CN102585754B - Solvent-type single-component polyurethane adhesive and preparation method thereof - Google Patents
Solvent-type single-component polyurethane adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a solvent-type single-component polyurethane adhesive and a preparation method thereof. The preparation method comprises the following steps: carrying out vacuumizing and water removal on 60-100 weight parts of polyether polyol; then adding 100 weight parts of methylene diphenyl diisocyanate into the polyether polyol; adding 40-80 weight parts of solvent and 0.5-2.5 weight parts of catalyst, and then reacting under stirring; and finally, adding 0.01-0.2 weight parts of stabilizing agent, reacting under stirring, filtering and discharging, and sealing and storing to obtain the polyurethane adhesive. Compared with the foam volume (3-4 times) of a common product, the foam volume of the adhesive is increased to 5-8 times, so that the adhesive can be integrated in a base material and a core material better, thereby achieving the best bonding state; and the storage period of the adhesive is prolonged from 3-6 months to 11 to 13 months, thereby solving the problem of inconvenience in production, application and storage of the adhesive for manufacturers and users.
Description
Technical field
The present invention relates to chemical sizing agent technical field, relate in particular to a kind of solvent-type single-component polyurethane adhesive and preparation method thereof.
Background technology
Because adhesive for polyurethane has toughness is adjustable, bonding process is simple, splendid resistance to low temperature and the features such as stability of item number, in recent years, become sizing agent with fastest developing speed at home and abroad.Adhesive for polyurethane generally is divided into five classes: polyisocyanates, two component response type, single-component response type, solvent-borne type and dispersion build, and wherein solvent-type single-component polyurethane adhesive is hydroxyl polyurethane and the solvent composition by high molecular; And the relatively two component sizing agents of single-component solvent-based adhesive have the characteristics such as easy to use of processing.So the purposes of solvent-type single-component polyurethane adhesive is more and more extensive, it can be used for many industries such as automobile, decorative heat preservation, Men Ye.But the gas release of present most of solvent-type single-component polyurethane adhesive is less, can not meet the bonding of some hole cores such as rock wool, perlite and base material; And the storage period of most of solvent-type single-component polyurethane adhesive is shorter, generally at 3 to 6 months, this has brought inconvenience to producer and user on producing and using, preserve; And in solvent-type single-component polyurethane adhesive, solvent commonly used is benzene kind solvent, contaminate environment, can not meet an urgent demand of client to its feature of environmental protection.
Research contents
The technical problem to be solved in the present invention is, the problems such as the storage period of solvent-type single-component polyurethane adhesive is shorter, gas release is less, a kind of solvent-type single-component polyurethane adhesive is provided, its gas release is large, storage period long, of many uses, easy construction and pollution-free, nontoxic, and its preparation technology is provided.
For achieving the above object, technical scheme of the present invention is: a kind of preparation method of solvent-type single-component polyurethane adhesive, the polyether glycol that at first its processing step is is 60-100 part by parts by weight vacuumizes and dewaters, then add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, add again the catalyzer that solvent that parts by weight are 40-80 part and umber are 0.5-2.5 part, stirring reaction, finally add the stablizer that parts by weight are 0.01-0.2 part, stirring reaction, filter discharging, sealing is preserved, and obtains adhesive for polyurethane.
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that its processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 95-120 ℃, the polyether glycol that is 60-100 part by parts by weight vacuumizes the 0.5-2h that dewaters;
2) be cooled to 50-80 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 55-90 ℃, and the time is 1-3h;
3) then be cooled to 40-70 ℃, add the catalyzer that solvent that parts by weight are 40-80 part and umber are 0.5-2.5 part, stirring reaction, the reaction times is 0.3-2h;
4) add the stablizer that parts by weight are 0.01-0.2 part, stirring reaction, the reaction times is 0.3-2h, filters discharging, sealing is preserved.
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that the parts by weight of described each component are as follows: diphenylmethanediisocyanate is that 100 parts, polyether glycol are that 70-90 part, solvent are that 50-70 part, catalyzer are 1-2 part, stablizer 0.05-0.15 part.
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that described diphenylmethanediisocyanate (MDI) is the liquid 4 of modification, the 4-diphenylmethanediisocyanate.
The preparation method of a kind of solvent-type single-component polyurethane adhesive of the present invention, described stablizer is organism, organic acid or mineral acid, is preferably any one or more mixtures that form by any part by weight in Benzoyl chloride, acetic acid, formic acid, lactic acid, hydrochloric acid, nitric acid, phosphoric acid.
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that described polyether glycol is any one or more mixtures that form by any part by weight in dihydroxyl polyoxytrimethylene ether (different molecular weight has 1000 and 2,000 two kinds), trihydroxy-polyoxygenated ether (molecular weight 3000).
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that described solvent is any one or more mixtures that form by any part by weight in acetone, ethyl acetate, methylene dichloride.
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention preferred version is that described catalyzer is dibutyl tin laurate, 2, any one or more mixtures that form by any part by weight in the 2-dual-morpholinyl diethyl ether.
The invention still further relates to a kind of solvent-type single-component polyurethane adhesive, it utilizes any preparation method of the claims 1-7 to make.
A kind of solvent-type single-component polyurethane adhesive of the present invention, its normal temperature preservation period is 11-13 month.
The performance of the solvent-type single-component polyurethane adhesive that the present invention is made has been carried out analyzing and testing, adopt the equipment such as sealing storage tank, blast dry oven, karl Fischer titration apparatus and gas chromatograph according to the method in volumetric method, observation and GB 18583-2008, it to be measured, its result is as shown in table 1.
The analyzing and testing result of table 1 solvent-type single-component polyurethane adhesive provided by the invention
The present invention, by the choosing and the optimization of each component concentration of solvent in adhesive for polyurethane and polyether glycol kind, increases substantially its foam performance.Acetone, ethyl acetate and methylene dichloride etc. are as good solvent, and its boiling point is low, can be vaporized by the reaction producing heat, and the foam generated body, in addition, its molecular weight is low, and expansion ratio is high, thereby effectively increase, has beaten foam expansion.The gas release of sizing agent doubly has been increased to 5-8 doubly by the 3-4 of usual production, can have better incorporated base material and core, reached best bond state.
Add stablizer in adhesive for polyurethane of the present invention, acid stabilizer can suppress the production reaction of biuret, thereby suppresses crosslinking reaction, simultaneously in energy and the alkaline substance in the major ingredient polyethers, thereby has increased shelf lives of sizing agent.
Extended to 11-13 month by 3-6 month the storage period of sizing agent, solved manufacturer and user produce and use, very large problem in preservation.
For the consideration of meeting the market requirement and environmental factors, the present invention utilizes green and environment-friendly solvent to replace benzene kind solvent, has realized the product nontoxic pollution-free.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 110 ℃, the dihydroxyl polyoxytrimethylene ether that is 60 parts by parts by weight vacuumizes the 1h that dewaters;
2) be cooled to 75 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 80 ℃, and the time is 1.5h;
3) then be cooled to 60 ℃, add the dibutyl tin laurate that ethyl acetate that parts by weight are 40 parts and umber are 0.5 part, stirring reaction, the reaction times is 0.3h;
4) add the Benzoyl chloride that parts by weight are 0.01 part, stirring reaction, the reaction times is 2h, filters discharging, sealing is preserved, and obtains adhesive for polyurethane.The adhesive for polyurethane that this embodiment is prepared has carried out the test of correlated performance, and test result is as table 2.
The analyzing and testing result of the adhesive for polyurethane of table 2 embodiment 1 preparation
Embodiment 2
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 95 ℃, the trihydroxy-polyoxygenated ether that the dihydroxyl polyoxygenated ether that is 62 parts by parts by weight and parts by weight are 38 parts vacuumizes the 2h that dewaters;
2) be cooled to 50 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 55 ℃, and the time is 3h;
3) then be cooled to 40 ℃, add the dibutyl tin laurate that methylene dichloride that parts by weight are 80 parts and umber are 2.5 parts, stirring reaction, the reaction times is 1.5h;
4) add Benzoyl chloride that parts by weight are 0.04 part and the formic acid of 0.03 part, stirring reaction, the reaction times is 0.5h, filters discharging, sealing is preserved, and obtains adhesive for polyurethane.The adhesive for polyurethane that this embodiment is prepared has carried out the test of correlated performance, and test result is as table 3.
The analyzing and testing result of the adhesive for polyurethane of table 3 embodiment 2 preparations
Embodiment 3
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 100 ℃, the dihydroxyl polyoxytrimethylene ether that is 73 parts by parts by weight vacuumizes the 1.5h that dewaters;
2) be cooled to 65 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 70 ℃, and the time is 2h;
3) then be cooled to 45 ℃, add acetone that parts by weight are 60 parts and umber be 1.3 parts 2, the 2-dual-morpholinyl diethyl ether, stirring reaction, the reaction times is 2h;
4) adding parts by weight is 0.05 part of hydrochloric acid, 0.05 part of nitric acid and 0.03 part of lactic acid, stirring reaction, and the reaction times is 0.7h, filters discharging, sealing is preserved, and obtains adhesive for polyurethane.The adhesive for polyurethane that this embodiment is prepared has carried out the test of correlated performance, and test result is as table 4.
The analyzing and testing result of the adhesive for polyurethane of table 4 embodiment 3 preparations
Embodiment 4
The preparation method's of a kind of solvent-type single-component polyurethane adhesive of the present invention processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 120 ℃, the dihydroxyl polyoxytrimethylene ether that is 80 parts by parts by weight vacuumizes the 0.5h that dewaters;
2) be cooled to 80 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 90 ℃, and the time is 1h;
3) then be cooled to 70 ℃, add dibutyl tin laurate that ethyl acetate that parts by weight are 10 parts, 40 parts of methylene dichloride and umber are 0.7 part, 0.9 part 2, the 2-dual-morpholinyl diethyl ether, stirring reaction, the reaction times is 1h;
4) adding parts by weight is 0.05 part of acetic acid and 0.15 part of phosphoric acid, stirring reaction, and the reaction times is 0.3h, filters discharging, sealing is preserved, and obtains adhesive for polyurethane.The adhesive for polyurethane that this embodiment is prepared has carried out the test of correlated performance, and test result is as table 5.
The analyzing and testing result of the adhesive for polyurethane of table 5 embodiment 4 preparations
Claims (5)
1. the preparation method of a solvent-type single-component polyurethane adhesive, is characterized in that, its processing step is:
1), under the condition that in vacuum tightness be more than 0.09Mpa, temperature is 95-120 ℃, the polyether glycol that is 60-100 part by parts by weight vacuumizes the 0.5-2h that dewaters;
2) be cooled to 50-80 ℃, start stirring, add the diphenylmethanediisocyanate that parts by weight are 100 parts to be reacted, temperature of reaction is controlled at 55-90 ℃, and the time is 1-3h;
3) then be cooled to 40-70 ℃, add the catalyzer that solvent that parts by weight are 40-80 part and umber are 0.5-2.5 part, stirring reaction, the reaction times is 0.3-2h;
4) add the stablizer that parts by weight are 0.05-0.15 part, stirring reaction, the reaction times is 0.3-2h, filters discharging, sealing is preserved, and obtains adhesive for polyurethane;
Described stablizer is any one or more mixtures that form by any part by weight in Benzoyl chloride, acetic acid, formic acid, lactic acid, hydrochloric acid, nitric acid, phosphoric acid;
Described solvent is any one or more mixtures that form by any part by weight in acetone, ethyl acetate, methylene dichloride;
Described polyether glycol is that molecular weight is any one or more mixtures that form by any part by weight in 1000 or 2000 dihydroxyl polyoxytrimethylene ethers, the molecular weight trihydroxy-polyoxygenated ether that is 3000.
2. the preparation method of a kind of solvent-type single-component polyurethane adhesive according to claim 1, it is characterized in that, the parts by weight of described each component are as follows: diphenylmethanediisocyanate is that 100 parts, polyether glycol are that 70-90 part, solvent are that 50-70 part, catalyzer are 1-2 part, stablizer 0.05-0.15 part.
3. the preparation method of a kind of solvent-type single-component polyurethane adhesive according to claim 1, it is characterized in that, described catalyzer is dibutyl tin laurate, 2, any one or more mixtures that form by any part by weight in the two morpholinyl ethyl ethers of 2-.
4. a solvent-type single-component polyurethane adhesive, is characterized in that, utilizes any preparation method of the claims 1-3 to make.
5. a kind of solvent-type single-component polyurethane adhesive according to claim 4, is characterized in that, its normal temperature preservation period is 11-13 month.
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| CN 201210012211 CN102585754B (en) | 2012-01-13 | 2012-01-13 | Solvent-type single-component polyurethane adhesive and preparation method thereof |
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| CN 201210012211 CN102585754B (en) | 2012-01-13 | 2012-01-13 | Solvent-type single-component polyurethane adhesive and preparation method thereof |
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| CN103013425B (en) * | 2012-12-27 | 2014-06-04 | 南通高盟新材料有限公司 | Adhesive for solid wood floor and preparation method thereof |
| CN104046314A (en) * | 2013-03-12 | 2014-09-17 | 杭州宝力物资再生利用有限公司 | Diphenyl-methane-diisocyanate (MDI)-type mono-component moisture-curable polyurethane adhesive and manufacturing method thereof |
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| CN106883807A (en) * | 2017-03-10 | 2017-06-23 | 上海回天新材料有限公司 | One-component solvent-free type polyurethane adhesive and its preparation method and application |
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| CN111320959B (en) * | 2020-03-24 | 2021-08-06 | 上海汉司实业有限公司 | Polyurethane structural adhesive and preparation method and application thereof |
| CN111517736B (en) * | 2020-04-29 | 2022-02-11 | 廊坊市北辰创业树脂材料股份有限公司 | Light non-combustible sound insulation board and preparation method thereof |
| CN113462340A (en) * | 2021-03-31 | 2021-10-01 | 山西维力固科技股份有限公司 | Non-combustible solvent type single-component polyurethane adhesive and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130680A (en) * | 2007-09-29 | 2008-02-27 | 山东东大一诺威聚氨酯有限公司 | Environment protection type single-component polyurethane binder, production and use method of the same |
| CN101781518A (en) * | 2010-02-08 | 2010-07-21 | 广州市台实防水补强有限公司 | Single component colour polyurethane waterproof paint and preparation method thereof |
| CN101805582A (en) * | 2010-03-17 | 2010-08-18 | 山东德宝建筑节能技术有限公司 | Polyurethane adhesive |
| US20110154772A1 (en) * | 2009-12-31 | 2011-06-30 | Bostik, Inc. | Moisture Curable Adhesive Composition and Method for Installing Hardwood Floors |
-
2012
- 2012-01-13 CN CN 201210012211 patent/CN102585754B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130680A (en) * | 2007-09-29 | 2008-02-27 | 山东东大一诺威聚氨酯有限公司 | Environment protection type single-component polyurethane binder, production and use method of the same |
| US20110154772A1 (en) * | 2009-12-31 | 2011-06-30 | Bostik, Inc. | Moisture Curable Adhesive Composition and Method for Installing Hardwood Floors |
| CN101781518A (en) * | 2010-02-08 | 2010-07-21 | 广州市台实防水补强有限公司 | Single component colour polyurethane waterproof paint and preparation method thereof |
| CN101805582A (en) * | 2010-03-17 | 2010-08-18 | 山东德宝建筑节能技术有限公司 | Polyurethane adhesive |
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