CN101314699B - Water-based adhesion agent and preparation thereof - Google Patents
Water-based adhesion agent and preparation thereof Download PDFInfo
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- CN101314699B CN101314699B CN2008101244313A CN200810124431A CN101314699B CN 101314699 B CN101314699 B CN 101314699B CN 2008101244313 A CN2008101244313 A CN 2008101244313A CN 200810124431 A CN200810124431 A CN 200810124431A CN 101314699 B CN101314699 B CN 101314699B
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Abstract
The invention relates to a waterborne adhesive and the preparation method thereof. The waterborne adhesive is prepared from deionized water, nano-SiO2, polyvinyl alcohol PVA17-99, polyvinyl alcohol PVA17-88, emulsifying agent, vinyl acetate, acrylic acid, ammonium persulfate, TXIB, preservative, and defoaming agent at a certain weight ratio. The preparation method comprises the following steps: adding nano-SiO2 into the waterborne adhesive, and adding TXIB dropwise through a flowmeter before and after polymerization of the waterborne adhesive, thus improving the brittleness, the water resistance and the glossiness of the waterborne adhesive, reducing the bottom film-forming temperature, remarkably improving the bonding strength of the adhesive, reducing the toxicity of the waterborne adhesive and lowering the production cost. The product can be widely used for self-adhesion and crossed adhesion of various kinds of non-metal materials such as paper sheets, wood material, fiber board and textiles, and has the advantages of environment-friendliness, economic and practical use, board range of application, etc.
Description
Technical field
The invention belongs to adhesive area, be specifically related to a kind of water-based adhesion agent and preparation method thereof.
Background technology
Water-based adhesion agent be a kind of be dispersion medium with water, by adding the aqueous adhesive that monomer etc. is polymerized, be mainly used in the bonding of non-metallic material, especially for wood working, indoor decoration, very high to its environmental requirement, must meet GB18583 " limits of harmful substances in the indoor decorating adhesive ".At present, Chinese patent application 200710030506.7 discloses a kind of novel copolymerized white latex, its batching comprises: polyvinyl alcohol, deionized water, sodium bicarbonate, vinyl acetate between to for plastic, butyl acrylate, tertiary monocarboxylic acid ethene vinegar, dispersion agent, defoamer, ammonium persulphate, softening agent, the pH value conditioning agent, polyreaction is carried out in glassed steel reaction vessels, at first the polyvinyl alcohol deionized water is dropped in the reactor, intensification makes its dissolving, the cooling back adds dispersion agent, defoamer, add reaction monomers again, at normal pressure, temperature is to carry out polyreaction under 72～80 ℃ of whipped states, add an amount of pH value conditioning agent then, make pH value between 6.0～7.0, add Plasticizer DBP at last, constitute product.Wherein softening agent is a dibutyl phthalate (DBP), because it contains benzene liver class objectionable impurities, human body is had injury, even can be carcinogenic.In addition, plasticizer dosage is bigger, and promptly 2.5～6%, increased production cost.
The preparation method and the application of Chinese patent application 200610156025.6 disclosed a kind of water resistant starch-base timber adhesives.Its preparation method is: the crosslinked graft copolymers of (1) starch-vinyl acetate synthetic; With starch is raw material, is catalyzer with hydrochloric acid, is initiator with the ammonium persulphate, with the vinyl acetate is monomer, connects the skill copolyreaction under acidic conditions, then with N, N1-methylene-bis acryloyl is a linking agent, carries out crosslinking reaction and the crosslinked graft copolymers of synthetic starch-vinyl acetate; (2) the crosslinked graft copolymers of starch-vinyl acetate and auxiliary agent mixes; The crosslinked graft copolymers of starch-vinyl acetate is a properties-correcting agent with polyvinyl alcohol 124 under neutrallty condition, is the secondary crosslinking agent with the borax, after the gelatinization, be thinner with urea, glycerine is softening agent, tbp is a defoamer, obtains water resistant starch-base timber adhesive after the mixing.Wherein, softening agent is a glycerine, and its consumption is 10%～15% of a starch quality.Because the plasticization effect of glycerine is relatively poor, its consumption is corresponding just bigger, thereby has increased production cost.In addition, add softening agent glycerine does not have thickening and improves bonding strength in aqueous adhesive effect, aqueous adhesive does not generally use glycerine to make softening agent on the existing market.
In addition, China Patent No. is 02109564.7 disclosed a kind of multifunctional aqueous adhesive and method for making thereof.It is made up of first, second two components.The first component is made up of a certain amount of polyvinyl alcohol ethylenic unsaturated acid ester, ethylenic unsaturated acid acid anhydride or acid, emulsifier op-10, dodecyl phenenyl sulfate, ammonium persulphate, dibutyl phthalate (DBP), defoamer and water; The second component is made up of a certain amount of organic compound, polyisocyanates, organic acid acetic that contains one or more hydroxyls.Wherein softening agent also is a dibutyl phthalate, and its consumption reaches 5%～10%, large usage quantity.Therefore, O-phthalic ester dibutylester commonly used in the market hardly realizes that as primary plasticizer dibutyl phthalate (DBP) has injury to human body, and animal experiment shows that liver and kidney are had injury effect, even can be carcinogenic.Dibutyl phthalate usefulness is the primary plasticizer in the water-based adhesion agent, has been difficult to satisfy environmental requirement, and the application in water-based adhesion agent of green, environmental protection, superplastiser has become trend of the times.
Summary of the invention
In order to overcome the shortcoming that prior art exists, the purpose of this invention is to provide a kind of water-based adhesion agent of economical and practical, green, environmental protection.
Said water-based adhesion agent, it is made by following materials of weight proportions:
Deionized water 100
Nano silicon 0.2～1.0
PVAC polyvinylalcohol 17-99 2～4
PVAC polyvinylalcohol 17-88 3～6
Emulsifying agent 0.6～1.2
Vinyl acetate between to for plastic 80～100
Vinylformic acid 0.2～1.6
Ammonium persulphate 0.1～0.3
2,2,4-trimethylammonium 1,3-pentanediol diisobutyrate (TXIB) 1～7
Sanitas 0.1～0.3
Defoamer 0.01～0.04
Further, described emulsifying agent preferred emulsifier OP-10, emulsifying agent NP-40, emulsifying agent NP-10, emulsifying agent EFS-470, emulsifying agent LB-100;
The preferred magnificent section 981 of described sanitas, magnificent outstanding A-04, Xin Ke-OIC, WAP202, HM-01;
The preferred defoamer SPA-202 of described defoamer, defoamer 470, defoamer BEK-750, water-based froth breaking suds suppressor 1183.
Another object of the present invention provides the preparation method of above-mentioned water-based adhesion agent, and its method is as follows:
(1) weighs raw material by above-mentioned weight proportion;
(2) vinyl acetate between to for plastic, vinylformic acid are mixed the formation mix monomer;
(3) nano silicon is scattered in formation nano silicon solution in the deionized water;
(4) add nano silicon solution, PVAC polyvinylalcohol 17-99, PVAC polyvinylalcohol 17-88, defoamer in reactor, heat temperature raising to 85～95 ℃ pass vapour insulation 1～3 hour is cooled to 40～50 ℃ after the dissolving fully;
(5) in reactor, add 5%～20% of emulsifying agent and TXIB total amount again, stir;
(6) in reactor, continue to add 10%～20% of mix monomer total amount, be warming up to 65 ℃～75 ℃, the 30%-35% that adds the ammonium persulphate total amount, initiated polymerization generates seed emulsion, heat temperature raising to 75 ℃～85 ℃, drip mix monomer surplus and ammonium persulphate surplus again, dripped in 4～7 hours;
(7) drip the end post-heating and be warming up to 90 ℃, insulation slaking reaction 1 hour drips the TXIB surplus, drips in 20～40 minutes, and insulation reaction is cooled to 40～50 ℃ after 0.5～1 hour, add sanitas at last and stir, and detects discharging.
The present invention has the following advantages:
1, adds nano silicon before the reaction, utilize the small-size effect of nanoparticle self, surface effects, quantum effect by the Van der Waals force effect, significantly improves the cohesive strength of water-based adhesion agent, compare with the water-based adhesion agent that traditional method makes, bonding strength has improved more than 40%, simultaneously, has improved curing speed, weathering resistance of water-based adhesion agent etc.
2, before the water-based adhesion agent polymerization, after the polymerization, accurately drip asepsis environment-protecting respectively, do not contain the TXIB of phthalic anhydride class objectionable impurities, fragility, water tolerance, the glossiness of water-based adhesion agent glued membrane have been improved, improved the bonding strength of water-based adhesion agent, significantly reduced minimum film-forming temperature, minimum film-forming temperature than the water-based adhesion agent that makes with traditional method has descended 5～7 ℃, thereby has improved the resistance to low temperature of water-based adhesion agent.And in process for preparation, do not re-use Plasticizer DBP, reduced the toxicity of water-based adhesion agent, got rid of because of using Plasticizer DBP to cause carcinogenic possibility.
3, by dripping softening agent TXIB before the polymerization, regulate the denseness of water-based adhesion agent, thereby effectively control the viscosity of water-based adhesion agent.
4, TXIB has plasticity efficiently, has replaced the use of poisonous softening agent, environmental protection, and reduced production cost.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
(1) takes by weighing raw material by table 1 proportioning.
(2) vinyl acetate between to for plastic, vinylformic acid are mixed, make mix monomer.
(3) rotating speed of nano silicon with 1500 rev/mins is scattered in the deionized water, forms nano silicon solution.
(4) add nano silicon solution, polyvinyl alcohol, defoamer in reactor, heat temperature raising to 85 ℃ pass gas insulation 3 hours is cooled to 40 ℃ after the dissolving fully.
(5) in reactor, add 5% of emulsifying agent and TXIB total amount again, stir.
(6) continue to add 10% of mix monomer in reactor, be warming up to 65 ℃, add 30% of ammonium persulphate total amount, initiated polymerization generates seed emulsion, and heat temperature raising to 75 ℃ drips mix monomer and ammonium persulphate surplus again.
(7) drip to finish post-heating and be warming up to 90 ℃, insulation slaking reaction 1 hour drips the TXIB surplus, drips in 20 minutes, and insulation reaction is after 0.5 hour, is cooled to 40 ℃ and adds the sanitass back that stirs and detect discharging.
Embodiment 2:
(1) takes by weighing raw material by table 1 proportioning.
(2) vinyl acetate between to for plastic, vinylformic acid are mixed, make mix monomer.
(3) rotating speed of nano silicon with 1500 rev/mins is scattered in the deionized water, forms nano silicon solution.
(4) add nano silicon solution, polyvinyl alcohol, defoamer in reactor, heat temperature raising to 95 ℃ pass gas insulation 1 hour is cooled to 50 ℃ after the dissolving fully.
(5) in reactor, add 20% of emulsifying agent and TXIB total amount again, stir.
(6) continue to add 20% of mix monomer in reactor, be warming up to 75 ℃, add 35% of ammonium persulphate total amount, initiated polymerization generates seed emulsion, and heat temperature raising to 85 ℃ drips mix monomer and ammonium persulphate surplus again.
(7) drip to finish post-heating and be warming up to 90 ℃, insulation slaking reaction 1 hour drips the TXIB surplus, drips in 40 minutes, and insulation reaction is after 1 hour, is cooled to 50 ℃ and adds the sanitass back that stirs and detect discharging.
Embodiment 3:
(1) takes by weighing raw material by table 1 proportioning.
(2) vinyl acetate between to for plastic, vinylformic acid are mixed, make mix monomer.
(3) rotating speed of nano silicon with 1500 rev/mins is scattered in the deionized water, forms nano silicon solution.
(4) add nano silicon solution, polyvinyl alcohol, defoamer in reactor, heat temperature raising to 90 ℃ pass gas insulation 2 hours is cooled to 45 ℃ after the dissolving fully.
(5) in reactor, add 10% of emulsifying agent and TXIB total amount again, stir.
(6) continue to add 15% of mix monomer in reactor, be warming up to 70 ℃, add 33% of ammonium persulphate total amount, initiated polymerization generates seed emulsion, and heat temperature raising to 80 ℃ drips mix monomer and ammonium persulphate surplus again.
(7) drip to finish post-heating and be warming up to 90 ℃, insulation slaking reaction 1 hour drips the TXIB surplus, drips in 30 minutes, and insulation reaction is after 45 minutes, is cooled to 45 ℃ and adds the sanitass back that stirs and detect discharging.
The set of dispense ratio of table 1 embodiment 1-3
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Nano silicon | 0.2g | 1.0g | 0.6g |
| PVAC polyvinylalcohol 17-99 | 2g | 4g | 3g |
| PVAC polyvinylalcohol 17-88 | 6g | 4g | 3g |
| Deionized water | 100g | 100g | 100g |
| Emulsifying agent (OP-10) | 0.6g | 1.2g | 0.8g |
| Vinyl acetate between to for plastic | 80g | 100g | 90g |
| Vinylformic acid | 0.2g | 1.6g | 1.0g |
| Ammonium persulphate | 0.1g | 0.3g | 0.2g |
| 2,4-trimethylammonium 1,3-pentanediol diisobutyrate (TXIB) | 1g | 7g | 5g |
| Sanitas (magnificent section 981) | 0.1g | 0.3g | 0.2g |
| Defoamer (SPA-202) | 0.01g | 0.04g | 0.02g |
Embodiment 4: substantially the same manner as Example 1, difference is: emulsifying agent is emulsifying agent EFS-470, and sanitas is magnificent outstanding A-04, and defoamer is a defoamer 470.
Embodiment 5: substantially the same manner as Example 2, difference is: emulsifying agent is emulsifying agent LB-100, and sanitas is Xin Ke-OIC, and defoamer is defoamer BEK-750.
Embodiment 6: substantially the same manner as Example 3, difference is: emulsifying agent is emulsifying agent NP-40, and sanitas is sanitas WAP-202, and defoamer is a water-based froth breaking suds suppressor 1183.
Embodiment 7: substantially the same manner as Example 3, difference is: emulsifying agent is emulsifying agent NP-10, and sanitas is sanitas HM-01.
The detected result of the resultant water-based adhesion agent of the foregoing description 1-7 sees Table 2
Table 2 embodiment 1-7 detected result
In the foregoing description, the magnificent section 981 of described sanitas, magnificent outstanding A-04, Xin Ke-OIC, WAP202, HM-01 beautify factory from Shanxi Petro-Chemical Design Inst., Shanghai Hua Jie Fine Chemical Co., Ltd, the vast biochemical company limited in Nantong, Guangdong Dimei Biological Technology Co., Ltd., Linqu County, Shandong Province ring and buy gained.
Claims (4)
1. the preparation method of a water-based adhesion agent is characterized in that, comprises the following steps:
(1) weigh raw material by following weight proportion:
(2) vinyl acetate between to for plastic, vinylformic acid are mixed the formation mix monomer;
(3) nano silicon is scattered in formation nano silicon solution in the deionized water;
(4) add nano silicon solution, PVAC polyvinylalcohol 17-99, PVAC polyvinylalcohol 17-88, defoamer in reactor, heat temperature raising to 85～95 ℃ be incubateds 1～3 hour, are cooled to 40-50 ℃ after dissolving fully;
(5) in reactor, add emulsifying agent and 2,2 again, 4-trimethylammonium 1, the 5%-20% of 3-pentanediol diisobutyrate total amount stirs;
(6) 10%-20% of continuation adding mix monomer total amount in reactor, be warming up to 65 ℃～75 ℃, add 30%～35% of ammonium persulphate total amount, initiated polymerization generates seed emulsion, heat temperature raising to 75 ℃～85 ℃, drip mix monomer surplus and ammonium persulphate surplus again, dripped in 4～7 hours;
(7) drip the end post-heating and be warming up to 90 ℃, insulation slaking reaction 1 hour drips the TXIB surplus, drips in 20～40 minutes, and insulation reaction is cooled to 40～50 ℃ after 0.5～1 hour, add sanitas at last and stir, and detects discharging.
2. the preparation method of a kind of water-based adhesion agent according to claim 1 is characterized in that, described emulsifying agent is emulsifier op-10, emulsifying agent NP-40, emulsifying agent NP-10, emulsifying agent EFS-470 or emulsifying agent LB-100.
3. the preparation method of a kind of water-based adhesion agent according to claim 1 is characterized in that, described sanitas is Hua Ke-981, magnificent outstanding A-04, new OIC, WAP202 or HM-01.
4. the preparation method of a kind of water-based adhesion agent according to claim 1 is characterized in that, described defoamer is defoamer SPA-202, defoamer 470, defoamer BEK-750 or water-based froth breaking suds suppressor 1183.
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| CN101851475B (en) * | 2010-05-25 | 2011-09-21 | 江苏黑松林粘合剂厂有限公司 | Preparation method of energy-saving, environment-protecting and sag-resistant water-based instant adhesive |
| CN102516857B (en) * | 2011-11-25 | 2015-04-29 | 东营市盛基环保工程有限公司 | Formaldehyde-free cementing compound for profiled artificial board and preparation method thereof |
| CN110055004A (en) * | 2019-04-24 | 2019-07-26 | 中山市旭森涂层材料有限公司 | A kind of aqueous PP faces patch and its manufacture craft directly |
| CN113416507B (en) * | 2021-07-14 | 2023-02-10 | 湖北恒阳科技发展有限公司 | Ultrahigh-speed nozzle connecting adhesive and preparation method thereof |
| CN115368848A (en) * | 2022-09-19 | 2022-11-22 | 河南通宇胶业科技有限公司 | Manual hot-sticking veneer glue and preparation method thereof |
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| CN1342735A (en) * | 2001-09-30 | 2002-04-03 | 中山大学 | Aqueous emulsion type nm adhesive for paper or plastics and its preparing process |
| CN1544565A (en) * | 2003-11-24 | 2004-11-10 | 中国石油天然气集团公司 | Granulating process for thiofide CBS and preparing method thereof |
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