CN101864024A - Polyacrylic ester coating adhesive emulsion and preparation method thereof - Google Patents
Polyacrylic ester coating adhesive emulsion and preparation method thereof Download PDFInfo
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- CN101864024A CN101864024A CN 201010202309 CN201010202309A CN101864024A CN 101864024 A CN101864024 A CN 101864024A CN 201010202309 CN201010202309 CN 201010202309 CN 201010202309 A CN201010202309 A CN 201010202309A CN 101864024 A CN101864024 A CN 101864024A
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- monomer
- coating adhesive
- polyacrylic ester
- adhesive emulsion
- emulsion
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- 239000000839 emulsion Substances 0.000 title claims abstract description 67
- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 238000000576 coating method Methods 0.000 title claims abstract description 53
- 239000000853 adhesive Substances 0.000 title claims abstract description 41
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 41
- 150000002148 esters Chemical class 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000004945 emulsification Methods 0.000 title description 8
- 239000000178 monomer Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000004132 cross linking Methods 0.000 claims abstract description 30
- 239000003999 initiator Substances 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 10
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 9
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 4
- -1 alkyl methacrylate Chemical compound 0.000 claims description 30
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 8
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 6
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 6
- 125000005250 alkyl acrylate group Chemical group 0.000 claims description 5
- 125000000746 allylic group Chemical group 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- 239000012966 redox initiator Substances 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- ROLAGNYPWIVYTG-UHFFFAOYSA-N 1,2-bis(4-methoxyphenyl)ethanamine;hydrochloride Chemical compound Cl.C1=CC(OC)=CC=C1CC(N)C1=CC=C(OC)C=C1 ROLAGNYPWIVYTG-UHFFFAOYSA-N 0.000 claims description 2
- XUIKGJQOQAHGQE-UHFFFAOYSA-N CC(=CC)[Na] Chemical compound CC(=CC)[Na] XUIKGJQOQAHGQE-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920006387 Vinylite Polymers 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 claims description 2
- GYDSPAVLTMAXHT-UHFFFAOYSA-N pentyl 2-methylprop-2-enoate Chemical compound CCCCCOC(=O)C(C)=C GYDSPAVLTMAXHT-UHFFFAOYSA-N 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 159000000000 sodium salts Chemical class 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 36
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 abstract 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 abstract 1
- 125000005907 alkyl ester group Chemical group 0.000 abstract 1
- 239000011976 maleic acid Substances 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 20
- 239000000126 substance Substances 0.000 description 16
- 235000019395 ammonium persulphate Nutrition 0.000 description 11
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical class [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 10
- 238000007599 discharging Methods 0.000 description 10
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 10
- 239000002245 particle Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 description 1
- 239000004160 Ammonium persulphate Substances 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004159 Potassium persulphate Substances 0.000 description 1
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a polyacrylic ester coating adhesive emulsion, which is prepared from the following raw materials by weight percent: 20-50% of soft monomer, 5-20% of hard monomer, 0.5-2.0% of monomer containing carboxyl group, 1-5% of crosslinking monomer, 1-5% of emulsifier, 0.2-0.7% of initiator and the balance of deionized water, wherein the soft monomer is crylic acid alkyl ester; the hard monomer is one or two of methylpropenoic acid alkyl ester and styrene; the monomer containing carboxyl group is one or more of methacrylic acid, itaconic acid and maleic acid; and the corsslinking monomer is one or two of non-formaldehyde crosslinking monomer and inner crosslinking monomer containing two or more double bonds. The emulsion has good safety, no toxicity, low cost, high hydraulic pressure resistance, wide application range and the content of the formaldehyde of the coating accords with the European Union exit criteria. The invention also discloses a preparation method of the polyacrylic ester coating adhesive emulsion, which is simple to operate and is suitable for industrialized production.
Description
Technical field
The present invention relates to weaving and use the fine chemicals field, be specifically related to a kind of polyacrylic ester coating adhesive emulsion and preparation method thereof.
Background technology
The high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type system is based on the high-molecular copolymer of acrylate, and it can be widely used in needs high water pressure resistance and the strict fabric coating of formaldehyde content control.Early stage coating adhesive is the solvent-type acrylic ester copolymer, be with benzene-like compounds as solvent, toxicity is big, inflammable and cost is high, not environmental protection.Developed into the water soluble acrylic acid ester copolymer emulsion afterwards gradually, but its linking agent is many based on N hydroxymethyl acrylamide, in cross-linking process, can produce the formaldehyde material, cause the content of formaldehyde in the acrylate copolymer emulsion that makes higher, human body is produced harm, thereby the outlet of such coating prod is subjected to very big restriction.In recent years domestic-developed some water soluble acrylic acid ester coating adhesive emulsion liquid, its composition mainly is main monomer with the butyl acrylate, common methacrylic compounds is a function monomer; Meet the requirements though such water soluble acrylic acid ester coating adhesive emulsion pendular ring is protected, coating adhesion is poor, water-fast forcing down.
In addition, existing aqueous polyurethane emulsion mainly is to be made by raw material reaction such as polyether glycol (or polyester polyol) and isocyanic ester, chainextender dimethylol propionic acid, though its coating water pressure resistance height, raw materials cost is high a lot of than water-and acrylate, the sexual valence ratio.Therefore, develop a kind of low cost again the polyacrylic ester coating adhesive emulsion of the high hydraulic pressure of ability extensive market prospects will be arranged.
Summary of the invention
The invention provides the high water pressure resistance polyacrylic ester coating adhesive emulsion of a kind of environment-friendly type, its security is good, and is nontoxic, cost is low, can select comonomer and ratio according to different fabric materials and processing requirements, reach the feel and the water pressure resistance index that need, the cost performance height.
The present invention also provides a kind of preparation method of polyacrylic ester coating adhesive emulsion, and this method is easy and simple to handle, is suitable for suitability for industrialized production.
A kind of polyacrylic ester coating adhesive emulsion, make by following raw materials by weight percent:
Soft monomer 20%～50%
Hard monomer 5%～20%
Contain carboxylic monomer 0.5%～2.0%
Cross-linking monomer 1%～5%
Emulsifying agent 1%～5%
Initiator 0.2%～0.7%
The deionized water surplus.
Wherein, described soft monomer is an alkyl acrylate;
Described hard monomer is selected from one or both in alkyl methacrylate, the vinylbenzene;
The described carboxylic monomer that contains is selected from methacrylic acid, methylene-succinic acid, the toxilic acid one or more;
Described cross-linking monomer is selected from no aldehyde cross-linking monomer, have in the interior cross-linking monomer of two or more pairs key one or both.
As preferably:
Described polyacrylic ester coating adhesive emulsion, make by following raw materials by weight percent:
Soft monomer 25%～35%
Hard monomer 5%～15%
Contain carboxylic monomer 0.5%～1.5%
Cross-linking monomer 1.5%～3.5%
Emulsifying agent 1%～5%
Initiator 0.2%～0.7%
The deionized water surplus.
Wherein, described soft monomer is an alkyl acrylate; Described alkyl acrylate is selected from one or more in ethyl propenoate, butyl acrylate, the ethyl acrylate, further preferred butyl acrylate.
Described hard monomer is selected from one or both in alkyl methacrylate, the vinylbenzene; Described alkyl methacrylate is selected from one or more in methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, methacrylic acid pentyl ester, the N-Hexyl methacrylate, further the preferable methyl methyl acrylate.
The described carboxylic monomer that contains is selected from methacrylic acid, methylene-succinic acid, the toxilic acid one or more.
Described cross-linking monomer is selected from no aldehyde cross-linking monomer, have in the interior cross-linking monomer of two or more pairs key one or both; Described no aldehyde cross-linking monomer is selected from one or more in diacetone-acryloamide(DAA), double bond containing urea heterocyclic compound, the hydroxyl-products such as Vinylite derivative; Such no aldehyde cross-linking monomer does not have free formaldehyde, can make to meet international environmental protection standard, and the polyacrylic ester coating adhesive emulsion that coating adhesion is good, water pressure resistance is high; Wherein, the molecular formula of described double bond containing urea heterocyclic compound is: (HC=COOCH
2CH
2-NCH
2CH
2-NHC=O)
2, can select the commercially available prod for use, the V-100M that produces as the loyal chemical company in Shanghai etc.; Described interior cross-linking monomer with two or more pairs key is selected from one or more in Phthalic acid, diallyl ester, diallyl isophthalate, the phthalic acid ethylene glycol bisthioglycolate allyl ester etc.; The interior cross-linking monomer that introducing has two or more pairs key helps improving the molecular weight of polymkeric substance.
Described initiator is selected from persulphate or persulphate-hydrosulphite redox initiation system, can select in ammonium persulphate, Potassium Persulphate, Sodium Persulfate or the ammonium persulfate-sodium bisulfite redox initiation system one or more for use; Further initiator system of ammonium persulfate-sodium bisulfite redox initiation system.Adopt such initiator, the polyreaction gentleness, the molecular weight distribution that obtains is even.
Described emulsifying agent is selected from one or more in ethoxylated alkyl ether ammonium sulfate (as CO-436, the loyal chemical company in Shanghai), the reactive emulsifier, the mixture of further preferred ethoxylated alkyl ether ammonium sulfate and reactive emulsifier; Wherein, described reactive emulsifier is selected for use and is contained allylic alkyl sulfo-succinic acid dibasic acid esters sodium salt (as M-10S, the loyal chemical company in Shanghai), methylpropenyl sodium sulfonate, double bond containing alcohol ether sulfo-succinic acid ester sodium salt are (as NRS-138, the loyal chemical company in Shanghai) one or more in, such emulsifying agent can improve the water tolerance of coating.
Raw material of the present invention all can be selected the commercially available prod for use.
The preparation method of described polyacrylic ester coating adhesive emulsion comprises the steps:
(1) with whole soft monomers, hard monomer, to contain carboxylic monomer, cross-linking monomer, emulsifying agent and consumption be that the deionized water of deionized water gross weight 40%～45% mixes, and makes pre-emulsion;
(2) be that the deionized water of deionized water gross weight 40%～45% and pre-emulsion that consumption is above-mentioned pre-emulsion gross weight 3%～10% mix as seed liquor with consumption, after being warming up to 60 ℃～85 ℃, adding consumption is the initiator of initiator gross weight 5%～25%, react the initiator solution that adds remaining pre-emulsion after 5 minutes～30 minutes continuously and make by the initiator and the remaining deionized water of remainder, be controlled at and added in 2 hours～6 hours, add back insulation 1 hour～2 hours, be cooled to below 40 ℃, obtain polyacrylic ester coating adhesive emulsion after filtration.
The high water pressure resistance polyacrylic ester coating adhesive emulsion of described environment-friendly type can be widely used in needs high water pressure resistance and the strict fabric coating of formaldehyde content control.
The present invention has following advantage:
The high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of the present invention, security is good, nontoxic, cost is low, can select comonomer and ratio according to different fabric materials and processing requirements, reach the water pressure resistance index and the fabric feeling that need, can be widely used in umbrella cloth, tent, clothes overcoat lining paint coating, the coating formaldehyde content is extremely low, and one water pressure resistance of coating can reach 1000mmH
2More than the O.
The preparation method of polyacrylic ester coating adhesive emulsion of the present invention is simple to operate, need not special equipment, and the reaction be easy to control, be applicable to suitability for industrialized production.
Embodiment
Embodiment 1
Having agitator, in the reactor of reflux exchanger and thermometer, add 15.0 kilograms of deionized waters earlier, add 0.3 kilogram of ethoxylated alkyl ether ammonium sulfate (CO-436 again, the loyal chemical company in Shanghai produces), 1.3 kilograms of methylpropenyl sodium sulfonates, 0.83 kilogram of methacrylic acid, double bond containing urea heterocyclic compound (V-100M, the loyal chemical company in Shanghai produces) 0.2 kilogram of 1.31 kilograms and interior cross-linking monomer Phthalic acid, diallyl ester, mix the back and add 20.0 kilograms of butyl acrylates, 3.5 kilograms of 3.5 kilograms of methyl methacrylates and vinylbenzene, emulsification after 1 hour discharging as pre-emulsion.
In empty still, add 15.0 kilograms of deionized waters and 1.6 kilograms of above-mentioned pre-emulsions as seed liquor, be warming up to 80 ℃, add 32 gram ammonium persulphates and 28 gram sodium bisulfites, reacted 15 minutes, do not have till the backflow, slowly drip the above-mentioned pre-emulsion of residue again, be controlled at and dripped off in 3 hours, drip respectively simultaneously: add 2.5 kilograms of deionized waters and add the initiator solution that 2.5 kilograms of deionized waters are formed by 112 gram sodium bisulfites by 128 gram ammonium persulphates, be controlled at and dripped off in 3 hours, drip back insulation 2 hours, be cooled to below 40 ℃, filter discharging, obtaining solid content is 42.5% (weight percent), particle diameter is about 180nm, the high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of band blue light.
This polyacrylic ester coating adhesive emulsion one coat water pressure resistance reaches 1050mmH
2O, formaldehyde content is less than 10ppm.
Embodiment 2
Having agitator, in the reactor of reflux exchanger and thermometer, add 15.0 kilograms of deionized waters earlier, add 0.3 kilogram of ethoxylated alkyl ether ammonium sulfate (CO-436 again, the loyal chemical company in Shanghai produces), 1.3 kilograms of methylpropenyl sodium sulfonates, 0.83 kilogram of methacrylic acid, double bond containing urea heterocyclic compound (V-100M, the loyal chemical company in Shanghai produces) 0.3 kilogram of 1.5 kilograms and interior cross-linking monomer Phthalic acid, diallyl ester, mix the back and add 20.0 kilograms of butyl acrylates, 3.5 kilograms of 3.5 kilograms of methyl methacrylates and vinylbenzene, emulsification after 1 hour discharging as pre-emulsion.
In empty still, add 15.0 kilograms of deionized waters and 1.6 kilograms of above-mentioned pre-emulsions as seed liquor, be warming up to 80 ℃, add 32 gram ammonium persulphates and 28 gram sodium bisulfites, reacted 15 minutes, do not have till the backflow, slowly drip the above-mentioned pre-emulsion of residue again, be controlled at and dripped off in 3 hours, drip simultaneously respectively simultaneously: add 2.5 kilograms of deionized waters and add the initiator solution that 2.5 kilograms of deionized waters are formed by 112 gram sodium bisulfites by 128 gram ammonium persulphates, be controlled at and dripped off in 3 hours, drip back insulation 2 hours, be cooled to below 40 ℃, filter discharging, obtaining solid content is 42.0% (weight percent), particle diameter is about 180nm, the high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of band blue light.
This polyacrylic ester coating adhesive emulsion one coat water pressure resistance reaches 1250mmH
2O, formaldehyde content is less than 10ppm.
Embodiment 3
Having agitator, in the reactor of reflux exchanger and thermometer, add 15.0 kilograms of deionized waters earlier, add 0.3 kilogram of ethoxylated alkyl ether ammonium sulfate (CO-436 again, the loyal chemical company in Shanghai produces), contain allylic alkyl sulfo-succinic acid dibasic acid esters sodium salt (M-10S, the production of the loyal chemical company in Shanghai) 1.3 kilograms, 0.83 kilogram of methacrylic acid, 0.2 kilogram of 1.5 kilograms of diacetone-acryloamide(DAA)s and interior cross-linking monomer Phthalic acid, diallyl ester, mix the back and add 20.0 kilograms of butyl acrylates, 3.5 kilograms of 3.5 kilograms of methyl methacrylates and vinylbenzene, emulsification after 1 hour discharging as pre-emulsion.
In empty still, add 15.0 kilograms of deionized waters and 1.6 kilograms of above-mentioned pre-emulsions as seed liquor, be warming up to 80 ℃, add 32 gram ammonium persulphates and 28 gram sodium bisulfites, reacted 15 minutes, do not have till the backflow, slowly drip the above-mentioned pre-emulsion of residue again, be controlled at and dripped off in 3 hours, drip simultaneously respectively simultaneously: add 2.5 kilograms of deionized waters and add the initiator solution that 2.5 kilograms of deionized waters are formed by 112 gram sodium bisulfites by 128 gram ammonium persulphates, be controlled at and dripped off in 3 hours, drip back insulation 2 hours, be cooled to below 40 ℃, filter discharging, obtaining solid content is 42.5% (weight percent), particle diameter is about 180nm, the high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of band blue light.
This polyacrylic ester coating adhesive emulsion one coat water pressure resistance reaches 1010mmH
2O, formaldehyde content is less than 10ppm.
Embodiment 4
Having agitator, in the reactor of reflux exchanger and thermometer, add 15.0 kilograms of deionized waters earlier, add 0.5 kilogram of ethoxylated alkyl ether ammonium sulfate (CO-436 again, the loyal chemical company in Shanghai produces), 1.0 kilograms of methylpropenyl sodium sulfonates, 0.83 kilogram of methacrylic acid, double bond containing urea heterocyclic compound (V-100M, the loyal chemical company in Shanghai produces) 0.2 kilogram of 1.31 kilograms and interior cross-linking monomer Phthalic acid, diallyl ester, mix the back and add 18.0 kilograms of butyl acrylates, 4.5 kilograms of 4.5 kilograms of methyl methacrylates and vinylbenzene, emulsification after 1 hour discharging as pre-emulsion.
In empty still, add 15.0 kilograms of deionized waters and 1.6 kilograms of above-mentioned pre-emulsions as seed liquor, be warming up to 80 ℃, add 32 gram ammonium persulphates and 28 gram sodium bisulfites, reacted 15 minutes, do not have till the backflow, slowly drip the above-mentioned pre-emulsion of residue again, be controlled at and dripped off in 3 hours, drip respectively simultaneously: add 2.5 kilograms of deionized waters and add the initiator solution that 2.5 kilograms of deionized waters are formed by 112 gram sodium bisulfites by 128 gram ammonium persulphates, be controlled at and dripped off in 3 hours, drip back insulation 2 hours, be cooled to below 40 ℃, filter discharging, obtaining solid content is 42.5% (weight percent), particle diameter is about 150nm, the high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of band blue light.
This polyacrylic ester coating adhesive emulsion one coat water pressure resistance reaches 1150mmH
2O, formaldehyde content is less than 10ppm.
Embodiment 5
Having agitator, in the reactor of reflux exchanger and thermometer, add 15.0 kilograms of deionized waters earlier, add 0.5 kilogram of ethoxylated alkyl ether ammonium sulfate (CO-436 again, the loyal chemical company in Shanghai produces), contain allylic alkyl sulfo-succinic acid dibasic acid esters sodium salt (M-10S, the production of the loyal chemical company in Shanghai) 1.3 kilograms, 0.6 kilogram of methylene-succinic acid, double bond containing urea heterocyclic compound (V-100M, the loyal chemical company in Shanghai produces) 0.2 kilogram of 1.31 kilograms and interior cross-linking monomer Phthalic acid, diallyl ester, mix the back and add 18.0 kilograms of butyl acrylates, 4.5 kilograms of 4.5 kilograms of methyl methacrylates and vinylbenzene, emulsification after 1 hour discharging as pre-emulsion.
In empty still, add 15.0 kilograms of deionized waters and 1.6 kilograms of above-mentioned pre-emulsions as seed liquor, be warming up to 80 ℃, add 32 gram ammonium persulphates and 28 gram sodium bisulfites, reacted 15 minutes, do not have till the backflow, slowly drip the above-mentioned pre-emulsion of residue again, be controlled at and dripped off in 3 hours, drip respectively simultaneously: add 2.5 kilograms of deionized waters and add the initiator solution that 2.5 kilograms of deionized waters are formed by 112 gram sodium bisulfites by 128 gram ammonium persulphates, be controlled at and dripped off in 3 hours, drip back insulation 2 hours, be cooled to below 40 ℃, filter discharging, obtaining solid content is 42.5% (weight percent), particle diameter is about 150nm, the high water pressure resistance polyacrylic ester coating adhesive emulsion of environment-friendly type of band blue light.
This polyacrylic ester coating adhesive emulsion one coat water pressure resistance reaches 1150mmH
2O, formaldehyde content is less than 10ppm.
Claims (10)
1. polyacrylic ester coating adhesive emulsion, make by following raw materials by weight percent:
Soft monomer 20%～50%
Hard monomer 5%～20%
Contain carboxylic monomer 0.5%～2.0%
Cross-linking monomer 1%～5%
Emulsifying agent 1%～5%
Initiator O.2%～0.7%
The deionized water surplus;
Wherein, described soft monomer is an alkyl acrylate;
Described hard monomer is selected from one or both in alkyl methacrylate, the vinylbenzene;
The described carboxylic monomer that contains is selected from methacrylic acid, methylene-succinic acid, the toxilic acid one or more;
Described cross-linking monomer is selected from no aldehyde cross-linking monomer, have in the interior cross-linking monomer of two or more pairs key one or both.
2. polyacrylic ester coating adhesive emulsion according to claim 1 is characterized in that, is made by following raw materials by weight percent:
Soft monomer 25%～35%
Hard monomer 5%～15%
Contain carboxylic monomer 0.5%～1.5%
Cross-linking monomer 1.5%～3.5%
Emulsifying agent 1%～5%
Initiator 0.2%～0.7%
The deionized water surplus.
3. polyacrylic ester coating adhesive emulsion according to claim 1 is characterized in that described alkyl acrylate is selected from one or more in ethyl propenoate, butyl acrylate, the ethyl acrylate.
4. polyacrylic ester coating adhesive emulsion according to claim 1, it is characterized in that described alkyl methacrylate is selected from one or more in methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, methacrylic acid pentyl ester, the N-Hexyl methacrylate.
5. polyacrylic ester coating adhesive emulsion according to claim 1 is characterized in that, described no aldehyde cross-linking monomer is selected from one or more in diacetone-acryloamide(DAA), double bond containing urea heterocyclic compound, the hydroxyl-Vinylite derivative;
Wherein, the molecular formula of described double bond containing urea heterocyclic compound is: (HC=COOCH
2CH
2-NCH
2CH
2-NHC=O)
2
6. polyacrylic ester coating adhesive emulsion according to claim 1, it is characterized in that described interior cross-linking monomer with two or more pairs key is selected from one or more in Phthalic acid, diallyl ester, diallyl isophthalate, the phthalic acid ethylene glycol bisthioglycolate allyl ester.
7. polyacrylic ester coating adhesive emulsion according to claim 1 is characterized in that, described initiator is selected from persulphate or persulphate-hydrosulphite redox initiation system.
8. polyacrylic ester coating adhesive emulsion according to claim 1 is characterized in that described emulsifying agent is selected from one or more in ethoxylated alkyl ether ammonium sulfate, the reactive emulsifier;
Wherein, described reactive emulsifier is selected for use and is contained allylic alkyl sulfo-succinic acid dibasic acid esters sodium salt, methylpropenyl sodium sulfonate, contains in allylic ether alcohol sulfate or the double bond containing alcohol ether sulfo-succinic acid ester sodium salt one or more.
9. according to the preparation method of each described polyacrylic ester coating adhesive emulsion of claim 1～8, comprise the steps:
(1) with whole soft monomers, hard monomer, to contain carboxylic monomer, cross-linking monomer, emulsifying agent and consumption be that the deionized water of deionized water gross weight 40%～45% mixes, and makes pre-emulsion;
(2) be that the deionized water of deionized water gross weight 40%～45% and pre-emulsion that consumption is above-mentioned pre-emulsion gross weight 3%～10% mix as seed liquor with consumption, after being warming up to 60 ℃～85 ℃, adding consumption is the initiator of initiator gross weight 5%～25%, react the initiator solution that adds remaining pre-emulsion after 5 minutes～30 minutes continuously and make by the initiator and the remaining deionized water of remainder, be controlled at and added in 2 hours～6 hours, add back insulation 1 hour～2 hours, be cooled to below 40 ℃, obtain polyacrylic ester coating adhesive emulsion after filtration.
10. according to the application of each described polyacrylic ester coating adhesive emulsion of claim 1～8 in the preparation fabric coating.
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