CN112625282A - Production and processing technology of pearl graphene - Google Patents
Production and processing technology of pearl graphene Download PDFInfo
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- CN112625282A CN112625282A CN202011586123.XA CN202011586123A CN112625282A CN 112625282 A CN112625282 A CN 112625282A CN 202011586123 A CN202011586123 A CN 202011586123A CN 112625282 A CN112625282 A CN 112625282A
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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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
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
Abstract
The invention belongs to the technical field of graphene fibers, and particularly relates to a production and processing technology of pearl graphene, aiming at the problems of complex production and processing process and high manufacturing and processing cost of the existing pearl graphene, the following scheme is proposed at present: (1) prefabrication of graphite oxide: adding 20-35 mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.4-0.9 g of sodium nitrate and 3.5-3.8 g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow; (2) preparing graphite oxide: the mixture obtained in step (1) was filtered, and washed with a mixture of 64mL of water and 10mL of hydrochloric acid. The invention has the advantages of low price of raw materials, good strength and toughness, greatly improved strength and toughness of the composite material, good conductivity and tribology performance, stable performance, greatly reduced manufacturing and processing cost, and wide popularization and application.
Description
Technical Field
The invention relates to the technical field of graphene fibers, in particular to a production and processing technology of pearl graphene.
Background
The graphene fiber is prepared by attaching a graphene raw material to other fiber materials in a physical or chemical mode or doping graphene into artificial fiber slurry in a certain proportion, changes the physical and chemical properties of original fibers through the characteristics of the graphene, belongs to a new material, and can improve the mechanical strength by 2-3 times compared with the traditional material, namely a mother-of-pearl-like structure material, namely a bionic material. However, the defect of limited mechanical performance of the single-kind nano unit reinforced organic matter exists in the nacre-like structure material. In the development process of the fiber, graphene, clay sheets and LDH sheets are used as two-dimensional nano units, and cellulose fibers are used as one-dimensional nano units to enhance the mechanical property. Of these materials, some graphene-based composites, such as graphene/cellulose films, are of greatest interest. The composite material has the characteristics of good mechanical strength, large special surface area, low cost, abundant natural reserves, environmental friendliness and the like.
At present, due to the fact that protein materials capable of well connecting cellulose nanofibers and graphene are obtained, the nacre-like structure graphene fiber film with good mechanical strength is obtained, however, for the existing fiber film materials, the production and processing process is complex, the manufacturing and processing cost is high, and the pearl graphene production and processing process cannot be widely popularized and applied.
Disclosure of Invention
The production and processing technology of the pearl graphene provided by the invention solves the problems that the production and processing technology of the graphene fiber film with the pearl layer structure in the prior art is complex in process and high in manufacturing and processing cost, and cannot be widely popularized and applied.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production and processing technology of pearl graphene comprises the following steps:
(1) prefabrication of graphite oxide: adding 20-35 mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.4-0.9 g of sodium nitrate and 3.5-3.8 g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 2-3 h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.5-5.8 g of pearl powder, 6.0-6.8 g of oyster shell powder, 1-3 g of clam shell powder and 5-8 g of alginate fibers into 125-140 mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form a suspension, adding polyvinyl alcohol into the suspension, homogenizing under high pressure, uniformly stirring, extruding and granulating by a screw extruder, and rolling the extruded and granulated particles to form a film.
Preferably, the amount of the liquid nitrogen used in the step (5) is 8-10L.
Preferably, in the step (5), the pressure of the freeze dryer is less than 1Pa, and the freeze-drying temperature is-60 to-80 ℃.
Preferably, the algin weighed in the step (4) is dissolved in deionized water with the concentration of 40mg/ml, the stirring time is 20-30 min, the mixed solution is subjected to ultrasonic treatment for 30-50 min, and then the mixed solution is stirred for 6-8 h.
Compared with the prior art, the invention has the beneficial effects that:
the pearl-structure graphene fiber film prepared by the invention has the advantages of simple processing technology, low price of raw materials, good strength and toughness, stable performance, simple used equipment, greatly reduced manufacturing and processing cost and contribution to wide popularization and application, and the strength and toughness of the composite material are greatly improved, and good conductivity and tribology performance are obtained.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
The first embodiment is as follows:
a production and processing technology of pearl graphene comprises the following steps:
(1) prefabrication of graphite oxide: adding 20mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.4g of sodium nitrate and 3.5g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 2h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.5g of pearl powder, 6.0g of oyster shell powder, 1g of freshwater mussel shell powder and 5g of alginate fiber into 125mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form suspension, adding polyvinyl alcohol into the suspension, homogenizing and stirring uniformly under high pressure, extruding and granulating by a screw extruder, and rolling the extruded and granulated granules to form a film.
Wherein the dosage of the liquid nitrogen in the step (5) is 8L.
Wherein in the step (5), the pressure of a freeze dryer is less than 1Pa, and the freeze-drying temperature is-60 ℃.
Wherein, the algin weighed in the step (4) is dissolved in deionized water with the concentration of 40mg/ml, the stirring time is 20min, the mixed solution is subjected to ultrasonic treatment for 30min, and then the mixed solution is stirred for 6 h.
Example two:
a production and processing technology of pearl graphene comprises the following steps:
(1) prefabrication of graphite oxide: adding 25mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.6g of sodium nitrate and 3.6g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 2h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.5g of pearl powder, 6.0g of oyster shell powder, 1g of freshwater mussel shell powder and 5g of alginate fiber into 130mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form a suspension, adding polyvinyl alcohol into the suspension, homogenizing and stirring uniformly under high pressure, extruding and granulating by a screw extruder, and rolling the extruded and granulated granules to form a film.
Wherein the dosage of the liquid nitrogen in the step (5) is 8L.
Wherein in the step (5), the pressure of a freeze dryer is less than 1Pa, and the freeze-drying temperature is-60 ℃.
Wherein, the algin weighed in the step (4) is dissolved in deionized water with the concentration of 40mg/ml, the stirring time is 20min, the mixed solution is subjected to ultrasonic treatment for 30min, and then the mixed solution is stirred for 6 h.
Example three:
a production and processing technology of pearl graphene comprises the following steps:
(1) prefabrication of graphite oxide: adding 30mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.4g of sodium nitrate and 3.5g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 2h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.6g of pearl powder, 6.0g of oyster shell powder, 1g of freshwater mussel shell powder and 5g of alginate fiber into 133mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form a suspension, adding polyvinyl alcohol into the suspension, homogenizing and stirring uniformly under high pressure, extruding and granulating by a screw extruder, and rolling the extruded and granulated granules to form a film.
Wherein the dosage of the liquid nitrogen in the step (5) is 9L.
Wherein in the step (5), the pressure of a freeze dryer is less than 1Pa, and the freeze-drying temperature is-70 ℃.
Wherein, the algin weighed in the step (4) is dissolved in deionized water with the concentration of 40mg/ml, the stirring time is 20min, the mixed solution is subjected to ultrasonic treatment for 30min, and then the mixed solution is stirred for 7 h.
Example four:
a production and processing technology of pearl graphene comprises the following steps:
(1) prefabrication of graphite oxide: adding 35mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.9g of sodium nitrate and 3.8g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 3h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.8g of pearl powder, 6.8g of oyster shell powder, 3g of mussel shell powder and 8g of alginate fiber into 140mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form a suspension, adding polyvinyl alcohol into the suspension, homogenizing and stirring uniformly under high pressure, extruding and granulating by a screw extruder, and rolling the extruded and granulated granules to form a film.
Wherein the dosage of the liquid nitrogen in the step (5) is 10L.
Wherein in the step (5), the pressure of a freeze dryer is less than 1Pa, and the freeze-drying temperature is-80 ℃.
Wherein, the algin weighed in the step (4) is dissolved in deionized water with the concentration of 40mg/ml, the stirring time is 30min, the mixed solution is subjected to ultrasonic treatment for 50min, and then the mixed solution is stirred for 8 h.
According to the production and processing technology of the pearl graphene, the prepared pearl-structure graphene fiber film is simple in processing technology, low in raw material price, good in strength and toughness, stable in performance, simple in used equipment, and beneficial to wide popularization and application, and the strength and toughness of the composite material are greatly improved, and good conductivity and tribology performance are obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. The production and processing technology of the pearl graphene is characterized by comprising the following steps:
(1) prefabrication of graphite oxide: adding 20-35 mL of sulfuric acid into a beaker into dried 2g of graphite powder, stirring, adding 0.4-0.9 g of sodium nitrate and 3.5-3.8 g of potassium permanganate after 50min, heating to 35 ℃ after 1h for reaction for 2h, and then adding 35% of hydrogen peroxide until the reaction solution is changed from brown to bright yellow;
(2) preparing graphite oxide: filtering the mixed solution prepared in the step (1), washing with the mixed solution of 64mL of water and 10mL of hydrochloric acid, centrifugally washing with a large amount of deionized water to neutrality, finally filling the mixed solution into a dialysis bag, and dialyzing for about ten days to prepare graphite oxide;
(3) preparing a graphene oxide solution: carrying out ultrasonic treatment on the graphite oxide prepared in the step (2) by using an ultrasonic cell crusher to obtain a brown graphene oxide dispersion liquid, and freeze-drying the obtained graphene oxide dispersion liquid and then retaining the graphene oxide dispersion liquid;
(4) preparing a graphene oxide algin solution: weighing algin, dissolving the algin in deionized water, taking 350mL of graphene oxide solution prepared in the step (3) and 450mL of algin solution, mixing the graphene oxide solution and the algin solution, stirring, performing ultrasonic treatment, and stirring again to obtain a uniform solution;
(5) preparing a graphene oxide alginate ridge beam: adding 800mL of the graphite oxide alginate solution prepared in the step (4) into a mold, adding liquid nitrogen, standing for 1h until the solution is completely frozen, taking out the solution from the mold, and freezing the solution in a freeze dryer for 2-3 h to obtain a graphene oxide alginate ridge beam with a laminated structure;
(6) preparing a pearl graphite fiber film; adding 5.5-5.8 g of pearl powder, 6.0-6.8 g of oyster shell powder, 1-3 g of clam shell powder and 5-8 g of alginate fibers into 125-140 mL of polylactide, stirring at the speed of 600rpm/min at 70 ℃ for 20min to form a suspension, adding polyvinyl alcohol into the suspension, homogenizing under high pressure, uniformly stirring, extruding and granulating by a screw extruder, and rolling the extruded and granulated particles to form a film.
2. The production and processing technology of pearl graphene according to claim 1, wherein the amount of liquid nitrogen used in step (5) is 8-10L.
3. The production and processing technology of pearl graphene according to claim 1, wherein in the step (5), the pressure of a freeze dryer is less than 1Pa, and the freeze-drying temperature is-60 ℃ to-80 ℃.
4. The production and processing technology of pearl graphene according to claim 1, wherein the algin weighed in the step (4) is dissolved in deionized water with a concentration of 40mg/ml, the stirring time is 20-30 min, the mixed solution is subjected to ultrasonic treatment for 30-50 min, and then the mixed solution is stirred for 6-8 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787317A (en) * | 2014-01-02 | 2014-05-14 | 上海应用技术学院 | Preparation method of graphene oxide dispersion liquid |
| CN104163423A (en) * | 2014-08-13 | 2014-11-26 | 东华大学 | Method for preparing spongy graphene by freeze drying |
| CN108559112A (en) * | 2018-03-20 | 2018-09-21 | 清远粤绿新材料技术有限公司 | A kind of preparation method of graphene-cellulose conductive composite film |
| CN109504012A (en) * | 2018-12-22 | 2019-03-22 | 穆凯鹏 | Graphene oxide-polyacrylic acid imitates the preparation method of shell mother-of-pearl layered composite film |
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2020
- 2020-12-29 CN CN202011586123.XA patent/CN112625282A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787317A (en) * | 2014-01-02 | 2014-05-14 | 上海应用技术学院 | Preparation method of graphene oxide dispersion liquid |
| CN104163423A (en) * | 2014-08-13 | 2014-11-26 | 东华大学 | Method for preparing spongy graphene by freeze drying |
| CN108559112A (en) * | 2018-03-20 | 2018-09-21 | 清远粤绿新材料技术有限公司 | A kind of preparation method of graphene-cellulose conductive composite film |
| CN109504012A (en) * | 2018-12-22 | 2019-03-22 | 穆凯鹏 | Graphene oxide-polyacrylic acid imitates the preparation method of shell mother-of-pearl layered composite film |
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