CN118062846A - Carbonization treatment of alkylated waste acid and method for preparing activated carbon - Google Patents
Carbonization treatment of alkylated waste acid and method for preparing activated carbon Download PDFInfo
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- CN118062846A CN118062846A CN202410102751.8A CN202410102751A CN118062846A CN 118062846 A CN118062846 A CN 118062846A CN 202410102751 A CN202410102751 A CN 202410102751A CN 118062846 A CN118062846 A CN 118062846A
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- acid
- sulfuric acid
- waste acid
- dilute sulfuric
- activated carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000002253 acid Substances 0.000 title claims abstract description 67
- 239000002699 waste material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000003763 carbonization Methods 0.000 title claims abstract description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- 239000005539 carbonized material Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000010000 carbonizing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229960000892 attapulgite Drugs 0.000 claims abstract description 7
- 229920005610 lignin Polymers 0.000 claims abstract description 7
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002028 Biomass Substances 0.000 claims abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 240000008042 Zea mays Species 0.000 claims abstract description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 3
- 235000005822 corn Nutrition 0.000 claims abstract description 3
- 239000002023 wood Substances 0.000 claims abstract description 3
- 239000000428 dust Substances 0.000 claims abstract 2
- 239000010902 straw Substances 0.000 claims abstract 2
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 14
- 238000005086 pumping Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- 238000005804 alkylation reaction Methods 0.000 claims description 7
- 238000000108 ultra-filtration Methods 0.000 claims description 7
- 230000029936 alkylation Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 4
- 238000001728 nano-filtration Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 230000003213 activating effect Effects 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 2
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 2
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- -1 as an optimal mode Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004028 organic sulfates Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a method for carbonizing alkylated waste acid and preparing activated carbon, which comprises the following steps: cleaning, drying, crushing and sieving biomass material wood dust and corn straw mainly containing lignin, adding attapulgite, mixing, adding clear water, stirring uniformly, soaking, adding cross-linking agent polyvinyl alcohol cross-linking agent, mixing uniformly, drying to prepare a decoloring agent, adding the decoloring agent into waste acid, introducing the adsorbed material into an acid-resistant reaction kettle, carrying out dehydration and carbonization reaction on the waste acid, the decoloring agent and adsorbed organic matters thereof, washing the carbonized reactant, and centrifuging to obtain dilute sulfuric acid; and activating the carbonized material produced by the reaction to prepare the activated carbon.
Description
Technical Field
The invention relates to the technical field of waste acid recycling regeneration, in particular to a carbonization treatment alkylation waste acid and a method for preparing activated carbon.
Background
Sulfuric acid is consumed in the production process of the sulfuric acid method alkylation device, the alkylation reaction needs to maintain the acid concentration to be more than 88.5%, the waste acid is discharged from the acid settling tank of the reaction system to the waste acid tank after the acid concentration is low, and the waste sulfuric acid of the alkylation device generally comprises the following components: 88.5 to 90.0 percent of titratable acid, 3 to 5 percent of organic hydrocarbon, 1.5 to 2 percent of liquefied gas, 1.0 to 1.5 percent of water, 0.5 to 1.0 percent of organic sulfate, a small amount of sulfonic acid and the like; wherein the organic hydrocarbon is primarily an isooctane fraction, which is not effectively recovered and utilized, and the isooctane entrained in the spent acid is not constant as it exits the system with the spent acid plant.
During the storage of the spent acid, the above components in the spent acid continue to react and react more rapidly as the temperature increases to ambient temperature. Organic hydrocarbons and organic sulphates react in spent acid storage tanks to produce high carbon chain polymers, commonly known as acid soluble oils or "red oils", containing large amounts of conjugated diolefins, C5 rings and branched compounds thereof, which are difficult to handle due to corrosiveness and complex composition.
The carbonized material is biochar formed by taking lignin as a main body and a decoloring agent and organic matters in acid through sulfuric acid treatment, and can be used for preparing active carbon through activation treatment. The activated carbon is prepared by high-temperature treatment, and the sulfuric acid is used for pretreating biological materials, so that the generation of tar during pyrolysis of raw materials can be inhibited, and pores generated by pyrolysis of the tar are prevented from being blocked by the tar. And simultaneously, the formation of carbon-containing volatile matters is inhibited, so that the yield of the activated carbon is improved.
Therefore, a method for preparing activated carbon by using industrial waste acid is needed, which not only can obtain high-quality activated carbon, but also can effectively treat the industrial waste acid.
Disclosure of Invention
In order to solve the problems, the invention provides a method for carbonizing alkylated waste acid and preparing active carbon, which can solve the problems of sulfuric acid recovery and purification and can obtain high-quality active carbon.
The invention provides a method for carbonizing alkylated waste acid and preparing active carbon, which comprises the steps of preparing a decoloring agent, treating waste sulfuric acid, preparing active carbon and treating system tail gas.
(1) Preparing a decoloring agent and treating waste sulfuric acid:
S1, cleaning, drying, crushing and sieving biomass materials to obtain lignin through a sieve of 50 meshes, and adding attapulgite, wherein the volume ratio of the lignin to the attapulgite is 6-12: 1, adding clear water with the volume of 5-8 times, uniformly stirring, soaking for 24 hours, adding a cross-linking agent polyvinyl alcohol, performing ultrasonic dispersion for 30 minutes, and drying;
S2, adding a decoloring agent into the waste acid, wherein the mass ratio of the waste acid to the decoloring agent is 10: 2-4, stirring for 10-15 min at a speed of 60-75 r/min to realize complete adsorption of organic matters and obtain adsorbed materials;
S3, pumping the adsorbed material into an acid-resistant reaction kettle, controlling the temperature to be 160-180 ℃ and heating for 60-90 min, wherein waste acid and a decolorizing agent are subjected to carbonization reaction, and part of waste gas in the reaction process is separated by a collecting tower and then is merged into a waste gas system for continuous treatment;
S4, washing reactants subjected to carbonization reaction for 5-6 times, adding clear water with the proportion being 1.5-2 times that of the waste acid, centrifugally separating to obtain dilute sulfuric acid, and washing residual dissolved matters in the carbonized material after filtration for three stages to obtain carbonized material;
s5, pumping dilute sulfuric acid into the ultrafiltration membrane by using a pump to further remove solid suspended matters, feeding the dilute sulfuric acid from the bottom of the ultrafiltration membrane, discharging the dilute sulfuric acid from the upper part of the ultrafiltration membrane, and automatically flowing into an acid cleaning tank;
S6, pumping dilute sulfuric acid in the acid cleaning tank into a security filter by using a pump, and pumping the dilute sulfuric acid into an acid-resistant nanofiltration membrane treatment device by using a high-pressure pump;
(2) Preparing active carbon:
S7, under the inert atmosphere, controlling the activation temperature to be 800-850 ℃, introducing water vapor at the rate of 0.5-1 ml/min for activation, and keeping the temperature for 1-1.5 hours to obtain active carbon, and cooling and cleaning the active carbon to obtain the active carbon;
(3) And (3) treating tail gas of a system: s3, S8, generating sulfur-containing tail gas, separating the tail gas in a collecting tower, and then, introducing the tail gas into a sodium method sulfur dioxide waste gas treatment system to prepare sodium sulfite.
According to the carbonization treatment alkylation waste acid and the method for preparing the activated carbon, the volume ratio of lignin to attapulgite is 8-10 as a preferable mode: 1.
According to the carbonization treatment alkylation waste acid and the method for preparing the activated carbon, as an optimal mode, biomass materials are wood chips and corn stalks.
The invention provides a method for carbonizing alkylated waste acid and preparing active carbon, which can solve the problems of sulfuric acid recovery and purification and can obtain high-quality active carbon.
Drawings
FIG. 1 is a flow chart of the process for treating waste sulfuric acid in a process for carbonizing alkylated waste acid and preparing activated carbon according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1
As shown in FIG. 1, 500ml of waste acid was taken with a density of about 1.7, according to the mass of acid and decolorizing agent of 6: adding a decoloring agent in a ratio of 1, stirring at a rotation speed of 75r/min for 15min in a kneading reaction kettle, entering a carbonization reaction kettle, controlling the temperature to 180 ℃, performing carbonization reaction for 90min, adding clear water into the carbonized material for cleaning, wherein the cleaning frequency is three times, the total amount of the added clear water is not more than 2 times of the amount of waste acid, obtaining 30-50% dilute sulfuric acid 1L, introducing water vapor into the carbonized material under an inert atmosphere (filled with nitrogen for 0.5 ml/min), controlling the activation temperature to 800 ℃, activating at a rate of 0.5ml/min, and preserving heat for 80min to obtain the activated carbon. The iodine adsorption value and the methylene blue adsorption value of the activated carbon obtained after cooling and cleaning are 709.3mg/g and 98.6mg/g respectively.
Example 2
As shown in FIG. 1, 500ml of waste acid was taken with a density of about 1.7, according to an acid and decolorizing agent mass of 8: adding a decoloring agent in a ratio of 1, stirring at a rotation speed of 75r/min for 15min in a kneading reaction kettle, entering a carbonization reaction kettle, controlling the temperature to 180 ℃, performing carbonization reaction for 90min, adding clear water into the carbonized material for cleaning, wherein the cleaning frequency is three times, the total amount of the added clear water is not more than 2 times of the amount of waste acid, obtaining 30-50% dilute sulfuric acid 1L, introducing water vapor into the carbonized material under an inert atmosphere (filled with nitrogen for 0.5 ml/min), controlling the activation temperature to 800 ℃, activating at a rate of 0.5ml/min, and preserving heat for 80min to obtain the activated carbon. The iodine adsorption value and the methylene blue adsorption value of the activated carbon obtained after cooling and cleaning are 800.5mg/g and 130.4mg/g respectively.
Example 3
As shown in FIG. 1, 500ml of waste acid was taken with a density of about 1.7, according to the mass of acid and decolorizing agent of 6: adding a decoloring agent in a ratio of 1, stirring at a rotation speed of 75r/min for 15min in a kneading reaction kettle, entering a carbonization reaction kettle, controlling the temperature to 180 ℃, performing carbonization reaction for 90min, adding clear water into the carbonized material for cleaning, wherein the cleaning frequency is three times, the total amount of the added clear water is not more than 2 times of the amount of waste acid, obtaining 30-50% dilute sulfuric acid 1L, introducing water vapor into the carbonized material under an inert atmosphere (filled with nitrogen for 0.5 ml/min), controlling the activation temperature to 800 ℃, activating at a rate of 0.5ml/min, and preserving heat for 80min to obtain the activated carbon. The activated carbon obtained after cooling and cleaning has iodine adsorption value and methylene blue adsorption value of 814.7mg/g and 127.5mg/g respectively.
Example 4
As shown in FIG. 1, 500ml of waste acid was taken with a density of about 1.7, based on the mass 12 of acid and decolorizing agent: adding a decoloring agent in a ratio of 1, stirring at a rotation speed of 75r/min for 15min in a kneading reaction kettle, entering a carbonization reaction kettle, controlling the temperature to 180 ℃, performing carbonization reaction for 90min, adding clear water into the carbonized material for cleaning, wherein the cleaning frequency is three times, the total amount of the added clear water is not more than 2 times of the amount of waste acid, obtaining 30-50% dilute sulfuric acid 1L, introducing water vapor into the carbonized material under an inert atmosphere (filled with nitrogen for 0.5 ml/min), controlling the activation temperature to 800 ℃, activating at a rate of 0.5ml/min, and preserving heat for 80min to obtain the activated carbon. The iodine adsorption value and the methylene blue adsorption value of the activated carbon obtained after cooling and cleaning are 800.2mg/g and 110mg/g respectively.
The foregoing description is intended to be illustrative only and not limiting, and it will be understood by those skilled in the art that any modifications, changes or equivalents may be made without departing from the spirit and scope of the invention as defined in the following claims.
Claims (7)
1. A carbonization treatment alkylation waste acid and a method for preparing active carbon are characterized in that: the method comprises the following steps:
s1, preparing a decoloring agent: cleaning, drying, crushing and sieving biomass materials, adding attapulgite, adding clear water, uniformly stirring, soaking, adding cross-linking agent polyvinyl alcohol, performing ultrasonic dispersion, and drying to obtain a decoloring agent A;
S2, treating waste sulfuric acid: adding the decoloring agent A into waste acid, stirring and adsorbing to obtain an adsorbed material B, pumping the adsorbed material B into an acid-resistant reaction kettle, performing carbonization reaction to obtain a carbonized material D and tail gas C, separating the tail gas C by a collecting tower, washing the carbonized material D with water, adding clear water, performing centrifugal separation to obtain dilute sulfuric acid E, and washing the filtered carbonized material to obtain a carbonized material F; pumping the dilute sulfuric acid E into an ultrafiltration membrane by using a pump to obtain dilute sulfuric acid G; pumping the dilute sulfuric acid G into a cartridge filter by a pump, and pumping the dilute sulfuric acid G into an acid-resistant nanofiltration membrane treatment device by a high-pressure pump;
S3, preparing active carbon: under inert atmosphere, controlling the activation temperature to be 800-850 ℃, introducing water vapor at the rate of 0.5-1 ml/min for activation, and keeping the temperature for 1-1.5 h to obtain active carbon, and cooling and cleaning the active carbon to obtain the active carbon;
S4, treating system tail gas: and (3) separating the tail gas C in a collecting tower, and then, merging the tail gas C into a sodium method sulfur dioxide waste gas treatment system to prepare sodium sulfite.
2. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: the step S1 comprises the following steps:
s11, cleaning, drying, crushing and sieving biomass materials to 50 meshes;
s12, adding clear water with the volume of 5-8 times, uniformly stirring, and soaking for 24 hours;
s13, adding a cross-linking agent polyvinyl alcohol, performing ultrasonic dispersion for 30min, and drying to obtain the decoloring agent A.
3. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: the step S2 comprises the following steps:
S21, adding the decoloring agent A into waste acid, controlling the stirring time to be 60-75 r/min, and stirring for 10-15 min to obtain an adsorbed material B after the organic matters are completely adsorbed;
S22, pumping the adsorbed material B into an acid-resistant reaction kettle, controlling the temperature to be 160-180 ℃ and heating for 60-90 min, wherein the waste acid and the decolorizing agent A undergo carbonization reaction to obtain carbonized material D and tail gas C, and the tail gas C is separated by a collecting tower and then is combined into an exhaust gas system for continuous treatment;
S23, washing the carbonized material D for 5-6 times, adding clear water with the proportion being 1.5-2 times that of the waste acid, centrifugally separating to obtain dilute sulfuric acid E, and washing the residual dissolved matter in the carbonized material after filtration for three stages to obtain carbonized material F;
S24, pumping the dilute sulfuric acid E into an ultrafiltration membrane by using a pump to further remove solid suspended matters, wherein the dilute sulfuric acid E enters from the bottom of the ultrafiltration membrane, is discharged from the upper part of the ultrafiltration membrane and flows into an acid cleaning tank to obtain dilute sulfuric acid G;
S25, pumping the dilute sulfuric acid G in the acid cleaning tank into a security filter by using a pump, and pumping the dilute sulfuric acid G into an acid-resistant nanofiltration membrane treatment device by using a high-pressure pump.
4. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: in the step S1, the ratio of the lignin to the attapulgite is 6-12: 1.
5. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: in the step S1, the volume ratio of the lignin to the attapulgite is 8-10: 1.
6. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: in the step S1, the biomass material is wood dust and corn straw.
7. The method for carbonizing alkylated waste acid and preparing activated carbon according to claim 1, wherein the method comprises the following steps: in the S21, the mass ratio of the waste acid to the decoloring agent A is 10:2 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410102751.8A CN118062846A (en) | 2024-01-24 | 2024-01-24 | Carbonization treatment of alkylated waste acid and method for preparing activated carbon |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410102751.8A CN118062846A (en) | 2024-01-24 | 2024-01-24 | Carbonization treatment of alkylated waste acid and method for preparing activated carbon |
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