CN114477166A - Preparation process of expandable graphite - Google Patents
Preparation process of expandable graphite Download PDFInfo
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- CN114477166A CN114477166A CN202210003565.XA CN202210003565A CN114477166A CN 114477166 A CN114477166 A CN 114477166A CN 202210003565 A CN202210003565 A CN 202210003565A CN 114477166 A CN114477166 A CN 114477166A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 57
- 239000010439 graphite Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 75
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 38
- 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 30
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000011084 recovery Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 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
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 15
- 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 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 6
- 239000003518 caustics Substances 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 239000000047 product Substances 0.000 abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 abstract description 4
- 239000011593 sulfur Substances 0.000 abstract description 4
- 238000007865 diluting Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000007599 discharging Methods 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
- 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
- 238000012216 screening 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- 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 crystalline flake graphite into a reaction kettle according to a certain proportion, soaking for 30min, adding hydrogen peroxide, heating to 50 ℃ and reacting for 30 min; 2. performing filter pressing deacidification on the reacted materials, recovering the filtrate to a concentrated acid recovery tank, transferring the deacidified graphite to a washing tank, washing, performing filter pressing and drying; 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 ratio, 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, performing filter pressing, washing, drying, and recovering filtrate. The recovery rate of the sulfuric acid reaches 95%, the sulfuric acid is recycled, and the sulfur content in the product is low; the washing water is recycled, the utilization rate of the water 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 comprises the following steps: under the condition of proper temperature, concentrated sulfuric acid, hydrogen peroxide and natural crystalline flake graphite are added into the reactor by different procedures, and the reactor is continuously stirred to react for a certain time, and then is washed by water, centrifuged, dehydrated and dried. In the preparation process, the washing water consumption is large, the sulfuric acid cannot be recycled, and a large amount of sulfuric acid is wasted by washing, so that the environmental pollution is caused.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation process of expandable graphite, aiming at solving 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 preparation process of expandable graphite comprises the following steps:
step 1), quantitatively adding concentrated acid and crystalline flake graphite into a reaction kettle according to a certain proportion, soaking for 30min, adding hydrogen peroxide, heating to 50 ℃ and reacting for 30 min;
step 2), performing plate-and-frame filter pressing deacidification on the reacted materials, recovering the filtrate to a concentrated acid recovery tank, transferring the deacidified graphite to a washing tank, adding water for washing, performing plate-and-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 crystalline 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 step 4), adding water for dilution, adding hydrogen peroxide for reaction for 20-30 min, performing plate-and-frame filter pressing on the materials, washing and drying filter cakes, and recovering the 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 adding amount of hydrogen peroxide in the step 1 is 12-18% of the crystalline flake graphite.
Preferably, the washing process comprises 7 times of washing, wherein the first 3 times of washing is carried out by adopting filter pressing recovered water, the last 4 times of washing is carried out by adopting clear water, the clear water is used for washing for 1 time, then ammonia water is added for soaking for 3 hours, and then the subsequent washing treatment is carried out.
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 crystalline flake graphite.
Preferably, the adding amount of 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, acid mist generated in the reaction process is discharged after being treated by a No. 1 alkali washing tower, and acid mist generated in the drying process is discharged after being treated by a No. 2 alkali washing tower.
Preferably, the fan power of the caustic tower No. 1 and the fan power of the caustic tower No. 2 are 5.5kW, and the air volume is 9660-4830m3/h。
After the technical scheme is adopted, the invention has the beneficial effects that:
1) the product is dried by heating with steam, so that part of sulfur remaining on the graphite can be removed, and the content of sulfur in the graphite is reduced;
2) the recovery rate of the sulfuric acid reaches 95 percent, and the efficient recovery and utilization of the sulfuric acid are realized;
3) the invention recycles the washing water, improves the utilization rate of the water and reduces the cost;
4) the invention adopts the heating washing under the stirring state to the washing process, and the ammonia water is added for soaking during the washing process, so that the content of sulfur in the graphite layer can be effectively reduced;
5) the acid mist in the production process is quickly discharged after being subjected to alkali washing treatment by the alkali washing tower, so that the resulfurization phenomenon can be avoided.
In conclusion, the invention solves the technical problems of large washing water consumption, non-recoverability, waste of sulfuric acid washing 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 process for preparing an expandable graphite according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention. In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art, unless otherwise specified.
Example 1
Adding 400Kg of graphite raw material and 1000Kg of concentrated sulfuric acid with the concentration of 98% 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 the acid mist enters a No. 1 alkaline tower for treatment through an exhaust funnel; the reacted materials are put into an acid-proof material storage tank, sent into a plate-and-frame filter press by high-pressure air (the pressure is generally 0.4 MPa), deacidified, and recovered into a concentrated acid recovery tank for a potassium permanganate method.
Placing deacidified graphite into washing tank, and folding according to each tankWashing the dried material with about 500Kg of water and ammonia water for 7 times, wherein the first three times are carried out by pressure filtration to recover water with the water consumption of about 5m3Then using clean water for four times, the water consumption is about 6m3(ii) a The waste water of the first four times of washing is about 6m3The waste water is discharged into a sewage treatment station, and the treated water is used for producing high-carbon high-purity graphite; the last three times of washing water is about 5m3Recycling, wherein after washing for four times, 25Kg of ammonia water is added into a washing tank, and the washing tank is soaked for about 3 hours and then subjected to subsequent washing; the washed materials are sent to a plate-and-frame filter press for dehydration, and filtrate is recycled (2 m can be recycled for each ton of materials)3) Steam drying the dehydrated material, wherein 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 product is about 500Kg, and the steam condensate water is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust funnel; and screening and deslagging the dried material, mixing the material according to the quality index requirement, packaging and warehousing.
Concentrated sulfuric acid recovered by a hydrogen peroxide method is used as a raw material, and a potassium permanganate method is adopted to continuously participate in the preparation of the expandable graphite. Sending the recovered concentrated sulfuric acid to a dilution cooling tower, adding tap water to dilute the concentrated sulfuric acid to a concentration of about 76%, and cooling the concentrated sulfuric acid to the 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, then 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 tower for treatment through an exhaust funnel; the reacted materials are conveyed to a plate-and-frame filter press through a pipeline, dilute sulfuric acid (the concentration is about 60%) 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.
The deacidified graphite is put into washing tanks, each tank is washed by water and ammonia water about 500Kg after dried, and the washing is carried out for 7 times, wherein the first three times are carried out for recovering water by filter pressing, and the water consumption is about 5m3Then using clean water for four times, the water consumption is about 6m3(ii) a The waste water of the first four times of washing is about 6m3The waste water is discharged into a sewage treatment station, and the treated reclaimed water is used for producing high-carbon high-purity graphite; the last three times of washing water is about 5m3Recycling, wherein after washing for four times, 25Kg of ammonia water is added into a washing tank, and the washing tank is soaked for about 3 hours and then is subjected to subsequent washing; steam drying the dehydrated material; steam pressure for drying is controlled to be below 0.3MPa, and the temperature of the final material is not more than 120 ℃; the steam consumption of each ton of product is about 500Kg, and the steam condensate water is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust funnel; and screening and deslagging the dried material, mixing the material according to the quality index requirement, packaging and warehousing.
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% 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 the acid mist enters a No. 1 alkaline tower for treatment through an exhaust funnel; the reacted materials are put into an acid-proof material storage tank, sent into a plate-and-frame filter press by high-pressure air (the pressure is generally 0.4 MPa), deacidified, and recovered into a concentrated acid recovery tank for a potassium permanganate method.
The deacidified graphite is put into washing tanks, each tank is washed by water and ammonia water about 500Kg after dried, and the washing is carried out for 7 times, wherein the first three times are carried out for recovering water by filter pressing, and the water consumption is about 5m3Then using clean water for four times, the water consumption is about 6m3(ii) a The waste water of the first four times of washing is about 6m3The waste water is discharged into a sewage treatment station, and the treated water is used for producing high-carbon high-purity graphite; the last three times of washing water is about 5m3Recycling, adding 25Kg of ammonia water into a washing tank after washing for four times, soaking for about 3 hours, then carrying out subsequent washing, feeding the washed materials into a plate-and-frame filter press for dehydration, and recycling filtrate (one ton of materials can be recycled by 2 m)3) And (3) drying the dehydrated material by steam, wherein 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 product is about 500Kg, and the steam condensate water is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust funnel; sieving and deslagging the dried material, and classifying according to qualityAnd (5) mixing materials, packaging and warehousing according to the requirement of the quantity index.
Concentrated sulfuric acid recovered by a hydrogen peroxide method is used as a raw material, and a potassium permanganate method is adopted to continuously participate in the preparation of the expandable graphite. Sending the recovered concentrated sulfuric acid to a dilution cooling tower, adding tap water to dilute the concentrated sulfuric acid to a concentration of about 76%, and cooling the concentrated sulfuric acid to the 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, then 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 tower for treatment through an exhaust funnel; the reacted materials are conveyed to a plate-and-frame filter press through a pipeline, dilute sulfuric acid (the concentration is about 60%) 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.
The deacidified graphite is put into washing tanks, each tank is washed by water and ammonia water about 500Kg after dried, and the washing is carried out for 7 times, wherein the first three times are carried out for recovering water by filter pressing, and the water consumption is about 5m3Then using clean water for four times, the water consumption is about 6m3(ii) a The waste water of the first four times of washing is about 6m3The waste water is discharged into a sewage treatment station, and the treated reclaimed water is used for producing high-carbon high-purity graphite; the last three times of washing water is about 5m3Recycling, wherein after washing for four times, 25Kg of ammonia water is added into a washing tank, and the washing tank is soaked for about 3 hours and then is subjected to subsequent washing; steam drying the dehydrated material, wherein the steam pressure for drying is controlled below 0.3MPa, and the final material temperature is not more than 120 ℃; the steam consumption of each ton of product is about 500Kg, and the steam condensate water is recycled; waste gas generated by drying materials enters a No. 2 alkaline washing tower for treatment and is discharged through an exhaust funnel; and screening and deslagging the dried material, mixing the material according to the quality index requirement, packaging and warehousing.
The method provided by the invention has the advantages that the recovery rate of concentrated sulfuric acid is more than 95%, and the concentration of sulfuric acid in the concentrated acid recovery tank is 94%.
Claims (8)
1. A preparation process of expandable graphite is characterized by comprising the following steps:
step 1), quantitatively adding concentrated acid and crystalline flake graphite into a reaction kettle according to a certain proportion, uniformly stirring, soaking for 30min, adding hydrogen peroxide, heating to 50 ℃ and reacting for 30 min;
step 2), performing filter pressing deacidification on the reacted materials, and recovering the filtrate to a concentrated acid recovery tank; transferring the deacidified graphite to a washing tank, adding water, heating to 50 ℃, washing, 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 crystalline 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 step 4), adding water for dilution, adding hydrogen peroxide for reaction for 20-30 min, performing filter pressing on the materials, washing and drying filter cakes, and recovering the filtrate to a dilute acid recovery tank.
2. The process for preparing expandable graphite according to claim 1, wherein in 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 hydrogen peroxide is 12-18% of the crystalline flake graphite.
3. The process for preparing expandable graphite according to claim 1, wherein in step 2, the washing process comprises 7 times of washing, the first 3 times of washing with filter-pressing recovered water, and the last 4 times of washing with clear water; and washing the mixture for 1 time by using clean water, adding ammonia water to soak the mixture for 3 hours, and then carrying out subsequent washing treatment.
4. The process for preparing expandable graphite according to claim 1, wherein in 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 crystalline flake graphite.
5. The process for preparing expandable graphite according to claim 1, wherein in the step 4, the amount of hydrogen peroxide added is 5-10% of the mass of the crystalline flake graphite.
6. The process of claim 1, wherein the drying is steam drying, and the steam temperature is less than 120 ℃.
7. The process for preparing expandable graphite according to claim 1, wherein the acid mist generated in the reaction process is discharged after being treated by a No. 1 caustic tower; and acid mist generated in the drying process is treated by a No. 2 alkaline washing tower and then is discharged.
8. The process for preparing expandable graphite as claimed in any one of claims 1 to 7, wherein the fans of the No. 1 alkali wash tower and the No. 2 alkali wash tower have 5.5kW power and 4830m air volume of 9660-3/h。
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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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2022
- 2022-01-05 CN CN202210003565.XA patent/CN114477166B/en active Active
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| US20050118506A1 (en) * | 2003-07-25 | 2005-06-02 | Yury Pustovalov | Carbon material for electrodes of lithium-ion power sources and method of production thereof |
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
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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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