CN115109313A - Preparation method of special auxiliary agent for polyurethane sponge based on increase of tensile force - Google Patents
Preparation method of special auxiliary agent for polyurethane sponge based on increase of tensile force Download PDFInfo
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- CN115109313A CN115109313A CN202210807937.4A CN202210807937A CN115109313A CN 115109313 A CN115109313 A CN 115109313A CN 202210807937 A CN202210807937 A CN 202210807937A CN 115109313 A CN115109313 A CN 115109313A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 28
- 239000004814 polyurethane Substances 0.000 title claims abstract description 28
- 239000012752 auxiliary agent Substances 0.000 title abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229920001661 Chitosan Polymers 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 27
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 230000036632 reaction speed Effects 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 52
- 229910021389 graphene Inorganic materials 0.000 claims description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 8
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 8
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical group CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 7
- 229920000053 polysorbate 80 Polymers 0.000 claims description 7
- 239000000661 sodium alginate Substances 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
- 229940005550 sodium alginate Drugs 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention discloses a preparation method of a special assistant for polyurethane sponge based on increasing tension, which comprises the following steps: adding modified graphene into 5-7 times of chitosan dispersant, reacting at 65-75 ℃ for 35-45min at the reaction speed of 500-1000r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution; and (3) placing the product obtained in the step (III) at the temperature of 300-400 ℃ for heat treatment for 10-20min, and after the treatment is finished, returning the temperature to the room temperature at the speed of 1-3 ℃/min to obtain the special additive. The chitosan dispersing agent disclosed by the invention is prepared by matching chitosan and a silane coupling agent with other raw materials, the effect of assisting the synergy of the modified graphene and the dispersed carbon nano tube can be enhanced, and the improved special auxiliary agent is applied to polyurethane sponge, so that the strength performance and the elongation at break of the product can be improved in a coordinated manner.
Description
Technical Field
The invention relates to the technical field of polyurethane sponge, in particular to a preparation method of a special auxiliary agent for polyurethane sponge based on tension increase.
Background
The sponge is a porous material, has good water absorption, can be used for cleaning articles, and is made of wood cellulose fiber or foamed plastic polymer. In addition, there are also natural sponges made of sponge animals, and most of the natural sponges are used for body cleaning or painting. In addition, there are three types of synthetic sponges made of other materials, low density polyether (non-absorbent sponge), polyvinyl alcohol (superabsorbent material, no significant air holes) and polyester, respectively.
The invention provides a preparation method of a special assistant for polyurethane sponge based on increasing tension, which is based on that the assistant adopted by the existing polyurethane sponge is difficult to improve the mechanical tension property of the sponge, the strength property is improved, and the elongation at break property of the product is reduced.
Disclosure of Invention
In view of the drawbacks of the prior art, the object of the present invention is to provide a process for the preparation of a special adjuvant for polyurethane sponges based on increasing the tensile force, in order to solve the problems set forth in the background above.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of a special assistant for polyurethane sponge based on increasing tension, which comprises the following steps:
the method comprises the following steps: adding modified graphene into 5-7 times of chitosan dispersant, reacting at 65-75 ℃ for 35-45min at the reaction speed of 500-1000r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion to obtain a dispersed carbon nano tube;
step three: adding 4-9% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with ultrasonic power of 450-550W and ultrasonic time of 30-40min, finishing ultrasonic treatment, washing with water, and drying;
step four: and (3) placing the product obtained in the step (III) at the temperature of 300-400 ℃ for heat treatment for 10-20min, and after the treatment is finished, returning the temperature to the room temperature at the speed of 1-3 ℃/min to obtain the special additive.
Preferably, the preparation method of the modified graphene comprises the following steps:
s1: 5-10 parts of graphene is sent into 10-20 parts of mixed acid, stirred and reacted for 10-20min at the temperature of 45-55 ℃, the stirring speed is 350-450r/min, and after stirring, water washing and drying are carried out;
s2: then placing the graphene of S1 in 6-10 times of modification liquid for ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 450-500W, and the ultrasonic time is 45-55 min;
s3: and then, the graphene of S2 is subjected to heat treatment at the temperature of 110-120 ℃ for 10-20min, and after the heat treatment is finished, the graphene is cooled to room temperature by water, so that the modified graphene is obtained.
Preferably, the mixed acid is one or a combination of acetic acid and phosphoric acid.
Preferably, the preparation method of the modifying solution comprises the following steps:
adding 2-4 parts of sodium dodecyl sulfate into 10-20 parts of deionized water, then adding 1-3 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 1-3 parts of lanthanum sulfate solution into 5-10 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
Preferably, the mass fraction of the lanthanum sulfate solution is 4-7%.
Preferably, the mass fraction of the lanthanum sulfate solution is 5.5%.
Preferably, the preparation method of the chitosan dispersant comprises the following steps:
adding 5-10 parts of chitosan into 10-15 parts of deionized water, then adding 2-4 parts of silane coupling agent, then adding 1-3 parts of tween 80 and 2-4 parts of additive, and fully stirring and mixing to obtain the chitosan dispersant.
Preferably, the silane coupling agent is a silane coupling agent KH 570.
Preferably, the additive is sodium alginate and citric acid which are mixed according to the weight ratio of 3: 1.
Preferably, the mass fraction of the hydrochloric acid solution in the second step is 4-8%.
Compared with the prior art, the invention has the following beneficial effects:
according to the special assistant for the polyurethane sponge, the modified graphene is matched with the chitosan dispersant and is assisted by the dispersion type carbon nano tubes, the activity of the graphene is enhanced by the modification method, the graphene is matched with the dispersion type carbon nano tubes, the dispersibility of the graphene is enhanced, the graphene can be added into a product, the strength, the toughness and other properties of the product can be improved, the chitosan dispersant is prepared by matching chitosan and a silane coupling agent with other raw materials, the effect of assisting and enhancing the modified graphene and the dispersion type carbon nano tubes can be enhanced, and the improved special assistant is applied to the polyurethane sponge, so that the strength property and the elongation at break of the product can be improved in a coordinated manner;
the graphene is modified by mixed acid to improve the activity energy, and then modified by a modification solution formed by matching sodium dodecyl sulfate, sodium pyrophosphate, lanthanum sulfate solution and sodium citrate, so that the activity is enhanced after modification, and meanwhile, after heat treatment, the flexibility is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 preparation method of the special assistant for polyurethane sponge based on increasing tension force of the embodiment comprises the following steps:
the method comprises the following steps: adding modified graphene into 5-7 times of chitosan dispersant, reacting at 65-75 ℃ for 35-45min at the reaction speed of 500-1000r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion to obtain a dispersed carbon nano tube;
step three: adding 4-9% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with the ultrasonic power of 450-550W and the ultrasonic time of 30-40min, and washing and drying after the ultrasonic treatment is finished;
step four: and (3) placing the product obtained in the step (III) at the temperature of 300-400 ℃ for heat treatment for 10-20min, and after the treatment is finished, returning the temperature to the room temperature at the speed of 1-3 ℃/min to obtain the special additive.
The preparation method of the modified graphene of the embodiment comprises the following steps:
s1: 5-10 parts of graphene is sent into 10-20 parts of mixed acid, stirred and reacted for 10-20min at the temperature of 45-55 ℃, the stirring speed is 350-450r/min, and after stirring, water washing and drying are carried out;
s2: then placing the graphene of S1 in 6-10 times of modification liquid for ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 450-500W, and the ultrasonic time is 45-55 min;
s3: and then, the graphene of S2 is subjected to heat treatment at the temperature of 110-120 ℃ for 10-20min, and after the heat treatment is finished, the graphene is cooled to room temperature by water, so that the modified graphene is obtained.
The mixed acid in this embodiment is one or a combination of acetic acid and phosphoric acid.
The preparation method of the modified solution in this example is as follows:
adding 2-4 parts of sodium dodecyl sulfate into 10-20 parts of deionized water, then adding 1-3 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 1-3 parts of lanthanum sulfate solution into 5-10 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
The mass fraction of the lanthanum sulfate solution of this example was 4-7%.
The mass fraction of the lanthanum sulfate solution of this example was 5.5%.
The preparation method of the chitosan dispersant of the embodiment comprises the following steps:
adding 5-10 parts of chitosan into 10-15 parts of deionized water, then adding 2-4 parts of silane coupling agent, then adding 1-3 parts of tween 80 and 2-4 parts of additive, and fully stirring and mixing to obtain the chitosan dispersant.
The silane coupling agent of this example was a silane coupling agent KH 570.
The additive of this example is sodium alginate and citric acid mixed in a weight ratio of 3: 1.
The mass fraction of the hydrochloric acid solution in the second step of this example is 4-8%.
Example 1.
The preparation method of the special assistant for polyurethane sponge based on increasing tension force of the embodiment comprises the following steps:
the method comprises the following steps: adding modified graphene into 5 times of chitosan dispersant, reacting at 65 ℃ for 35min at the reaction speed of 500r/min, washing with water, and drying to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion to obtain a dispersed carbon nano tube;
step three: adding 4% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with the ultrasonic power of 450W and the ultrasonic time of 30min, and after the ultrasonic treatment, washing and drying;
step four: and (3) placing the product obtained in the step three at 300 ℃ for heat treatment for 10min, and after the heat treatment is finished, returning the temperature to the room temperature at the speed of 1 ℃/min to obtain the special auxiliary agent.
The preparation method of the modified graphene of the embodiment comprises the following steps:
s1: 5 parts of graphene is fed into 10 parts of mixed acid, stirred and reacted for 10min at the temperature of 45 ℃, the stirring speed is 350r/min, and after stirring, water washing and drying are carried out;
s2: then placing the graphene of S1 in 6 times of modification liquid, and performing ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 450W, and the ultrasonic time is 45 min;
s3: and then, placing the graphene of S2 at 110 ℃ for heat treatment for 10min, and cooling the graphene to room temperature by water to obtain the modified graphene.
The mixed acid in this example is acetic acid.
The preparation method of the modified solution in this example is as follows:
adding 2 parts of sodium dodecyl sulfate into 10 parts of deionized water, then adding 1 part of sodium pyrophosphate, and fully stirring and mixing to obtain a first reaction solution;
adding 1 part of lanthanum sulfate solution into 5 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
The mass fraction of the lanthanum sulfate solution of this example was 4%.
The preparation method of the chitosan dispersant of the embodiment comprises the following steps:
adding 5 parts of chitosan into 10 parts of deionized water, then adding 2 parts of silane coupling agent, then adding 1 part of tween 80 and 2 parts of additive, and stirring and fully mixing to obtain the chitosan dispersant.
The silane coupling agent of this example was a silane coupling agent KH 570.
The additive of this example is sodium alginate and citric acid mixed in a weight ratio of 3: 1.
The mass fraction of the hydrochloric acid solution in the second step of this example was 4%.
Example 2.
The preparation method of the special assistant for polyurethane sponge based on increasing tension force of the embodiment comprises the following steps:
the method comprises the following steps: adding the modified graphene into 7 times of chitosan dispersant, reacting at 75 ℃ for 45min at the reaction speed of 1000r/min, washing with water, and drying to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion is finished to obtain a dispersed carbon nano tube;
step three: adding 9% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with the ultrasonic power of 550W and the ultrasonic time of 40min, washing and drying after the ultrasonic treatment is finished;
step four: and (3) placing the product obtained in the step (III) at 400 ℃ for heat treatment for 20min, and after the heat treatment is finished, returning the temperature to the room temperature at the speed of 3 ℃/min to obtain the special auxiliary agent.
The preparation method of the modified graphene of the embodiment comprises the following steps:
s1: feeding 10 parts of graphene into 20 parts of mixed acid, stirring and reacting for 20min at 55 ℃, wherein the stirring speed is 450r/min, and washing and drying after stirring;
s2: then placing the graphene of S1 in 10 times of modification liquid for ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 500W, and the ultrasonic time is 55 min;
s3: and then, placing the graphene of S2 at 120 ℃ for heat treatment for 20min, and cooling the graphene to room temperature by water to obtain the modified graphene.
The mixed acid of this example was phosphoric acid.
The preparation method of the modified solution in this example is as follows:
adding 4 parts of sodium dodecyl sulfate into 20 parts of deionized water, then adding 3 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 3 parts of lanthanum sulfate solution into 10 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
The mass fraction of the lanthanum sulfate solution of this example was 7%.
The preparation method of the chitosan dispersant of the embodiment comprises the following steps:
adding 10 parts of chitosan into 15 parts of deionized water, then adding 4 parts of silane coupling agent, then adding 3 parts of tween 80 and 4 parts of additive, and stirring and fully mixing to obtain the chitosan dispersant.
The silane coupling agent of this example was a silane coupling agent KH 570.
The additive of this example is sodium alginate and citric acid mixed in a weight ratio of 3: 1.
The mass fraction of the hydrochloric acid solution in the second step of this example was 8%.
Example 3.
The preparation method of the special assistant for polyurethane sponge based on increasing tension force of the embodiment comprises the following steps:
the method comprises the following steps: adding modified graphene into 6 times of chitosan dispersant, reacting at 70 ℃ for 40min at the reaction speed of 750r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion is finished to obtain a dispersed carbon nano tube;
step three: adding 7% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with the ultrasonic power of 500W and the ultrasonic time of 35min, and after the ultrasonic treatment, washing and drying;
step four: and (3) placing the product obtained in the step three at 350 ℃ for heat treatment for 15min, and after the heat treatment is finished, returning the temperature to the room temperature at the speed of 2 ℃/min to obtain the special auxiliary agent.
The preparation method of the modified graphene of the embodiment comprises the following steps:
s1: sending 7.5 parts of graphene into 15 parts of mixed acid, stirring and reacting for 15min at 50 ℃, wherein the stirring speed is 400r/min, and washing and drying after stirring;
s2: then, placing the graphene of S1 in 8 times of modified liquid, and performing ultrasonic dispersion until the graphene is sufficiently dispersed, wherein the ultrasonic power is 475W, and the ultrasonic time is 50 min;
s3: and then, placing the graphene of S2 at 115 ℃ for heat treatment for 15min, and cooling the graphene to room temperature by water to obtain the modified graphene.
The mixed acid in this example is acetic acid.
The preparation method of the modified solution in this example is as follows:
adding 3 parts of sodium dodecyl sulfate into 15 parts of deionized water, then adding 2 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 2 parts of lanthanum sulfate solution into 7.5 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
The mass fraction of the lanthanum sulfate solution of this example was 5.5%.
The preparation method of the chitosan dispersant of the embodiment comprises the following steps:
adding 7.5 parts of chitosan into 12.5 parts of deionized water, then adding 3 parts of silane coupling agent, then adding 2 parts of tween 80 and 3 parts of additive, and stirring and mixing fully to obtain the chitosan dispersant.
The silane coupling agent of this example was a silane coupling agent KH 570.
The additive of this example is sodium alginate and citric acid mixed in a weight ratio of 3: 1.
The mass fraction of the hydrochloric acid solution in the second step of this example was 6%.
Example 4
The preparation method of the special assistant for polyurethane sponge based on increasing tension force of the embodiment comprises the following steps:
the method comprises the following steps: adding modified graphene into 6 times of chitosan dispersant, reacting at 68 ℃ for 36min at the reaction speed of 750r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion to obtain a dispersed carbon nano tube;
step three: adding 5% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with the ultrasonic power of 500W and the ultrasonic time of 32min, and after the ultrasonic treatment, washing and drying;
step four: and (3) placing the product obtained in the step three at 320 ℃ for heat treatment for 12min, and after the heat treatment is finished, returning the temperature to the room temperature at the speed of 1.2 ℃/min to obtain the special auxiliary agent.
The preparation method of the modified graphene of the embodiment comprises the following steps:
s1: feeding 6 parts of graphene into 12 parts of mixed acid, stirring and reacting for 12min at 46 ℃, wherein the stirring speed is 360r/min, and washing and drying after stirring;
s2: then placing the graphene of S1 in 8 times of modification liquid for ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 460W, and the ultrasonic time is 42 min;
s3: and then, placing the graphene of S2 at 113 ℃ for heat treatment for 12min, and cooling the graphene to room temperature by water to obtain the modified graphene.
The mixed acid in this example is acetic acid.
The preparation method of the modified solution in this example is as follows:
adding 3 parts of sodium dodecyl sulfate into 12 parts of deionized water, then adding 2 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 2 parts of lanthanum sulfate solution into 6 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
The mass fraction of the lanthanum sulfate solution of this example was 5%.
The preparation method of the chitosan dispersant of the embodiment comprises the following steps:
adding 6 parts of chitosan into 12 parts of deionized water, then adding 3 parts of silane coupling agent, then adding 2 parts of tween 80 and 3 parts of additive, and fully stirring and mixing to obtain the chitosan dispersant.
The silane coupling agent of this example was a silane coupling agent KH 570.
The additive of this example is sodium alginate and citric acid mixed in a weight ratio of 3: 1.
The mass fraction of the hydrochloric acid solution in the second step of this example was 5%.
The products of examples 1 to 4 were applied to polyurethane sponges, and the results of the performance tests were as follows, in comparison with the use without special auxiliary agents:
| strength increasing ratio (%) | Elongation at Break increase (%) | |
| Example 1 | 9.8 | 11.5 |
| Example 2 | 9.9 | 11.6 |
| Example 3 | 10.1 | 11.7 |
| Example 4 | 10.0 | 10.8 |
The product of the invention was further tested by comparative example for properties:
comparative example 1.
Unlike example 3, no modified graphene was added.
Comparative example 2.
Unlike example 3, no chitosan dispersant was added.
Comparative example 3.
Unlike example 3, no dispersed carbon nanotubes were added.
Carrying out performance test on the products of comparative examples 1-3;
as can be seen from comparative examples 1 to 3 and examples 1 to 4;
the products of the embodiments 1 to 4 of the invention can obviously improve the strength and the elongation at break of the products, and simultaneously, the strength and the elongation at break can play a role in coordination and improvement, one of the modified graphene, the dispersed carbon nano tube and the chitosan dispersant is not added, so that the performance of the products is obviously reduced, the raw materials are mutually coordinated to jointly improve the performance of the products, and the products are promoted to play a role in coordination and improvement.
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 attributes 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 description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The preparation method of the special assistant for the polyurethane sponge based on increasing the tensile force is characterized by comprising the following steps:
the method comprises the following steps: adding modified graphene into 5-7 times of chitosan dispersant, reacting at 65-75 ℃ for 35-45min at the reaction speed of 500-1000r/min, washing with water and drying after the reaction is finished to obtain a composite modified solution;
step two: sending the carbon nano tube into 6 times of hydrochloric acid solution, stirring and dispersing uniformly, washing and drying after dispersion to obtain a dispersed carbon nano tube;
step three: adding 4-9% of dispersed carbon nano tubes into the composite modified solution, performing ultrasonic dispersion treatment with ultrasonic power of 450-550W and ultrasonic time of 30-40min, finishing ultrasonic treatment, washing with water, and drying;
step four: and (3) placing the product obtained in the step (III) at the temperature of 300-400 ℃ for heat treatment for 10-20min, and after the treatment is finished, returning the temperature to the room temperature at the speed of 1-3 ℃/min to obtain the special additive.
2. The preparation method of the special assistant for polyurethane sponge based on tension increase according to claim 1, wherein the preparation method of the modified graphene comprises the following steps:
s1: 5-10 parts of graphene is sent into 10-20 parts of mixed acid, stirred and reacted for 10-20min at the temperature of 45-55 ℃, the stirring speed is 350-450r/min, and after stirring, water washing and drying are carried out;
s2: then placing the graphene of S1 in 6-10 times of modification liquid for ultrasonic dispersion until the graphene is fully dispersed, wherein the ultrasonic power is 450-500W, and the ultrasonic time is 45-55 min;
s3: and then, the graphene of S2 is subjected to heat treatment at the temperature of 110-120 ℃ for 10-20min, and after the heat treatment is finished, the graphene is cooled to room temperature by water, so that the modified graphene is obtained.
3. The preparation method of the special assistant for polyurethane sponge based on tension increase as claimed in claim 2, wherein the mixed acid is one or more of acetic acid and phosphoric acid.
4. The preparation method of the special assistant for polyurethane sponge based on tension increase as claimed in claim 2, wherein the preparation method of the modifying solution is as follows:
adding 2-4 parts of sodium dodecyl sulfate into 10-20 parts of deionized water, then adding 1-3 parts of sodium pyrophosphate, and stirring and mixing fully to obtain a first reaction solution;
adding 1-3 parts of lanthanum sulfate solution into 5-10 parts of deionized water containing 3% by mass of sodium citrate, and uniformly stirring and dispersing to obtain a second reaction solution;
and mixing the second reaction solution and the first reaction solution according to the weight ratio of 1:5, and stirring and fully mixing to obtain the modified solution.
5. The preparation method of the special assistant for polyurethane sponge based on tension increase as claimed in claim 4, wherein the mass fraction of the lanthanum sulfate solution is 4-7%.
6. The preparation method of the special assistant for the polyurethane sponge based on the tension increasing function as claimed in claim 5, wherein the mass fraction of the lanthanum sulfate solution is 5.5%.
7. The preparation method of the special assistant for polyurethane sponge based on tension increase as claimed in claim 1, wherein the preparation method of the chitosan dispersant is as follows:
adding 5-10 parts of chitosan into 10-15 parts of deionized water, then adding 2-4 parts of silane coupling agent, then adding 1-3 parts of tween 80 and 2-4 parts of additive, and fully stirring and mixing to obtain the chitosan dispersant.
8. The preparation method of the special assistant for polyurethane sponge based on increasing tensile force according to claim 7, wherein the silane coupling agent is silane coupling agent KH 570.
9. The preparation method of the special assistant for the polyurethane sponge based on the increase of the tensile force as claimed in claim 7, wherein the additive is sodium alginate and citric acid which are mixed according to a weight ratio of 3: 1.
10. The preparation method of the special assistant for polyurethane sponge based on tension increase as claimed in claim 1, wherein the mass fraction of the hydrochloric acid solution in the second step is 4-8%.
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Address after: 226412 north side of Jiangming Road, Dong'an science and Technology Park, Tongzhou Bay Jianghai linkage development demonstration zone, Nantong City, Jiangsu Province Applicant after: Hengguang New Materials (Jiangsu) Co.,Ltd. Address before: 226412 north side of Jiangming Road, Dong'an science and Technology Park, Tongzhou Bay Jianghai linkage development demonstration zone, Nantong City, Jiangsu Province Applicant before: NANTONG HENGGUANGDA POLYURETHANE MATERIAL CO.,LTD. |
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Application publication date: 20220927 |