CN105367734A - High-adhesion aqueous polyurethane adhesive preparation method - Google Patents
High-adhesion aqueous polyurethane adhesive preparation method Download PDFInfo
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- CN105367734A CN105367734A CN201510800027.3A CN201510800027A CN105367734A CN 105367734 A CN105367734 A CN 105367734A CN 201510800027 A CN201510800027 A CN 201510800027A CN 105367734 A CN105367734 A CN 105367734A
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- aqueous polyurethane
- weight parts
- preparation
- polyurethane adhesives
- adhesion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4063—Mixtures of compounds of group C08G18/62 with other macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6212—Polymers of alkenylalcohols; Acetals thereof; Oxyalkylation products thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6644—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
Abstract
The present invention discloses a high-adhesion aqueous polyurethane adhesive preparation method comprising the following steps: (1) mixing process; (2) first-order reaction; (3) second-order reaction; and (4) tackifying treatment. The high-adhesion aqueous polyurethane adhesive preparation method is easy to operate and easy to implement, the adhesive prepared by the method is short in room temperature curing time, highly sticky, and broad in market prospects.
Description
Technical field
The present invention relates to sizing agent preparing technical field, particularly relate to a kind of preparation method of high-adhesion Aqueous Polyurethane Adhesives.
Background technology
Aqueous Polyurethane Adhesives, because having pollution-free, the feature such as transportation safety, good work environment, will become the main flow in sizing agent market gradually.But aqueous polyurethane (WPU) sizing agent exists the shortcomings such as the little and poor water resistance of slow, the first viscous force of rate of drying, especially cohesive strength is low has had a strong impact on its application.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of high-adhesion Aqueous Polyurethane Adhesives, can solve the above-mentioned shortcoming that Aqueous Polyurethane Adhesives exists.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of high-adhesion Aqueous Polyurethane Adhesives, comprises the steps:
(1) mixing treatment: add the polyester diol of 40 ~ 50 weight parts and the isoflurane chalcone diisocyanate of 20 ~ 30 weight parts in the reactor of band heated and stirred function, vacuumize dehydration;
(2) first order reaction: pass into rare gas element in the reactor in step (1) after processed, then add the dibutyl tin laurate of 1 ~ 3 weight part and the chainextender of 1 ~ 3 weight part under an inert atmosphere, heated and stirred makes it to react for some time;
(3) second order reaction: by the near certain temperature of reacted mixed solution in step (2), and then add the triethylamine of the polyol of 5 ~ 15 weight parts, the chainextender of 2 ~ 5 weight parts and 5 ~ 10 weight parts, stirring makes it reaction, obtains adhesive for polyurethane;
(4) tackified finish: will add the tackifier resin emulsion of 10 ~ 20 weight parts in the mixed solution obtained in step (3), under vacuumizing state, high-speed stirring mixes, and obtains described high-adhesion Aqueous Polyurethane Adhesives.
In a preferred embodiment of the present invention, in described step (1), described in vacuumize dehydration conditions and be: vacuum tightness 0.1 ~ 0.3MPa, time 1 ~ 1.5h; Water ratio after dehydration is 1 ~ 5%.
In a preferred embodiment of the present invention, in described step (2), described Heating temperature is 68 ~ 75 DEG C, and the time is 0.5 ~ 1h, and stir speed (S.S.) is 50 ~ 80r/min.
In a preferred embodiment of the present invention, in described step (3), described temperature is 35 ~ 45 DEG C, and the time is 1 ~ 3h, and stir speed (S.S.) is 50 ~ 80r/min.
In a preferred embodiment of the present invention, in described step (4), described vacuum tightness is 0.5 ~ 0.8MPa, and stir speed (S.S.) is 300 ~ 500r/min.
In a preferred embodiment of the present invention, described tackifier resin emulsion is aqueous tackifier Gum Rosin emulsion, C5 tackifier resin emulsion or C9 tackifier resin emulsion.
In a preferred embodiment of the present invention, described polyol is that mixing quality is than being the glucose of 1:1 ~ 2 and the mixture of polyvinyl alcohol.
The invention has the beneficial effects as follows: the preparation method of a kind of high-adhesion Aqueous Polyurethane Adhesives of the present invention, easy and simple to handle, easily realize, the self-vulcanizing time that prepared sizing agent has is short, and viscosity is large, wide market.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
A preparation method for high-adhesion Aqueous Polyurethane Adhesives, comprises the steps:
(1) mixing treatment: add the polyester diol of 40 weight parts and the isoflurane chalcone diisocyanate of 20 weight parts in the reactor of band heated and stirred function, vacuumize vacuum tightness 0.1MPa, then dewater 1.5h, makes the water ratio of mixture be 1 ~ 5%;
(2) first order reaction: pass into nitrogen gas in the reactor in step (1) after processed, then the dibutyl tin laurate of 1 weight part and the chainextender of 1 weight part is added in a nitrogen atmosphere, be heated to 68 DEG C, stir with the speed of 50r/min, make it to react 1h;
(3) second order reaction: by near 45 DEG C of reacted mixed solution in step (2), and then add the triethylamine of the polyol of 5 weight parts, the chainextender of 2 weight parts and 5 weight parts, stir 3h with the speed of 50r/min, make it reaction, obtain adhesive for polyurethane; Wherein, polyol is that mixing quality is than being the glucose of 1:1 and the mixture of polyvinyl alcohol;
(4) tackified finish: the aqueous tackifier Gum Rosin emulsion of 10 weight parts will be added in the mixed solution obtained in step (3), being evacuated to vacuum tightness is 0.5MPa, mix with the speed high-speed stirring of 300r/min, obtain described high-adhesion Aqueous Polyurethane Adhesives.
Embodiment 2
A preparation method for high-adhesion Aqueous Polyurethane Adhesives, comprises the steps:
(1) mixing treatment: add the polyester diol of 50 weight parts and the isoflurane chalcone diisocyanate of 30 weight parts in the reactor of band heated and stirred function, vacuumize vacuum tightness 0.3MPa, then dewater 1h, makes the water ratio of mixture be 1 ~ 5%;
(2) first order reaction: pass into nitrogen gas in the reactor in step (1) after processed, then the dibutyl tin laurate of 3 weight parts and the chainextender of 3 weight parts is added in a nitrogen atmosphere, be heated to 75 DEG C, stir with the speed of 80r/min, make it to react 0.5h;
(3) second order reaction: by near 35 DEG C of reacted mixed solution in step (2), and then add the triethylamine of the polyol of 15 weight parts, the chainextender of 5 weight parts and 10 weight parts, stir 1h with the speed of 80r/min, make it reaction, obtain adhesive for polyurethane; Wherein, polyol is that mixing quality is than being the glucose of 1:2 and the mixture of polyvinyl alcohol;
(4) tackified finish: will add the C5 tackifier resin emulsion of 20 weight parts in the mixed solution obtained in step (3), being evacuated to vacuum tightness is 0.8MPa, mixes with the speed high-speed stirring of 500r/min, obtains described high-adhesion Aqueous Polyurethane Adhesives.
Embodiment 3
A preparation method for high-adhesion Aqueous Polyurethane Adhesives, comprises the steps:
(1) mixing treatment: add the polyester diol of 45 weight parts and the isoflurane chalcone diisocyanate of 25 weight parts in the reactor of band heated and stirred function, vacuumize vacuum tightness 0.2MPa, then dewater 1h, makes the water ratio of mixture be 1 ~ 5%;
(2) first order reaction: pass into nitrogen gas in the reactor in step (1) after processed, then the dibutyl tin laurate of 2 weight parts and the chainextender of 2 weight parts is added in a nitrogen atmosphere, be heated to 70 DEG C, stir with the speed of 60r/min, make it to react 0.5h;
(3) second order reaction: by near 40 DEG C of reacted mixed solution in step (2), and then add the triethylamine of the polyol of 10 weight parts, the chainextender of 4 weight parts and 8 weight parts, stir 2h with the speed of 60r/min, make it reaction, obtain adhesive for polyurethane; Wherein, polyol is that mixing quality is than being the glucose of 1:1 and the mixture of polyvinyl alcohol;
(4) tackified finish: the C9 tackifier resin emulsion of 15 weight parts will be added in the mixed solution obtained in step (3), being evacuated to vacuum tightness is 0.50.8MPa, mix with the speed high-speed stirring of 400r/min, obtain described high-adhesion Aqueous Polyurethane Adhesives.
After tested, the adhesive solidification time of Aqueous Polyurethane Adhesives 30 DEG C time prepared by aforesaid method is 58 ~ 65min, and stripping strength is 100 ~ 110N/ (2.5cm).
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (7)
1. a preparation method for high-adhesion Aqueous Polyurethane Adhesives, is characterized in that, comprises the steps:
(1) mixing treatment: add the polyester diol of 40 ~ 50 weight parts and the isoflurane chalcone diisocyanate of 20 ~ 30 weight parts in the reactor of band heated and stirred function, vacuumize dehydration;
(2) first order reaction: pass into rare gas element in the reactor in step (1) after processed, then add the dibutyl tin laurate of 1 ~ 3 weight part and the chainextender of 1 ~ 3 weight part under an inert atmosphere, heated and stirred makes it to react for some time;
(3) second order reaction: by the near certain temperature of reacted mixed solution in step (2), and then add the triethylamine of the polyol of 5 ~ 15 weight parts, the chainextender of 2 ~ 5 weight parts and 5 ~ 10 weight parts, stirring makes it reaction, obtains adhesive for polyurethane;
(4) tackified finish: will add the tackifier resin emulsion of 10 ~ 20 weight parts in the mixed solution obtained in step (3), under vacuumizing state, high-speed stirring mixes, and obtains described high-adhesion Aqueous Polyurethane Adhesives.
2. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, in described step (1), described in vacuumize dehydration conditions and be: vacuum tightness 0.1 ~ 0.3MPa, time 1 ~ 1.5h; Water ratio after dehydration is 1 ~ 5%.
3. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, in described step (2), described Heating temperature is 68 ~ 75 DEG C, and the time is 0.5 ~ 1h, and stir speed (S.S.) is 50 ~ 80r/min.
4. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, in described step (3), described temperature is 35 ~ 45 DEG C, and the time is 1 ~ 3h, and stir speed (S.S.) is 50 ~ 80r/min.
5. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, in described step (4), described vacuum tightness is 0.5 ~ 0.8MPa, and stir speed (S.S.) is 300 ~ 500r/min.
6. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, described tackifier resin emulsion is aqueous tackifier Gum Rosin emulsion, C5 tackifier resin emulsion or C9 tackifier resin emulsion.
7. the preparation method of high-adhesion Aqueous Polyurethane Adhesives according to claim 1, is characterized in that, described polyol is that mixing quality is than being the glucose of 1:1 ~ 2 and the mixture of polyvinyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510800027.3A CN105367734A (en) | 2015-11-19 | 2015-11-19 | High-adhesion aqueous polyurethane adhesive preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510800027.3A CN105367734A (en) | 2015-11-19 | 2015-11-19 | High-adhesion aqueous polyurethane adhesive preparation method |
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| CN105367734A true CN105367734A (en) | 2016-03-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510800027.3A Pending CN105367734A (en) | 2015-11-19 | 2015-11-19 | High-adhesion aqueous polyurethane adhesive preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433541A (en) * | 2016-08-26 | 2017-02-22 | 枣阳市恒泰化工有限公司 | High-temperature-resistant high-bonding-performance waterborne polyurethane bonding agent and preparation method thereof |
| CN110368516A (en) * | 2019-07-06 | 2019-10-25 | 袁斯曼 | A kind of preparation method of high bonding degradable adhesive fibrin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845133A (en) * | 2010-04-01 | 2010-09-29 | 陕西科技大学 | Method for preparing natural polyhydroxy compound modified aqueous polyurethane emulsion |
| CN103013420A (en) * | 2012-11-30 | 2013-04-03 | 三棵树涂料股份有限公司 | Environment-friendly anti-yellowing water-based universal polyurethane adhesive |
| CN103589135A (en) * | 2013-10-17 | 2014-02-19 | 常州大学 | Preparation method of polyvinyl alcohol modified waterborne polyurethane |
-
2015
- 2015-11-19 CN CN201510800027.3A patent/CN105367734A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845133A (en) * | 2010-04-01 | 2010-09-29 | 陕西科技大学 | Method for preparing natural polyhydroxy compound modified aqueous polyurethane emulsion |
| CN103013420A (en) * | 2012-11-30 | 2013-04-03 | 三棵树涂料股份有限公司 | Environment-friendly anti-yellowing water-based universal polyurethane adhesive |
| CN103589135A (en) * | 2013-10-17 | 2014-02-19 | 常州大学 | Preparation method of polyvinyl alcohol modified waterborne polyurethane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433541A (en) * | 2016-08-26 | 2017-02-22 | 枣阳市恒泰化工有限公司 | High-temperature-resistant high-bonding-performance waterborne polyurethane bonding agent and preparation method thereof |
| CN110368516A (en) * | 2019-07-06 | 2019-10-25 | 袁斯曼 | A kind of preparation method of high bonding degradable adhesive fibrin |
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Application publication date: 20160302 |
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