CN110643016A - Preparation method of carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion - Google Patents
Preparation method of carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion Download PDFInfo
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- CN110643016A CN110643016A CN201910982422.6A CN201910982422A CN110643016A CN 110643016 A CN110643016 A CN 110643016A CN 201910982422 A CN201910982422 A CN 201910982422A CN 110643016 A CN110643016 A CN 110643016A
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- carbon nanotube
- nano silver
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- modified polyurethane
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 72
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 71
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000004814 polyurethane Substances 0.000 title claims abstract description 56
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 5
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- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 4
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- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 claims description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 claims description 2
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- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
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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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/04—Carbon
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a preparation method of a carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion, which relates to the field of polymer chemistry. The carbon nano tube loaded nano silver wire is used as an additive and uniformly dispersed in a polyurethane matrix, and the coating film can meet the use requirements under the conditions of high stretching and high thermal stability and has good enough antistatic performance.
Description
Technical Field
The invention relates to the field of polymer chemistry, in particular to a preparation method of a modified polyurethane antistatic emulsion with carbon nano tube loaded with nano silver wires.
Background
The waterborne polyurethane takes water as a solvent, has the characteristics of environmental protection, safe transportation, good weather resistance and the like, and with the demand of people on novel multifunctional materials, researchers try to compound a certain material with outstanding performance with the polyurethane so as to expand the application range of the waterborne polyurethane in actual production, and the waterborne polyurethane is used in the aspects of building coatings, leather, textiles, packaging films, sealing materials, fibers and the like. Because polyurethane materials do not have natural conductivity, the surface resistance is high, the electrical insulation is good, static accumulation is easy to cause, once static is charged, static is not easy to eliminate, when static is accumulated to a certain degree, the practical application value of the polyurethane is directly influenced, the static accumulation is usually realized not by changing the polyurethane per se but by adding a certain form of conductive filler, and the conductive filler generally increases the difficulty and the cost of production and is usually mixed with fillers such as carbon nanotubes, graphene, clay nanomaterials, glass fibers and the like. Generally, these fillers do increase the conductivity of the polyurethane, but in practice unmodified fillers generally contribute little or no to the conductivity of the polymer composite.
Carbon nanotubes are an attractive material with excellent electrical, thermal and mechanical properties, extremely high weight, very toughness, good elasticity and repair properties. The carbon nano tube/polyurethane composite material can be widely applied to polymer foam, elastomers, coatings and textile fabrics. The electrical conductivity of the traditional resin is usually provided by a single filler, and metal particles or metal oxides can be loaded on the surface of the carbon nano tube through covalent-non-covalent coating, so that the carbon nano tube is endowed with good physical and chemical properties, the composite material has better and excellent performance, is dispersed into a polyurethane matrix, enhances the electrostatic dissipation of the composite material, improves the electrical conductivity of the composite material while enhancing the mechanical property, weather resistance and thermal stability, and meets the requirements of people on functional composite materials.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a modified polyurethane antistatic emulsion with carbon nano tube loaded nano silver wires, so as to solve the technical problems of poor antistatic performance of aqueous polyurethane and the like in the prior art.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a carbon nanotube loaded nano silver wire modified polyurethane antistatic emulsion, which comprises the following steps:
step 1, preparation of carbon nano tube loaded nano silver wire
Adding trihydroxymethyl aminomethane into 350mL of deionized water, stirring to dissolve the trihydroxymethyl aminomethane, and dropwise adding 0.1mol/L hydrochloric acid solution to adjust the pH value of the system to obtain a buffer solution; adding the multi-walled carbon nanotube into the buffer solution, performing ultrasonic dispersion for 5-8h to form a uniform suspension, adding dopamine, placing at 25-35 ℃, performing magnetic stirring for 2-10h, then adding a nano silver linear alcohol solution, and continuing to react for 2-6 h; adding a silane coupling agent, violently stirring for 2-6h, repeatedly centrifuging, washing with ethanol and deionized water for 2-5 times respectively, and vacuum drying the product at 60 ℃ for 24h to obtain a nano silver wire hybrid carbon nanotube material;
step 2, preparation of waterborne polyurethane prepolymer
Carrying out vacuum-pumping drying dehydration on polyester diol at 110 ℃ for 2 h; putting the obtained polyester diol into a reaction vessel, heating to 70 ℃, adding diisocyanate for reaction for 1h, adding a catalyst, and controlling the reaction temperature to be 60-85 ℃ for continuous reaction for 1 h; adding a hydrophilic chain extender to react for 1.5-2.5h, finally adding a double cross-linking agent into a reaction container, continuing to react for 0.5-1h, stopping the reaction, and cooling to obtain a waterborne polyurethane prepolymer;
step 3, preparation of nano silver wire hybrid carbon nano tube reinforced antistatic polyurethane emulsion
And (3) adding the product prepared in the step (1) into the product prepared in the step (2), controlling the temperature to be 20-40 ℃, quickly stirring for 1h, then cooling to room temperature, dropwise adding an alkali neutralizing agent, slowly stirring for 10min, quickly adding deionized water at a high rotating speed of 1500r/min, emulsifying for 30min, and carrying out reduced pressure distillation after the reaction is finished to prepare the nano silver wire hybrid carbon nanotube reinforced antistatic polyurethane emulsion, wherein the solid content is controlled to be 25-35%.
Further, in the step 1, the pH value of the buffer solution is 7.5-8.5, and the mass ratio of the multi-walled carbon nanotube to the dopamine is 1: 2-3%, the concentration of the nano silver linear alcohol solution is 0.1mol/L, and the addition amount is 5-15 mL.
Further, the silane coupling agent in the step 1 is one or a mixture of more of gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-mercaptopropyltrimethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
Furthermore, the dosage of the silane coupling agent is 2-8 times of that of the multi-wall carbon nano tube.
Further, the mass ratio of the nano silver wire hybrid carbon nano tube to the waterborne polyurethane prepolymer in the step 3 is 0.05-0.2: 10.
further, the polyester diol in the step 2 is one or a mixture of more of polycarbonate diol, polybutylene adipate diol, dimer acid type polyester diol and polyhexamethylene adipate diol.
Further, the molecular weight of the polyester diol is 1000-3000.
Further, the diisocyanate in the step 2 is one or a mixture of several of isophorone diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, 1, 6-hexamethylene diisocyanate, dicyclohexylmethane diisocyanate and dimer acid diisocyanate.
Further, in the step 2, the hydrophilic chain extender is one group containing carboxylic acid, sulfonic acid and phosphate group, and is one or a mixture of several selected from dimethylolpropionic acid, dimethylolbutyric acid and 2- [ (2-aminoethyl) amino ] sodium sulfonate.
Further, in the step 2, the double cross-linking agent is one or a mixture of more of trihydroxypropane, glycerol and dipentaerythritol, the catalyst is one or a mixture of more of stannous octoate and dibutyltin dilaurate, and the alkali neutralizing agent is one or a mixture of more of triethylamine, N-dimethylethanolamine and sodium hydroxide.
The invention relates to a preparation method of a carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion, which can be applied to the field of biological medical treatment, and compared with the prior art, the invention has the beneficial effects that:
the existing waterborne polyurethane material has no natural conductivity, high surface resistance and good electrical insulation, is easy to cause static accumulation, is not easy to eliminate once being charged with static, directly influences the practical application value when the static is accumulated to a certain degree, and the carbon nano tube has excellent electrical property, thermal conductivity and mechanical property, extremely high weight, toughness, good elasticity and repair property, and is an attractive substance. The carbon nano tube/polyurethane composite material can be widely applied to polymer foam, elastomers, coatings and textile fabrics. The electrical conductivity of the traditional resin is usually provided by a single filler, and metal particles or metal oxides can be loaded on the surface of the carbon nano tube through covalent-non-covalent coating, so that the carbon nano tube is endowed with good physical and chemical properties, the composite material has better and excellent performance, is dispersed into a polyurethane matrix, enhances the electrostatic dissipation of the composite material, improves the electrical conductivity of the composite material while enhancing the mechanical property, weather resistance and thermal stability, and meets the requirements of people on functional composite materials.
The method for preparing the nano silver wire hybrid carbon nano tube has the advantages of mild conditions, simplicity, convenience, practicability, greenness, harmlessness and short reaction time, does not damage the self structure of the carbon nano tube, keeps the original attribute of the carbon nano tube, avoids waste acid and waste water generated by oxidizing the carbon nano tube by using strong acid, and reduces the cost to a certain extent.
The invention adopts dopamine autopolymerization to wrap the nano silver wire, and fixes the nano silver wire on the surface of the carbon nano tube by using the silane coupling agent, so that the carbon nano tube can be endowed with good physical and chemical properties, and the composite material has better and outstanding performance. There is practically no carbon nanotube material that has electrical conductivity and good mechanical durability without any special treatment, while the original properties of the material can be maintained by dopamine coating modification.
The invention utilizes the carbon nano tube silver-loaded material as the conductive filler, greatly enhances the mechanical property of the polyurethane material, obtains the antistatic effect and shows excellent practical effect.
Drawings
FIG. 1 is a flow chart of the functional modification of the surface of CNTs;
FIG. 2 is a schematic diagram of the preparation of nano silver wire hybrid carbon nanotubes;
FIG. 3 is a transmission electron micrograph of a surface-modified carbon nanotube-loaded silver, in which (a) is a partially enlarged TEM image of a carbon nanotube-loaded silver nanowire and (b) is a partially enlarged TEM image of a carbon nanotube-loaded silver nanowire;
fig. 4 is a thermogravimetric graph of the nano silver wire hybridized carbon nanotube reinforced antistatic polyurethane composite coating film.
Detailed Description
In order to make the technical solutions of the present application better understood by those skilled in the art, the technical solutions of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, 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 application.
It is noted that the term "comprising" in the description and claims of the present application is intended to cover a non-exclusive inclusion, e.g. a method comprising a list of steps is not necessarily limited to those steps explicitly listed, but may include other steps not explicitly listed or inherent to such methods. The embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail with reference to examples.
Example 1:
the experiment prepares the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion according to the following steps:
(1) preparation of carbon nano tube loaded nano silver wire
Combining the figure and 2, weighing a proper amount of tris (hydroxymethyl) aminomethane, adding the tris (hydroxymethyl) aminomethane into 350mL of deionized water, stirring to dissolve the tris (hydroxymethyl) aminomethane, dropwise adding 0.1mol/L hydrochloric acid solution to adjust the pH value of a system to 8.5, and using the solution before use as a buffer solution; adding 0.2g of multi-walled carbon nanotube into the prepared buffer solution, performing ultrasonic dispersion for 6 hours to form a uniform suspension, adding 0.42g of dopamine, placing at 25 ℃, performing magnetic stirring for 8 hours, adding 5mL of 0.1mol/L nano-silver linear alcohol solution, and continuing to react for 5 hours; adding 1.2g of gamma-aminopropyltriethoxysilane, violently stirring for 3h, repeatedly centrifuging, washing with ethanol and deionized water for 2 times respectively, and vacuum drying the product at 60 ℃ for 24h to obtain the carbon nanotube-loaded nano-silver wire material.
(2) Preparation of waterborne polyurethane prepolymer
20g of polyester diol is vacuumized, dried and dehydrated for 2.5 hours at the temperature of 110 ℃; putting the obtained polyester diol into a reaction vessel, heating to 70 ℃, adding 13.2g of diisocyanate, stirring and mixing, adding 2 drops of dibutyltin dilaurate, and controlling the reaction temperature to be 85 ℃ to continue reacting for 1.5 h; and adding 1.8g of dimethylolbutyric acid for reaction for 2 hours, finally adding the mixture into a reaction vessel of 0.3g of dipentaerythritol, continuing the reaction for 1 hour, stopping the reaction, and cooling to obtain the waterborne polyurethane prepolymer.
(3) Preparation of carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion
And (2) adding the product prepared in the step (1) into the step (2), controlling the temperature to be 20-40 ℃, quickly stirring for 1h, then dropwise adding an alkali neutralizing agent into the room temperature, slowly stirring for 10min, quickly adding deionized water at a high rotating speed of 1500r/min, emulsifying for 30min, and removing the solvent through reduced pressure distillation after the reaction is finished to prepare the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion.
The performance of the nano silver wire hybrid carbon nanotube reinforced antistatic polyurethane emulsion 1 obtained in example 1 was tested, and the obtained performance indexes are shown in Table 1
TABLE 1
Example 2:
the experiment prepares the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion according to the following steps:
(1) preparation of carbon nano tube loaded nano silver wire
Weighing a proper amount of tris (hydroxymethyl) aminomethane, adding the tris (hydroxymethyl) aminomethane into 350mL of deionized water, stirring to dissolve the tris (hydroxymethyl) aminomethane, dropwise adding 0.1mol/L hydrochloric acid solution to adjust the pH value of the system to 8.5, and using the solution as a buffer solution before use; adding 0.3g of multi-walled carbon nanotube into the prepared buffer solution, performing ultrasonic dispersion for 6 hours to form a uniform suspension, adding 0.62g of dopamine, placing at 25 ℃, performing magnetic stirring for 8 hours, adding 10mL of 0.1mol/L nano-silver linear alcohol solution, and continuing to react for 5 hours; adding 1.2g of gamma-aminopropyltriethoxysilane, violently stirring for 3h, repeatedly centrifuging, washing with ethanol and deionized water for 2 times respectively, and vacuum drying the product at 60 ℃ for 24h to obtain the carbon nanotube-loaded nano-silver wire material.
(2) Preparation of waterborne polyurethane prepolymer
15g of polyester diol is vacuumized, dried and dehydrated for 2.5 hours at the temperature of 110 ℃; putting the obtained polyester diol into a reaction vessel, heating to 70 ℃, adding 9.9g of diisocyanate, stirring and mixing, adding 2 drops of dibutyltin dilaurate, and controlling the reaction temperature to be 85 ℃ to continue reacting for 1.5 h; and adding 1.4g of dimethylolbutyric acid for reaction for 2 hours, finally adding the mixture into a reaction vessel of 0.2g of dipentaerythritol, continuing the reaction for 1 hour, stopping the reaction, and cooling to obtain the waterborne polyurethane prepolymer.
(3) Preparation of carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion
And (2) adding the product prepared in the step (1) into the step (2), controlling the temperature to be 35 ℃, quickly stirring for 1h, then dropwise adding an alkali neutralizing agent into the room temperature, slowly stirring for 10min, quickly adding deionized water at a high rotating speed of 1500r/min, emulsifying for 30min, and removing the solvent by reduced pressure distillation after the reaction is finished to prepare the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion.
The performance of the nano silver wire hybrid carbon nanotube reinforced antistatic polyurethane emulsion 2 obtained in example 2 was tested, and the obtained performance indexes are shown in Table 2
TABLE 2
Example 3:
the experiment prepares the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion according to the following steps:
(1) preparation of carbon nano tube loaded nano silver wire
Weighing a proper amount of tris (hydroxymethyl) aminomethane, adding the tris (hydroxymethyl) aminomethane into 350mL of deionized water, stirring to dissolve the tris (hydroxymethyl) aminomethane, dropwise adding 0.1mol/L hydrochloric acid solution to adjust the pH value of the system to 8.5, and using the solution as a buffer solution before use; adding 0.35g of multi-walled carbon nanotube into the prepared buffer solution, performing ultrasonic dispersion for 6 hours to form a uniform suspension, adding 0.72g of dopamine, placing at 25 ℃, performing magnetic stirring for 8 hours, adding 15mL of 0.1mol/L nano-silver linear alcohol solution, and continuing to react for 5 hours; adding 1.2g of gamma-aminopropyltriethoxysilane, violently stirring for 3h, repeatedly centrifuging, washing with ethanol and deionized water for 2 times respectively, and vacuum drying the product at 60 ℃ for 24h to obtain the carbon nanotube-loaded nano-silver wire material.
(2) Preparation of waterborne polyurethane prepolymer
25g of polyester diol is vacuumized, dried and dehydrated for 2.5 hours at the temperature of 110 ℃; putting the obtained polyester diol into a reaction vessel, heating to 70 ℃, adding 16.6g of diisocyanate, stirring and mixing, adding 2 drops of dibutyltin dilaurate, and controlling the reaction temperature to be 85 ℃ to continue reacting for 1.5 h; and adding 2.2g of dimethylolbutyric acid for reaction for 2 hours, finally adding the mixture into a reaction vessel of 0.4g of dipentaerythritol, continuing the reaction for 1 hour, stopping the reaction, and cooling to obtain the waterborne polyurethane prepolymer.
(3) Preparation of carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion
And (2) adding the product prepared in the step (1) into the step (2), controlling the temperature to be 35 ℃, quickly stirring for 1h, then dropwise adding an alkali neutralizing agent into the room temperature, slowly stirring for 10min, quickly adding deionized water at a high rotating speed of 1500r/min, emulsifying for 30min, and removing the solvent by reduced pressure distillation after the reaction is finished to prepare the carbon nano tube loaded nano silver wire modified polyurethane antistatic emulsion.
The performance of the nano silver wire hybridized carbon nanotube reinforced antistatic polyurethane emulsion 3 obtained in example 3 was tested, and the obtained performance indexes are shown in Table 3
TABLE 3
Comparative test
The carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion prepared in the examples 1-3 is mixed according to the proportion listed in the table 4, uniformly stirred, coated on the surface of the treated tinplate, dried and cured at 60 ℃ for 30min to form a film, and the hardness (GB/T6739-. And compared with comparative coating films 1 to 3 obtained by curing the nano silver wire without adding the carbon nanotube, as shown in table 5. Wherein the polyurethane emulsion used in the comparative example is obtained by curing and film-forming the polyurethane emulsion emulsified by the aqueous polyurethane prepared in the second step of example 1.
Proportioning of nano silver wire hybridized carbon nano tube and polyurethane emulsion
TABLE 4
Performance index of coating film
TABLE 5
As can be seen from Table 5, the physical properties of the coating film obtained from the carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion prepared by the invention include excellent adhesive force, pencil hardness and water resistance, and compared with the comparative example, the antistatic property of the coating film is greatly improved due to the introduction of the carbon nanotube-loaded nano silver wire.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
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.
The present invention is not limited to the above description of the embodiments, and those skilled in the art should, in light of the present disclosure, appreciate that many changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion is characterized by comprising the following steps:
step 1, preparation of carbon nano tube loaded nano silver wire
Adding trihydroxymethyl aminomethane into 350mL of deionized water, stirring to dissolve the trihydroxymethyl aminomethane, and dropwise adding 0.1mol/L hydrochloric acid solution to adjust the pH value of the system to obtain a buffer solution; adding the multi-walled carbon nanotube into the buffer solution, performing ultrasonic dispersion for 5-8h to form a uniform suspension, adding dopamine, placing at 25-35 ℃, performing magnetic stirring for 2-10h, then adding a nano silver linear alcohol solution, and continuing to react for 2-6 h; adding a silane coupling agent, violently stirring for 2-6h, repeatedly centrifuging, washing with ethanol and deionized water for 2-5 times respectively, and vacuum drying the product at 60 ℃ for 24h to obtain a nano silver wire hybrid carbon nanotube material;
step 2, preparation of waterborne polyurethane prepolymer
Carrying out vacuum-pumping drying dehydration on polyester diol at 110 ℃ for 2 h; putting the obtained polyester diol into a reaction vessel, heating to 70 ℃, adding diisocyanate for reaction for 1h, adding a catalyst, and controlling the reaction temperature to be 60-85 ℃ for continuous reaction for 1 h; adding a hydrophilic chain extender to react for 1.5-2.5h, finally adding a double cross-linking agent into a reaction container, continuing to react for 0.5-1h, stopping the reaction, and cooling to obtain a waterborne polyurethane prepolymer;
step 3, preparation of nano silver wire hybrid carbon nano tube reinforced antistatic polyurethane emulsion
And (3) adding the product prepared in the step (1) into the product prepared in the step (2), controlling the temperature to be 20-40 ℃, quickly stirring for 1h, then cooling to room temperature, dropwise adding an alkali neutralizing agent, slowly stirring for 10min, quickly adding deionized water at a high rotating speed of 1500r/min, emulsifying for 30min, and carrying out reduced pressure distillation after the reaction is finished to prepare the nano silver wire hybrid carbon nanotube reinforced antistatic polyurethane emulsion, wherein the solid content is controlled to be 25-35%.
2. The preparation method of the carbon nanotube-loaded nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 1, wherein the pH value of the buffer solution in the step 1 is 7.5-8.5, and the mass ratio of the multi-walled carbon nanotube to the dopamine is 1: 2-3%, the concentration of the nano silver linear alcohol solution is 0.1mol/L, and the addition amount is 5-15 mL.
3. The method for preparing the carbon nanotube-loaded nanosilver-modified polyurethane antistatic emulsion as claimed in claim 2, wherein the silane coupling agent in the step 1 is one or a mixture of more of gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-mercaptopropyltrimethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
4. The preparation method of the carbon nanotube-loaded nanosilver wire modified polyurethane antistatic emulsion as claimed in claim 3, wherein the amount of the silane coupling agent is 2-8 times that of the multiwall carbon nanotube.
5. The preparation method of the carbon nanotube-loaded nano silver wire modified polyurethane antistatic emulsion as claimed in claim 4, wherein the mass ratio of the nano silver wire hybrid carbon nanotube to the aqueous polyurethane prepolymer in the step 3 is 0.05-0.2: 10.
6. the method for preparing the carbon nanotube-loaded nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 5, wherein the polyester diol in the step 2 is one or a mixture of polycarbonate diol, polybutylene adipate diol, dimer acid type polyester diol and polyhexamethylene adipate diol.
7. The method for preparing the carbon nanotube-loaded nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 6, wherein the molecular weight of the polyester diol is 1000-3000.
8. The method for preparing the carbon nanotube-supported nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 7, wherein the diisocyanate in the step 2 is one or a mixture of isophorone diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, 1, 6-hexamethylene diisocyanate, dicyclohexylmethane diisocyanate and dimer acid diisocyanate.
9. The method for preparing the carbon nanotube-loaded nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 8, wherein the hydrophilic chain extender in step 2 is one group selected from carboxylic acid, sulfonic acid and phosphoric acid, and is one or more mixtures selected from dimethylolpropionic acid, dimethylolbutyric acid and sodium 2- [ (2-aminoethyl) amino ] sulfonate.
10. The method for preparing the carbon nanotube-loaded nanosilver wire-modified polyurethane antistatic emulsion as claimed in claim 9, wherein the double cross-linking agent in step 2 is one or a mixture of more of trimethylolpropane, glycerol and dipentaerythritol, the catalyst is one or a mixture of more of stannous octoate and dibutyltin dilaurate, and the alkali neutralizing agent is one or a mixture of more of triethylamine, N-dimethylethanolamine and sodium hydroxide.
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