparent after solidification.
Example 3
The high-thixotropy flame-retardant water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
firstly, preparation of Pre-emulsion
Adding 105g of deionized water, 14.5gSR-10 and 5.5gER-10 emulsifier in sequence into an emulsifying machine, and stirring for 1 hour until the mixture is uniformly dispersed; mixed monomers (98g of styrene, 168g of butyl acrylate, 14g of acrylic acid, 16g of 4-hydroxybutyl acrylate and 28.6g of hydroxyethyl methacrylate phosphate) are added dropwise into the emulsifier aqueous solution, and stirred for 1 hour until the mixture is uniformly dispersed, thereby obtaining 449.6g of pre-emulsion.
② preparation of seed emulsion
a. 2.0g of ammonium persulfate is dissolved in 10g of deionized water to prepare 12g of initiator aqueous solution;
b. adding 200g of deionized water, 2.0g of sodium citrate, 20g of pre-emulsion, 0.5gSR-10 and 0.5gER-10 of emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1h at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dropwise adding 429.6g of the rest total pre-emulsion and 8.7g of the rest initiator aqueous solution into the seed emulsion at the temperature of 79 +/-1 ℃, wherein the dropwise adding time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, glue preparation
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring at 600 +/-30 r/min, sequentially adding 2-amino-2-methyl-1-propanol (14.0 g), a bactericide CN-46 (1.4 g) and 20gHS-530K, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to prepare the high-thixotropy flame-retardant water-based transparent nail-free adhesive.
The nail-free glue prepared by the ingredients and the method is white before solidification, has excellent thixotropy, does not flow when standing upside down, and is transparent after solidification.
Comparative example 1
This comparative example is the case of a nail-free adhesive prepared using a conventional thickening thixotropic agent (fumed silica) and the product obtained is a nontransparent product. It is considered in the industry that the adhesive force of the transparent product is generally lower than that of the non-transparent product, but the product prepared according to the technical scheme provided by the invention, such as the products in the examples 1 and 2, is a transparent product, but the adhesive force of the product can reach or even be better than that of the product in the comparative example 1.
The novel environment-friendly water-based nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
putting the VAE emulsion into a high-speed dispersion power mixer, adding water, chlorinated fatty acid methyl ester, a dispersing agent 5040, a defoaming agent DF-681 and a foam inhibitor DF-814, and stirring for 30min until the mixture is uniformly dispersed.
Adding heavy calcium carbonate, and stirring for 30-50 min until the mixture is uniformly dispersed.
And thirdly, adding fumed silica, and stirring for 40-60 min until the fumed silica is uniformly dispersed to prepare the novel environment-friendly water-based nail-free glue.
Comparative example 2
The comparative example is a compounding system and a preparation method of a solvent type transparent nail-free glue. The transparency of the solvent type nail-free glue is the best transparency of all the nail-free glues, and the nail-free glue prepared by adopting the technical scheme of the invention is a water-based product, does not add an organic solvent and a tackifying emulsion, and achieves the transparency level of the solvent type nail-free glue after being cured.
The preparation method of the transparent nail-free glue comprises the following steps: adding 10 parts of cyclohexane, 2 parts of methylal, 8 parts of ethyl acetate and 10 parts of tetrachloroethylene into a reaction kettle according to the weight part ratio of the formula, adding 25 parts of SEBS, 7 parts of rosin resin, 4 parts of terpene resin and 4 parts of tackifier AT-90X under the stirring state, uniformly stirring, adding 10 parts of transparent powder, BP-186B5 parts of organic bentonite, 2450.7 parts of antioxidant, HP-1361.7 parts and 7700.7 parts of hindered amine light stabilizer, stirring until the materials are completely dissolved, filtering and discharging to obtain the transparent nail-free glue.
Comparative example 3
In comparison to the batch system of the present invention, no silica sol was added to this comparative example.
The flame-retardant water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
preparation of a Pre-emulsion
Adding 105g of deionized water, 3.0gSR-10 and 3.0gER-10 emulsifiers into an emulsifying machine in sequence, and stirring for 1 hour until the mixture is uniformly dispersed; obtaining an emulsifier aqueous solution;
the mixed monomers (110g of styrene, 189g of butyl acrylate, 16g of acrylic acid, 14g of 4-hydroxybutyl acrylate and 28g of hydroxyethyl methacrylate phosphate) are added dropwise into the aqueous solution of the emulsifier and stirred for 1 hour until the mixture is uniformly dispersed, thus obtaining the pre-emulsion.
② preparation of seed emulsion
a. Dissolving 1.40g of ammonium persulfate in 10g of deionized water to prepare an initiator aqueous solution;
b. adding 200g of deionized water, 1.40g of sodium citrate, 20g of pre-emulsion, 0.5gSR-10 and 0.5gER-10 of emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1 hour at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dripping all the residual pre-emulsion and the initiator aqueous solution into the seed emulsion at the temperature of 83 +/-2 ℃, wherein the dripping time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, glue preparation
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring at 600 +/-30 r/min, sequentially adding 7.0g of 2-amino-2-methyl-1-propanol and 0.7g of bactericide CN-46, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to obtain the flame-retardant water-based transparent nail-free adhesive.
Comparative example 4
In comparison with the compounding system of the present invention, no functional monomer was added in this comparative example.
The flame-retardant water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
preparation of a Pre-emulsion
Adding 105g of deionized water, 3.0gSR-10 and 3.0gER-10 emulsifier in sequence into an emulsifying machine, and stirring for 1h until the mixture is uniformly dispersed; the mixed monomer (110g of styrene, 189g of butyl acrylate, 16g of acrylic acid and 28g of hydroxyethyl methacrylate phosphate) is added dropwise into the emulsifier aqueous solution, and the mixture is stirred for 1 hour until the mixture is uniformly dispersed, so that the pre-emulsion is prepared.
② preparation of seed emulsion
a. Dissolving 1.40g of ammonium persulfate in 10g of deionized water to prepare an initiator aqueous solution;
b. adding 200g of deionized water, 1.40g of sodium citrate, 20g of pre-emulsion, 0.5gSR-10 and 0.5gER-10 of emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1h at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dripping all the residual pre-emulsion and the initiator aqueous solution into the seed emulsion at the temperature of 79 +/-1 ℃, wherein the dripping time is 4.0 +/-0.5 h; after the dropwise addition is finished, the reaction is carried out for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, glue preparation
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring at 600 +/-30 r/min, sequentially adding 7.0g of 2-amino-2-methyl-1-propanol, 0.7g of bactericide CN-46 and 17.5g of HS-530K, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to obtain the flame-retardant water-based transparent nail-free adhesive.
Comparative example 5
In this comparative example, no flame retardant monomer was used, as compared to the compounding system of the present invention.
The high thixotropic water-based transparent nail-free glue comprises the following components in percentage by weight:
the preparation method comprises the following steps:
preparation of a Pre-emulsion
Adding 105g of deionized water, 3.0gSR-10 and 3.0gER-10 emulsifier in sequence into an emulsifying machine, and stirring for 1 hour until the mixture is uniformly dispersed; the mixed monomers (110g of styrene, 189g of butyl acrylate, 16g of acrylic acid and 14g of 4-hydroxybutyl acrylate) are added dropwise to the aqueous emulsifier solution and stirred for 1h until the mixture is uniformly dispersed, thus obtaining the pre-emulsion.
② preparation of seed emulsion
a. Dissolving 1.40g of ammonium persulfate in 10g of deionized water to prepare an initiator aqueous solution;
b. adding 200g of deionized water, 1.40g of sodium citrate, 20g of pre-emulsion, 0.5gSR-10 and 0.5gER-10 of emulsifier into a reaction kettle in sequence, stirring and heating to 78 ℃; adding 3.3g of initiator aqueous solution into the reaction kettle, and carrying out heat preservation reaction for 1h at the temperature of 79 +/-1 ℃ to obtain the seed emulsion showing blue light.
Preparation of aqueous base stock
Simultaneously dripping all the residual pre-emulsion and the initiator aqueous solution into the seed emulsion at the temperature of 79 +/-1 ℃, wherein the dripping time is 3.5-4.0 h; after the dropwise addition is finished, the reaction is carried out for 2 hours at the temperature of 83 +/-2 ℃ to obtain the aqueous base material.
Fourthly, preparing the glue
Putting the water-based base material into a high-speed dispersion power mixer, starting stirring at 600r/min +/-30 r/min, sequentially adding 7.0g of 2-amino-2-methyl-1-propanol, 0.7g of bactericide CN-46 and 17.5g of HS-530K, and dispersing for 15 +/-2 min until the materials are uniformly dispersed to obtain the high-thixotropy water-based transparent nail-free adhesive.
The relative performance of the nail-free glues of examples 1-3 and comparative examples 1-5 was tested using the following method:
test of tensile shear Strength
And testing according to a method for testing the tensile shear strength of 24h and 168h in standard nail-free glue for indoor wall surface light decorative plates JC/T2186-2013.
② thixotropic ability
The thixotropic capacity of the nail-free glue is measured by taking the sag as an index, and the detection method is tested according to a sag test method in standard nail-free glue for indoor wall surface light decorative plates JC/T2186-2013.
Flame retardant ability
The glass rod was inserted into the gel to a depth of 10mm, and then taken out and cured at room temperature for 7 days. After the glue had solidified, the alcohol lamp was lit for 3s, the lamp was removed and the duration of the open flame on the sample after removal of the lamp was measured with a stopwatch with a minimum graduation of 0.1 s. And evaluating the flame retardant capability of the cured glue solution by taking the duration of the open flame as an index. The test method refers to HG/T3659-2020 Chlorella adhesive for quick bonding conveyer belt.
Fourthly, transparency
Comparative nail-free glue clarity tests for examples 1-3 and comparative examples 1-2 were conducted as follows:
the transparent PVC plastic (50 mm. times.50 mm. times.2 mm) was bonded with the appropriate amounts of examples 1-3 and comparative examples 1-2. And curing the sample for 48 hours at room temperature, and comparing the transparencies of different samples.
The results of the performance tests on the nail-free adhesives obtained in examples 1 to 3 and comparative examples 1 to 5 are shown in Table 1.
TABLE 1 test results of examples and comparative examples
From the detection results, it can be seen that:
comparison of tensile shear strengths:
the conclusion obtained from the test results of the shear strength of 24h and 168h is that the tensile shear strength of the nail-free glue obtained by applying the technical scheme of the invention can reach or even be superior to that of the nail-free glue in the comparative example.
② comparison result of thixotropic ability:
comparative examples 1, 2, 3 and 5 show the sag of the nail-free glue prepared by using the functional monomer 4-hydroxy butyl acrylate and silica sol HS-530K, and the performance test results are 0.5mm, 0.4mm and 0.5 mm; comparative example 3 with the addition of a functional monomer and without the addition of silica sol data 5.2mm, and comparative example 4 with the addition of silica sol and without the addition of a functional monomer data 7.2 mm.
Therefore, when only the functional monomer 4-hydroxybutyl acrylate is matched with the silica sol HS-530K for use, the sag of the glue solution is smaller, and the glue solution has better thixotropy.
③ the comparison result of flame retardant ability:
the open flame duration data shows that: in comparative example 1, example 2, example 3, comparative example 3 and comparative example 4, the flame-retardant monomer hydroxyethyl methacrylate phosphate is used for polymerization, and the obtained nail-free glue has excellent flame retardant capability; the hydroxyethyl methacrylate phosphate which is not used as a flame retardant monomer in comparative example 5 participates in polymerization and has no flame retardant ability.
Comparison result of transparency:
the transparency of the nail-free glue prepared in the embodiments 1, 2 and 3 of the invention can reach the level of the solvent type transparent nail-free glue in the comparative example 2.
The data in Table 1 show that the high-thixotropy flame-retardant water-based transparent nail-free glue obtained by the invention has high bonding strength, meets the related index requirements in the standard JC/T2186-2013, has extremely high transparency and good flame retardance, and is obviously superior to the products in the prior art.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. The high-thixotropy flame-retardant water-based transparent nail-free glue is characterized by comprising the following components in percentage by mass:
2. the highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the reaction monomer is a mixture of styrene, butyl acrylate and acrylic acid, wherein the mass percentage ratio of the styrene to the butyl acrylate to the acrylic acid is 34-40: 50-61: 2-5.5.
3. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the functional monomer is 4-hydroxy butyl acrylate.
4. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the flame-retardant monomer is hydroxyethyl methacrylate phosphate.
5. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the composite emulsifier is a mixture of SR-10 and ER-10, and the mass fraction ratio of SR-10 to ER-10 is 1-4: 1.
6. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the pH regulator is 2-amino-2-methyl-1-propanol.
7. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the antibacterial agent is CN-46.
8. The highly thixotropic flame retardant water-based transparent nail-free adhesive according to claim 1, which is characterized in that: the silica sol is a dispersion liquid with the mass fraction of 28-32% of silica, the pH value of the silica sol is 9.0-11.0, and the average particle size of the silica in the silica sol is 3-5 nm.
9. The preparation method of the high thixotropic flame retardant water-based transparent nail-free glue according to any one of claims 1 to 8, which is characterized by comprising the following specific steps:
preparation of pre-emulsion:
adding a composite emulsifier and deionized water into an emulsifying machine, and stirring for 1h until the mixture is dispersed to prepare an emulsifier aqueous solution with the mass percentage concentration of 5-16%; dropwise adding a reaction monomer, a functional monomer and a flame-retardant monomer into the emulsifier aqueous solution, and stirring for 1h until the mixture is uniformly dispersed to obtain a pre-emulsion;
preparing a seed emulsion:
dissolving ammonium persulfate in deionized water to prepare an initiator aqueous solution with the mass percentage concentration of 12-17%; according to the weight ratio of sodium citrate: pre-emulsion: emulsifier: deionized water is 1.4-2: 20: 1: 181-200, stirring and heating to 78 ℃; adding an aqueous initiator solution to the reaction kettle when the temperature rises to 78 ℃, wherein the ratio of the aqueous initiator solution: the mass ratio of the sodium citrate is 3.3: 1.3-2.1; reacting for 1h at the temperature of 79 +/-1 ℃ to obtain seed emulsion;
preparing the water-based base material:
at the temperature of 79 +/-1 ℃, dropwise adding the pre-emulsion and the initiator aqueous solution into the seed emulsion again, wherein the dropwise adding of the pre-emulsion and the initiator aqueous solution is carried out simultaneously, wherein the initiator aqueous solution: pre-emulsion: the mass ratio of the sodium citrate is 8.0-9.0: 446-450: 1.3-2.1, wherein the dripping time is 4.0 +/-0.5 h; after the dropwise addition is finished, heating and raising the temperature, and carrying out heat preservation reaction for 1-2 h at the temperature of 83 +/-2 ℃ to obtain a water-based base material;
fourthly, preparing glue:
and (3) putting the water-based base material into a high-speed dispersion power mixer, sequentially adding the pH regulator, the bactericide and the silica sol at the rotating speed of 600 +/-30 r/min, and stirring for 15 +/-2 min until the materials are uniformly dispersed to prepare the high-thixotropy flame-retardant water-based transparent nail-free adhesive.
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| DE10343675A1 (en) * | 2003-09-18 | 2005-04-14 | Bayer Materialscience Ag | Aqueous adhesive dispersions |
| CN102391800A (en) * | 2011-09-13 | 2012-03-28 | 北京高盟新材料股份有限公司 | Water-based flame-retardant acrylate pressure sensitive adhesive and preparation method thereof |
| KR101683739B1 (en) * | 2016-09-20 | 2016-12-07 | 주식회사 코스펙스 | An emulsion adhesive composition for manufacturing polystyrene foam and the making method thereof |
| CN111040684A (en) * | 2019-12-28 | 2020-04-21 | 太仓运通新材料科技有限公司 | Preparation method of flame-retardant modified acrylate pressure-sensitive adhesive |
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- 2022-03-16 CN CN202210257079.0A patent/CN114525092A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10343675A1 (en) * | 2003-09-18 | 2005-04-14 | Bayer Materialscience Ag | Aqueous adhesive dispersions |
| CN102391800A (en) * | 2011-09-13 | 2012-03-28 | 北京高盟新材料股份有限公司 | Water-based flame-retardant acrylate pressure sensitive adhesive and preparation method thereof |
| KR101683739B1 (en) * | 2016-09-20 | 2016-12-07 | 주식회사 코스펙스 | An emulsion adhesive composition for manufacturing polystyrene foam and the making method thereof |
| CN111040684A (en) * | 2019-12-28 | 2020-04-21 | 太仓运通新材料科技有限公司 | Preparation method of flame-retardant modified acrylate pressure-sensitive adhesive |
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