KR100890561B1 - Oxidation colloid nano graphite manufacturing method - Google Patents

Abstract

A method for manufacturing oxidation colloid nano graphite is provided to manufacture the oxidation colloid nano graphite electrochemically after heating up the graphite in a furnace. A method for manufacturing oxidation colloid nano graphite comprises the following steps of: pulverizing high pure graphite to a corpuscle; mixing pulverized high pure graphite, nitric acid, sulfuric acid, distilled water and ammonium nitrate; maturing the mixed contents; stabilizing air for removing nitrogen; cooling quickly the matured contents after heating up; dehydrating the cooled contents in a dehydrator to paper; neutralizing the colloidal graphite by injecting the contents into the oxidation colloidal graphite; dehydrating again the neutralized graphite.

Description

Oxidation colloid nano Graphite Manufacturing method

The present invention relates to a method for producing colloidal nano graphite oxide to be used as a variety of new materials in the field of lithium batteries, high conductivity ink, corrosion-resistant corrosion, solar heat collection material, carbon fiber substitute composite materials.

In general, graphite is composed of carbon such as coke and diamond, but has a unique layered crystal structure in which a hexagonal structure composed of carbon atoms is layered. When such graphite is treated with a suitable oxidizing agent, chemical species such as SO ₃ ^{2 -} and NO ₃ ^- are introduced between the graphite layers to form interlayer compounds.

High-purity graphite has generally increased the purity of graphite by heating the secondary graphite material treated in the graphitization furnace in a reaction furnace and removing impurities contained in the secondary graphite material by combining with chlorine gas or hydrogen hydrogen gas. . For example of other methods

In Korean Patent Registration No. 10-0694649, carbon black is selected and carbonized at a high temperature in heating materials that can be used for heating, hot water supply, drying, food cooking, and equipment that require high temperature or heat. To obtain the first pulverized, the first pulverized carbon black to a cake state, and then pulverized and sieved to obtain purified carbon as a 60 ~ 70 micron powder before heat treatment at 200 degrees before crushing; distilled water and silicon dioxide and potassium oxide To obtain a water glass by mixing a predetermined ratio; 15 to 40 parts by weight of purified carbon, 0.3 to 1.0 parts by weight of water-based acid powder, 0.2 to 1.0 parts by weight of a silicone antifoaming agent is pulverized under vibration by mixing 100 parts by weight of water glass To obtain a colloidal carbon solution; A conductive carbon thin film exothermic material provided through is described,

Patent Publication No. 10-0675992 describes carbon nanorods, comprising a carbon hexagonal mesh with a central axis extending in one direction,

Publication No. 10-0254483 discloses the steps of oxidizing graphite by dry contact with SO 3 gas generated from fuming sulfuric acid or sulfuric anhydride; Irradiating microwaves to the oxidized graphite; And it is described a method of producing expanded graphite comprising the step of expanding the thermally expanded graphite oxide irradiated with microwaves,

Korean Patent Publication No. 10-238015 is filled with a main raw material mainly composed of a mixture of coke and silica in a furnace of an electric resistance heating furnace to obtain a high-purity graphitized graphite in a small number of processing fixtures. A preliminary step of arranging the carbon material in the part, energizing the positive electrode, energizing the positive electrode continuously in a preliminary step of generating an ingot group of silicon carbide around the core part by reduction carbonization of silicon, and The ingot of silicon carbide is transformed into high-purity graphite by heating the incot to a temperature above the sublimation temperature of silicon and below the sublimation temperature of graphite, and thermally dissociating the silicon atoms in the silicon carbide to oxidize and remove the ingot outside. It is known a method for producing graphite, comprising a purifying step to

In the method for producing expanded graphite molded article described in Japanese Patent Application Laid-Open No. 59-35078, expanded graphite is produced by heat-treating graphite deposited at a mixed acid of 50% sulfuric acid and 60% perchloric acid in a weight ratio of 100: 5 at 1000 ° C. Technology is described,

Japanese Patent Laid-Open No. 61-72609 describes a method for producing expanded graphite using sodium and tetrahydrofuran,

Japanese Patent Laid-Open Publication Nos. 62-170332, 63-3939081, 3086538 and 4-21509 use a mixture of sulfuric acid and hydrogen peroxide, sulfuric acid and nitric acid and boric acid, and concentrated sulfuric acid and concentrated nitric acid as oxidizing agents. , A method for producing expanded graphite that can be used as a composite material of cement and mortar, expanded graphite sheet, and the like,

Japanese Patent Application Laid-Open Nos. 7-136501, 8-143856, and U.S. Patent No. 5,149,518 use mixed acids based on sulfuric acid as oxidants, which can be used as expanded graphite sheets, oil adsorbents and inorganic fiber composite materials. A method for producing expanded graphite is disclosed,

US Pat. No. 5,503,717 discloses a process for producing expanded graphite by electrochemically injecting ZnCl 2 into graphite layers and then heat treating them.

As described above, when the mixed acid based on sulfuric acid is used as the oxidizing agent, the consumption of acid is caused by directly impregnating graphite particles in a large amount (1.5 times or more of graphite) in a concentrated mixed acid stock solution for a long time. In order to solve this very many disadvantages, it is a problem to be solved by the present invention to provide a method for producing a colloidal nano-graphite graphite electrochemically by heating the graphite in the furnace with an electrode, and then using nitric acid sulfate and calcium nitrate.

The present invention is to solve the problems of the prior art, as an improvement of the domestic patent application No. 10-2006-36087, the applicant filed earlier,

The graphite minerals are placed in a kiln and reheated, mixed with nitric acid, sulfuric acid, calcium nitrate and nitrogen dioxide valence, heated, diluted with ammonia and caustic soda mixture to pH 2-3, washed, dried and Therefore, to provide a method for producing colloidal oxide nanographium oxide is prepared by dilution in water is a problem solving means to achieve the present invention.

The present invention is obtained by using a furnace using an electrode electrode of high purity graphite, and then acid treated with nitric acid, sulfuric acid, calcium nitrate and nitrogen dioxide gas, it is possible to eliminate the risk due to NO2 gas, and also separately expensive moisture purification device It is possible to omit the NO2 gas by using a high pressure pump, which can be omitted, and to dehydrate the graphite suspension treated with acid diluted with ammonia and caustic soda mixture. It can reduce size 10 ~ 30 times, and it is a manufacturing method of colloidal nano graphite oxide which is used by adding water or alcohol to water 3: 1 paste as needed afterwards. It is economical by simplifying removal and greatly reducing installation cost and production cost. Academically than opening the way to producing a new material oxide nano-colloidal graphite is produced with the new technology, which will also have an innovative effect.

In order to achieve the above object, the present invention provides a general graphite mineral in an electric furnace.

Obtaining high purity graphite by high temperature firing at 2600 ~ 3200 ℃:

Grinding the high purity graphite obtained by the high temperature firing into 0.1-3 μm fine particles:

Reacting by adding 1 ~ 10 kg of 1N carnitrate 400g 1N nitric acid 2.5kg, 1N sulfuric acid 7.5kg distilled water to 1kg to 5kg of 1N ammonium nitrate in 1kg

Stabilizing step characterized in that the mixed content of the reaction in the aging period for 10 to 14 hours and put in air to remove nitrogen, aeration by stabilizing treatment:

Heating and cooling step of heating and quenching 70 ~ 100 ℃, 2 to 4 hours to the mature content:

The first step of dewatering by filtering the paper in the dehydrator after the heating, quenching:

6-10 L of distilled water was added to the paste-type high-purity graphite collected by the first dehydration, and 1N ammonia and 1N caustic soda were mixed in the same amount, and the mixture was stirred until pH 2-3, to neutralize colloidal graphite. Neutralization stage

It relates to a method for producing colloidal nano-oxide oxide consisting of a second step of dewatering the content of the pH 2-3 using a paper again in the dehydrator.

Graphite manufacturing is to prepare three container boxes of 500 ~ 1000㎛ particles of graphite minerals 700mm length 350mm height 350mm of graphite material and fill the same graphite mineral particles 500 ~ 1000㎛ particles in it and maintain airtightness,

(See Figs. 1 and 2) After stacking firebrick having a width of 4700 mm and a width of 1300 mm and a thickness of 500 mm, the graphite of (Fig. 1) prepared in a box having a bottom thickness of 300 mm is placed in a container box (Fig. 2) and the cover closed. ,

Since 100 전극 or more electricity is connected to both sides of the graphite electrode rod as shown in FIG. Oxidation is prevented by maintaining the vacuum, and when the high temperature is continuously heated at a temperature of 2600 ~ 3200 ℃ for a certain time, impurities in the graphite mineral are calcined, thereby obtaining pure graphite having a purity of 99.98% or more.

The graphite thus obtained is pulverized through a conventional pulverizer and the pulverized fine particles are sorted through a sorting machine to separate small and small particles to obtain small particles, and the large particles are pulverized again to obtain small particles.

This produces graphite powder particles with a diameter of 0.1-3 μm.

In the present invention, NO2 gas is generated, which must be removed to eliminate the dangers caused by NO2 gas in the next process, and also to remove NO2 gas by using a high pressure pump at a low cost by omitting an expensive moisture purification device. Way

In the present invention, when the NO 2 gas is injected into the NO 2 gas remover using a high pressure pump with a jet nozzle, the NaOH solution and the NO 2 gas are inhaled to remove the NO 2 gas, and also prevent the fusion of nitrogen oxide during the operation and lower concentration than usual in the reactor. So that it does not react with foreign matter,

Since the amount of the drug used in the present invention is various, and the result of finding the best amount of experiment results over several decades, the colloidal graphite oxide is produced even if the process time is different or less than the amount described above, but the quality and characteristics The quality of the colloidal graphite may be deteriorated over time or due to changes in temperature, pressure, and humidity of the surrounding environment.

In the present invention, the air is stirred and aerated, and then heated in a heater at 80 to 100 ° C. for 2 to 4 hours, followed by quenching and stabilizing. After stabilizing, the contents are filtered by primary paper and dewatered once in advance. More filtering and dehydration can reduce the use of demineralized water in the work process by 10 ~ 20 times and greatly reduce the working time.

After the first dehydration, add 6-10 liters of distilled water to the high-purity graphite paste collected, and stir until the mixture of 1N ammonia and 1N caustic soda is brought to pH 2-3 and neutralize colloidal graphite solution. Can be greatly reduced,

A method for manufacturing a colloidal graphite graphite, which neutralizes colloidal graphite oxidized to pH 2 to 3, and then filter the filter in the second dewatering process, which also facilitates the filtering, and decomposes colloidal oxide oxide of graphite, which is a precipitate after dehydration. will be.

Hereinafter, the present invention will be described in detail with reference to the following Examples.

Example

1st process

Prepare three container boxes with graphite mineral 500 ~ 1000㎛ particles of 700mm length 350mm height 350mm made of graphite material, fill them with the same graphite mineral diameter 500 ~ 1000㎛ particles, and maintain airtightness.

After stacking fire bricks 4700mm wide by 1300mm wide and 500mm thick, and putting the prepared graphite minerals in a box with a floor thickness of 300mm in the container box and closing the cover,

Connect electricity over 100㎾ to both sides of graphite electrode rod and flow it (by adding nitrogen as needed), and heat the temperature of 2600 ~ 3200 ℃, and maintain the airtightness of surrounding graphite minerals so that no oxygen is added, so vacuum is maintained by oxidation. To prevent incineration of impurities in the graphite, thus obtaining pure graphite with a purity of 99% or higher,

After the baked particles are put into a grinder and continuously pulverized with a graphite powder of diameter 05. ~ 2 ㎛, and after sorting the graphite pulverized into fine particles with a diameter of 0.1 ~ 3 ㎛ through a separator,

2nd process

After 1 kg of pulverized high-purity graphite as described above, 1 N Carri nitrate 400 g 1 N nitrate 2.5 kg, 1 N sulfuric acid 7.5 kg distilled water 8-12 L, 1 N ammonia nitrate 5-10 g was added to the reactor, followed by reaction.

(If the NO2 gas is injected into the NO2 gas remover using the high pressure pump with a jet nozzle, the NO2 gas is sucked into the NaOH mixture solution to remove the NO2 gas and, if necessary, removed using a carbon filter.)

After transferring the mixed reaction contents to a ripening machine for 10 to 14 hours, and aeration by stabilizing by adding air using a pipe connected to the aeration tank connected to the compressor to remove nitrogen,

After transferring the aged contents to a heater and heating at 70-100 ° C. for 2 to 4 hours, after transferring to a quenching machine and quenching,

After the heating and quenching, transfer to a vacuum dehydrator and filter by paper in the vacuum dehydrator to the first dehydration,

Transfer the colloidal graphite paste sifted after the first dehydration to a neutralization tank, add 6-10 L of distilled water, and stir the mixed solution of 1N ammonia and 1N caustic soda until pH 2 ~ 3 to neutralize colloidal graphite.

The contents of pH 2-3 were transferred to a vacuum dehydrator to filter and dewater using paper again to prepare colloidal nano graphite oxide.

Hereinafter, the colloidal oxide nanographite production apparatus of the present invention will be described with reference to the drawings.

1 and 2 show a detailed view of the graphite production apparatus of the present invention, Figure 3 shows a detailed view of the colloidal graphite production apparatus of the present invention, the cover 10, the wall 20, the container box 30, the floor 40 ), See-through port 50, supporter 70, electrode rod 80, distilled water supply tank 101, sulfuric acid supply tank 102, nitric acid supply tank 103, calcium nitrate supply tank 104, graphite supply tank (105), reactor temperature control jacket 110, nitrogen dioxide discharge pipe 150, high pressure pump 155, jet nozzle 151, caustic soda supply tank 160, caustic dinitrogen oxide absorption tank 170, carbon filtration tank (180). Ammonia supply tank 190, distilled water supply pipe (195), reactor temperature control jacket (250), compressor (310), hot water boiler (410), heating jacket (450), cooling pump (510), cooling jacket (550) ), Wastewater collection tank 710, vacuum tank 720, vacuum pump 740, colloidal graphite outlet 800, screen and paper filter (850), reactor (A), aging machine (B), aeration tank (C ), Heater (D), cooler (E), neutralization tank (F), and vacuum dehydrator (G).

Looking at the structure, the colloidal nano graphite manufacturing apparatus is composed of a graphite manufacturing apparatus and a colloidal graphite manufacturing apparatus,

Graphite manufacturing apparatus is shown in Figure 1 to 2,

A cover 10 formed on the upper portion, a bottom 40 installed as a refractory brick, four walls 20 installed as a refractory brick so that a working space is formed inside the floor 40, and the wall. The cover 10 is installed as a refractory brick on the upper portion of the upper portion 20, the cover 10 is provided to be opened up and down, the container box 30 is installed in the inner working space to produce pure graphite, and the wall 20 Is connected to one side of the container box 30 and the through-hole 50 is installed through the outside,

It is a structure of the graphite manufacturing apparatus composed of the electrode rod 80 provided on the other side of the wall 20 and both ends of the container box 30.

Colloidal graphite manufacturing apparatus as shown in Figure 3,

Raw materials are sequentially pumped to the reactor (A), ripening (B), aeration tank (C), heater (D), cooler (E), vacuum dehydrator (G), neutralization tank (F), and vacuum dehydrator (G). A device for producing colloidal graphite while being circulated by

Distilled water supply tank 101, sulfuric acid supply tank 102, nitric acid supply tank 103, nitrogen nitrate supply tank which are respectively installed in the reactor (A) and the upper portion of the reactor (A) to inject each raw material into an automatic feeder. 104, composed of a graphite supply tank 105,

Reactor temperature control jacket 110 installed outside the reactor (A), a stirring motor provided on one side of the outside of the reactor (A), a stirrer connected to the stirring motor and installed inside the reactor (A), the reactor ( The lower side of A) is connected to a plurality of ripening machine (B) and aeration tank (C) by the discharge pipe,

The nitrogen dioxide discharge pipe 150 is connected to one side of the reactor (A) to discharge the nitrogen dioxide gas generated in the reactor (A), the jet nozzle 151 installed at the end of the nitrogen dioxide discharge pipe 150, and the nitrogen dioxide discharge pipe Jet nozzle 151 is provided at the end of the 150 is connected to the nitrogen dioxide absorption tank 170, the high pressure pump 155 installed on one side of the nitrogen dioxide absorption tank 170, and the nitrogen dioxide absorption tank 170 It is composed of a caustic soda tank 160 connected, and a carbon filter 180 connected to the nitrogen dioxide absorption tank 170,

The aging machine (B) is composed of 12, connected by the discharge pipe of the reactor (A), the stirring motor is installed on the upper outside, the stirrer connected to the stirring motor and installed inside the stirrer, and the compressor It is connected to the aeration tank (C) receiving oxygen from the leasher 310 is connected with the valve to the pipe to receive oxygen,

The upper part of each ripening machine (B) is connected to the nitrogen dioxide absorption tank 170 by a discharge pipe for discharging the generated nitrogen dioxide, the lower portion is composed of discharge pipe,

Three heaters (D) are installed and connected to pipes at 12 aging (B) and aeration tank (C) at the top, and installed outside, and receives the hot water from the boiler 410 to heat the heater (D). Jacket 450, the discharge pipe installed in the lower part,

It is composed of a stirring motor installed in the upper upper portion, a stirrer connected to the stirring motor and installed inside the heater,

The cooler (E) is connected to three heaters (D) by a pipe and a cooling jacket 550 connected to a cooling pump 510 installed outside to cool the introduced mixture to the pipe, and a discharge pipe installed below; It is composed of a stirring motor installed in the upper upper portion, a stirrer connected to the stirring motor and installed inside the cooler,

The vacuum dehydrator (G) is connected to the heater (D) and the cooler (E) and the pipe at the top, the inlet pipe connected to the neutralization tank (F) on one side, the screen and paper filter 850 installed on the middle one side ), A colloidal graphite outlet 800 installed at one side of the screen and paper filter 850, and a discharge pipe connected to the neutralization tank F and installed at the other side of the screen and paper filter 850,

And the waste water collection tank 710 installed below the screen and paper filter 850,

It is installed on one side of the wastewater collection tank 710 is composed of a vacuum tank 720 connected to the vacuum pump 740 to maintain a vacuum,

The neutralization tank (F) is connected to the discharge pipe of the vacuum dehydrator (G),

A stirring motor installed at an upper portion of the outer side, a stirrer connected to the stirring motor and penetrating the neutralization tank and installed therein;

Caustic soda supply pipe is installed on the upper side and connected to the caustic soda supply tank 160,

A caustic soda supply pipe which is installed under the gas feed soda supply pipe and supplied by an automatic feeder by an ammonia supply tank 190 for supplying ammonia,

It can be seen that the structure is connected to the distilled water supply pipe 195 for supplying distilled water, and the lower structure is composed of a discharge pipe connected to the neutralization tank (F).

Referring to the operating state of the device of the present invention.

The operation method of high purity graphite manufacturing apparatus is to prepare three container boxes with 500 ~ 1000㎛ particle of graphite mineral and 700mm length 350mm height 350mm of graphite material, and fill the same graphite mineral diameter 500 ~ 1000㎛ particle and keep airtight. next,

(See Figs. 1 and 2) The graphite minerals of Fig. 1 were placed in a container box (Fig. 2) and the cover was closed by stacking fire bricks 4700 mm wide by 1300 mm thick and 500 mm thick, and placed in a box having a floor thickness of 300 mm vertically. after,

100 ㎾ or more electricity is connected to both sides of the graphite electrode rod as shown in FIG. 1, and the temperature is heated to 2600 ~ 3200 ℃ by adding nitrogen as needed. Is maintained to prevent oxidation and the impurities in the graphite are incinerated, thus obtaining pure graphite having a purity of 99% or higher,

The baked particles are put into a grinder and continuously pulverized into graphite powder, and continuously passed through a sorting machine to sort and operate the graphite pulverized into fine particles of 0.1 ~ 3㎛ diameter.

The method of operating the colloidal manufacturing apparatus is

After the graphite pulverized into 0.1 ~ 3㎛ diameter particles produced in the graphite manufacturing apparatus as described above into the graphite supply tank 105, distilled water supply tank 101, sulfuric acid supply tank 102, nitric acid supply tank 103 , Respectively, is installed in the upper portion of the reactor (A) connected to the calcium nitrate supply tank (104), the graphite supply tank (105) to feed each raw material into the automatic feeder, the reactor temperature control jacket (110) installed outside the reactor (A) By adjusting the temperature, and mixing the raw materials introduced by the stirring motor installed on one side of the reactor (A) with the stirring motor connected to the stirring motor and installed inside the reactor (A),

The lower one side of the reactor (A) is transferred to 12 ripening machines (B) and aeration tank (C) by discharge pipes,

(Nitrogen dioxide gas generated in the mixing process in the reactor (A) is caustic soda connected to the jet nozzle 51 installed at the end of the nitrogen dioxide discharge pipe 150 through the nitrogen dioxide discharge pipe 150 by the operation of the high-pressure pump 155 Absorbed from the built-in nitrogen dioxide absorption tank 170, and treated with a carbon filter 180 connected to the nitrogen dioxide absorption tank 170, if necessary)

Each of the 12 ripening machines (B) is connected to the aeration tank (C) receiving oxygen from the compressor (310) to introduce a stirring motor installed in the outer upper portion and the stirring motor connected to the stirring motor in the same manner as the reactor. Then aerated with oxygen inside the ripening machine (B),

(At this time, the nitrogen dioxide generated during the aging process of each aging machine (B) is moved to absorb the nitrogen dioxide absorption tank 170 containing the caustic soda described above through the discharge pipe, and, if necessary, the nitrogen dioxide absorption tank ( 170) and the carbon filter connected to 180)

The heater D is transferred to three heaters D by a discharge pipe connected to the lower part, and the heater D is heated by a heating jacket 450 installed outside the heater D by receiving hot water from the boiler 410. At the same time as the stirring motor provided on the outer upper portion of the heater (D) and the mixture of the inside of the heater (D) by the stirring motor,

It is transferred to the cooler (E) to cool the mixture introduced by the cooling jacket 550 connected to the external cooling pump 510, and at the same time, the stirring motor is installed on the outer upper portion, connected to the stirring motor and passes through the cooler. After stirring with a stirrer installed inside,

Transfer to the vacuum dehydrator (G) by the discharge pipe, and then installed on one side of the waste water collection tank 710 installed below the screen and paper filter 850 and connected to the vacuum pump 740 to maintain a vacuum ( 720, the inside of the vacuum dehydrator (G) is maintained in a vacuum state, firstly filtered through the screen and paper filter 850 installed on one side of the middle and the filtrate is discharged through the waste water collection tank 710 of the lower, filtered mixture of

After the transfer to the neutralization tank (F), the caustic soda supply pipe connected to the caustic soda supply tank 160 installed on one side of the upper side, and installed in the lower portion of the condensed soda supply pipe by an ammonia supply tank 190 by an automatic feeder While caustic soda, ammonia and distilled water are automatically supplied to the ammonia supply pipe and the distilled water supply pipe 195,

 After the stirring motor is installed on the outer top, the stirring motor is connected to the stirring motor and stirred sufficiently by the stirrer installed inside,

Again, the vacuum tank 720 is transferred to the vacuum dehydrator (G) and then installed on one side of the wastewater collection tank 710 installed under the screen and paper filter 850 and connected to the vacuum pump 740 to maintain the vacuum. By maintaining the vacuum inside the vacuum dehydrator (G) in a vacuum state, the screen and the paper filter 850 installed on one side of the secondary filtration and the filtrate is discharged through the waste water collection tank 710 of the lower, secondary filtration The colloidal graphite is a method of operating the colloidal graphite nano-graphite device for discharging through the colloidal graphite outlet 800 installed on the upper side of the screen and paper filter 850.

In the above, each chemical and distilled water supply pipe is provided with an automatic feeder to supply a predetermined amount according to a preset instruction. Since the automatic feeder is a common technique widely used in the art, specific details will not be described.

1 and 2 detailed view of the graphite manufacturing apparatus of the present invention

Figure 3 is a detailed view of the clad graphite production apparatus of the present invention

Explanation of symbols in the drawings

Cover (10), wall (20), container box (30), bottom (40), sight hole (50), support (70), electrode (80), distilled water supply tank (101), sulfuric acid supply tank (102) , Nitric acid supply tank (103), nitrate supply tank (104), graphite supply tank (105), reactor temperature control jacket (110), nitrogen dioxide discharge pipe (150), high pressure pump (155), jet nozzle (151), caustic Soda supply tank 160, caustic dinitrogen oxide absorption tank 170, carbon filtration tank 180. Ammonia supply tank 190, distilled water supply pipe (195), reactor temperature control jacket (250), compressor (310), hot water boiler (410), heating jacket (450), cooling pump (510), cooling jacket (550) ), Wastewater collection tank 710, vacuum tank 720, vacuum pump 740, colloidal graphite outlet 800, screen and paper filter (850), reactor (A), aging machine (B), aeration tank (C ), Heater (D), cooler (E), neutralization tank (F), vacuum dehydrator (G)

Claims (12)

In the method for producing colloidal nanographite oxide, Obtaining high-purity graphite from ordinary graphite mineral by high-temperature firing at 2600 ~ 3200 ℃ in electric furnace: Grinding the high purity graphite obtained by the high temperature firing into 0.1-3 μm fine particles:  Reacting by adding 8 ~ 1L of distilled water 400g 1N nitrate 2.5kg, 7.5kg 1N sulfuric acid to 1kg of the grinding wire fine particles high-purity graphite 1N ammonium nitrate 5-10g added to the reactor: Stabilizing step characterized in that the mixed content of the contents aged in the aging period for 10 to 14 hours and put the air to remove nitrogen, aeration to stabilize the treatment: Heating and cooling step of heating and quenching 70 ~ 100 ℃, 2 to 4 hours to the mature content: The first step of dewatering by filtering the paper in the dehydrator after the heating, quenching: 6-10 L of distilled water was again added to the colloidal graphite in the paste form obtained by the first dehydration, and the same amount of 1N ammonia and 1N caustic soda was mixed. Then, the mixture was stirred until pH 2-3, and colloidal graphite was added. Neutralization step to neutralize: The method of producing a colloidal nano-graphite oxide, characterized in that the content of the pH 2-3 is filtered through a second dehydration step: using paper again in the dehydrator. The method of claim 1, wherein the obtaining of high purity graphite A method of producing colloidal nanographite oxides characterized in that calcination of ordinary graphite minerals in a high temperature electric furnace at 2600-3200 ° C. produces 99.98% or more of high purity graphite, and the step of pulverizing into fine particles is pulverized into fine particles having a diameter of 0.1 to 3 μm. . The method of claim 1, wherein the step of reacting colloidal nanoparticles, characterized in that 1 to 3 hours of mixed reaction for 1 hour to 3 hours to 1 kg of particulate graphite having a diameter of 0.1 ~ 3㎛ 400g nitric acid 2.5kg sulfuric acid 7.5kg distilled water 8-12L Method of producing graphite. According to claim 1, When the mixture is reacted in the reaction step by adding ammonia nitrate when the reaction is oxidized colloidal nano, characterized in that the reaction is promoted to increase the oxidation of the mixture even if the concentration of nitric acid is insufficient Method of producing graphite. The method of claim 1, wherein the nitrogen dioxide gas generated in the reacting step is removed using a high pressure pump to remove nitrogen dioxide gas. According to claim 5, Nitrogen dioxide gas produced in the reaction step using a high pressure pump, the nitrogen dioxide gas with a jet nozzle installed at the end of the nitrogen dioxide gas discharge pipe suction nitrogen injection with caustic soda into the nitrogen dioxide absorption tank to remove nitrogen dioxide Method for producing a colloidal nano graphite oxide, characterized in that. The method of claim 1, wherein the stabilizing step is a method of producing a colloidal nano-graphite oxide, characterized in that the contents of the mixed reaction aged in the aging period for 10 to 14 hours. The method of claim 1, wherein the stabilizing step is performed by agitation by adding air to discharge the generated nitrogen dioxide gas, and performing aeration. The method of claim 1, wherein the heating and cooling step of the colloidal nano-graphite oxide, characterized in that by stirring the air in the heater and the cooler, aeration, and then heated in a heater to 80 ~ 100 ℃ for 2 to 4 hours and then quenched Manufacturing method The method of claim 1, wherein the primary dewatering step is performed by filtering the paper installed on the upper portion of the primary screen in a vacuum dehydrator. The method of claim 1, wherein the neutralizing step is added to the colloidal graphite paste collected after the first dehydration to 6 ~ 10ℓ of distilled water and stirred to neutralize by stirring until the concentration is pH 2 ~ 3 with a mixture of caustic soda and ammonia. Method for producing a colloidal nano-graphite oxide characterized in that. The method of claim 1, wherein the secondary dehydration step is to filter the neutralized mixed solution with paper to secondary dehydration with a vacuum dehydrator.

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