CN117186825A - Foaming waterproof polyurethane environment-friendly adhesive and preparation method thereof - Google Patents
Foaming waterproof polyurethane environment-friendly adhesive and preparation method thereof Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims abstract description 72
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 72
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 71
- 239000004814 polyurethane Substances 0.000 title claims abstract description 71
- 238000005187 foaming Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 121
- 239000003607 modifier Substances 0.000 claims abstract description 64
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 59
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 59
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 55
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- 239000011159 matrix material Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims description 105
- 238000003756 stirring Methods 0.000 claims description 53
- 239000010456 wollastonite Substances 0.000 claims description 43
- 229910052882 wollastonite Inorganic materials 0.000 claims description 43
- -1 rare earth lanthanum sulfate Chemical class 0.000 claims description 32
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 32
- 238000000498 ball milling Methods 0.000 claims description 27
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229920001661 Chitosan Polymers 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 235000011056 potassium acetate Nutrition 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 230000002457 bidirectional effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 239000008055 phosphate buffer solution Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- RPDJEKMSFIRVII-UHFFFAOYSA-N oxomethylidenehydrazine Chemical group NN=C=O RPDJEKMSFIRVII-UHFFFAOYSA-N 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a foaming waterproof polyurethane environment-friendly adhesive, which comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 10-15% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 5-10% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix. The polyurethane environment-friendly adhesive adopts a polyurethane adhesive matrix to match with a flaky graphene modifier and nano silicon dioxide double-adjusting agent, and the two are improved in a bidirectional coordination manner to cooperate together, so that the waterproof performance and the heat resistance of a product system are improved in a coordinated manner, and the service efficiency of the product is improved.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a foaming waterproof polyurethane environment-friendly adhesive and a preparation method thereof.
Background
Polyurethane is a high molecular compound containing isocyanate groups or amino isocyanate groups, which is prepared by reacting dihydric or polyhydric alcohol with isocyanate, and can be used for preparing foams, adhesives, elastomers and the like, the waterproof performance and heat resistance of the existing polyurethane adhesive are difficult to coordinate and improve, and the service efficiency of the product is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a foaming waterproof polyurethane environment-friendly adhesive and a preparation method thereof, so as to solve the problems in the background art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a foaming waterproof polyurethane environment-friendly adhesive, which comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 10-15% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 5-10% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
Preferably, the preparation method of the flaky graphene modifier comprises the following steps:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 1-2h, and the preparation method comprises the steps of washing and drying after ultrasonic treatment is finished;
s02: adding wollastonite modifier accounting for 5-10% of the total weight of the S01 product into the S01 product, ball milling for 1-2h at the rotating speed of 1000-1500r/min, and obtaining a ball milling body after ball milling;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 2-5% of the total weight of the rare earth lanthanum sulfate solution, and uniformly stirring to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
Preferably, the mixed acid solution is prepared by mixing hydrochloric acid solution with the mass fraction of 2%, citric acid solution with the mass fraction of 5% and sulfuric acid solution with the mass fraction of 8% according to the weight ratio of 4:1:1.
Preferably, the rare earth lanthanum sulfate solution has a mass fraction of 5-10% and the chitosan solution has a mass fraction of 4-6%.
Preferably, the rotation speed of the stirring modification treatment is 500-1000r/min, and the stirring time is 1-2h.
Preferably, the preparation method of the wollastonite modifier comprises the following steps:
adding 5-10 parts of wollastonite into 20-30 parts of ethanol solvent, uniformly stirring, adding 2-5 parts of phosphoric acid buffer solution and 1-3 parts of potassium acetate solution, and stirring fully to obtain wollastonite liquid;
and (3) the wollastonite liquid is sent into 3-5 times of sodium dodecyl sulfate solution to be stirred uniformly, and then the wollastonite liquid is washed and dried to obtain the wollastonite modifier.
Preferably, the pH of the phosphate buffer solution is 5.0; the mass fraction of the potassium acetate solution is 5-9%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%.
Preferably, the preparation method of the nano silicon dioxide double-dispensing agent comprises the following steps:
the nano silicon dioxide is sent to 120-130 ℃ for heat treatment for 1-2h, then cooled to 45-50 ℃ at the speed of 1-3 ℃/min, the nano silicon dioxide agent is obtained, yttrium nitrate solution with the total amount of 10-15% of the nano silicon dioxide agent and triisostearyl isopropyl titanate with the total amount of 1-3% of the nano silicon dioxide agent are added into the nano silicon dioxide agent, ball milling is carried out for 1-2h at the speed of 1000-1500r/min, and then water washing and drying are carried out, thus obtaining the nano silicon dioxide double-dispensing agent.
Preferably, the yttrium nitrate solution has a mass fraction of 3-6%.
The invention also provides a preparation method of the foaming waterproof polyurethane environment-friendly adhesive, which comprises the following steps: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
Compared with the prior art, the invention has the following beneficial effects:
the polyurethane environment-friendly adhesive adopts a polyurethane adhesive matrix to match with a flaky graphene modifier and nano silicon dioxide double-adjusting agent, and the two are improved in a bidirectional coordination manner to cooperate together, so that the waterproof performance and the heat resistance of a product system are improved in a coordinated manner, and the service efficiency of the product is improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The environment-friendly polyurethane adhesive comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 10-15% of the total weight of the polyurethane adhesive matrix and nano silicon dioxide double-dispensing agent accounting for 5-10% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
The preparation method of the flaky graphene modifier in the embodiment comprises the following steps:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 1-2h, and the preparation method comprises the steps of washing and drying after ultrasonic treatment is finished;
s02: adding wollastonite modifier accounting for 5-10% of the total weight of the S01 product into the S01 product, ball milling for 1-2h at the rotating speed of 1000-1500r/min, and obtaining a ball milling body after ball milling;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 2-5% of the total weight of the rare earth lanthanum sulfate solution, and uniformly stirring to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
The mixed acid solution in this embodiment is formed by mixing a hydrochloric acid solution with a mass fraction of 2%, a citric acid solution with a mass fraction of 5% and a sulfuric acid solution with a mass fraction of 8% according to a weight ratio of 4:1:1.
The rare earth lanthanum sulfate solution in the embodiment has the mass fraction of 5-10% and the chitosan solution has the mass fraction of 4-6%.
The rotational speed of the stirring modification treatment in the embodiment is 500-1000r/min, and the stirring time is 1-2h.
The preparation method of the wollastonite modifier in the embodiment comprises the following steps:
adding 5-10 parts of wollastonite into 20-30 parts of ethanol solvent, uniformly stirring, adding 2-5 parts of phosphoric acid buffer solution and 1-3 parts of potassium acetate solution, and stirring fully to obtain wollastonite liquid;
and (3) the wollastonite liquid is sent into 3-5 times of sodium dodecyl sulfate solution to be stirred uniformly, and then the wollastonite liquid is washed and dried to obtain the wollastonite modifier.
The pH of the phosphate buffer solution of this example was 5.0; the mass fraction of the potassium acetate solution is 5-9%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%.
The preparation method of the nano silicon dioxide double-dispensing agent in the embodiment comprises the following steps:
the nano silicon dioxide is sent to 120-130 ℃ for heat treatment for 1-2h, then cooled to 45-50 ℃ at the speed of 1-3 ℃/min, the nano silicon dioxide agent is obtained, yttrium nitrate solution with the total amount of 10-15% of the nano silicon dioxide agent and triisostearyl isopropyl titanate with the total amount of 1-3% of the nano silicon dioxide agent are added into the nano silicon dioxide agent, ball milling is carried out for 1-2h at the speed of 1000-1500r/min, and then water washing and drying are carried out, thus obtaining the nano silicon dioxide double-dispensing agent.
The mass fraction of the yttrium nitrate solution in the embodiment is 3-6%.
The preparation method of the foaming waterproof polyurethane environment-friendly adhesive comprises the following steps: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
Example 1
The environment-friendly adhesive for the foaming waterproof polyurethane comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 10% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 5% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
The preparation method of the flaky graphene modifier in the embodiment comprises the following steps:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 450W, the ultrasonic time is 1h, and the preparation method comprises the steps of finishing ultrasonic treatment, washing with water and drying;
s02: adding wollastonite modifier accounting for 5% of the total weight of the S01 product into the S01 product, and ball-milling for 1h at the rotating speed of 1000r/min, wherein ball milling is finished to obtain a ball-milled body;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 2% of the total weight of the rare earth lanthanum sulfate solution, and stirring and uniformly mixing to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
The mixed acid solution in this embodiment is formed by mixing a hydrochloric acid solution with a mass fraction of 2%, a citric acid solution with a mass fraction of 5% and a sulfuric acid solution with a mass fraction of 8% according to a weight ratio of 4:1:1.
The rare earth lanthanum sulfate solution in this embodiment has a mass fraction of 5% and the chitosan solution has a mass fraction of 4%.
The rotational speed of the stirring modification treatment in this example was 500r/min, and the stirring time was 1h.
The preparation method of the wollastonite modifier in the embodiment comprises the following steps:
adding 5 parts of wollastonite into 20 parts of ethanol solvent, uniformly stirring, adding 2 parts of phosphoric acid buffer solution and 1 part of potassium acetate solution, and fully stirring to obtain wollastonite liquid;
and (3) feeding the wollastonite liquid into a 3-time sodium dodecyl sulfate solution, uniformly stirring, and then washing and drying to obtain the wollastonite modifier.
The pH of the phosphate buffer solution of this example was 5.0; the mass fraction of the potassium acetate solution is 5%; the mass fraction of the sodium dodecyl sulfate solution is 10%.
The preparation method of the nano silicon dioxide double-dispensing agent in the embodiment comprises the following steps:
and (3) sending the nano silicon dioxide into a reactor at 120 ℃ for heat treatment for 1h, cooling to 45 ℃ at a speed of 1 ℃/min to obtain a nano silicon dioxide agent, adding yttrium nitrate solution accounting for 10% of the total amount of the nano silicon dioxide agent and triisostearyl isopropyl titanate accounting for 1% of the total amount of the nano silicon dioxide agent into the nano silicon dioxide agent, ball-milling for 1h at a rotating speed of 1000r/min, washing with water, and drying to obtain the nano silicon dioxide double-regulating agent.
The mass fraction of the yttrium nitrate solution of this example was 3%.
The preparation method of the foaming waterproof polyurethane environment-friendly adhesive comprises the following steps: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
Example 2
The environment-friendly adhesive for the foaming waterproof polyurethane comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 15% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 10% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
The preparation method of the flaky graphene modifier in the embodiment comprises the following steps:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 550W, the ultrasonic time is 2h, and the preparation method comprises the steps of finishing ultrasonic treatment, washing with water and drying;
s02: adding wollastonite modifier accounting for 10% of the total weight of the S1 product into the S1 product, ball-milling for 2 hours at the rotating speed of 1500r/min, and obtaining a ball-milled body after ball milling;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 5% of the total weight of the rare earth lanthanum sulfate solution, and stirring and uniformly mixing to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
The mixed acid solution in this embodiment is formed by mixing a hydrochloric acid solution with a mass fraction of 2%, a citric acid solution with a mass fraction of 5% and a sulfuric acid solution with a mass fraction of 8% according to a weight ratio of 4:1:1.
The rare earth lanthanum sulfate solution in this embodiment has a mass fraction of 10% and the chitosan solution has a mass fraction of 6%.
The rotational speed of the stirring modification treatment in this example was 1000r/min, and the stirring time was 2h.
The preparation method of the wollastonite modifier in the embodiment comprises the following steps:
adding 10 parts of wollastonite into 30 parts of ethanol solvent, uniformly stirring, adding 5 parts of phosphoric acid buffer solution and 3 parts of potassium acetate solution, and fully stirring to obtain wollastonite liquid;
and (3) feeding the wollastonite liquid into 5 times of sodium dodecyl sulfate solution, uniformly stirring, and then washing and drying to obtain the wollastonite modifier.
The pH of the phosphate buffer solution of this example was 5.0; the mass fraction of the potassium acetate solution is 9%; the mass fraction of the sodium dodecyl sulfate solution is 15%.
The preparation method of the nano silicon dioxide double-dispensing agent in the embodiment comprises the following steps:
and (3) sending the nano silicon dioxide into 130 ℃ for heat treatment for 2 hours, then cooling to 50 ℃ at the speed of 3 ℃/min to obtain a nano silicon dioxide agent, adding yttrium nitrate solution accounting for 15% of the total amount of the nano silicon dioxide agent and triisostearyl isopropyl titanate accounting for 3% of the total amount of the nano silicon dioxide agent into the nano silicon dioxide agent, ball-milling for 2 hours at the rotating speed of 1500r/min, washing with water, and drying to obtain the nano silicon dioxide double-regulating agent.
The mass fraction of the yttrium nitrate solution of this example was 6%.
The preparation method of the foaming waterproof polyurethane environment-friendly adhesive comprises the following steps: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
Example 3
The environment-friendly polyurethane adhesive comprises a polyurethane adhesive matrix, wherein a flake graphene modifier accounting for 12.5% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 7.5% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
The preparation method of the flaky graphene modifier in the embodiment comprises the following steps:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 500W, the ultrasonic time is 1.5h, and the preparation method comprises the steps of washing with water and drying;
s02: adding wollastonite modifier accounting for 7.5 percent of the total weight of the S1 product into the S1 product, and ball-milling for 1.5 hours at the rotating speed of 1250r/min, wherein the ball milling is finished to obtain a ball-milled body;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 3.5% of the total weight of the rare earth lanthanum sulfate solution, and uniformly stirring to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
The mixed acid solution in this embodiment is formed by mixing a hydrochloric acid solution with a mass fraction of 2%, a citric acid solution with a mass fraction of 5% and a sulfuric acid solution with a mass fraction of 8% according to a weight ratio of 4:1:1.
The rare earth lanthanum sulfate solution in this embodiment has a mass fraction of 7.5% and the chitosan solution has a mass fraction of 5%.
The rotational speed of the stirring modification treatment in this example was 750r/min, and the stirring time was 1.5h.
The preparation method of the wollastonite modifier in the embodiment comprises the following steps:
adding 7.5 parts of wollastonite into 25 parts of ethanol solvent, uniformly stirring, adding 3.5 parts of phosphoric acid buffer solution and 2 parts of potassium acetate solution, and stirring fully to obtain wollastonite liquid;
and (3) conveying the wollastonite liquid into 4 times of sodium dodecyl sulfate solution, uniformly stirring, and then washing and drying to obtain the wollastonite modifier.
The pH of the phosphate buffer solution of this example was 5.0; the mass fraction of the potassium acetate solution is 7%; the mass fraction of the sodium dodecyl sulfate solution is 12.5%.
The preparation method of the nano silicon dioxide double-dispensing agent in the embodiment comprises the following steps:
and (3) sending the nano silicon dioxide into 125 ℃ for heat treatment for 1.5 hours, then cooling to 47 ℃ at a speed of 2 ℃/min to obtain a nano silicon dioxide agent, adding yttrium nitrate solution accounting for 12.5% of the total amount of the nano silicon dioxide agent and triisostearyl isopropyl titanate accounting for 2% of the total amount of the nano silicon dioxide agent into the nano silicon dioxide agent, ball-milling for 1.5 hours at a rotating speed of 1250r/min, washing with water, and drying to obtain the nano silicon dioxide double-regulating agent.
The mass fraction of the yttrium nitrate solution of this example was 4.5%.
The preparation method of the foaming waterproof polyurethane environment-friendly adhesive comprises the following steps: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
Comparative example 1.
Unlike example 3, a flaky graphene modifier was not added.
Comparative example 2.
The difference from example 3 is that the graphene platelet modifier is replaced with graphene platelets.
Comparative example 3.
The difference from example 3 is that the preparation method of the flaky graphene modifier is different; the wollastonite modifier is not used for treatment.
Comparative example 4.
The difference from example 3 is the wollastonite modifier preparation; the uniform stirring treatment in the sodium dodecyl sulfate solution is not adopted.
Comparative example 5.
The difference from example 3 is that the preparation method of the flaky graphene modifier is different; the rare earth compound agent is not adopted for treatment.
Comparative example 6.
The difference from example 3 is that no nano silica twin-toner is added.
Comparative example 7.
The difference from example 3 is that no yttrium nitrate solution was added in the preparation of the nano-silica twin-dose.
And placing the product under the water mist condition for 12 hours, testing the water resistance, treating the product at 60 ℃ for 12 hours, and testing the temperature resistance.
The results of the performance measurements of examples 1-3 and comparative examples 1-6 are as follows
The product of the invention has excellent peel strength under the conventional conditions, can achieve the coordination effect under the water-resistant condition and the temperature-resistant condition, and can achieve the coordination significant improvement of water resistance and temperature resistance; the product performance is obviously reduced without adding one of the flaky graphene modifier and the nano silicon dioxide double-regulating agent, the flaky graphene modifier and the nano silicon dioxide double-regulating agent are matched and synergistic together, and the product performance can be optimized in a coordinated manner;
meanwhile, the flaky graphene modifier is replaced by flaky graphene, and the preparation methods of the flaky graphene modifier are different; the wollastonite modifier is not adopted for treatment, and the preparation method of the wollastonite modifier is different; the method does not adopt uniform stirring treatment in a sodium dodecyl sulfate solution, the preparation method of the flaky graphene modifier is different, the preparation method of the flaky graphene is not adopted, the rare earth compound agent is not adopted, the product has different flaky graphene performance, the product performance tends to be poor, and only the flaky graphene prepared by the method has the most obvious product performance effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The environment-friendly polyurethane adhesive comprises a polyurethane adhesive matrix, and is characterized in that a flake graphene modifier accounting for 10-15% of the total weight of the polyurethane adhesive matrix and a nano silicon dioxide double-dispensing agent accounting for 5-10% of the total weight of the polyurethane adhesive matrix are added into the polyurethane adhesive matrix.
2. The environment-friendly foaming waterproof polyurethane adhesive of claim 1, wherein the preparation method of the flaky graphene modifier is as follows:
s01: adding the flaky graphene into a mixed acid solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 1-2h, and the preparation method comprises the steps of washing and drying after ultrasonic treatment is finished;
s02: adding wollastonite modifier accounting for 5-10% of the total weight of the S01 product into the S01 product, ball milling for 1-2h at the rotating speed of 1000-1500r/min, and obtaining a ball milling body after ball milling;
s03: uniformly mixing a rare earth lanthanum sulfate solution and a chitosan solution according to a weight ratio of 3:1, then adding a silane coupling agent KH560 accounting for 2-5% of the total weight of the rare earth lanthanum sulfate solution, and uniformly stirring to obtain the rare earth lanthanum sulfate solution;
s04: adding the ball-milling body into the rare earth compound agent according to the weight ratio of 1:5, stirring and modifying, and washing and drying after stirring is finished to obtain the flaky graphene modifier.
3. The environment-friendly foaming waterproof polyurethane adhesive according to claim 2, wherein the mixed acid solution is prepared by mixing hydrochloric acid solution with the mass fraction of 2%, citric acid solution with the mass fraction of 5% and sulfuric acid solution with the mass fraction of 8% according to the weight ratio of 4:1:1.
4. The environment-friendly foaming waterproof polyurethane adhesive of claim 2, wherein the rare earth lanthanum sulfate solution is 5-10% in mass fraction and the chitosan solution is 4-6% in mass fraction.
5. The environment-friendly foaming waterproof polyurethane adhesive according to claim 2, wherein the rotational speed of the stirring modification treatment is 500-1000r/min, and the stirring time is 1-2h.
6. The environment-friendly foaming waterproof polyurethane adhesive according to claim 2, wherein the wollastonite modifier is prepared by the following steps:
adding 5-10 parts of wollastonite into 20-30 parts of ethanol solvent, uniformly stirring, adding 2-5 parts of phosphoric acid buffer solution and 1-3 parts of potassium acetate solution, and stirring fully to obtain wollastonite liquid;
and (3) the wollastonite liquid is sent into 3-5 times of sodium dodecyl sulfate solution to be stirred uniformly, and then the wollastonite liquid is washed and dried to obtain the wollastonite modifier.
7. The environment-friendly adhesive for foaming waterproof polyurethane as claimed in claim 6, wherein the pH value of the phosphoric acid buffer solution is 5.0; the mass fraction of the potassium acetate solution is 5-9%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%.
8. The environment-friendly foaming waterproof polyurethane adhesive according to claim 1, wherein the preparation method of the nano silicon dioxide double-dispensing agent is as follows:
the nano silicon dioxide is sent to 120-130 ℃ for heat treatment for 1-2h, then cooled to 45-50 ℃ at the speed of 1-3 ℃/min, the nano silicon dioxide agent is obtained, yttrium nitrate solution with the total amount of 10-15% of the nano silicon dioxide agent and triisostearyl isopropyl titanate with the total amount of 1-3% of the nano silicon dioxide agent are added into the nano silicon dioxide agent, ball milling is carried out for 1-2h at the speed of 1000-1500r/min, and then water washing and drying are carried out, thus obtaining the nano silicon dioxide double-dispensing agent.
9. The environment-friendly foaming waterproof polyurethane adhesive of claim 8, wherein the mass fraction of the yttrium nitrate solution is 3-6%.
10. The preparation method of the foaming waterproof polyurethane environment-friendly adhesive is characterized by comprising the following steps of: and uniformly stirring and mixing the polyurethane adhesive matrix, the flaky graphene modifier and the nano silicon dioxide double-modifier to obtain the foaming waterproof polyurethane environment-friendly adhesive.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311074497.7A CN117186825A (en) | 2023-08-24 | 2023-08-24 | Foaming waterproof polyurethane environment-friendly adhesive and preparation method thereof |
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| CN202311074497.7A CN117186825A (en) | 2023-08-24 | 2023-08-24 | Foaming waterproof polyurethane environment-friendly adhesive and preparation method thereof |
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