CN115584224B - Preparation method of environment-friendly water-based adhesive - Google Patents
Preparation method of environment-friendly water-based adhesive Download PDFInfo
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- CN115584224B CN115584224B CN202211305399.5A CN202211305399A CN115584224B CN 115584224 B CN115584224 B CN 115584224B CN 202211305399 A CN202211305399 A CN 202211305399A CN 115584224 B CN115584224 B CN 115584224B
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 50
- 239000000853 adhesive Substances 0.000 title claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000839 emulsion Substances 0.000 claims abstract description 42
- -1 acrylic ester Chemical class 0.000 claims abstract description 22
- 229920001577 copolymer Polymers 0.000 claims abstract description 15
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical compound ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- 229920001084 poly(chloroprene) Polymers 0.000 claims abstract description 13
- 239000004816 latex Substances 0.000 claims abstract description 12
- 229920000126 latex Polymers 0.000 claims abstract description 12
- VGQLLUIFOUVAPI-UHFFFAOYSA-N [Cl].OC(=O)C=C Chemical compound [Cl].OC(=O)C=C VGQLLUIFOUVAPI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 24
- 239000007822 coupling agent Substances 0.000 claims description 15
- 239000003431 cross linking reagent Substances 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000003995 emulsifying agent Substances 0.000 claims description 13
- 230000000149 penetrating effect Effects 0.000 claims description 13
- 239000002562 thickening agent Substances 0.000 claims description 13
- 239000005995 Aluminium silicate Substances 0.000 claims description 12
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 12
- 235000012211 aluminium silicate Nutrition 0.000 claims description 12
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 12
- 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 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical group COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical group CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- BRNFYNCAGBJLOZ-UHFFFAOYSA-N penta-1,3-diene hydrate Chemical compound CC=CC=C.O BRNFYNCAGBJLOZ-UHFFFAOYSA-N 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 abstract description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 36
- 238000012360 testing method Methods 0.000 description 7
- 239000003522 acrylic cement Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000037303 wrinkles Effects 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 description 1
- VPAHRARWPRHPQN-UHFFFAOYSA-M [Cl+].[O-]C(=O)C=C Chemical compound [Cl+].[O-]C(=O)C=C VPAHRARWPRHPQN-UHFFFAOYSA-M 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229950006451 sorbitan laurate Drugs 0.000 description 1
- 235000011067 sorbitan monolaureate Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention discloses a preparation method of an environment-friendly aqueous adhesive, and belongs to the technical field of preparation of aqueous acrylic ester adhesives. Under the acidic condition, the invention copolymerizes aqueous acrylic ester and pentadiene to obtain pentadiene-aqueous acrylic ester emulsion, and then blends the emulsion with VAE emulsion and neoprene latex to obtain acrylic acid chloride Ding Yin ion copolymerization emulsion; the environment-friendly aqueous adhesive is prepared by taking the acrylic acid chlorine Ding Yinli sub-copolymer emulsion as a main adhesive and adding various auxiliary agents, can well overcome the defects of slower volatilization speed and poorer water resistance of the traditional aqueous acrylic acid ester adhesive, has the advantages of simple preparation method, environmental protection, no pollution, suitability for industrial production and good market competitiveness.
Description
Technical Field
The invention belongs to the technical field of preparation of aqueous acrylic ester adhesives, and particularly relates to a preparation method of an environment-friendly aqueous adhesive.
Background
With the increasing strictness of environmental regulations and the increasing environmental awareness of people, the requirements of various application fields on adhesives are becoming stricter nowadays. The solvent-type adhesive contains a large amount of volatile organic solvents such as benzene, toluene and the like, seriously harms human health and pollutes the environment, and also has the risks of combustion and explosion in the storage and preparation processes. Unlike solvent-based adhesives, the aqueous adhesives use natural polymers or synthetic polymers as adhesives and water as solvents or dispersants, and have remarkable advantages in clean production and safe use. The aqueous adhesive can be classified into polyurethane aqueous adhesives, epoxy aqueous adhesives, phenolic aqueous adhesives, organosilicon aqueous adhesives, acrylic aqueous adhesives, rubber aqueous adhesives and the like according to materials; however, since the research of the water-based adhesive in China is started later, most of the existing products in China still have more defects in practical application, and better development and application cannot be achieved.
The aqueous acrylic ester adhesive is an aqueous adhesive with more applications, belongs to an emulsifying system, and has the advantages of no change of viscosity along with the change of the molecular weight of a polymer, environmental protection, no flammability, wide solid content range, adjustable permeation and the like; however, at the same time, the method has the defects of slower volatilization speed, poorer initial viscosity, poor wettability to partial plastics and poor water resistance. Along with the development of science and technology, the improvement of economic level and the improvement of the quality of life level of people, the development of high-performance environment-friendly aqueous adhesives has become a necessary trend, so that the curing of the aqueous acrylic ester adhesives is controlled, and the defect of usability of the aqueous acrylic ester adhesives is overcome.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art in the background art, the invention aims to provide a preparation method of an environment-friendly aqueous adhesive, which aims to overcome the shortcomings of the traditional aqueous acrylic adhesive and prepare a high-performance aqueous acrylic adhesive which can be quickly volatilized and dried and has excellent early water resistance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of an environment-friendly water-based adhesive, which comprises the following steps:
step 1): mixing and dispersing the acrylic acid chloride Ding Yin ion copolymer emulsion, a cross-linking agent, a dispersing agent, an emulsifying agent, a penetrating agent and a film forming auxiliary agent;
step 2): adding nano calcium carbonate and kaolin into the mixture obtained in the step 1) for multiple times for continuous dispersion, vacuumizing after the material addition is finished, and heating to 40-50 ℃;
step 3): continuously adding dioctyl phthalate, a coupling agent and a thickening agent into the mixture obtained in the step 2), and stirring in vacuum to obtain the water-based acrylic ester adhesive.
Preferably, the preparation method of the chlorine acrylate Ding Yinli sub-copolymer emulsion in the step 1) comprises the following steps: under the acidic condition, copolymerizing aqueous acrylic ester and pentadiene to obtain pentadiene-aqueous acrylic ester emulsion, and then blending the emulsion with VAE emulsion and neoprene latex to obtain acrylic acid chloride Ding Yin ion copolymer emulsion.
Preferably, the neoprene latex is anionic neoprene latex, the solid content of which is 46+/-2 percent, and the viscosity of which is 1200 mPa.s.
Preferably, the vinyl acetate content of the VAE emulsion is 92±2%.
Preferably, the raw materials used in each step are as follows in parts by weight: 50-60 parts of acrylic acid chlorine Ding Yinli seed copolymerization emulsion, 0.3-0.6 part of cross-linking agent, 2-5 parts of dispersing agent, 3-7 parts of emulsifying agent, 2-6 parts of penetrating agent, 1.5-3 parts of film forming auxiliary agent, 20-30 parts of nano calcium carbonate, 5-12 parts of kaolin, 5-8 parts of dioctyl phthalate, 0.2-0.5 part of coupling agent and 1-5 parts of thickening agent.
Preferably, the raw materials used in each step are as follows in parts by weight: 56 parts of acrylic acid chloride Ding Yin ion copolymer emulsion, 0.5 part of cross-linking agent, 3.5 parts of dispersing agent, 5 parts of emulsifying agent, 4 parts of penetrating agent, 2.2 parts of film forming auxiliary agent, 24 parts of nano calcium carbonate, 9 parts of kaolin, 7 parts of dioctyl phthalate, 0.4 part of coupling agent and 3 parts of thickening agent.
Preferably, the cross-linking agent is aminopropyl triethoxysilane; the coupling agent is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane.
Preferably, the film forming aid is dipropylene glycol monomethyl ether.
Compared with the prior art, the invention has the beneficial effects that:
under the acidic condition, the invention copolymerizes aqueous acrylic ester and pentadiene to obtain pentadiene-aqueous acrylic ester emulsion, and then blends the emulsion with VAE emulsion and neoprene latex to obtain acrylic acid chloride Ding Yin ion copolymerization emulsion; the environment-friendly aqueous adhesive is prepared by taking the acrylic acid chlorine Ding Yinli sub-copolymer emulsion as a main adhesive and adding various auxiliary agents, can well overcome the defects of slower volatilization speed and poorer water resistance of the traditional aqueous acrylic acid ester adhesive, has the advantages of simple preparation method, environmental protection, no pollution, suitability for industrial production and good market competitiveness.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described in the following examples. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the test of the invention, aminopropyl triethoxysilane is adopted as the crosslinking agent, sorbitan laurate is adopted as the dispersing agent, polyoxyethylene styryl phenyl ether is adopted as the emulsifying agent, JFC is adopted as the penetrating agent, dipropylene glycol monomethyl ether is adopted as the film forming auxiliary agent, N- (beta-aminoethyl) -gamma aminopropyl trimethoxysilane is adopted as the coupling agent, and hydroxymethyl cellulose is adopted as the thickening agent.
Example 1
An environment-friendly aqueous acrylic adhesive, the preparation method of which comprises the following steps:
1. accurately weighing the preparation raw materials: 56 parts of acrylic acid chloride Ding Yin ion copolymer emulsion (prepared by copolymerizing 120 parts by weight of aqueous acrylic ester and 0.5 part by weight of dicyclopentadiene at a pH value of 4.6 and then blending with 25 parts by weight of VAE emulsion and 40 parts by weight of neoprene latex), 0.5 part of cross-linking agent, 3.5 parts of dispersing agent, 5 parts of emulsifying agent, 4 parts of penetrating agent, 2.2 parts of film forming auxiliary agent, 24 parts of nano calcium carbonate, 9 parts of kaolin, 7 parts of dioctyl phthalate, 0.4 part of coupling agent and 3 parts of thickening agent.
2. Adding the acrylic acid chloride Ding Yinli sub-copolymer emulsion into a dispersing machine, regulating the pH value to 4.2, respectively setting the dispersing shaft, the wall-mounted rotating speed to 40Hz and 25Hz, mechanically stirring for 30 minutes, continuously adding the cross-linking agent, the dispersing agent, the emulsifying agent, the penetrating agent and the film-forming auxiliary agent into the dispersing machine, and keeping the parameters and continuously mechanically stirring for 30 minutes.
3. The nano calcium carbonate and the kaolin are put into a dispersing machine in batches, the temperature is raised to 30 ℃ when the input amount reaches two thirds, then the rest powder is put into the dispersing machine, the vacuum is started to-0.1 MPa, and the auxiliary temperature is raised to 45 ℃; and finally, putting dioctyl phthalate, a coupling agent and a thickening agent into a dispersing machine, starting vacuum to-0.12 MPa, mechanically stirring for 30 minutes, controlling the temperature of the materials to be 45 ℃, and discharging to obtain the adhesive.
The adhesive prepared in the embodiment is uniformly coated on the surface of a steel plate, and the thickness is 1.5mm; based on the template, the adhesive of the embodiment is tested for partial performance:
the steel plates are respectively placed in different humidity environments to detect the drying speed of the coating film: surface drying at 25 ℃ under the condition of 25% humidity for 5.8 h/real drying for 25h; surface drying at 25 ℃ under 50% humidity for 5.8 h/real drying for 25.5h; surface drying at 25deg.C under 80% humidity for 5.9 hr/real drying for 26.5 hr.
And (3) water resistance test: drying the steel plate for 1.5h, placing the edge seal in distilled water at 25 ℃ (2/3 of the edge seal is immersed in the water), observing the state of a coating film every 3h, judging damage when the coating film bubbles and wrinkles are reached, and recording the damage time as an early water resistance index; the steel plate is dried for 72 hours, the edge sealing is placed in distilled water at 25 ℃ (2/3 of the edge sealing is immersed in the water), the coating state is observed every 12 hours, the damage is judged when the coating bubbles and wrinkles are reached, and the damage time is recorded as a final water resistance index. The test results are: early water resistance 105h and final water resistance 26.5d.
Example 2
An environment-friendly aqueous acrylic adhesive, the preparation method of which comprises the following steps:
1. accurately weighing the preparation raw materials: 50 parts of acrylic acid chloride Ding Yin ion copolymerization emulsion (prepared by copolymerizing 120 parts by weight of aqueous acrylic ester and 0.5 part by weight of dicyclopentadiene at a pH value of 4.6 and then blending with 25 parts by weight of VAE emulsion and 40 parts by weight of neoprene latex), 0.3 part of cross-linking agent, 4.5 parts of dispersing agent, 3.5 parts of emulsifying agent, 6 parts of penetrating agent, 2.8 parts of film forming additive, 28 parts of nano calcium carbonate, 6 parts of kaolin, 5 parts of dioctyl phthalate, 0.2 part of coupling agent and 1.5 parts of thickening agent.
2. Adding the acrylic acid chloride Ding Yinli sub-copolymer emulsion into a dispersing machine, regulating the pH value to 4.2, respectively setting the dispersing shaft, the wall-mounted rotating speed to 40Hz and 25Hz, mechanically stirring for 30 minutes, continuously adding the cross-linking agent, the dispersing agent, the emulsifying agent, the penetrating agent and the film-forming auxiliary agent into the dispersing machine, and keeping the parameters and continuously mechanically stirring for 30 minutes.
3. The nano calcium carbonate and the kaolin are put into a dispersing machine in batches, the temperature is raised to 30 ℃ when the input amount reaches two thirds, then the rest powder is put into the dispersing machine, the vacuum is started to-0.1 MPa, and the auxiliary temperature is raised to 45 ℃; and finally, putting dioctyl phthalate, a coupling agent and a thickening agent into a dispersing machine, starting vacuum to-0.12 MPa, mechanically stirring for 30 minutes, controlling the temperature of the materials to be 45 ℃, and discharging to obtain the adhesive.
The adhesive properties prepared in this example were tested as in example 1:
drying speed: surface drying at 25 ℃ under 25% humidity for 5.9 h/real drying for 27h; surface drying at 25 ℃ under 50% humidity for 6.0 h/real drying for 27.5h; surface drying at 25deg.C under 80% humidity for 6.0 h/real drying for 28.5h.
And (3) water resistance test: early water resistance 94h and final water resistance 24d.
Example 3
An environment-friendly aqueous acrylic adhesive, the preparation method of which comprises the following steps:
1. accurately weighing the preparation raw materials: 60 parts of acrylic acid chloride Ding Yin ion copolymer emulsion (prepared by copolymerizing 120 parts by weight of aqueous acrylic ester and 0.5 part by weight of dicyclopentadiene at a pH value of 4.6 and then blending with 25 parts by weight of VAE emulsion and 40 parts by weight of neoprene latex), 0.6 part of cross-linking agent, 2.5 parts of dispersing agent, 7 parts of emulsifying agent, 2.5 parts of penetrating agent, 1.6 parts of film forming additive, 20 parts of nano calcium carbonate, 12 parts of kaolin, 8 parts of dioctyl phthalate, 0.5 part of coupling agent and 4.5 parts of thickening agent.
2. Adding the acrylic acid chloride Ding Yinli sub-copolymer emulsion into a dispersing machine, regulating the pH value to 4.2, respectively setting the dispersing shaft, the wall-mounted rotating speed to 40Hz and 25Hz, mechanically stirring for 30 minutes, continuously adding the cross-linking agent, the dispersing agent, the emulsifying agent, the penetrating agent and the film-forming auxiliary agent into the dispersing machine, and keeping the parameters and continuously mechanically stirring for 30 minutes.
3. The nano calcium carbonate and the kaolin are put into a dispersing machine in batches, the temperature is raised to 30 ℃ when the input amount reaches two thirds, then the rest powder is put into the dispersing machine, the vacuum is started to-0.1 MPa, and the auxiliary temperature is raised to 45 ℃; and finally, putting dioctyl phthalate, a coupling agent and a thickening agent into a dispersing machine, starting vacuum to-0.12 MPa, mechanically stirring for 30 minutes, controlling the temperature of the materials to be 45 ℃, and discharging to obtain the adhesive.
The adhesive properties prepared in this example were tested as in example 1:
drying speed: surface drying at 25 ℃ under 25% humidity for 5.8 h/real drying for 26h; surface drying at 25 ℃ under 50% humidity for 5.9 h/real drying for 27.5h; surface drying at 25deg.C under 80% humidity for 6.0 h/real drying for 28h.
And (3) water resistance test: early water resistance of 102h and final water resistance of 25.5d.
Comparative example 1
The acrylic acid chloride Ding Yinli sub-copolymer emulsion is prepared by only adopting the blending of the aqueous acrylic ester emulsion and the VAE emulsion and the neoprene emulsion, and the rest of the steps have the same parameters as those of the embodiment 1.
The adhesive properties prepared in this comparative example were tested as in example 1:
drying speed: surface drying at 25 ℃ under the condition of 25% humidity for 5.8 h/real drying for 25.5h; surface drying at 25 ℃ under 50% humidity for 5.9 h/real drying for 29.5h; surface drying at 25deg.C under 80% humidity for 9.5 h/real drying for 47.5h.
And (3) water resistance test: early water resistance 103h and final water resistance 26d.
Comparative example 2
The acrylic acid chlorine Ding Yinli sub-copolymer emulsion is prepared by only adopting the blending of the pentadiene-water acrylic ester emulsion and the neoprene latex, and the rest of the steps have the same parameters as those of the example 1 to prepare the adhesive.
The adhesive properties prepared in this comparative example were tested as in example 1:
drying speed: surface drying at 25 ℃ under the condition of 25% humidity for 5.9 h/real drying for 25h; surface drying at 25 ℃ under 50% humidity for 6.0 h/real drying for 26h; surface drying at 25deg.C under 80% humidity for 6.0 h/real drying for 27h.
And (3) water resistance test: early water resistance for 48h and final water resistance for 24.5d.
The embodiments described above represent only a few preferred embodiments of the present invention, which are described in more detail and are not intended to limit the present invention. It should be noted that various changes and modifications can be made to the present invention by those skilled in the art, and any modifications, equivalent substitutions, improvements, etc. which are within the spirit and principle of the present invention are included in the scope of the present invention.
Claims (6)
1. The preparation method of the environment-friendly water-based adhesive is characterized by comprising the following steps of:
step 1): mixing and dispersing the acrylic acid chloride Ding Yin ion copolymer emulsion, a cross-linking agent, a dispersing agent, an emulsifying agent, a penetrating agent and a film forming auxiliary agent; the preparation method of the acrylic acid chlorine Ding Yinli sub-copolymerization emulsion comprises the following steps: under an acidic condition, copolymerizing 120 parts by weight of water-based acrylic ester and 0.5 part by weight of dicyclopentadiene to obtain pentadiene-water-based acrylic ester emulsion, and then blending the obtained emulsion with 25 parts by weight of VAE emulsion and 40 parts by weight of neoprene latex;
step 2): adding nano calcium carbonate and kaolin into the mixture obtained in the step 1) for multiple times for continuous dispersion, vacuumizing after the material addition is finished, and heating to 40-50 ℃;
step 3): continuously adding dioctyl phthalate, a coupling agent and a thickening agent into the mixture obtained in the step 2), and stirring in vacuum to obtain a water-based acrylic ester adhesive;
wherein, the raw materials used in each step are as follows according to parts by weight: 50-60 parts of acrylic acid chlorine Ding Yinli seed copolymerization emulsion, 0.3-0.6 part of cross-linking agent, 2-5 parts of dispersing agent, 3-7 parts of emulsifying agent, 2-6 parts of penetrating agent, 1.5-3 parts of film forming auxiliary agent, 20-30 parts of nano calcium carbonate, 5-12 parts of kaolin, 5-8 parts of dioctyl phthalate, 0.2-0.5 part of coupling agent and 1-5 parts of thickening agent.
2. The method for preparing the environment-friendly water-based adhesive according to claim 1, wherein the neoprene latex is anionic neoprene latex, the solid content of which is 46%, and the viscosity of which is 1200 mpa.s.
3. The method for preparing the environment-friendly water-based adhesive according to claim 1, wherein the vinyl acetate content of the VAE emulsion is 92+/-2%.
4. The preparation method of the environment-friendly water-based adhesive according to claim 1, which is characterized in that the raw materials used in each step are as follows in parts by weight: 56 parts of acrylic acid chloride Ding Yin ion copolymer emulsion, 0.5 part of cross-linking agent, 3.5 parts of dispersing agent, 5 parts of emulsifying agent, 4 parts of penetrating agent, 2.2 parts of film forming auxiliary agent, 24 parts of nano calcium carbonate, 9 parts of kaolin, 7 parts of dioctyl phthalate, 0.4 part of coupling agent and 3 parts of thickening agent.
5. The method for preparing the environment-friendly water-based adhesive according to claim 1, wherein the cross-linking agent is aminopropyl triethoxysilane; the coupling agent is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane.
6. The method for preparing the environment-friendly water-based adhesive according to claim 1, wherein the film forming additive is dipropylene glycol monomethyl ether.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4309330A (en) * | 1981-02-19 | 1982-01-05 | Hitachi Chemical Company Ltd. | Copolymer emulsion |
| CN101560367A (en) * | 2008-04-18 | 2009-10-21 | 黄楚填 | Aqueousneoprene type environment-friendly glue and preparation method thereof |
| CN103805097A (en) * | 2012-11-14 | 2014-05-21 | 深圳市顾康力化工有限公司 | Environment-friendly water-based chloroprene universal rubber and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4309330A (en) * | 1981-02-19 | 1982-01-05 | Hitachi Chemical Company Ltd. | Copolymer emulsion |
| CN101560367A (en) * | 2008-04-18 | 2009-10-21 | 黄楚填 | Aqueousneoprene type environment-friendly glue and preparation method thereof |
| CN103805097A (en) * | 2012-11-14 | 2014-05-21 | 深圳市顾康力化工有限公司 | Environment-friendly water-based chloroprene universal rubber and preparation method thereof |
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