CN114477166B - Preparation process of expandable graphite - Google Patents
Preparation process of expandable graphite Download PDFInfo
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- CN114477166B CN114477166B CN202210003565.XA CN202210003565A CN114477166B CN 114477166 B CN114477166 B CN 114477166B CN 202210003565 A CN202210003565 A CN 202210003565A CN 114477166 B CN114477166 B CN 114477166B
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- acid
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 54
- 239000010439 graphite Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 84
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 40
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000011084 recovery Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 11
- 238000010790 dilution Methods 0.000 claims abstract description 10
- 239000012895 dilution Substances 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 239000003595 mist Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 238000007865 diluting Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 239000002912 waste gas Substances 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation process of expandable graphite, which relates to the technical field of graphite preparation and comprises the following steps: 1. quantitatively adding concentrated acid and flake graphite into a reaction kettle according to a certain proportion, soaking for 30min, adding hydrogen peroxide, and heating to 50 ℃ for reaction for 30min; 2. the reacted materials are subjected to filter pressing and deacidification, filtrate is recovered to a concentrated acid recovery tank, graphite after deacidification is transferred to a washing tank, washing, filter pressing and drying are carried out; 3. transferring the acid solution recovered in the step 2 to a dilution cooling tower, diluting, transferring dilute sulfuric acid and crystalline flake graphite to a reaction kettle according to a proportion, uniformly stirring, adding potassium permanganate, heating to 30-60 ℃, and reacting for 30-45 min; 4. adding water for dilution, adding hydrogen peroxide for reaction for 20-30 min, press filtering, washing, drying and recovering filtrate. The sulfuric acid recovery rate reaches 95%, the sulfuric acid is recycled, and the sulfur content in the product is low; the washing water is recycled, the water utilization rate is improved, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of graphite preparation, in particular to a preparation process of expandable graphite.
Background
The preparation method of the expandable graphite comprises a chemical intercalation method, an electrochemical method, an ultrasonic oxidation method, a gas-phase diffusion method, a molten salt method and the like, wherein the traditional process flow of the chemical intercalation method is as follows: under the condition of proper temperature, concentrated sulfuric acid, hydrogen peroxide and natural crystalline flake graphite are added in different procedures, reacted for a certain time under continuous stirring, and then washed, centrifuged, dehydrated and dried. In the preparation process, the consumption of washing water is large, the washing water can not be recovered, a large amount of sulfuric acid is wasted by washing water, and environmental pollution is caused.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation process of expandable graphite, which aims to solve the technical problems of large washing water consumption, waste of sulfuric acid by washing and environmental pollution in the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a process for preparing expandable graphite, comprising the steps of:
step 1), quantitatively adding concentrated acid and flake graphite into a reaction kettle according to a certain proportion, soaking for 30min, adding hydrogen peroxide, and heating to 50 ℃ for reaction for 30min;
step 2), carrying out plate-frame filter pressing deacidification on the reacted materials, recovering filtrate to a concentrated acid recovery tank, transferring graphite after deacidification to a washing tank, washing by adding water, carrying out plate-frame filter pressing, and drying;
step 3), transferring the acid solution recovered in the step 2 to a dilution cooling tower, adding water for dilution, quantitatively transferring dilute sulfuric acid and flake graphite to a reaction kettle according to a certain proportion, uniformly stirring, adding potassium permanganate, heating to 30-60 ℃, and reacting for 30-45 min;
and 4) adding water for dilution, adding hydrogen peroxide for reaction for 20-30 min, carrying out plate-frame filter pressing on the materials, washing and drying filter cakes, and recovering filtrate to a dilute acid recovery tank.
Preferably, the concentrated acid is 98% concentrated sulfuric acid, the mass ratio of the concentrated sulfuric acid to the crystalline flake graphite is 2.5:1, and the addition amount of the hydrogen peroxide in the step 1 is 12-18% of the mass of the crystalline flake graphite.
Preferably, the washing process comprises 7 times of washing, wherein the first 3 times of washing are performed by adopting filter pressing recycled water, the second 4 times of washing are performed by adopting clear water, and the clear water is added into ammonia water for soaking for 3 hours after 1 time of washing, and then subsequent washing treatment is performed.
Preferably, the concentration of the dilute sulfuric acid is 76%, the mass ratio of the dilute sulfuric acid to the crystalline flake graphite is 1.6:1, and the addition amount of the potassium permanganate is 10-15% of the mass of the crystalline flake graphite.
Preferably, the adding amount of the hydrogen peroxide in the step 4 is 5-10% of the mass of the crystalline flake graphite.
Preferably, the drying mode is steam drying, and the steam temperature is less than 120 ℃.
Preferably, the acid mist generated in the reaction process is discharged after being treated by a No. 1 alkaline washing tower, and the acid mist generated in the drying process is discharged after being treated by a No. 2 alkaline washing tower.
Preferably, the blower power of the No. 1 alkaline washing tower and the No. 2 alkaline washing tower is 5.5kW, and the air quantity is 9660-4830m 3 /h。
After the technical scheme is adopted, the invention has the beneficial effects that:
1) According to the invention, the product is dried by adopting steam heating, so that part of sulfur remained on the graphite can be removed, and the sulfur content in the graphite is reduced;
2) The sulfuric acid recovery rate reaches 95%, so that the high-efficiency recovery and utilization of sulfuric acid are realized;
3) The invention recycles the washing water, improves the utilization rate of the water and reduces the cost;
4) According to the invention, the stirring state is adopted in the washing process, the temperature is raised for washing, and ammonia water is added for soaking during washing, so that the sulfur content in the graphite layer can be effectively reduced;
5) The invention adopts the alkaline washing tower to carry out alkaline washing treatment on the acid mist in the production process and then rapidly discharges the acid mist, thereby avoiding the phenomenon of sulfur recovery.
In summary, the invention solves the technical problems of large consumption of washing water, irrecoverable washing water, waste of sulfuric acid caused by washing water and environmental pollution in the prior art.
Drawings
FIG. 1 is a flow chart of a process for preparing expandable graphite according to the present invention.
Detailed Description
The following is a detailed description of a process for preparing expandable graphite according to the present invention, but should not be construed as limiting the scope of the invention. In the present invention, all the preparation materials are commercially available products well known to those skilled in the art unless specified otherwise.
Example 1
Adding 400Kg of graphite raw material and 1000Kg of concentrated sulfuric acid with the concentration of 98 percent into a reaction kettle, uniformly stirring, adding 60Kg of hydrogen peroxide, heating to 50 ℃ for reaction for 30min, and discharging acid mist generated in the reaction process after entering a No. 1 alkaline washing tower for treatment; the reacted material is put into an acid-resistant storage tank, and is sent into a plate-and-frame filter press by high-pressure air (the pressure is generally 0.4 MPa) to deacidify, and the acid is recovered into a concentrated acid recovery tank for the potassium permanganate method.
Putting deacidified graphite into a washing tank, washing with about 500Kg of water and ammonia water according to the dry material folded in each tank, and washing for 7 times, wherein the last three times use filter pressing to recycle water, and the water consumption is about 5m 3 The clean water is used for the last four times, and the water consumption is about 6m 3 The method comprises the steps of carrying out a first treatment on the surface of the Waste water from the first four washes is about 6m 3 Discharging into a sewage treatment station, wherein the treated water is used for producing high-carbon high-purity graphite; the washing water of the last three times is about 5m 3 Recycling, wherein after four times of washing, 25Kg of ammonia water is added into a washing tank, soaking is carried out for about 3 hours, and then subsequent washing is carried out; the washed material is sent into a plate-and-frame filter press for dehydration, and the filtrate is recycled (2 m of material can be recycled per ton) 3 ) Drying the dehydrated material by steam, and controlling the pressure of the dried material by steamThe temperature of the final material is not more than 120 ℃ when the temperature is below 0.3 MPa; the steam consumption of each ton of the product is about 500Kg, and the steam condensate is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust drum; and (5) screening the dried materials, mixing, packaging and warehousing according to the quality index requirements.
And taking the concentrated sulfuric acid recovered by the hydrogen peroxide method as a raw material, and adopting a potassium permanganate method to continuously participate in preparing the expandable graphite. The recovered concentrated sulfuric acid is sent to a dilution cooling tower, is diluted to about 76% by tap water, and is cooled to normal temperature; adding 400Kg of graphite raw material and 6400Kg of concentrated sulfuric acid with the concentration of 76% into a reaction kettle, uniformly stirring, adding 50Kg of potassium permanganate, heating to 50 ℃, reacting for 30min, adding 200Kg of tap water and 30Kg of hydrogen peroxide, reacting for about 20min, and discharging acid mist generated in the reaction process after entering a No. 1 alkaline washing tower for treatment through an exhaust funnel; the reacted material is conveyed to a plate-and-frame filter press through a pipeline, so that dilute sulfuric acid (the concentration is about 60%) is separated from the material, the separated dilute sulfuric acid enters a dilute acid recovery tank, and graphite is conveyed to a washing tank for washing.
Putting deacidified graphite into a washing tank, washing about 500Kg of dry material in each tank with water and ammonia water for 7 times, wherein the last three times use filter pressing to recycle water, and the water consumption is about 5m 3 The clean water is used for the last four times, and the water consumption is about 6m 3 The method comprises the steps of carrying out a first treatment on the surface of the Waste water from the first four washes is about 6m 3 Discharging the waste water into a sewage treatment station, wherein the treated reclaimed water is used for producing high-carbon high-purity graphite; the washing water of the last three times is about 5m 3 Recycling, wherein 25Kg of ammonia water is added into a washing tank after four times of washing, soaking is carried out for about 3 hours, and then subsequent washing is carried out; drying the dehydrated material by steam; the steam pressure for drying is controlled below 0.3MPa, and the temperature of the final material is not more than 120 ℃; the steam consumption of each ton of the product is about 500Kg, and the steam condensate is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust drum; and (5) screening the dried materials, mixing, packaging and warehousing according to the quality index requirements.
According to the method provided by the invention, the recovery rate of the concentrated sulfuric acid is 95%, and the concentration of the sulfuric acid in the concentrated acid recovery tank is 93%.
Example 2
Adding 400Kg of graphite raw material and 1000Kg of concentrated sulfuric acid with the concentration of 98 percent into a reaction kettle, uniformly stirring, adding 72Kg of hydrogen peroxide, heating to 50 ℃ for reaction for 30min, and discharging acid mist generated in the reaction process after entering a No. 1 alkaline washing tower for treatment through an exhaust funnel; the reacted material is put into an acid-resistant storage tank, and is sent into a plate-and-frame filter press by high-pressure air (the pressure is generally 0.4 MPa) to deacidify, and the acid is recovered into a concentrated acid recovery tank for the potassium permanganate method.
Putting deacidified graphite into a washing tank, washing about 500Kg of dry material in each tank with water and ammonia water for 7 times, wherein the last three times use filter pressing to recycle water, and the water consumption is about 5m 3 The clean water is used for the last four times, and the water consumption is about 6m 3 The method comprises the steps of carrying out a first treatment on the surface of the Waste water from the first four washes is about 6m 3 Discharging into a sewage treatment station, wherein the treated water is used for producing high-carbon high-purity graphite; the washing water of the last three times is about 5m 3 Recycling, wherein after four times of washing, 25Kg of ammonia water is added into a washing tank, soaking is carried out for about 3 hours, then subsequent washing is carried out, the washed material is sent into a plate-and-frame filter press for dehydration, and filtrate is recycled (ton of material can be recycled for 2 m) 3 ) And (3) drying the dehydrated material by steam, wherein the pressure of the steam for drying is controlled below 0.3MPa, and the temperature of the final material is not more than 120 ℃. The steam consumption of each ton of the product is about 500Kg, and the steam condensate is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust drum; and (5) screening the dried materials, mixing, packaging and warehousing according to the quality index requirements.
And taking the concentrated sulfuric acid recovered by the hydrogen peroxide method as a raw material, and adopting a potassium permanganate method to continuously participate in preparing the expandable graphite. The recovered concentrated sulfuric acid is sent to a dilution cooling tower, is diluted to about 76% by tap water, and is cooled to normal temperature; adding 400Kg of graphite raw material and 6400Kg of concentrated sulfuric acid with the concentration of 76% into a reaction kettle, uniformly stirring, adding 60Kg of potassium permanganate, heating to 50 ℃, reacting for 30min, adding 200Kg of tap water and 40Kg of hydrogen peroxide, reacting for about 20min, and discharging acid mist generated in the reaction process after entering a No. 2 alkaline washing tower for treatment through an exhaust funnel; the reacted material is conveyed to a plate-and-frame filter press through a pipeline, so that dilute sulfuric acid (the concentration is about 60%) is separated from the material, the separated dilute sulfuric acid enters a dilute acid recovery tank, and graphite is conveyed to a washing tank for washing.
Putting deacidified graphite into a washing tank, washing about 500Kg of dry material in each tank with water and ammonia water for 7 times, wherein the last three times use filter pressing to recycle water, and the water consumption is about 5m 3 The clean water is used for the last four times, and the water consumption is about 6m 3 The method comprises the steps of carrying out a first treatment on the surface of the Waste water from the first four washes is about 6m 3 Discharging the waste water into a sewage treatment station, wherein the treated reclaimed water is used for producing high-carbon high-purity graphite; the washing water of the last three times is about 5m 3 Recycling, wherein 25Kg of ammonia water is added into a washing tank after four times of washing, soaking is carried out for about 3 hours, and then subsequent washing is carried out; drying the dehydrated material by steam, wherein the pressure of the dried material by the steam is controlled below 0.3MPa, and the temperature of the final material is not more than 120 ℃; the steam consumption of each ton of the product is about 500Kg, and the steam condensate is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust drum; and (5) screening the dried materials, mixing, packaging and warehousing according to the quality index requirements.
The method provided by the invention has the advantages that the recovery rate of the concentrated sulfuric acid is more than 95%, and the concentration of the sulfuric acid in the concentrated acid recovery tank is 94%.
Claims (4)
1. A process for preparing expandable graphite, comprising the steps of:
step 1), quantitatively adding concentrated acid and flake graphite into a reaction kettle according to a certain proportion, uniformly stirring, soaking for 30min, adding hydrogen peroxide, and heating to 50 ℃ for reaction for 30min;
step 2), carrying out filter pressing deacidification on the reacted materials, and recovering filtrate to a concentrated acid recovery tank; transferring the deacidified graphite to a washing tank, adding water, heating to 50 ℃, washing, press-filtering and drying;
step 3), transferring the acid solution recovered in the step 2 to a dilution cooling tower, adding water for dilution, quantitatively transferring dilute sulfuric acid and flake graphite to a reaction kettle according to a certain proportion, uniformly stirring, adding potassium permanganate, heating to 30-60 ℃, and reacting for 30-45 min;
step 4), adding water for dilution, adding hydrogen peroxide for reaction for 20-30 min, carrying out filter pressing on materials, washing and drying filter cakes, and recycling filtrate to a dilute acid recycling tank;
in the step 2, the washing process comprises 7 times of washing, wherein the first 3 times of washing are carried out by adopting filter pressing reclaimed water, and the last 4 times of washing are carried out by adopting clear water; washing with clear water for 1 time, adding ammonia water, soaking for 3 hours, and then carrying out subsequent washing treatment; the washing water of the last 3 times is recycled;
in the step 4, the reacted materials are conveyed to a plate-and-frame filter press through a pipeline, so that dilute sulfuric acid is separated from the materials, the separated dilute sulfuric acid enters a dilute acid recovery tank, and graphite is conveyed to a washing tank for washing;
in the step 1, the concentrated acid is 98% concentrated sulfuric acid, the mass ratio of the concentrated sulfuric acid to the crystalline flake graphite is 2.5:1, and the addition amount of the hydrogen peroxide is 12-18% of the crystalline flake graphite;
in the step 4, the addition amount of the hydrogen peroxide is 5-10% of the mass of the crystalline flake graphite;
acid mist generated in the reaction process is treated by a No. 1 alkaline washing tower and then discharged; acid mist generated in the drying process is treated by a No. 2 alkaline washing tower and then discharged.
2. The process for preparing expandable graphite according to claim 1, wherein in the step 3, the concentration of the dilute sulfuric acid is 76%, the mass ratio of the dilute sulfuric acid to the crystalline flake graphite is 1.6:1, and the addition amount of the potassium permanganate is 10-15% of the mass of the crystalline flake graphite.
3. The process of claim 1, wherein the drying is steam drying, and the steam temperature is less than 120 ℃.
4. The process for preparing expandable graphite according to claim 1, wherein the blower power of the No. 1 alkaline washing tower and the No. 2 alkaline washing tower is 5.5kW, and the air quantity is 9660-4830m 3 /h。
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| CN105502360A (en) * | 2015-12-25 | 2016-04-20 | 燕山大学 | Preparation method of sulfur-free expansible graphite |
| CN106564895A (en) * | 2016-11-14 | 2017-04-19 | 滨州英特石化配件有限公司 | Preparation technology and system of expandable graphite |
| CN108862271A (en) * | 2018-09-28 | 2018-11-23 | 辽宁大学 | A kind of expansible graphite preparation method of proportion optimizing intercalator |
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| JP2021501111A (en) * | 2017-10-31 | 2021-01-14 | 日東電工株式会社 | Method for chemically exfoliating graphite |
| CN113735111A (en) * | 2021-10-08 | 2021-12-03 | 黑龙江哈工石墨科技有限公司 | Preparation process method of low-sulfur expandable graphite |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA72692C2 (en) * | 2003-07-25 | 2007-06-25 | Ener 1 Subsidiary Entpr With F | Process for preparation of carbon material for electrodes of lithium-ion current sources |
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2022
- 2022-01-05 CN CN202210003565.XA patent/CN114477166B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN103145119A (en) * | 2013-03-14 | 2013-06-12 | 内蒙古瑞盛新能源有限公司 | Preparation method of expandable graphite |
| CN105502360A (en) * | 2015-12-25 | 2016-04-20 | 燕山大学 | Preparation method of sulfur-free expansible graphite |
| CN106564895A (en) * | 2016-11-14 | 2017-04-19 | 滨州英特石化配件有限公司 | Preparation technology and system of expandable graphite |
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| JP2021501111A (en) * | 2017-10-31 | 2021-01-14 | 日東電工株式会社 | Method for chemically exfoliating graphite |
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| CN113735111A (en) * | 2021-10-08 | 2021-12-03 | 黑龙江哈工石墨科技有限公司 | Preparation process method of low-sulfur expandable graphite |
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