CN113292739A - Production method of high-graphene-concentration latex - Google Patents
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- 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
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Abstract
The invention discloses a production method of high-graphene-concentration latex, which is characterized in that the incompatibility of graphene oxide and latex is reduced by adopting a method for carrying out composite modification on the surface of the graphene oxide, casein, aromatic hydrocarbon amine and water-soluble organic polyamine are used as modifiers, the pH is adjusted by ammonia water to be modified in an alkaline environment, the obtained concentrated graphene slurry is mixed with the latex while maintaining alkalinity, the weight proportion of the modified graphene in the solid content of the latex is 1-10 wt%, the mechanical stability of the modified graphene latex exceeds 100 seconds, and the multifunctional properties of the graphene latex/rubber, namely the functions of high heat conduction, high electric conduction, high strength, bacteriostasis and the like, are realized. The thermal conductivity of the latex sponge produced by the high-graphene-concentration latex prepared by the method is more than one time of that of the common latex sponge. The method can realize continuous large-scale production and has low production cost.
Description
Technical Field
The invention relates to the technical field of graphene latex preparation, in particular to a large-scale production method of latex sponge with high graphene concentration.
Background
The thermal conductivity of common organic matters such as rubber and plastic is about 0.2W/mK, and the organic matters are electric insulating materials; the thermal conductivity of the foaming material is about 0.02W/mK, and the foaming material is a heat-insulating material. Compared with organic matters such as latex, plastic, resin and the like, the thermal conductivity and the electric conductivity of the graphene are more than ten thousand times of those of common organic matters, so that the electric and thermal properties of the materials can be greatly improved by adding the graphene. And the increase of the electrical conductivity and the thermal conductivity is in positive correlation with the concentration of graphene in the composite material, and the higher the concentration of graphene is, the faster the physical properties are increased, and the simple linear increase is not realized, so that the thermal conductivity and the electrical conductivity of the organic material with high graphene concentration are higher.
The natural latex is an emulsion dispersion liquid with polypentadiene as a main component, the average particle size of latex particles is in a micrometer range, a small amount of protein, organic acid and the like play a role of a surfactant as a dispersing agent, the natural latex is stable in an alkaline environment and poor in stability, and the storage stability needs to be improved by adding ammonia water after filtration, purification and concentration. The added ammonia water needs to be deaminated by a deamination process before use, the deaminated latex needs to be added with other types of stabilizers to increase the stability, particularly the mechanical stability, so as to ensure the stable performance of the latex in the use process, and casein, gelatin, potassium hydroxide/sodium, ammonium laurate, sodium oleyl sulfate and the like are widely applied to the latex industry as the stabilizers.
Graphene is a neutral material, has poor dispersibility in water, is slightly acidic in graphene oxide, is not compatible with latex which is stable under an alkaline condition although the dispersibility in water is relatively good, and can cause a gelling phenomenon after mixing, particularly the stability of the latex is reduced after high-concentration addition, and the gelling phenomenon occurs in the mixing process of graphene and latex or in a high-speed stirring foaming process. This is related to the high aspect ratio of graphene and the sharpness of the blade as analyzed, which cuts the particles of the latex during stirring, creating a new latex interface. The new interface is lipophilic and incompatible with the water-based graphene, the stability of the latex is damaged, and the lipophilic latex is polymerized.
The addition of the graphene into the latex is also a conventional process for preparing the graphene rubber, and compared with mixed graphene addition processes such as banburying, open milling and the like, the shear stress is moderate, and the tearing damage of the graphene is light. However, the mechanical properties of the latex or rubber can be changed due to the high-concentration addition of the graphene, and the mechanical strength of the graphene latex can be increased due to the functional groups capable of reacting with the latex/rubber on the surface of the graphene in the vulcanization process.
Therefore, there is a need to develop a production process capable of increasing the concentration of graphene in the latex.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a production method of high-graphene-concentration latex, which is simpler in process method, takes natural concentrated latex and graphene oxide as raw materials, and realizes the multifunctionality of graphene latex/rubber, namely the functions of high heat conductivity, high electric conductivity, high strength, bacteriostasis and the like, through the mixing compatibility of surface-modified graphene oxide and latex, the mechanical stability of the graphene latex and the chemical combination of rubber molecules and graphene.
In order to solve the technical problems, the invention adopts the following technical scheme: a production method of high-graphene-concentration latex is characterized by comprising the following steps:
a) taking graphene oxide as a raw material, wherein the oxygen content of the graphene oxide is 5-30%;
b) dispersing graphene oxide in deionized water by adopting high shear or ultrasonic technology and the like to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 0.1-10 wt%;
c) mixing the graphene oxide slurry with casein, aromatic hydrocarbon amine, water-soluble organic polyamino and ammonia water in a heating reaction kettle in a proportion order, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: aromatic hydrocarbon amine: water-soluble organic polyammonia: ammonia water with a concentration of 20% is 100: 0.1 to 11: 0.01-1: 0.01-1: 0.01-1: 0.01 to 0.05;
d) firstly, adding aromatic hydrocarbon amine, continuously stirring, raising the temperature in a kettle to 70-95 ℃, maintaining for 3-5 hours, then adding casein, water-soluble organic polyamino and ammonia water with the concentration of 20% in proportion, and continuously reacting for 3-10 hours to obtain modified graphene slurry;
e) dehydrating the modified graphene slurry, washing for 3 times, and dehydrating to obtain a modified graphene concentrate, wherein the content of the modified graphene is 5-25%;
f) and mixing the modified graphene concentrate with natural latex in different proportions, wherein the weight proportion of the modified graphene in the solid content of the latex is 1-10 wt%, and the mechanical stability of the modified graphene latex exceeds 100 seconds.
In the step a), the graphene oxide has an oxygen content of 5-30%, a pH value of less than 7, and a specific surface area of 50-500 m2Per g, the particle size is 1-20 mu m, the length-thickness ratio is more than 500, the preferred oxygen content is 7-20%, and the preferred specific surface area is 70-200 m2The preferable particle size is 3-15 μm, and the production process can adopt a combination of a chemical oxidation method, an electrolysis method, a physical mechanical stripping method and a surface oxidation method, or can adopt aqueous slurry which is dispersed well without adding a dispersing agent.
In the step b), the dispersion process of the graphene oxide is a high shear method or an ultrasonic method and the like, and the high shear process adopts a high-speed colloid mill with the rotating speed of more than 2500rpm, an ultrahigh pressure homogenizer with the pressure of more than 50MPa and a nanometer sand mill with the rotating speed of more than 700 rpm; the ultrasonic method uses high-power ultrasonic equipment with power more than 3kW, and the graphene oxide is uniformly dispersed in deionized water at high concentration after dispersion without any agglomeration. This step is avoided if the starting material is an aqueous slurry of graphene oxide.
In the step c), adding ammonia water to adjust the pH value to be 9-12.
In the step d), the temperature in the kettle is 70-95 ℃, the total reaction time is 6-15 hours, firstly, aromatic hydrocarbon amine is added, the reaction is maintained for 3-5 hours, then casein, water-soluble organic polyamino and ammonia water with the concentration of 20% are added according to the proportion, the reaction is continued for 3-10 hours, the pH value is maintained between 9-12 in the reaction process through adding the ammonia water, the stirring speed ensures that the oxidized graphene slurry and each reactant are uniformly mixed, the temperature in the kettle is uniform, the concentration of each reactant is constant when the reaction is finished, and the pH value can be maintained to be unchanged when the ammonia water is not added.
In the step e), in order to remove unreacted raw materials, the modified graphene slurry is dehydrated and washed for 3 times and then dehydrated and concentrated, deionized water is used for washing the modified graphene slurry, the concentration of the modified graphene in water in the washing process is not more than 5%, a filter pressing or centrifugal separation method is adopted for dehydration, the pressure of the filter pressing is more than 0.5MPa, the rotation speed of centrifugal separation is more than 800rpm, a high-speed dispersion machine is adopted when the filter cake is re-dispersed in the deionized water, the rotation speed is more than 1000rpm, and the uniformity and no agglomeration of the modified graphene in the re-dispersed slurry are ensured. And finally, the content of the modified graphene in the dehydrated filter cake is 5-25%, and the preferable content is 10-20%.
In the step f), the weight ratio of the modified graphene in the solid content of the latex is 1-10 wt%, preferably more than 3%, the concentration of the latex is more than 50%, preferably more than 55%, and the mechanical stability test method of the modified graphene latex is according to the national standard GST 8301-2001.
Wherein casein is natural phosphorus-containing protein dissolved in alkaline water, aromatic hydrocarbon amine is aniline, phenethylamine, benzylamine or 2-methyl-6-ethyl aniline, etc., and water-soluble organic polyamine is amino-terminated polyether, triethylene tetramine or diethylene triamine, etc.
The high-graphene-concentration latex can be used for producing a latex foam material, wherein the high-speed stirring foaming time of the latex sponge in the production process is within 30 seconds, the time from foaming to injection molding is not more than 90 seconds, and the gel time is within 2 minutes; or adding acid formic acid to solidify the latex, and drying and dehydrating to obtain the graphene natural rubber.
According to the invention, natural concentrated latex and graphene oxide are used as raw materials, and through the mixing compatibility of surface modified graphene oxide and latex, the mechanical stability of graphene latex and the chemical combination of rubber molecules and graphene, the weight proportion of modified graphene in the solid content of the latex is 1-10 wt%, the mechanical stability of the modified graphene latex exceeds 100 seconds, and the multifunctional properties of the graphene latex/rubber, namely the functions of high heat conductivity, high electric conductivity, high strength, bacteriostasis and the like, are realized.
Detailed Description
The following is further described in conjunction with the detailed description:
embodiment 1, a method for producing a high graphene concentration latex, comprising the steps of:
a) graphene oxide with the oxygen content of 12 percent is taken as a raw material, and the specific surface area of the graphene oxide is about 180m2The grain diameter is about 7 mu m, and the length-thickness ratio is about 1500;
b) dispersing graphene oxide in deionized water by adopting a high shear process to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 4 wt%, and circularly dispersing for 30 minutes by adopting a high-speed colloid mill with the rotating speed of 5000rpm to obtain graphene oxide slurry, wherein the pH value is 6;
c) stirring and mixing the graphene oxide slurry, casein, aniline, amino-terminated polyether and ammonia water in a heating reaction kettle in proportion and sequence, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: aniline: amino-terminated polyether: ammonia water with a concentration of 20% ═ 100: 4.15: 0.2: 0.2: 0.1: 0.01 to 0.05;
d) firstly, adding aniline, continuously stirring, raising the temperature in a kettle to 90 ℃, and maintaining for 3 hours; adding casein, amino-terminated polyether and ammonia water with the concentration of 20% in proportion, keeping the temperature in the kettle unchanged, adjusting the pH to 9.5, and continuously reacting for 6 hours to obtain modified graphene slurry;
e) and (3) dehydrating the modified graphene slurry, washing the modified graphene slurry for 3 times by using deionized water, and then dehydrating the modified graphene slurry, wherein the concentration of the slurry is 4% during washing. Dispersing the filter cake in deionized water by using a high-speed dispersion machine, and performing filter pressing by using a plate and frame filter press under the pressure of 0.6MPa to obtain a modified graphene concentrate, wherein the content of the modified graphene is 18%;
f) mixing the modified graphene concentrate with natural latex with the concentration of 60%, wherein the weight ratio of the natural latex to the graphene concentrate is 100: 15.8. the weight proportion of the modified graphene in the solid content of the latex is 5 wt%, and the mechanical stability of the modified graphene latex is tested according to the national standard GST 8301-2001, wherein the stability is more than 200 seconds.
The modified graphene concentration latex is used for producing the latex mattress, the production process is a Dunlop method, and the problems of product quality, production line pause and the like caused by gel do not occur in the production process.
The density of the mattress is 80kg/m3The thermal conductivity of the graphene latex sponge is 0.048W/mK.
Embodiment 2, a method for producing a high graphene concentration latex, comprising the steps of:
a) graphene oxide with the oxygen content of 15 percent is taken as a raw material, and the specific surface area is about 250m2The grain diameter is about 7 mu m, and the length-thickness ratio is about 2000;
b) dispersing graphene oxide in deionized water by adopting a high shear process to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 3.5 wt%, and circularly dispersing for 30 minutes by adopting a high-speed colloid mill with the rotating speed of 5000rpm to obtain graphene oxide slurry, wherein the pH value is 6;
c) stirring and mixing the graphene oxide slurry, casein, phenethylamine, diethylenetriamine and ammonia water in a heating reaction kettle according to the proportion and the sequence, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: phenylethylamine: diethylenetriamine: ammonia water with a concentration of 20% ═ 100: 3.6: 0.25: 0.3: 0.12: 0.01 to 0.05;
d) firstly, adding aniline, continuously stirring, raising the temperature in a kettle to 85 ℃, and maintaining for 4 hours; adding casein, diethylenetriamine and ammonia water with the concentration of 20% according to the proportion, keeping the temperature in the kettle unchanged, adjusting the pH value to 9.5, and continuously reacting for 8 hours to obtain modified graphene slurry;
e) dehydrating the modified graphene slurry, washing the modified graphene slurry for 3 times by using deionized water, and then dehydrating the modified graphene slurry, wherein the concentration of the slurry is 3.5% during washing; dispersing the filter cake in deionized water by using a high-speed dispersion machine, and performing filter pressing by using a plate and frame filter press under the pressure of 0.6MPa to obtain a modified graphene concentrate, wherein the content of the modified graphene is 16%;
f) mixing the modified graphene concentrate with natural latex with the concentration of 60%, wherein the weight ratio of the natural latex to the graphene concentrate is 100: 11. the weight proportion of the modified graphene in the solid content of the latex is 3 wt%, and the mechanical stability of the modified graphene latex is tested according to the national standard GST 8301-2001, wherein the stability is more than 250 seconds.
The modified graphene concentration latex is used for producing the latex mattress, the production process is a Dunlop method, and the problems of product quality, production line pause and the like caused by gel do not occur in the production process.
The density of the mattress is 80kg/m3The thermal conductivity of the graphene latex sponge is 0.037W/mK.
Embodiment 3, a method for producing a high graphene concentration latex, comprising the steps of:
a) graphene oxide with the oxygen content of 9 percent is taken as a raw material, and the specific surface area is about 100m2The grain diameter is about 10 mu m, and the length-thickness ratio is about 1200;
b) dispersing graphene oxide in deionized water by adopting a high shear process to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 5 wt%, and circularly dispersing for 30 minutes by adopting a high-speed colloid mill with the rotating speed of 5000rpm to obtain graphene oxide slurry, wherein the pH value is 6.5;
c) stirring and mixing the graphene oxide slurry, casein, benzylamine, amino-terminated polyether and ammonia water in a heating reaction kettle in proportion and sequence, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: benzylamine: amino-terminated polyether: ammonia water with a concentration of 20% ═ 100: 5.15: 0.15: 0.15: 0.1: 0.01 to 0.05;
d) firstly, adding benzylamine, continuously stirring, raising the temperature in the kettle to 90 ℃, and maintaining for 4 hours; adding casein, amino-terminated polyether and ammonia water with the concentration of 20% in proportion, keeping the temperature in the kettle unchanged, adjusting the pH to 9.5, and continuously reacting for 8 hours to obtain modified graphene slurry;
e) dehydrating the modified graphene slurry, washing the modified graphene slurry for 3 times by using deionized water, and then dehydrating the modified graphene slurry, wherein the concentration of the slurry is 5% during washing; dispersing the filter cake in deionized water by using a high-speed dispersion machine, and performing filter pressing by using a plate and frame filter press under the pressure of 0.6MPa to obtain a modified graphene concentrate, wherein the content of the modified graphene is 20%;
f) mixing the modified graphene concentrate with natural latex with the concentration of 60%, wherein the weight ratio of the natural latex to the graphene concentrate is 100: 19.5. the weight proportion of the modified graphene in the solid content of the latex is 7 wt%, and the mechanical stability of the modified graphene latex is tested according to the national standard GST 8301-2001, wherein the stability is more than 200 seconds.
The modified graphene concentration latex is used for producing the latex mattress, the production process is a Dunlop method, and the problems of product quality, production line pause and the like caused by gel do not occur in the production process.
The density of the mattress is 80kg/m3In the case, the thermal conductivity of the graphene latex sponge is 0.061W/mK.
Embodiment 4, a method for producing a high graphene concentration latex, comprising the steps of:
a) graphene oxide with the oxygen content of 9 percent is taken as a raw material, and the specific surface area is about 100m2The grain diameter is about 10 mu m, and the length-thickness ratio is about 1200;
b) dispersing graphene oxide in deionized water by adopting a high shear process to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 6 wt%, and circularly dispersing for 30 minutes by adopting a high-speed colloid mill with the rotating speed of 5000rpm to obtain graphene oxide slurry, wherein the pH value is 6.4;
c) stirring and mixing the graphene oxide slurry, casein, phenethylamine, diethylenetriamine and ammonia water in a heating reaction kettle according to the proportion and the sequence, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: phenylethylamine: diethylenetriamine: ammonia water with a concentration of 20% ═ 100: 6.2: 0.1: 0.1: 0.12: 0.01 to 0.05;
d) firstly, adding phenylethylamine, continuously stirring, raising the temperature in the kettle to 85 ℃, and maintaining for 4 hours; adding casein, diethylenetriamine and ammonia water with the concentration of 20% according to the proportion, keeping the temperature in the kettle unchanged, adjusting the pH value to 10, and continuously reacting for 8 hours to obtain modified graphene slurry;
e) dehydrating the modified graphene slurry, washing the modified graphene slurry for 3 times by using deionized water, and then dehydrating the modified graphene slurry, wherein the concentration of the slurry is 6% during washing; dispersing the filter cake in deionized water by using a high-speed dispersion machine, and performing filter pressing by using a plate and frame filter press under the pressure of 0.6MPa to obtain a modified graphene concentrate, wherein the content of the modified graphene is 21%;
f) mixing the modified graphene concentrate with natural latex with the concentration of 60%, wherein the weight ratio of the natural latex to the graphene concentrate is 100: 26, the weight proportion of the modified graphene in the solid content of the latex is 10 wt%.
g) Slowly adding formic acid into the graphene slurry, simultaneously condensing the graphene and the latex, dehydrating by using the same filter press, wherein the filter pressing pressure is 0.6MPa, drying at low temperature to obtain a concentrated material of the graphene rubber, wherein the concentrated material can be added into various rubber products to increase the thermal conductivity and the electric conductivity of the rubber, reduce the air permeability and the like.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The present invention has been described in detail, and it should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Claims (9)
1. A production method of high-graphene-concentration latex is characterized by comprising the following steps: the method comprises the following steps:
a) selecting graphene oxide as a raw material, wherein the oxygen content of the graphene oxide is 5-30%;
b) dispersing graphene oxide in deionized water to prepare aqueous slurry, wherein the concentration of the graphene oxide in the slurry is 0.1-10 wt%;
c) mixing the graphene oxide slurry with casein, aromatic hydrocarbon amine, water-soluble organic polyamino and ammonia water in a heating reaction kettle in a proportion order, wherein the weight ratio of each component is as follows: and (3) graphene oxide: casein: aromatic hydrocarbon amine: water-soluble organic polyammonia: ammonia water with a concentration of 20% is 100: 0.1 to 11: 0.01-1: 0.01-1: 0.01-1: 0.01 to 0.05;
d) firstly, adding aromatic hydrocarbon amine, and continuously stirring; adding casein, water-soluble organic multi-ammonia and ammonia water with the concentration of 20% according to the proportion, and continuously reacting to obtain modified graphene slurry;
e) dehydrating, washing and dehydrating the modified graphene slurry to obtain a modified graphene concentrate, wherein the graphene content of the modified graphene concentrate is 5-25%;
f) and mixing the modified graphene concentrate with natural latex to obtain the high-graphene-concentration latex, wherein the weight ratio of the modified graphene in the solid content of the latex is 1-10 wt%, and the mechanical stability of the modified graphene latex exceeds 100 seconds.
2. The method for producing the high graphene concentration latex according to claim 1, wherein: in the step a), the pH value of the graphene oxide is less than 7, and the specific surface area is 50-500 m2The particle size is 1-20 mu m, and the length-thickness ratio is more than 500; the graphene oxide is prepared by combining a chemical oxidation method, an electrolytic method, a physical mechanical stripping method and a surface oxidation method, or by adopting an aqueous slurry which is well dispersed without adding a dispersing agent.
3. The method for producing the high graphene concentration latex according to claim 2, wherein: in the step b), the dispersion process of the graphene oxide is a high shear or ultrasonic method, and the high shear process is processed by adopting a high-speed colloid mill with the rotating speed of more than 2500rpm, an ultrahigh pressure homogenizer with the pressure of more than 50MPa and a nanometer sand mill with the rotating speed of more than 700 rpm; the ultrasonic method uses high-power ultrasonic equipment with power more than 3kW, and the graphene oxide is uniformly dispersed in deionized water at high concentration after dispersion without any agglomeration.
4. The method for producing the high graphene concentration latex according to claim 1, wherein: in the step c), adding ammonia water and adjusting the pH value to be 9-12.
5. The method for producing the high graphene concentration latex according to claim 1, wherein: in the step d), the temperature in the kettle is raised to 70-95 ℃, firstly, aromatic hydrocarbon amine is added, the reaction is maintained for 3-5 hours, then casein, water-soluble organic polyamino and ammonia water with the concentration of 20% are added according to the proportion, the reaction is continued for 3-10 hours, the pH value is maintained between 9 and 12 in the reaction process through adding the ammonia water, the stirring speed ensures that the oxidized graphene slurry and each reactant are uniformly mixed, the temperature in the kettle is uniform, and the concentration of each reactant tends to be constant when the reaction is finished.
6. The method for producing the high graphene concentration latex according to claim 1, wherein: in the step e), the modified graphene slurry is dehydrated and washed for 3 times, then is dehydrated and concentrated, the modified graphene slurry is washed by deionized water, and the concentration of the modified graphene in water in the washing process is not more than 5%; dehydrating by adopting a filter pressing or centrifugal separation method, wherein the pressure of the filter pressing is more than 0.5MPa, and the rotating speed of the centrifugal separation is more than 800 rpm; and (3) when the filter cake is redispersed in deionized water, a high-speed dispersion machine is adopted, the rotating speed is more than 1000rpm, the modified graphene in the redispersed slurry is ensured to be uniform and not to be agglomerated, and finally, the content of the modified graphene in the dehydrated filter cake is 5-25%.
7. The method for producing the high graphene concentration latex according to claim 1, wherein: in the step f), the weight proportion of the modified graphene in the solid content of the latex is more than 3%, and the mechanical stability test method of the modified graphene latex is according to the national standard GST 8301-2001.
8. The method for producing a high graphene concentration latex according to any one of claims 1 to 7, wherein: casein is natural phosphorus-containing protein dissolved in alkaline water; the aromatic hydrocarbon amine is aniline, phenethylamine, benzylamine or 2-methyl-6-ethyl aniline; the water-soluble organic polyamine is amino-terminated polyether, triethylene tetramine or diethylenetriamine.
9. The method for producing a high graphene concentration latex according to any one of claims 1 to 8, wherein: the high-graphene-concentration latex is used for producing a latex foam material, wherein the high-speed stirring foaming time of the latex sponge in the production process is within 30 seconds, the time from foaming to injection molding is not more than 90 seconds, and the gel time is within 2 minutes; or adding acid formic acid to solidify the latex, and drying and dehydrating to obtain the graphene natural rubber.
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| CN111218090A (en) * | 2020-03-04 | 2020-06-02 | 昆明理工大学 | Preparation method of anisotropic modified graphene epoxy resin composite material |
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| CN106947128A (en) * | 2017-04-19 | 2017-07-14 | 扬州大学 | A kind of preparation method of graphene compounded latex sponge |
| CN109250711A (en) * | 2017-07-13 | 2019-01-22 | 山东欧铂新材料有限公司 | A kind of preparation method of amination graphene oxide |
| CN109666259A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method of modified graphene oxide, modified graphene and modified graphene epoxy resin dispersion liquid |
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