CN1654577A - High strong adhesive and method for preparing same - Google Patents
High strong adhesive and method for preparing same Download PDFInfo
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- CN1654577A CN1654577A CN 200510032745 CN200510032745A CN1654577A CN 1654577 A CN1654577 A CN 1654577A CN 200510032745 CN200510032745 CN 200510032745 CN 200510032745 A CN200510032745 A CN 200510032745A CN 1654577 A CN1654577 A CN 1654577A
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- tackiness agent
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 12
- 239000000853 adhesive Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title description 4
- 229920001084 poly(chloroprene) Polymers 0.000 claims abstract description 42
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 31
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 38
- 238000002156 mixing Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 25
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000003112 inhibitor Substances 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- 230000008719 thickening Effects 0.000 claims description 16
- 239000000945 filler Substances 0.000 claims description 14
- 239000013008 thixotropic agent Substances 0.000 claims description 14
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 13
- 239000003502 gasoline Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 claims description 8
- 238000012856 packing Methods 0.000 claims description 8
- 238000005502 peroxidation Methods 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- RNYJXPUAFDFIQJ-UHFFFAOYSA-N hydron;octadecan-1-amine;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[NH3+] RNYJXPUAFDFIQJ-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 244000043261 Hevea brasiliensis Species 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 229920003052 natural elastomer Polymers 0.000 claims description 4
- 229920001194 natural rubber Polymers 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 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 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- CUOZYXPNIFEQTK-UHFFFAOYSA-N benzenesulfonic acid;formaldehyde Chemical compound O=C.OS(=O)(=O)C1=CC=CC=C1 CUOZYXPNIFEQTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000007859 condensation product Substances 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 159000000000 sodium salts Chemical class 0.000 claims description 3
- 150000003505 terpenes Chemical class 0.000 claims description 3
- 235000007586 terpenes Nutrition 0.000 claims description 3
- 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 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- UBUCNCOMADRQHX-UHFFFAOYSA-N N-Nitrosodiphenylamine Chemical compound C=1C=CC=CC=1N(N=O)C1=CC=CC=C1 UBUCNCOMADRQHX-UHFFFAOYSA-N 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical group O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- NWHVZAGJLOWTDI-UHFFFAOYSA-N C1=CC(=CC=C1O)C.[N+](=O)([O-])C1=CC=CC(=C1)[N+](=O)[O-] Chemical compound C1=CC(=CC=C1O)C.[N+](=O)([O-])C1=CC=CC(=C1)[N+](=O)[O-] NWHVZAGJLOWTDI-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 5
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- 239000002318 adhesion promoter Substances 0.000 abstract 1
- 230000003712 anti-aging effect Effects 0.000 abstract 1
- 239000003963 antioxidant agent Substances 0.000 abstract 1
- 230000003078 antioxidant effect Effects 0.000 abstract 1
- 239000011449 brick Substances 0.000 abstract 1
- 239000004566 building material Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000004567 concrete Substances 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 229920001971 elastomer Polymers 0.000 abstract 1
- 229910052602 gypsum Inorganic materials 0.000 abstract 1
- 239000010440 gypsum Substances 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000005060 rubber Substances 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000005034 decoration Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 6
- 238000010074 rubber mixing Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 235000010216 calcium carbonate Nutrition 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 235000019241 carbon black Nutrition 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011178 precast concrete Substances 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- -1 catalyzer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The powerful adhesive includes neoprene, grafting monomer, thickener, dispersant, adhesion promoter, catalyst, antioxidant, solvent, stuffing, etc. The present invention also discloses the preparation process of the adhesive, and the preparation includes introducing grafting monomer to neoprene molecule chain to raise the adhesion strength, selecting proper adhesion promoting resin to increase the initial adhesion force, and adopting mixed solvent to form high adhering performance. The adhesive has high solid content and excellent environment protecting performance, and has also excellent antiageing performance, high resistance to heat, oil, chemical and corrosion, high weather resistance, good mildew-proof performance, antibiotic performance, etc. and may be used for adhering timber, concrete, rubber, metal, gypsum board, brick and other building material.
Description
Technical field
The present invention relates to be applied to the tackiness agent of material of construction, specifically reference and a kind of high-strength adhesive and its preparation Method.
Background technology
In the continuous progressive of the house fitting-up epoch, in order to reach firm effect attractive in appearance, increasing people wishes that finishing does not re-use iron nail, screw, but directly bonding with strong adhesive.Traditional tackiness agent can not satisfy people's desired chemical material articles for use safety and harmony attractive in appearance.They have significant limitation in decorations or aspect sticking mutually to differing materials; Because of the chemical property instability, do not reach the minimum standard of national interior decoration finishing material limits of harmful substances in the residual objectionable impurities in bonding back.On the market high-quality tackiness agent of some high-performance and auxiliary agent product can't production or product performance and quality can't reach the needs in market.Tackiness agent is a kind of novel material of construction, and research abroad is also also few.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention provides the environment-friendly type high intensity power tackiness agent of the antimildew and antibacterial performance of a kind of high solids content, favorable environment protection energy and excellence.
Another object of the present invention provides the preparation method of above-mentioned tackiness agent.
Primary and foremost purpose of the present invention is achieved through the following technical solutions: tackiness agent of the present invention comprises following components by weight portions:
Chloroprene rubber 100
Grafted monomer 20～120
Thickening material 2～5
Dispersion agent 0.3～0.6
Thixotropic agent 1～5
Catalyzer 0.2～1.6
Stopper 2.2～3.3
Oxidation inhibitor 1～5
Solvent 400～600
Tackifying resin 30～50
Filler 80～150
As a kind of improvement, tackiness agent of the present invention comprises following components by weight portions:
Chloroprene rubber 100
Grafted monomer 75
Thickening material 3
Dispersion agent 0.45
Thixotropic agent 3
Catalyzer 0.2
Stopper 3
MgO?????????????????????????????????1
Solvent 460
Tackifying resin 45
Filler 120
Described grafted monomer can be methyl methacrylate (MMA) or butyl acrylate (BA) or vinylformic acid (AA) etc.
Described thickening material can be white carbon black or Walocel MT 20.000PV, natural rubber etc.;
Described tackifying resin is modified phenolic resins, terpine resin, terpene phenolic resin, modified rosin resin or petroleum resin etc.
Described dispersion agent mainly is an industrial surface activity agent, as two octadecyl ammonium chloride, Phenylsulfonic acid formaldehyde condensation products sodium salt, paraffin etc.; Described thixotropic agent mainly is wilkinite, polyether silane etc.; Described catalyzer mainly is a peroxide, as benzoyl peroxide, two formyls of peroxidation, 2, this formyl of 4-dichloro peroxidation etc.; Described stopper mainly is a phenols, as 2,6 di-t-butyls-4-sylvan, 2, and 6-dinitrobenzene p-cresol, N nitrosodiphenyl amine etc.; Described filler can be lime carbonate, nano-calcium carbonate, light calcium carbonate, kaolin, polynite etc.
Described solvent is toluene, hexanaphthene, acetone, butanone, normal hexane, 1, and two or more mixes the mixed solvent that uses 1-dichloro hexane, gasoline etc., and its solubility parameter is δ=9～9.5.
The preparation method of environment-friendly type high intensity power tackiness agent of the present invention comprises the steps:
A, that 100 parts of chloroprene rubbers are put into mill is mixing, adds thickening material after 10 minutes, mixing 10～20 minutes;
B, in reactor, add solvent, tackifying resin, stir, add oxidation inhibitor, continue to stir 4～6 hours;
C, will put into reactor, add grafted monomer, dispersion agent, catalyzer, stir, dissolving, be warmed up to 40～60 ℃, react 4～8 hours through mixing chloroprene rubber, the adding stopper, and cool to room temperature discharging.
D, the chloroprene rubber after the grafting is joined in the planetary mixer, start stir about 10 minutes adds filler, thixotropic agent, continues to stir discharging, packing, finished product 1～2 hour.
Strong adhesive of the present invention at first is in reactor resol to be carried out modification, form the complex compound of resol, metal oxide, add therein then and add thickening material also through the chloroprene rubber after mixing, then add grafted monomer, catalyzer, dispersion agent etc., under the free radical effect, grafted monomer becomes monomer free radical (radical), by chain transfer reaction and chloroprene rubber (CR) graft copolymerization, forms complicated graft copolymerization mixture.Utilize the grafted method in the chloroprene rubber molecular chain, to introduce grafted monomer, to improve its bonding strength; Select for use through suitable tackifying resin to increase the initial bonding strength of tackiness agent; And the mixed solvent that lower boiling combines in adopting makes the environment-friendly type tackiness agent for building with higher adhesiveproperties.
This strong adhesive has good physics, chemical property, big as bonding force, smell is little, waterproof, certain elasticity and filling properties etc. are arranged, can replace traditional iron nail, screw, in construction industry, be used in the bonding of seam crossings such as panel, door frame, precast concrete form, factory building in a large number, aspect the interior decoration decoration, can be used on the bonding and filling between the materials such as kitchen guarding's ceramic tile, bathtub, tank, lamp decoration, furniture manufacturing, also can be in leather and sheet material manufacturing in a large number as bonding.
Tackiness agent of the present invention is compared with prior art, has following advantage and effect:
(1) the present invention forms the complex compound of tackifying resin, metal oxide by to the modification of tackifying resin, makes in its next step the graft reaction and has played certain crosslinked action, has improved initial bonding strength, the stripping strength of chloroprene rubber.
(2) the present invention adopts the composite method of novel process, by selecting suitable thickening, dispersion agent, filler, solvent etc. for use, improves the chloroprene rubber solid content, and has kept its good thixotropy.
After testing, every technical indicator of environment-friendly type high intensity power tackiness agent of the present invention is as follows:
| Sequence number | Interventions Requested | Unit | Standard-required | Assay |
| ????1 | Solid content | ????(％) | About 50 | About 65 |
| ????2 | Denseness | ????9-12 | ????9-12 | |
| ????3 | Extrudability | ????ml/s | ????≥80 | ????≥80 |
| ????4 | Sag | ??mm | ????0.8 | ????0.5 |
| ????5 | Surface drying time | ??min | ????3-5 | ????3-5 |
| ????6 | Shearing resistance | ??MPa | ????2.0 | ????3.1 |
As seen, tackiness agent of the present invention owing to have 〉=50% high solids content, favorable environment protection energy and excellent ageing-resistant, heat-resisting, oil resistant, resistance to chemical attack, weathering resistance, mildew-resistant, performance such as antibiotic, can substitute traditional iron nail, screw, on indoor and outdoor decoration is decorated, play vital role.Aspect civilian, be used in the bonding of seam crossings such as panel, door frame, precast concrete form, factory building in the construction industry in a large number; Aspect the interior decoration decoration, can be used on the bonding and filling between the materials such as kitchen guarding's ceramic tile, bathtub, tank, lamp decoration, furniture manufacturing; Also can be in leather and sheet material manufacturing in a large number as bonding.Product of the present invention does not contain harmful materials such as benzene,toluene,xylene, and the content of free formaldehyde also is lower than standard-required content, and environmental protection safe in utilization has boundless market outlook.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 3 parts of thickening material white carbon blacks after 10 minutes, mixing evenly.
2, pre-reaction
In reactor, add 600 parts of solvents (mixed solvent that toluene, hexanaphthene and gasoline are formed, toluene: hexanaphthene: the gasoline proportioning is 4: 3: 3), 50 parts of modified phenolic resinss (commercially available), stir, add 2 parts of oxidation inhibitor MgO therein, continue to stir 4 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 70 parts of grafted monomer methymethacrylates (MMA), 0.6 part of two octadecyl ammonium chloride of dispersion agent, 0.34 part of catalyzer benzoyl peroxide, stir, dissolve, be warmed up to 60 ℃, reacted 4 hours, add 2.5 parts of stoppers 2 immediately, 6 di-t-butyls-4-sylvan (dilutes with butanone, extension rate 1: 10), and cools to room temperature polyreaction is stopped, discharging.
4, the preparation of tackiness agent
Chloroprene rubber after the above-mentioned grafting is joined in the planetary mixer, and start stir about 10 minutes adds 120 parts of filler-calcium carbonates, 1 part of thixotropic agent polyether silane, continues to stir discharging, packing, finished product 1 hour.
Embodiment 2
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 2 parts of thickening material white carbon blacks after 10 minutes, mixing evenly.
2, pre-reaction
In reactor, add 400 parts of solvents (mixed solvent that toluene, normal hexane and gasoline are formed, toluene: normal hexane: the gasoline proportioning is 4: 4: 2), 30 parts of terpine resins, stir, add 3 parts of oxidation inhibitor MgO therein, continue to stir 4 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 20 parts of grafted monomer methymethacrylates, 0.6 part of dispersion agent Phenylsulfonic acid formaldehyde condensation products sodium salt, 0.2 part of catalyzer benzoyl peroxide, stir, dissolve, be warmed up to 40 ℃, reacted 6 hours, add 2.2 parts of stoppers 2 immediately, 6 di-t-butyls-4-sylvan (dilutes with butanone, extension rate 1: 10), and cools to room temperature polyreaction is stopped, discharging.
4, the preparation of tackiness agent
Chloroprene rubber after the grafting is joined in the planetary mixer, and start stir about 10 minutes adds 150 parts of filler polynites, 3.1 parts of thixotropic agent polyether silanes, continues to stir discharging, packing, finished product 2 hours.
Embodiment 3
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 5 parts of thickening material Walocel MT 20.000PVs, mixing 18 minutes after 10 minutes.
2, pre-reaction
In reactor, add 500 parts of solvents (mixed solvent that toluene, butanone and gasoline are formed, toluene: butanone: the gasoline proportioning is 4: 3: 3), 50 parts of terpene phenolic resins, stir, add 1 part of oxidation inhibitor MgO therein, continue to stir 6 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 43 parts of grafted monomer butyl acrylates (BA), 0.5 part of dispersion agent paraffin, two formyls of 0.24 part of catalyzer peroxidation, stir, dissolve, be warmed up to 60 ℃, reacted 5 hours, add 3.3 parts of stoppers 2 immediately, 6 di-t-butyls-4-sylvan (dilutes with butanone, extension rate 1: 10), and cools to room temperature polyreaction is stopped, discharging.
4, the preparation of tackiness agent
Chloroprene rubber after the grafting is joined in the planetary mixer, and start stir about 10 minutes adds 100 parts of filler kaolin, 5 parts of thixotropic agent polyether silanes, continues to stir discharging, packing, finished product 2 hours.
Embodiment 4
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 3 parts of thickening material Walocel MT 20.000PVs, mixing 15 minutes after 10 minutes.
2, pre-reaction
In reactor, add 530 parts of solvent (mixed solvents of toluene, normal hexane, toluene: the normal hexane proportioning is 6: 4), 50 parts of tackifying resin modified rosin resins (commercially available), stir, add 4 parts of oxidation inhibitor MgO therein, continue to stir 5 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 63 parts of grafted monomer vinylformic acid (AA), the two octadecyl ammonium chloride of 0.4 part of dispersion agent, two formyls of 1.2 parts of catalyzer peroxidation, stir, dissolve, be warmed up to 60 ℃, reacted 8 hours, and added 2.8 parts of stopper N nitrosodiphenyl amines (with butanone dilution, extension rate 1: 10) immediately, and cool to room temperature polyreaction is stopped, discharging.4, the preparation of tackiness agent
Chloroprene rubber after the grafting is joined in the planetary mixer, and start stir about 10 minutes adds 150 parts of filler light calcium carbonates, 2.3 parts of thixotropic agent polyether silanes, continues to stir discharging, packing, finished product 2 hours.
Embodiment 5
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 5 parts of thickening material natural rubbers, mixing 10 minutes after 10 minutes.
2, pre-reaction
In reactor, add 480 parts of solvent (toluene, 1, the mixed solvent that 1-dichloro hexane and gasoline are formed, toluene: 1, the 1-dichloro hexane: the gasoline proportioning is 5: 2: 3), 30 parts of tackifying resin petroleum resin, stir, add 5 parts of oxidation inhibitor MgO therein, continue to stir 4 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 120 parts of grafted monomer methymethacrylates, 0.3 part of two octadecyl ammonium chloride of dispersion agent, 1.6 parts of catalyzer 2, this formyl of 4-dichloro peroxidation stirs, dissolves, and is warmed up to 50 ℃, reacted 7 hours, add 3.1 parts of stoppers 2 immediately, 6-dinitrobenzene p-cresol (with butanone dilution, extension rate 1: 10), and cool to room temperature polyreaction is stopped, discharging.
4, the preparation of tackiness agent
Chloroprene rubber after the grafting is joined in the planetary mixer, and start stir about 10 minutes adds 80 parts of filler nanometer calcium carbonates, 2.5 parts of thixotropic agent wilkinites, continues to stir discharging, packing, finished product 1.5 hours.
Embodiment 6
1, chloroprene rubber mixing
Getting 100 parts of chloroprene rubbers, to put into mill mixing, adds 3 parts of thickening material natural rubbers, mixing 20 minutes after 10 minutes.
2, pre-reaction
In reactor, add 460 parts of solvents (mixed solvent that toluene, acetone and gasoline are formed, toluene: acetone: the gasoline proportioning is 4: 2: 4), 45 parts of tackifying resin petroleum resin, stir, add 1 part of oxidation inhibitor MgO therein, continue to stir 4 hours, make and carry out complex reaction between tackifying resin and the oxidation inhibitor.
3, grafting
To join through mixing chloroprene rubber in the reactor, add 75 parts of grafted monomer methymethacrylates, 0.45 part of two octadecyl ammonium chloride of dispersion agent, 0.2 part of catalyzer 2, this formyl of 4-dichloro peroxidation stirs, dissolves, and is warmed up to 60 ℃, reacted 8 hours, add 3 parts of stoppers 2 immediately, 6-dinitrobenzene p-cresol (with butanone dilution, extension rate 1: 10), and cool to room temperature polyreaction is stopped, discharging.
4, the preparation of tackiness agent
Chloroprene rubber after the grafting is joined in the planetary mixer, and start stir about 10 minutes adds 120 parts of filler nanometer calcium carbonates, 3 parts of thixotropic agent wilkinites, continues to stir discharging, packing, finished product 1.5 hours.
Claims (9)
1, a kind of high strong adhesive is characterized in that, comprises following components by weight portions:
Chloroprene rubber 100
Grafted monomer 20～120
Thickening material 2～5
Dispersion agent 0.3～0.6
Thixotropic agent 1～5
Catalyzer 0.2～1.6
Stopper 2.2～3.3
Oxidation inhibitor 1～5
Solvent 400～600
Tackifying resin 30～50
Filler 80～150
2, tackiness agent according to claim 1 is characterized in that, described tackiness agent comprises following components by weight portions:
Chloroprene rubber 100
Grafted monomer 75
Thickening material 3
Dispersion agent 0.45
Thixotropic agent 3
Catalyzer 0.2
Stopper 3
MgO?????????????????????????????1
Solvent 460
Tackifying resin 45
Filler 120
3, tackiness agent according to claim 1 is characterized in that, described grafted monomer is methyl methacrylate, butyl acrylate or vinylformic acid.
4, tackiness agent according to claim 1 is characterized in that, described thickening material is white carbon black, Walocel MT 20.000PV or natural rubber.
5, tackiness agent according to claim 1 is characterized in that, described tackifying resin is modified phenolic resins, terpine resin, terpene phenolic resin, modified rosin resin or petroleum resin.
6, tackiness agent according to claim 1 is characterized in that, described dispersion agent is two octadecyl ammonium chloride, Phenylsulfonic acid formaldehyde condensation products sodium salt, paraffin; Described thixotropic agent is wilkinite, polyether silane; Described catalyzer is benzoyl peroxide, two formyls of peroxidation, 2, this formyl of 4-dichloro peroxidation; Described stopper is 2,6 di-t-butyls-4-sylvan, 2,6-dinitrobenzene p-cresol, N nitrosodiphenyl amine;
7, tackiness agent according to claim 1 is characterized in that, described filler is lime carbonate, nano-calcium carbonate, light calcium carbonate, kaolin, polynite.
8, tackiness agent according to claim 1, it is characterized in that, described solvent is toluene, hexanaphthene, acetone, butanone, normal hexane, 1, the mixed solvent that 1-dichloro hexane, two or more mixing of gasoline are used, and its solubility parameter is δ=9～9.5.
9, the preparation method of the described high strong adhesive of claim 1 is characterized in that, comprises the steps:
A, that 100 parts of chloroprene rubbers are put into mill is mixing, adds thickening material after 10 minutes, mixing 10～20 minutes;
B, in reactor, add solvent, tackifying resin, stir, add oxidation inhibitor MgO, continue to stir 4～6 hours;
C, will put into reactor, add grafted monomer, dispersion agent, catalyzer, stir, dissolving, be warmed up to 40～60 ℃, react 4～8 hours through mixing chloroprene rubber, the adding stopper, and cool to room temperature discharging;
D, the chloroprene rubber after the grafting is joined in the planetary mixer, start was stirred 10 minutes, added filler, thixotropic agent, stirred discharging, packing, finished product 1～2 hour.
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Assignee: Hubei Bluesky New Material Inc. Assignor: Mo Wanquan Contract fulfillment period: 2006.12.28 to 2013.12.28 contract change Contract record no.: 2009420000083 Denomination of invention: High strong adhesive and method for preparing same Granted publication date: 20061206 License type: Exclusive license Record date: 2009.8.10 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.12.28 TO 2013.12.28; CHANGE OF CONTRACT Name of requester: HUBEI XIANTAO BLUE SKY CHEMICAL CO., LTD. Effective date: 20090810 |
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Effective date of registration: 20111222 Address after: 510450, Guangzhou, Guangzhou City, Baiyun District, Xin Guang highway, Pui Pui section, Liwan (Jiang Gao) Industrial Zone, B141408, Guangdong Patentee after: Guangzhou Glorystar Chemical Co., Ltd. Address before: 510450 Guangdong Guangzhou first grade highway, Pui Bei section, Liwan Economic Development Zone, Guangzhou Gao Shi Industrial Co., Ltd. Patentee before: Mo Wanquan |