CN112479247A - Method for preparing lead sulfide by using industrial desulfurization waste liquid - Google Patents
Method for preparing lead sulfide by using industrial desulfurization waste liquid Download PDFInfo
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- CN112479247A CN112479247A CN202011481453.2A CN202011481453A CN112479247A CN 112479247 A CN112479247 A CN 112479247A CN 202011481453 A CN202011481453 A CN 202011481453A CN 112479247 A CN112479247 A CN 112479247A
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- waste liquid
- lead sulfide
- lead
- desulfurization waste
- lead acetate
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- 239000007788 liquid Substances 0.000 title claims abstract description 60
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 44
- 230000023556 desulfurization Effects 0.000 title claims abstract description 44
- 229940056932 lead sulfide Drugs 0.000 title claims abstract description 44
- 229910052981 lead sulfide Inorganic materials 0.000 title claims abstract description 44
- 239000002699 waste material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 34
- 229940046892 lead acetate Drugs 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 17
- 239000003245 coal Substances 0.000 description 10
- 238000004939 coking Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229940083037 simethicone Drugs 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- -1 sulfide ions Chemical class 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a method for preparing lead sulfide by using industrial desulfurization waste liquid, which synthesizes a lead sulfide material by a wet chemical method. The industrial desulfurization waste liquid and lead acetate are used as raw materials, and lead sulfide is prepared through a series of processes of oil bath heating, stirring, filtering, drying and the like. The method can be used for preparing the lead sulfide functional material quickly and efficiently, shortens the synthesis time, enlarges the yield of the synthesized lead sulfide, has high efficiency, low energy consumption and high yield of the lead sulfide material, and does not cause pollution to the environment. The method solves the problems that the traditional process needs to prepare the lead sulfide material in a high-temperature and high-pressure environment, the quantity of reaction raw materials is limited, and the cooling time is long.
Description
Technical Field
The invention relates to a method for preparing a lead sulfide functional material by using industrial desulfurization waste liquid.
Background
Lead sulfide is an important semiconductor material, the research of nano materials has become a research hotspot worldwide in recent years, and the lead sulfide material is also deeply researched due to important application in many fields. For example, an infrared detector prepared by utilizing lead sulfide nanocrystals is an infrared detector which has high sensitivity in a near infrared region and can work at normal temperature only by refrigeration of a conductor refrigerator. Has unique effect in military affairs, civil economy and other aspects. Meanwhile, the lead sulfide powder can be used as raw materials in the aspects of luminescent materials, anti-counterfeiting materials, coating materials, electroluminescent powder, nonlinear optical materials, photoelectric conversion materials and the like, is generally used for developing photoelectric detector materials in the photoelectric field, and has the characteristics of quick response, capability of working at room temperature and the like.
In addition, the coal chemical industry in China is developed rapidly, the three wastes generated in the coal processing and production process are much higher than those of petroleum and natural gas, and the coal chemical industry causes serious pollution to the atmosphere and water body environment. The sulfur-containing waste gas is one of the main gas pollutants in the production process of coal chemical enterprises, and has great threat to the environment and the health of people. Therefore, the desulfurization process is adopted to reduce the influence of the gas pollutants on the environment. The desulfurization process commonly adopted by domestic and foreign coal chemical industry enterprises mainly comprises dry desulfurization and wet desulfurization, the wet desulfurization is a desulfurization process commonly adopted by domestic coal chemical industry enterprises, and a large amount of desulfurization waste liquid can be generated in the desulfurization process. The desulfurization waste liquid is obtained by absorbing H in coal gas by using ammonia as an alkali source for desulfurization in the coking process of a coking plant2S and other sulfides, and sulfur-containing liquid generated after sulfur removal. The treatment of the desulfurization waste liquid becomes a difficult problem to be solved urgently by the coal coking enterprises after long-term accumulation.
At present, under the requirement of national environmental protection policy, coal coke chemical enterprises must solve the problems of cyclic utilization of a large amount of desulfurization waste liquid, waste residue and waste water which are difficult to treat, and the like, so as to ensure that the desulfurization efficiency cannot be influenced and the continuous production is realized. Therefore, enterprises adopt various methods to treat the waste liquid so as to realize recycling, for example, the waste liquid is utilized to prepare byproducts such as sulfur and the like. Therefore, the invention improves the added value of the ammonia desulphurization byproduct on the premise of reducing the environmental pollution as much as possible, not only meets the requirement of the environmental protection policy, but also brings great economic benefit to the coking enterprises.
Disclosure of Invention
The invention aims to provide a method for preparing lead sulfide by using industrial desulfurization waste liquid, which synthesizes a lead sulfide material by a wet chemical method. The industrial desulfurization waste liquid and lead acetate are used as raw materials, and lead sulfide is prepared through a series of processes of oil bath heating, stirring, filtering, drying and the like. The method can be used for preparing the lead sulfide functional material quickly and efficiently, shortens the synthesis time, enlarges the yield of the synthesized lead sulfide, has high efficiency, low energy consumption and high yield of the lead sulfide material, and does not cause pollution to the environment.
The method for preparing the lead sulfide by using the industrial desulfurization waste liquid comprises the following steps:
a. filtering the 900-plus-1000 mL desulfurization waste liquid by using a 0.45-micron microporous filter membrane to remove residues in the waste liquid, and reserving the filtered desulfurization waste liquid for later use;
b. weighing 9-10g of lead acetate powder, adding the lead acetate powder into 100mL of deionized water, and stirring until the lead acetate powder is completely dissolved to obtain a lead acetate solution;
c. adding the lead acetate solution obtained in the step b into the desulfurization waste liquid obtained in the step a, continuously stirring for 10-20min, and then adjusting the pH value of the solution to 7-8 by using glacial acetic acid;
d. c, placing the solution obtained in the step c into an oil bath pot containing the dimethyl silicone oil for reaction, continuously stirring, heating to 160 ℃ for heat preservation for 6-8h, stopping heating and stirring, and naturally cooling to room temperature to obtain a solid-liquid mixture;
e. d, performing solid-liquid separation on the solid-liquid mixture after the reaction in the step d by using a centrifugal machine to obtain a lead sulfide material;
f. and e, putting the lead sulfide material obtained after separation in the step e into an oven, and drying for 4-6h at the temperature of 80 ℃ to finally obtain the lead sulfide material.
Compared with the existing preparation method, the method for preparing the lead sulfide by using the industrial desulfurization waste liquid has the advantages that:
more desulfurization waste liquid can be consumed in one experiment, and more lead sulfide functional materials can be obtained at the same time.
The supernatant obtained by the experiment can continuously react with lead acetate until the divalent sulfide ions in the mixed solution are completely consumed, and the continuous preparation of the lead sulfide functional material can be realized.
The oil bath kettle has the advantages of high heating rate, high reaction efficiency and high cooling rate due to the connection with the external environment, can raise the temperature by 120 ℃ in a short time, and is short in experimental period and low in energy consumption.
The invention is applied to coal coking enterprises, can create extremely high profits for the enterprises, can quickly solve a series of problems caused by excessive desulfurization waste liquid, and provides a good scheme for the aspect of environmental protection.
The invention adopts the centrifuge to carry out solid-liquid separation on the solid-liquid mixture after the reaction is finished, thereby shortening the time for separating the lead sulfide material. Compared with suction filtration, the method has the advantages of simple process, short time and thorough separation.
The desulfurization waste liquid is obtained by introducing coal flue gas into industrial ammonia water, so that the solution is alkaline, glacial acetic acid is required to be added after mixing to adjust the pH value of the mixed solution to 8, and the generation of lead sulfide during reaction is facilitated.
The used industrial desulfurization waste liquid is obtained by directly introducing the coal flue gas subjected to dust removal and cooling treatment into industrial ammonia water to simulate the environment absorbed by the industrial flue gas.
The pH of the mixed solution was adjusted to 8. The reaction rate of the desulfurization waste liquid and the lead acetate is improved, the cooling process is reduced, the reaction period is shortened, a large amount of desulfurization waste liquid can be treated in one experiment, and contribution is made to environmental protection.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
Example 1
a. Filtering 950mL of desulfurization waste liquid by using a 0.45-micron microporous filter membrane, removing residues in the waste liquid, and reserving the filtered desulfurization waste liquid for later use;
b. weighing 9g of lead acetate powder, adding the lead acetate powder into 100mL of deionized water, and stirring until the lead acetate powder is completely dissolved to obtain a lead acetate solution;
c. adding the lead acetate solution obtained in the step b into the desulfurization waste liquid obtained in the step a, continuously stirring for 15min, and then adjusting the pH value of the solution to 7 by using glacial acetic acid;
d. c, placing the solution obtained in the step c into an oil bath pot containing simethicone for reaction, continuously stirring, heating to 140 ℃, then preserving heat for 6 hours, stopping heating and stirring, and naturally cooling to room temperature to obtain a solid-liquid mixture;
e. d, performing solid-liquid separation on the solid-liquid mixture after the reaction in the step d by using a centrifugal machine to obtain a lead sulfide material;
f. and e, putting the lead sulfide material obtained after separation in the step e into an oven, and drying for 4 hours at the temperature of 80 ℃ to finally obtain the lead sulfide material.
Example 2
a. Filtering 900mL of desulfurization waste liquid by using a 0.45-micron microporous filter membrane, removing residues in the waste liquid, and reserving the filtered desulfurization waste liquid for later use;
b. 9.882g of lead acetate powder is weighed and added into 100mL of deionized water, and the mixture is stirred until the lead acetate powder is completely dissolved to obtain a lead acetate solution;
c. adding the lead acetate solution obtained in the step b into the desulfurization waste liquid obtained in the step a, continuously stirring for 10min, and then adjusting the pH value of the solution to 8 by using glacial acetic acid;
d. c, placing the solution obtained in the step c into an oil bath pot containing simethicone for reaction, continuously stirring, heating to 120 ℃, then preserving heat for 8 hours, stopping heating and stirring, and naturally cooling to room temperature to obtain a solid-liquid mixture;
e. d, performing solid-liquid separation on the solid-liquid mixture after the reaction in the step d by using a centrifugal machine to obtain a lead sulfide material;
f. and e, putting the lead sulfide material obtained after separation in the step e into an oven, and drying for 4 hours at the temperature of 80 ℃ to finally obtain the lead sulfide material.
Example 3
a. Filtering 1000mL of desulfurization waste liquid by using a 0.45-micron microporous filter membrane, removing residues in the waste liquid, and reserving the filtered desulfurization waste liquid for later use;
b. weighing 10g of lead acetate powder, adding the lead acetate powder into 100mL of deionized water, and stirring until the lead acetate powder is completely dissolved to obtain a lead acetate solution;
c. adding the lead acetate solution obtained in the step b into the desulfurization waste liquid obtained in the step a, continuously stirring for 20min, and then adjusting the pH value of the solution to 8 by using glacial acetic acid;
d. c, placing the solution obtained in the step c into an oil bath pot containing simethicone for reaction, continuously stirring, heating to 160 ℃, then preserving heat for 7 hours, stopping heating and stirring, and naturally cooling to room temperature to obtain a solid-liquid mixture;
e. d, performing solid-liquid separation on the solid-liquid mixture after the reaction in the step d by using a centrifugal machine to obtain a lead sulfide material;
f. and e, putting the lead sulfide material obtained after separation in the step e into an oven, and drying for 5 hours at the temperature of 80 ℃ to finally obtain the lead sulfide material.
The method can improve the yield of the lead sulfide functional material, reduce energy consumption, shorten reaction time, simplify operation, replace a larger container for preparation and improve the amount of the generated lead sulfide.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (1)
1. A method for preparing lead sulfide by using industrial desulfurization waste liquid is characterized by comprising the following steps:
a. filtering the 900-plus-1000 mL desulfurization waste liquid by using a 0.45-micron microporous filter membrane to remove residues in the waste liquid, and reserving the filtered desulfurization waste liquid for later use;
b. weighing 9-10g of lead acetate powder, adding the lead acetate powder into 100mL of deionized water, and stirring until the lead acetate powder is completely dissolved to obtain a lead acetate solution;
c. adding the lead acetate solution obtained in the step b into the desulfurization waste liquid obtained in the step a, continuously stirring for 10-20min, and then adjusting the pH value of the solution to 7-8 by using glacial acetic acid;
d. c, placing the solution obtained in the step c into an oil bath pot containing the dimethyl silicone oil for reaction, continuously stirring, heating to 160 ℃ for heat preservation for 6-8h, stopping heating and stirring, and naturally cooling to room temperature to obtain a solid-liquid mixture;
e. d, performing solid-liquid separation on the solid-liquid mixture after the reaction in the step d by using a centrifugal machine to obtain a lead sulfide material;
f. and e, putting the lead sulfide material obtained after separation in the step e into an oven, and drying for 4-6h at the temperature of 80 ℃ to finally obtain the lead sulfide material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011481453.2A CN112479247A (en) | 2020-12-16 | 2020-12-16 | Method for preparing lead sulfide by using industrial desulfurization waste liquid |
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| CN202011481453.2A CN112479247A (en) | 2020-12-16 | 2020-12-16 | Method for preparing lead sulfide by using industrial desulfurization waste liquid |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104692454A (en) * | 2015-02-12 | 2015-06-10 | 洛阳师范学院 | Method for preparing lead sulfide nano-particles through reflux precipitation |
| CN108793235A (en) * | 2018-09-20 | 2018-11-13 | 昌吉学院 | A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid |
-
2020
- 2020-12-16 CN CN202011481453.2A patent/CN112479247A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104692454A (en) * | 2015-02-12 | 2015-06-10 | 洛阳师范学院 | Method for preparing lead sulfide nano-particles through reflux precipitation |
| CN108793235A (en) * | 2018-09-20 | 2018-11-13 | 昌吉学院 | A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid |
Non-Patent Citations (2)
| Title |
|---|
| 李静文;: "硫化钠沉淀法处理含铅废水研究" * |
| 郝浩博等: ""利用脱硫废液通过水热法制备硫化铅"" * |
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