CN112473067A - Preparation method of graphene composite graphite micro-powder foam extinguishing agent and product thereof - Google Patents
Preparation method of graphene composite graphite micro-powder foam extinguishing agent and product thereof Download PDFInfo
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- CN112473067A CN112473067A CN202011604077.1A CN202011604077A CN112473067A CN 112473067 A CN112473067 A CN 112473067A CN 202011604077 A CN202011604077 A CN 202011604077A CN 112473067 A CN112473067 A CN 112473067A
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- extinguishing agent
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- micropowder
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0007—Solid extinguishing substances
- A62D1/0014—Powders; Granules
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0071—Foams
- A62D1/0078—Foams containing proteins or protein derivatives
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Carbon And Carbon Compounds (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention discloses a graphene composite graphite micropowder foam extinguishing agent, a preparation method thereof and a product thereof. By compounding the graphene on the surface of the graphite micropowder, the surface action sites of the graphite micropowder are greatly increased, and the dispersibility of the graphite micropowder in a foam extinguishing agent solution is improved. The protein hydrolysis process is combined with the composite process of the graphite micro powder, so that the extra energy consumption is reduced, and the practicability is high.
Description
Technical Field
The invention relates to the field of fire extinguishing agents, in particular to a foam extinguishing agent, and especially relates to a preparation method and a product of a graphene composite graphite micro powder foam extinguishing agent.
Background
The main component of the protein foam extinguishing agent is hydrolyzed protein, which is a harmless and cheap extinguishing agent. Heating the industrial protein under acidic conditions produces hydrolyzed protein, the degree of hydrolysis being related to the ability of the fire extinguishing agent to foam. The graphite and the expanded graphite micropowder can be used as a dry powder extinguishing agent to extinguish fires caused by metals such as sodium, potassium and the like. Recently, researches show that the anti-burning capacity of the foam fire extinguishing agent can be enhanced by adding graphite and expanded graphite micro powder into the protein foam fire extinguishing agent to form a three-phase fire extinguishing agent (Hanbaoling, the research on the fire extinguishing performance of the graphite protein foam fire extinguishing agent on oil fire [ J ]. China science and technology vertical and horizontal, 2017, 000(002): 165-166.; Jiansheng, Zhai-changeable, Xujian nan, and the like. In order to ensure the flame-retardant effect, more than 10% of graphite micro powder by mass is often required to be added into the foam extinguishing agent, and a large amount of graphite micro powder is deposited at the bottom of the extinguishing agent and is not beneficial to extinguishing fire.
Graphene Oxide (GO) is graphene having an oxygen-containing functional group, and can be uniformly dispersed in water, and can support a protein by the action of the oxygen-containing functional group thereon, and the dispersibility in water is further improved. The dispersibility of graphene oxide is also related to the pH value, and the lower the pH, the lower the dispersibility. In addition, the graphene-based material is also a good refractory material (DouChong, Lindaoli. graphene-based composite material flame retardant performance research [ J ]. fire-fighting science and technology, 2013, 32(10): 1145 + 1147.), and has primary application in the field of fire extinguishing agents (Chinese patent CN 108079477A, Chinese patent CN 106823229A and Chinese patent CN 108273225A), but the graphene-based material is high in price and difficult to popularize and apply.
In order to improve the rheological property of the graphite micropowder in the foam extinguishing agent, the graphite surface needs to be modified, and the graphite has high chemical inertness and is difficult to modify the surface through direct chemical reaction. One solution is to coat the graphite with other carbon materials such as graphene, pitch, etc. using the natural affinity between the carbon material and graphite to form a so-called pure carbon composite. The pure carbon compound not only keeps the basic properties of graphite, but also greatly improves the chemical inertness of the surface of the graphite, and has more applications in the field of energy sources.
Disclosure of Invention
Aiming at the problem that the graphite micropowder is unstable to disperse in an aqueous solution, the invention aims to provide a preparation method of a graphene composite graphite micropowder foam extinguishing agent. The foam extinguishing agent is prepared by compounding graphene on the surface of graphite micropowder and further compounding hydrolyzed protein.
It is yet another object of the present invention to provide: a graphene composite graphite micropowder foam extinguishing agent product prepared by the method.
The purpose of the invention is realized by the following scheme: a preparation method of a graphene composite graphite micropowder foam extinguishing agent comprises the following steps of firstly compounding graphene with graphite micropowder in an acid sedimentation mode, then further modifying the surface of the graphene by utilizing hydrolyzed protein to obtain a high-dispersity compound, and further compounding to obtain a practical foam extinguishing agent, wherein the preparation method comprises the following steps:
(1) fully and uniformly mixing graphite micro powder and a graphene oxide solution by rapid stirring and ultrasound;
(2) adding acid into the solution obtained in the step (1), so that the dispersibility of the graphene oxide is reduced and the graphene oxide is coated on the surface of graphite;
(3) adding industrial gelatin into the dispersion liquid obtained in the step (2), continuously stirring, and then sealing into a hydrothermal kettle for heating;
(4) and (4) cooling the product obtained in the step (3), adjusting the pH value, performing ultrasonic dispersion, and adding a foam stabilizer to obtain the graphene composite graphite micropowder foam extinguishing agent.
The mesh number of the graphite micro powder in the step (1) is at least 1000 meshes.
Preferably, the particle size of the graphite micropowder used in the step (1) is 3000 meshes.
The mass ratio of the graphene oxide to the graphite particles in the step (1) is 1: 50 to 1: 200.
the acid added in the step (2) is hydrochloric acid or acetic acid, and the hydrolysis degree of the industrial protein in the step (3) can be regulated and controlled by regulating the dosage, so that the foaming performance and rheological property of the fire extinguishing agent are regulated and controlled.
Preferably, the acid used in step (2) is acetic acid.
In the step (3), the total concentration of the industrial gelatin added in the fire extinguishing agent is 8 percent.
In the step (4), lauryl alcohol (lauryl alcohol) is used as a foam stabilizer, and the concentration is 4 g L-1。
The invention provides a graphene composite graphite micropowder foam extinguishing agent which is prepared by any one of the methods.
According to the invention, graphene is firstly compounded with graphite micropowder in an acid sedimentation mode, then the surface of the graphene is further modified by utilizing hydrolyzed protein to obtain a high-dispersity compound, and then the high-dispersity compound is compounded to obtain a practical foam extinguishing agent.
The invention has the advantages that: by compounding the graphene on the surface of the graphite micropowder, the surface action sites of the graphite micropowder are greatly increased, and the dispersibility of the graphite micropowder in a foam extinguishing agent solution is improved. The protein hydrolysis process is combined with the composite process of the graphite micro powder, so that the extra energy consumption is reduced, and the practicability is high.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1.
A method of manufacturing a semiconductor device, comprising the steps of 1: the 50-type graphene composite graphite micropowder foam extinguishing agent is prepared by firstly compounding graphene with graphite micropowder in an acid precipitation mode, then further modifying the surface of the graphene by utilizing hydrolyzed protein to obtain a high-dispersity compound, and further compounding to obtain a practical foam extinguishing agent, and the preparation method comprises the following steps:
(1) preparing a mixture of graphene oxide and graphite micropowder:
adding 0.4 g of graphene oxide powder into 200 mL of water at room temperature, and stirring and ultrasonically dissolving to obtain a graphene oxide solution; fully and uniformly mixing 20 g of graphite micropowder and graphene oxide solution with ultrasound by quickly stirring for 2 hours to obtain a mixed solution;
(2) acidifying to form a graphene oxide-graphite micropowder composite:
adding 1 mL of commercially available concentrated hydrochloric acid into the mixed solution obtained in the step (1), and continuing to react for 0.5 h, wherein the dispersibility of the graphene oxide in water is reduced and the graphene oxide is coated on the surface of the graphite micropowder to form a composite dispersion liquid;
(3) complex formation with hydrolyzed protein:
adding 185 mL of industrial gelatin containing 32 g of gelatin into the dispersion liquid obtained in the step (2), continuously stirring for 0.5 h, sealing the obtained dispersion liquid into a hydrothermal kettle, heating for 2 h at 120 ℃, and hydrolyzing the gelatin and preliminarily combining the gelatin with the graphene-graphite micro powder compound;
(4) the pH was adjusted back and complexes formed:
cooling the product obtained in the step (3), adjusting the pH value to 9, continuously stirring for 2 h, under an alkaline condition, reforming hydrogen bonds between the hydrolyzed protein and oxygen-containing functional groups of the graphene to finally form composite particles with high dispersibility, adding 1.6 g of lauryl alcohol serving as a foam stabilizer, and continuously stirring for 15 min to obtain the product 1: 50 type graphene composite graphite micropowder foam extinguishing agent.
Example 2.
A method of manufacturing a semiconductor device, comprising the steps of 1: the 200-type graphene composite graphite micropowder foam extinguishing agent is similar to the step of the embodiment 1, and is prepared by the following steps:
(1) preparing a mixture of graphene oxide and graphite micropowder:
adding 0.1 g of graphene oxide powder into 200 mL of water at room temperature, and stirring and ultrasonically dissolving to obtain a graphene oxide solution; fully and uniformly mixing 20 g of graphite micropowder and the graphene oxide solution by quickly stirring for 2 hours to obtain a mixed solution;
(2) acidifying to form a graphene oxide-graphite micropowder composite:
keeping stirring, adding 2 mL of glacial acetic acid into the mixed solution obtained in the step (1), and continuing to react for 0.5 h, wherein the dispersibility of the graphene oxide in water is reduced and the graphene oxide is coated on the surface of the graphite micropowder to form a composite dispersion solution;
(3) complex formation with hydrolyzed protein:
adding 160 mL of industrial gelatin solution containing 32 percent of gelatin into the compound dispersion liquid obtained in the step (2), continuously stirring for 0.5 h, sealing the obtained dispersion liquid into a hydrothermal kettle, heating for 2 h at 120 ℃ to obtain dispersion liquid, and hydrolyzing the gelatin and preliminarily combining the gelatin with the graphene-graphite micro powder compound;
(4) the pH was adjusted back and complexes formed:
cooling the dispersion obtained in step (3) and adding an appropriate amount of sodium hydroxide solution to increase the pH to 9. Continuously stirring for 2 h, under the alkaline condition, hydrogen bonds are formed again between the hydrolyzed protein and the oxygen-containing functional groups of the graphene, and finally composite particles with high dispersity are formed, and sodium acetate left in the solution also plays a certain role in stabilizing the composite. Adding 1.6 g of lauryl alcohol as a foam stabilizer, and continuously stirring for 15 min to obtain a mixture of 1: 200 type graphene composite graphite micropowder foam extinguishing agent.
The above examples are merely illustrative for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (8)
1. A preparation method of a graphene composite graphite micropowder foam extinguishing agent is characterized by firstly compounding graphene with graphite micropowder in an acid sedimentation mode, then further modifying the surface of the graphene by utilizing hydrolyzed protein to obtain a high-dispersity compound, and further compounding to obtain a practical foam extinguishing agent, and comprises the following steps:
(1) the method comprises the following steps of fully and uniformly mixing graphite micro powder and a graphene oxide solution through rapid stirring and ultrasound, wherein the mass ratio of the graphene oxide to graphite particles is 1: 50 to 1: 200 of a carrier;
(2) adding acid into the solution obtained in the step (1), so that the dispersibility of the graphene oxide is reduced and the graphene oxide is coated on the surface of graphite;
(3) adding industrial gelatin into the dispersion liquid obtained in the step (2), continuously stirring, sealing the mixture in a hydrothermal kettle and heating, wherein the total concentration of the industrial gelatin in the fire extinguishing agent is not more than 10%;
(4) and (4) cooling the product obtained in the step (3), adjusting the pH value, performing ultrasonic dispersion, and adding lauryl alcohol serving as a foam stabilizer to obtain the graphene composite graphite micropowder foam extinguishing agent.
2. The preparation method of the graphene composite graphite micropowder foam fire extinguishing agent according to claim 1, wherein the mesh number of the graphite micropowder in the step (1) is at least 1000 meshes.
3. The method for preparing the graphene composite graphite micropowder foam extinguishing agent according to claim 1, wherein the particle size of the graphite micropowder is 3000 meshes.
4. The preparation method of the graphene composite graphite micropowder foam fire extinguishing agent according to claim 1, wherein the acid added in the step (2) is hydrochloric acid or acetic acid.
5. The preparation method of the graphene composite graphite micropowder foam fire extinguishing agent according to claim 1, wherein the acid used in the step (2) is acetic acid.
6. The method for preparing the graphene composite graphite micropowder foam fire extinguishing agent according to claim 1, wherein the total concentration of industrial gelatin added in the fire extinguishing agent in the step (3) is 8%.
7. The preparation method of the graphene composite graphite micropowder foam fire extinguishing agent according to claim 1, wherein the foam stabilizer in the step (4) is 4 g L-1。
8. A graphene composite graphite micropowder foam extinguishing agent, which is characterized by being prepared according to the method of any one of claims 1 to 7.
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| CN202011604077.1A CN112473067B (en) | 2020-12-30 | 2020-12-30 | Preparation method of graphene composite graphite micro-powder foam extinguishing agent and product thereof |
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| CN202011604077.1A CN112473067B (en) | 2020-12-30 | 2020-12-30 | Preparation method of graphene composite graphite micro-powder foam extinguishing agent and product thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280079A (en) * | 2016-08-04 | 2017-01-04 | 桐乡市小老板特种塑料制品有限公司 | A kind of fire extinguishing band |
| CN106377862A (en) * | 2016-08-31 | 2017-02-08 | 胡泽军 | Fire extinguishing agent prepared from grapheme and superfine materials |
| CN108864839A (en) * | 2017-05-12 | 2018-11-23 | 力王新材料（惠州）有限公司 | A kind of expanded graphite flame-retarding fire-extinguishing material and preparation method thereof |
| WO2019054861A1 (en) * | 2017-09-13 | 2019-03-21 | Technische Universiteit Delft | Fire extinguishing solution |
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- 2020-12-30 CN CN202011604077.1A patent/CN112473067B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280079A (en) * | 2016-08-04 | 2017-01-04 | 桐乡市小老板特种塑料制品有限公司 | A kind of fire extinguishing band |
| CN106377862A (en) * | 2016-08-31 | 2017-02-08 | 胡泽军 | Fire extinguishing agent prepared from grapheme and superfine materials |
| CN108864839A (en) * | 2017-05-12 | 2018-11-23 | 力王新材料（惠州）有限公司 | A kind of expanded graphite flame-retarding fire-extinguishing material and preparation method thereof |
| WO2019054861A1 (en) * | 2017-09-13 | 2019-03-21 | Technische Universiteit Delft | Fire extinguishing solution |
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