CN111393602A - Polyvinyl alcohol modified water-absorbent polyurethane and preparation method thereof - Google Patents
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G2230/00—Compositions for preparing biodegradable polymers
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- 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
- C08K3/20—Oxides; Hydroxides
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Abstract
The invention discloses polyvinyl alcohol modified water-absorbent polyurethane and a preparation method thereof, belonging to the technical field of water-absorbent polyurethane, and comprising a group A raw material and a group B raw material: the group A raw materials are prepared from the following materials in percentage; the content of oligomeric diol is 6-10%, the content of diisocyanate is 15-25%, the content of corundum micropowder is 10-15%, the content of copper powder is 10-15%, the content of polyester diol is 20-30%, the content of chain extender is 3-6% and the content of polyvinyl alcohol is 30-35%, the material with higher tensile strength is obtained by adding the corundum micropowder, the peel strength and the tensile strength of the material with higher tensile strength are obviously improved before being modified, and the polyvinyl alcohol modified polyurethanes of A type and B type are combined to obtain the polyurethane alcohol modified water-soluble polyurethane material, wherein the peel strength and the tensile strength of the polyurethane alcohol modified water-soluble polyurethane material are obviously improved before being modified, so that the higher elongation at break is kept, the polyurethane modified water-soluble polyurethane material can be repeatedly used, and the environment is protected and energy is saved.
Description
Technical Field
The invention relates to the technical field of water-absorbent polyurethane, in particular to polyvinyl alcohol modified water-absorbent polyurethane and a preparation method thereof.
Background
Polyurethane is a high molecular material with excellent performance, has the advantages of low temperature resistance, chemical corrosion resistance, friction resistance, good flexibility and the like, and is widely applied as coating, adhesive, fabric finishing agent and the like at present. The waterborne polyurethane takes water as a dispersion medium, does not contain or contain a small amount of organic solvent, has the advantages of low toxicity, nonflammability, low pollution and the like compared with the traditional solvent type polyurethane, and is an environment-friendly material. Meanwhile, the molecular structure of the waterborne polyurethane contains a large amount of carbamate groups, so that the waterborne polyurethane is a biodegradable material. In recent years, waterborne polyurethane has a good market prospect and is widely applied to various industries. However, the price of the waterborne polyurethane is relatively high, the strength is not high, and the high temperature resistance is poor, so that the further application of the waterborne polyurethane is limited.
In the preparation method of the polyvinyl alcohol modified waterborne polyurethane disclosed in application No. CN201310484625.5, an urethane bond in a waterborne polyurethane chain segment and a hydroxyl group in polyvinyl alcohol can form an intermolecular hydrogen bond effect, so that the polyurethane chain segment and the hydroxyl group in the polyvinyl alcohol have good compatibility, the price of the polyvinyl alcohol is relatively low, the cost of the material can be reduced while the mechanical property of the material is met by adding the polyvinyl alcohol into the waterborne polyurethane, but the strength is low, and the strength of the breaking elongation is also low.
Disclosure of Invention
The invention aims to provide polyvinyl alcohol modified water-absorbent polyurethane and a preparation method thereof, and the obtained polyvinyl alcohol modified water-soluble polyurethane material has the advantages that the peel strength and the tensile strength are obviously improved compared with those before modification, higher elongation at break is kept, the material can be repeatedly used, the environment is protected, and energy is saved, so that the problems in the background art are solved.
In order to achieve the purpose, the invention provides the following technical scheme: the polyvinyl alcohol modified water-absorbent polyurethane comprises a group A raw material and a group B raw material: the group A raw materials are prepared from the following materials in percentage; 6-10% of oligomeric diol, 15-25% of diisocyanate, 10-15% of corundum micropowder, 10-15% of copper powder, 20-30% of polyester diol, 3-6% of chain extender and 30-35% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; 15-20% of trimethylene carbonate, 23-29% of caprolactone, 37-43% of powdery anhydride, 16-25% of acrylic acid and 30-35% of polyvinyl alcohol.
Further, the raw material A comprises 7-9% of oligomeric diol, 18-20% of diisocyanate, 12-14% of corundum micropowder, 12-14% of copper powder, 24-26% of polyester diol, 4-5% of chain extender and 32-34% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; 16-18% of trimethylene carbonate, 25-27% of caprolactone, 39-41% of powdery anhydride, 18-20% of acrylic acid and 32-34% of polyvinyl alcohol.
Further, the raw materials of the group A comprise 8% of oligomeric diol, 19% of diisocyanate, 13% of corundum micropowder, 13% of copper powder, 25% of polyester diol, 4% of chain extender and 33% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; the content of trimethylene carbonate was 17%, the content of caprolactone was 26%, the content of powdery acid anhydride was 40%, the content of acrylic acid was 19%, and the content of polyvinyl alcohol was 33%.
Further, modified epoxy resin is added in the process of mixing and stirring the raw materials of the group A at the temperature of 150-200 ℃.
The other technology provided by the invention comprises a preparation method of polyvinyl alcohol modified water-absorbent polyurethane, which comprises the following steps:
s1: adding two equal parts of polyvinyl alcohol into water, putting the mixture into an oven, heating the mixture to 90-100 ℃, stirring the mixture for 3-5 hours until the mixture is completely dissolved, and pouring the mixture into the same container A and container B respectively;
s2: pouring the oligomeric diol and the diisocyanate into a container A, stirring and mixing, adding diethyl tin, stirring and reacting for 3-5 hours at 80-100 ℃ to obtain a polyurethane prepolymer, and adding a small amount of acetone to degrade and bond in the reaction process;
s3: cooling the reactant obtained in the step S2 to below 60 ℃, then adding copper powder and corundum micropowder, adding water for high-speed dispersion, adding a chain extender, performing chain extension reaction for 20-30 minutes at 60-70 ℃, and then vacuumizing to remove hot gas to obtain a waterborne polyurethane emulsion with the solid content of 10-30%;
s4: adding the emulsion of S3 into a container A, and mechanically stirring to uniformly mix the emulsion to obtain class A polyvinyl alcohol modified polyurethane;
s5: dissolving anhydride in an organic solvent, adding trimethylene carbonate and caprolactone, heating and stirring to perform heterogeneous reaction, and esterifying partial hydroxyl formed after copolymerization and modification of acrylic acid to introduce carboxyl to obtain a waterborne polyurethane emulsion with the solid content of 12-25%;
s6: adding the emulsion of S5 into a container B, mechanically stirring to uniformly mix the emulsion and the emulsion to obtain B type polyvinyl alcohol modified polyurethane, adding the B type polyvinyl alcohol modified polyurethane and the A type polyvinyl alcohol modified polyurethane into a vacuum rotary instrument for concentration, slowly adding 2 times of deionized water into the concentrated solution while stirring until the volume is one eighth, cooling for 2-4h in an environment at 4 ℃, and centrifuging for 10min at 1200rpm to obtain the mixed polyvinyl alcohol modified water-absorbing polyurethane.
Further, in S5, white corundum micropowder and copper powder are added into the aqueous polyurethane emulsion, wherein the mass of the corundum micropowder and the copper powder accounts for 6-12% of the total mass of the oligodiol and the diisocyanate.
Compared with the prior art, the invention has the beneficial effects that: the water absorption mechanism of the polyvinyl alcohol modified polyurethane of the A type is that the content of polyglycol and diisocyanate is low, the corundum micropowder is added, the material with higher tensile strength is provided, the peel strength and the tensile strength of the material are obviously improved compared with those before modification, so that the water-absorbing gel has high strength, the polyvinyl alcohol modified polyurethane of the A type and the B type are combined, the peel strength and the tensile strength of the obtained polyvinyl alcohol modified water-soluble polyurethane material are obviously improved compared with those before modification, and higher elongation at break is kept.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
referring to fig. 1, a polyvinyl alcohol-modified water-absorbent polyurethane includes group a raw materials and group B raw materials: the group A raw materials are prepared from the following materials in percentage; 6-10% of oligomeric diol, 15-25% of diisocyanate, 10-15% of corundum micropowder, 10-15% of copper powder, 20-30% of polyester diol, 3-6% of chain extender and 30-35% of polyvinyl alcohol, and modified epoxy resin is also added in the process of mixing and stirring the raw materials of the group A at the temperature of 150-200 ℃.
The group B raw materials are prepared from the following materials in percentage; 15-20% of trimethylene carbonate, 23-29% of caprolactone, 37-43% of powdery anhydride, 16-25% of acrylic acid and 30-35% of polyvinyl alcohol.
Example two:
the group A raw materials comprise 7-9% of oligomeric diol, 18-20% of diisocyanate, 12-14% of corundum micropowder, 12-14% of copper powder, 24-26% of polyester diol, 4-5% of chain extender and 32-34% of polyvinyl alcohol, and modified epoxy resin is also added in the process of mixing and stirring the group A raw materials at the temperature of 150-200 ℃.
The group B raw materials are prepared from the following materials in percentage; 16-18% of trimethylene carbonate, 25-27% of caprolactone, 39-41% of powdery anhydride, 18-20% of acrylic acid and 32-34% of polyvinyl alcohol.
Example three:
the group A raw materials comprise 8% of oligomeric diol, 19% of diisocyanate, 13% of corundum micropowder, 13% of copper powder, 25% of polyester diol, 4% of chain extender and 33% of polyvinyl alcohol, and modified epoxy resin is added in the process of mixing and stirring the group A raw materials at the temperature of 150-200 ℃.
The group B raw materials are prepared from the following materials in percentage; the content of trimethylene carbonate was 17%, the content of caprolactone was 26%, the content of powdery acid anhydride was 40%, the content of acrylic acid was 19%, and the content of polyvinyl alcohol was 33%.
And adding modified epoxy resin into the group A raw materials in the process of mixing and stirring at the temperature of 150-200 ℃.
In order to better show the flow of preparing the water-absorbent polyurethane, this example now proposes a method for preparing polyvinyl alcohol-modified water-absorbent polyurethane, which includes the following steps:
the method comprises the following steps: adding two equal parts of polyvinyl alcohol into water, putting the mixture into an oven, heating the mixture to 90-100 ℃, stirring the mixture for 3-5 hours until the mixture is completely dissolved, and pouring the mixture into the same container A and container B respectively;
step two: pouring the oligomeric diol and the diisocyanate into a container A, stirring and mixing, adding diethyl tin, stirring and reacting for 3-5 hours at 80-100 ℃ to obtain a polyurethane prepolymer, and adding a small amount of acetone to degrade and bond in the reaction process;
step three: cooling the reactant obtained in the step S2 to below 60 ℃, then adding copper powder and corundum micropowder, adding water for high-speed dispersion, adding a chain extender, performing chain extension reaction for 20-30 minutes at 60-70 ℃, and then vacuumizing to remove hot gas to obtain a waterborne polyurethane emulsion with the solid content of 10-30%;
step four: adding the emulsion of S3 into a container A, and mechanically stirring to uniformly mix the emulsion to obtain class A polyvinyl alcohol modified polyurethane;
step five: dissolving anhydride in an organic solvent, adding trimethylene carbonate and caprolactone, heating and stirring to perform heterogeneous reaction, esterifying partial hydroxyl formed after acrylic acid copolymerization modification to introduce carboxyl to obtain a waterborne polyurethane emulsion with the solid content of 12-25%, and adding white corundum micropowder and copper powder into the waterborne polyurethane emulsion to account for 6-12% of the total mass of the oligomeric diol and the diisocyanate;
step six: adding the emulsion of S5 into a container B, mechanically stirring to uniformly mix the emulsion and the emulsion to obtain B type polyvinyl alcohol modified polyurethane, adding the B type polyvinyl alcohol modified polyurethane and the A type polyvinyl alcohol modified polyurethane into a vacuum rotary instrument for concentration, slowly adding 2 times of deionized water into the concentrated solution while stirring until the volume is one eighth, cooling for 2-4h in an environment at 4 ℃, and centrifuging for 10min at 1200rpm to obtain the mixed polyvinyl alcohol modified water-absorbing polyurethane.
Comparative example one:
the group A raw materials comprise 8% of oligomeric diol, 19% of diisocyanate, 13% of corundum micropowder, 13% of copper powder, 25% of polyester diol, 4% of chain extender and 33% of polyvinyl alcohol, and modified epoxy resin is also added in the process of mixing and stirring the group A raw materials at the temperature of 150-200 ℃;
the group B raw materials are prepared from the following materials in percentage; the content of trimethylene carbonate was 17%, the content of caprolactone was 26%, the content of acrylic acid was 19% and the content of polyvinyl alcohol was 33%.
Comparative example two:
the group A raw materials comprise 8% of oligomeric diol, 19% of diisocyanate, 13% of copper powder, 25% of polyester diol, 4% of chain extender and 33% of polyvinyl alcohol, and modified epoxy resin is also added in the process of mixing and stirring the group A raw materials at the temperature of 150-200 ℃;
the group B raw materials are prepared from the following materials in percentage; the content of trimethylene carbonate was 17%, the content of caprolactone was 26%, the content of powdery acid anhydride was 40%, the content of acrylic acid was 19%, and the content of polyvinyl alcohol was 33%.
Comparing the first, second and third examples with the first and second comparative examples in Table I
TABLE-Effect of polyvinyl alcohol content on Properties of modified materials
The water absorption mechanism of the class A polyvinyl alcohol modified polyurethane is that the content of oligomeric diol and diisocyanate is low, the material with higher tensile strength is obtained by adding corundum micropowder, and the peel strength and the tensile strength of the material are obviously improved compared with those of the material before modification, so that the water-absorbing gel has high strength.
The polyvinyl alcohol modified polyurethane of B class is dissolved in organic solvent through anhydride, then trimethylene carbonate and caprolactone are added for heating and stirring, heterogeneous reaction is carried out, the copolymer is converted into a vinyl alcohol phase and acrylate phase block copolymer composite structure after saponification, the vinyl alcohol phase is partially crystallized during preparation, a crystallization area plays a role in crosslinking, the polyvinyl alcohol modified polyurethane of A class and B class is combined, the peel strength and the tensile strength of the obtained polyvinyl alcohol modified water-soluble polyurethane material are obviously improved compared with those before modification, and higher elongation at break is kept.
In summary, the following steps: the water absorption mechanism of the polyvinyl alcohol modified water-soluble polyurethane of the class A is that the content of polydihydric alcohol and diisocyanate is low, the material with higher tensile strength is obtained by adding corundum micropowder, the peel strength and the tensile strength of the material are obviously improved compared with those before modification, so that the water-absorbing gel has high strength, the peel strength and the tensile strength of the obtained polyvinyl alcohol modified water-soluble polyurethane material are obviously improved compared with those before modification by combining the class A and the class B polyvinyl alcohol modified polyurethanes, and higher elongation at break is kept.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (6)
1. The polyvinyl alcohol modified water-absorbent polyurethane is characterized by comprising a group A raw material and a group B raw material: the group A raw materials are prepared from the following materials in percentage; 6-10% of oligomeric diol, 15-25% of diisocyanate, 10-15% of corundum micropowder, 10-15% of copper powder, 20-30% of polyester diol, 3-6% of chain extender and 30-35% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; 15-20% of trimethylene carbonate, 23-29% of caprolactone, 37-43% of powdery anhydride, 16-25% of acrylic acid and 30-35% of polyvinyl alcohol.
2. The polyvinyl alcohol-modified water-absorbent polyurethane as claimed in claim 1, wherein the group A raw materials comprise 7 to 9% of oligomeric diol, 18 to 20% of diisocyanate, 12 to 14% of corundum micropowder, 12 to 14% of copper powder, 24 to 26% of polyester diol, 4 to 5% of chain extender and 32 to 34% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; 16-18% of trimethylene carbonate, 25-27% of caprolactone, 39-41% of powdery anhydride, 18-20% of acrylic acid and 32-34% of polyvinyl alcohol.
3. The polyvinyl alcohol-modified water-absorbent polyurethane according to claim 1, wherein the group A raw material comprises 8% of oligomeric diol, 19% of diisocyanate, 13% of corundum micropowder, 13% of copper powder, 25% of polyester diol, 4% of chain extender and 33% of polyvinyl alcohol;
the group B raw materials are prepared from the following materials in percentage; the content of trimethylene carbonate was 17%, the content of caprolactone was 26%, the content of powdery acid anhydride was 40%, the content of acrylic acid was 19%, and the content of polyvinyl alcohol was 33%.
4. The polyvinyl alcohol-modified water-absorbent polyurethane according to claim 1, wherein the group A raw materials are further added with a modified epoxy resin during mixing and stirring at a temperature of 150-200 ℃.
5. The method for preparing polyvinyl alcohol-modified water-absorbent polyurethane according to claim 1, comprising the steps of:
s1: adding two equal parts of polyvinyl alcohol into water, putting the mixture into an oven, heating the mixture to 90-100 ℃, stirring the mixture for 3-5 hours until the mixture is completely dissolved, and pouring the mixture into the same container A and container B respectively;
s2: pouring the oligomeric diol and the diisocyanate into a container A, stirring and mixing, adding diethyl tin, stirring and reacting for 3-5 hours at 80-100 ℃ to obtain a polyurethane prepolymer, and adding a small amount of acetone to degrade and bond in the reaction process;
s3: cooling the reactant obtained in the step S2 to below 60 ℃, then adding copper powder and corundum micropowder, adding water for high-speed dispersion, adding a chain extender, performing chain extension reaction for 20-30 minutes at 60-70 ℃, and then vacuumizing to remove hot gas to obtain a waterborne polyurethane emulsion with the solid content of 10-30%;
s4: adding the emulsion of S3 into a container A, and mechanically stirring to uniformly mix the emulsion to obtain class A polyvinyl alcohol modified polyurethane;
s5: dissolving anhydride in an organic solvent, adding trimethylene carbonate and caprolactone, heating and stirring to perform heterogeneous reaction, and esterifying partial hydroxyl formed after copolymerization and modification of acrylic acid to introduce carboxyl to obtain a waterborne polyurethane emulsion with the solid content of 12-25%;
s6: adding the emulsion of S5 into a container B, mechanically stirring to uniformly mix the emulsion and the emulsion to obtain B type polyvinyl alcohol modified polyurethane, adding the B type polyvinyl alcohol modified polyurethane and the A type polyvinyl alcohol modified polyurethane into a vacuum rotary instrument for concentration, slowly adding 2 times of deionized water into the concentrated solution while stirring until the volume is one eighth, cooling for 2-4h in an environment at 4 ℃, and centrifuging for 10min at 1200rpm to obtain the mixed polyvinyl alcohol modified water-absorbing polyurethane.
6. The method for preparing polyvinyl alcohol modified water-absorbent polyurethane as claimed in claim 5, wherein white corundum micropowder and copper powder account for 6-12% of the total mass of the oligodiol and the diisocyanate by adding the white corundum micropowder and the copper powder into the polyethylene aqueous polyurethane emulsion in S5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115159966A (en) * | 2022-06-30 | 2022-10-11 | 安徽瑞泰新材料科技有限公司 | High-strength refractory castable and preparation method thereof |
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| CN103589135A (en) * | 2013-10-17 | 2014-02-19 | 常州大学 | Preparation method of polyvinyl alcohol modified waterborne polyurethane |
| CN107163217A (en) * | 2017-05-22 | 2017-09-15 | 昆山嘉力普制版胶粘剂油墨有限公司 | A kind of preparation method of Nano diamond modified aqueous polyurethane |
| CN107267053A (en) * | 2017-05-12 | 2017-10-20 | 河北晨阳工贸集团有限公司 | Super industrial keyboard paint of water-fast, abrasion-resistance water and preparation method thereof |
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- 2020-05-27 CN CN202010462524.8A patent/CN111393602A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103589135A (en) * | 2013-10-17 | 2014-02-19 | 常州大学 | Preparation method of polyvinyl alcohol modified waterborne polyurethane |
| CN107267053A (en) * | 2017-05-12 | 2017-10-20 | 河北晨阳工贸集团有限公司 | Super industrial keyboard paint of water-fast, abrasion-resistance water and preparation method thereof |
| CN107163217A (en) * | 2017-05-22 | 2017-09-15 | 昆山嘉力普制版胶粘剂油墨有限公司 | A kind of preparation method of Nano diamond modified aqueous polyurethane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115159966A (en) * | 2022-06-30 | 2022-10-11 | 安徽瑞泰新材料科技有限公司 | High-strength refractory castable and preparation method thereof |
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Application publication date: 20200710 |