CN111995399A - Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid - Google Patents
Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid Download PDFInfo
- Publication number
- CN111995399A CN111995399A CN202010904989.4A CN202010904989A CN111995399A CN 111995399 A CN111995399 A CN 111995399A CN 202010904989 A CN202010904989 A CN 202010904989A CN 111995399 A CN111995399 A CN 111995399A
- Authority
- CN
- China
- Prior art keywords
- zinc sulfide
- waste liquid
- temperature
- desulfurization waste
- putting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing a zinc sulfide ceramic material by using coal coking desulfurization waste liquid, which takes the desulfurization waste liquid and zinc acetate as raw materials and is prepared by the processes of mixing and stirring, constant-temperature heating, filtering, drying, vacuum hot-pressing sintering, high-temperature annealing and the like, the zinc sulfide ceramic material obtained by the method can be used in the field of thermistors, has higher sensitivity, the resistance temperature coefficient is 10-100 times larger than that of metal, the temperature change at-50-100 ℃ can be detected, the product volume is small, the temperature of gaps, cavities and blood vessels in organisms which cannot be measured by other thermometers can be measured, the thermometer is easy to process into complex shapes, the zinc sulfide ceramic material prepared by the method has high compactness, hardness and corrosion resistance. The invention is based on the concept of changing waste into valuable, is beneficial to energy conservation, water conservation and resource recycling, effectively improves the resource utilization rate, increases the economic production benefit and provides an innovative idea for energy conservation and emission reduction.
Description
Technical Field
The invention relates to a method for preparing a zinc sulfide ceramic material by using coal coking desulfurization waste liquid.
Background
With the continuous development and progress of modern industrial production, the sulfur-containing waste liquid discharged in the production process of coal chemical enterprises in recent years has great threat to the ecological environment and the health of people. The main pollution components contained in the waste liquid are carbonate ions, thiocyanate ions, thiosulfate ions, divalent sulfide ions, sulfate ions and the like, and great harm is brought to the ecological environment. With the continuous development and research of desulfurization technology, ammonia desulfurization is adopted, but the mode of adding a desulfurizing agent in the ammonia desulfurization process is not environment-friendly, the subsequent wastewater is difficult to treat and exists in the form of waste liquid and waste residue, the environmental hazard is serious, and the sulfur in the desulfurization waste liquid is converted into sulfur with low added value through the ammonia desulfurization process; the existing desulfurization technology in the coking industry mainly comprises a lime-gypsum method, the main product is gypsum, the utilization rate of the existing gypsum is low, and the market is saturated. Many enterprises can convert sulfur-containing waste liquid into high-value-added functional powder materials such as sulfur, lead sulfide, zinc sulfide and the like after the sulfur-containing waste liquid is treated by a desulfurization process. Zinc sulfide is a typical direct wide-band-gap II-VI semiconductor material, and has a cubic phase forbidden band width of 3.72eV and a hexagonal phase of 3.77 eV. As a high value-added semiconductor material, zinc sulfide has been widely applied in the fields of electroluminescence, flat panel displays, light emitting diodes, lasers, nonlinear optical devices, photochemical catalysts, photosensitive sensors and the like, and the zinc sulfide generated under high temperature and high alkalinity has the characteristics of fine granularity, large specific surface and strong adsorbability, and can be used as a desulfurizing agent, a catalyst, a feed additive and the like for medicines, rubber, latex products, petrochemical industry and chemical industry.
At present, functional ceramic materials are generally prepared by adopting high-purity artificially synthesized raw materials and forming and sintering by using a precise control process, so that the functional ceramic has special mechanical, optical, acoustic, electrical, magnetic and thermal properties and the like so as to meet the requirements in production and life. According to the main components, oxide ceramics, nitride ceramics, carbide ceramics, sulfide ceramics, metal ceramics and the like are included, and the extracted sulfur element in the desulfurization waste liquid is converted into a zinc sulfide ceramic material, so that the zinc sulfide ceramic material can be used for the aspects of detection, control, compensation and the like of the environmental temperature. A common preparation method is Chemical Vapour Deposition (CVD), however this method is complex and time consuming, leading to sublimation of the compound phase transition at temperatures above 1200 c, cubic phase zinc sulphide is relatively structurally stable under nitrogen atmosphere, cubic phase transition to hexagonal phase up to 1010 c, and zinc sulphide sublimation starts at temperatures above 1100 c. To avoid oxidation by air, the sintering of the zinc sulfide should preferably be carried out at 1000 ℃ to minimize the conversion of cubic to hexagonal structure. Compared with the zinc sulfide ceramic material prepared by a chemical vapor deposition method, the vacuum hot-pressing ceramic material has the advantages of low cost, quick production period and higher surface hardness.
After retrieval: the invention relates to a method for preparing sulfur elementary substance by using coal coking desulfurization waste liquid (application number: CN 201811059440.9). the method comprises the steps of mixing the coal coking desulfurization waste liquid with carbon disulfide according to a certain proportion, using suspended sulfur in desulfurization liquid by a reduced pressure distillation method, and centrifuging to obtain a sulfur elementary substance product.
The invention discloses a method for preparing copper sulfide by using coal coking desulfurization waste liquid (application number: CN 201811059483.7). according to the method, the desulfurization waste liquid and a copper-containing solution are mixed and stirred uniformly, ammonia water is added, and a pH value is adjusted to obtain a copper sulfide sample.
A method for preparing zinc sulfide by using coal coking desulfurization waste liquid (application number: CN201710865031.7) comprises the steps of obtaining zinc sulfide powder by using desulfurization waste liquid and zinc acetate, and placing the obtained solution in a stainless steel reaction kettle for hydrothermal reaction in step c; and f, annealing the rough zinc sulfide powder obtained in the step f at high temperature under the protection of argon atmosphere.
The invention uses the desulfurization waste liquid as a sulfur source and zinc acetate as a zinc source, replaces sulfur-containing elements in the industrial waste water by a wet chemical method to generate zinc sulfide with high added value, and then sinters the zinc sulfide by a vacuum hot pressing method to prepare the zinc sulfide functional ceramic material with high purity and good compactness. The method has the advantages of realizing circular economy of coal chemical enterprises, being beneficial to energy conservation, water conservation and resource recycling, being simple in process operation, low in cost and high in recovery rate, reducing the industrial pollution control cost, improving the economic benefit of factories, and having great significance for the sustainable development of enterprises.
Disclosure of Invention
The invention aims to provide a method for preparing a zinc sulfide ceramic material by using coal coking desulfurization waste liquid, the method takes the desulfurization waste liquid and the zinc acetate as raw materials, and is prepared by the processes of mixing and stirring, constant-temperature heating, filtering, drying, vacuum hot-pressing sintering, high-temperature annealing and the like, the zinc sulfide ceramic material obtained by the method can be used in the field of thermistors, has higher sensitivity, the resistance temperature coefficient is 10-100 times larger than that of metal, the temperature change at-50-100 ℃ can be detected, the product volume is small, the temperature of gaps, cavities and blood vessels in organisms which cannot be measured by other thermometers can be measured, the thermometer is easy to process into complex shapes, the zinc sulfide ceramic material prepared by the method has high compactness, hardness and corrosion resistance. The invention is based on the concept of changing waste into valuable, is beneficial to energy conservation, water conservation and resource recycling, effectively improves the resource utilization rate, increases the economic production benefit and provides an innovative idea for energy conservation and emission reduction.
The invention relates to a method for preparing a zinc sulfide ceramic material by using coal coking desulfurization waste liquid, which takes the coal coking desulfurization waste liquid as a sulfur source to react with zinc acetate and is prepared by a wet chemical method, and the specific operation is carried out according to the following steps:
a. adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. c, dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to be 7-9, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. d, covering a preservative film on the opening of the beaker filled with the mixed solution obtained in the step c, putting the beaker into a water bath kettle, heating to 70-90 ℃, keeping the temperature for 2-6h, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven at 100 ℃ for 4-8 hours to obtain zinc sulfide powder with the purity of 99%;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the mold into a vacuum hot pressing furnace, vacuumizing to 10Pa, heating to 800 plus material 900 ℃ at the speed of 25 ℃/min, applying the pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic.
Compared with the prior art, the method for preparing the zinc sulfide ceramic material by using the coal coking desulfurization waste liquid has the following substantial characteristics:
1. the invention directly takes the desulfurization waste liquid discharged by coal coking enterprises as the raw material to prepare the high-purity zinc sulfide functional ceramic;
2. the reaction device for improving the experimental process flow is designed to cover the beaker with the film to manufacture a closed reaction environment, so that volatile matters generated in the reaction are attached to the film and are recovered from a gas state to a liquid state after being condensed when meeting cold, thereby recycling, avoiding air pollution and reactant loss and improving the utilization rate of raw materials;
3. the invention simplifies the preparation process of the zinc sulfide functional ceramic, and the prepared zinc sulfide functional ceramic has higher compactness, hardness and better corrosion resistance;
4. the invention is based on the concept of changing waste into valuable, is beneficial to energy conservation, water conservation and resource recycling, improves the resource utilization rate, increases the economic production benefit, and provides an innovative idea for energy conservation and emission reduction;
5. the invention adopts the vacuum hot-pressing sintering technology to prepare the zinc sulfide functional ceramic, the price of the required equipment is low, the preparation cost is reduced, the process route is simple and convenient to operate, the mass preparation can be realized, and a constructive idea is provided for optimizing the productivity structure.
Drawings
FIG. 1 is an X-ray diffraction pattern of a zinc sulfide ceramic material of the present invention at a powder preparation temperature of 80 ℃ and a calcination temperature of 900 ℃;
FIG. 2 is a scanning electron microscope image of the zinc sulfide ceramic material of the present invention;
FIG. 3 is an X-ray energy spectrum of the present invention.
Detailed Description
Example 1
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. c, dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 7, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. d, covering a preservative film on the opening of the beaker filled with the mixed solution obtained in the step c, putting the beaker into a water bath kettle, heating to 70 ℃, keeping the temperature for 2 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven constant at 100 ℃ for 4 hours to obtain zinc sulfide powder with the purity of 99 percent;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, putting 2g of zinc sulfide powder obtained in the step e into the mold, putting the mold into a vacuum hot pressing furnace, vacuumizing to 10Pa, heating to 800 ℃ at the speed of 25 ℃/min, applying the pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 2
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 8, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. d, covering a preservative film on the opening of the beaker filled with the mixed solution obtained in the step c, putting the beaker into a water bath kettle, heating to 80 ℃, keeping the temperature for 4 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven constant at 100 ℃ for 6 hours to obtain zinc sulfide powder with the purity of 99 percent;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the mold into a vacuum hot pressing furnace, vacuumizing to 10Pa, heating to 800 ℃ at the speed of 25 ℃/min, applying the pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 3
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 9, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. covering a preservative film on the mixed solution obtained in the step c, putting the beaker into a water bath kettle, heating to 90 ℃, keeping the temperature for 6 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven constant at 100 ℃ for 8 hours to obtain zinc sulfide powder with the purity of 99 percent;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the mold into a vacuum hot pressing furnace, vacuumizing to 10Pa, heating to 800 ℃ at the speed of 25 ℃/min, applying the pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 4
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. c, dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 7, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. covering a preservative film on the mixed solution obtained in the step c, putting the beaker into a water bath pot, heating to 75 ℃, keeping the temperature for 2.5 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven at 100 ℃ for 4-8 hours to obtain zinc sulfide powder with the purity of 99%;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the mold into a vacuum hot pressing furnace, vacuumizing to 10Pa, heating to 850 ℃ at the speed of 25 ℃/min, applying the pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 5
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 8, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. covering a preservative film on the mixed solution obtained in the step c, putting the beaker into a water bath pot, heating to 85 ℃, keeping the temperature for 3 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven constant at 100 ℃ for 5 hours to obtain zinc sulfide powder with the purity of 99 percent;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the zinc sulfide powder into the mold, putting the mold into a vacuum hot-pressing furnace, pumping to vacuum 10Pa, heating to 900 ℃ at the speed of 25 ℃/min, applying pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 6
a. Adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. c, dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to 9, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. covering a preservative film on the mixed solution obtained in the step c, putting the beaker into a water bath pot, heating to 90 ℃, keeping the temperature for 5 hours, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven constant at 100 ℃ for 7 hours to obtain zinc sulfide powder with the purity of 99 percent;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the zinc sulfide powder into the mold, putting the mold into a vacuum hot-pressing furnace, pumping to vacuum 10Pa, heating to 900 ℃ at the speed of 25 ℃/min, applying pressure to 40MPa, keeping the temperature for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic material.
Example 7
Any one of the zinc sulfide ceramic materials obtained in the examples 1-6 is tested by an X-ray energy spectrometer (EDS) to obtain a high-purity zinc sulfide ceramic material, wherein a small amount of zinc oxide is contained, and the purity of the material reaches more than 99%.
Example 8
The zinc sulfide ceramic material obtained in any one of the embodiments 1 to 6 is used in the field of thermistors, the zinc sulfide ceramic material has high sensitivity, the resistance temperature coefficient of the zinc sulfide ceramic material is 10 to 100 times larger than that of metal, the zinc sulfide ceramic material can detect temperature change of-50 to 100 ℃, the product volume is small, the zinc sulfide ceramic material can measure the temperature of gaps, cavities and blood vessels in organisms which cannot be measured by other thermometers, the zinc sulfide ceramic material is easy to process into complex shapes, automatic gain control can be realized by utilizing the self-heating characteristic of the negative temperature coefficient thermistor, and an RC oscillator amplitude stabilizing circuit, a delay circuit and a protection circuit are formed, so the thermistor can also be used as an electronic circuit element for instrument circuit temperature compensation, thermocouple cold end temperature compensation and the.
Claims (1)
1. A method for preparing a zinc sulfide ceramic material by using coal coking desulfurization waste liquid is characterized in that the method takes the coal coking desulfurization waste liquid as a sulfur source to react with zinc acetate, and the zinc sulfide ceramic material is prepared by a wet chemical method, and the specific operation is carried out according to the following steps:
a. adding 9.7g of zinc acetate into 90mL of deionized water, and stirring for 10min on a magnetic stirrer until the zinc acetate is dissolved;
b. measuring 900mL of desulfurization waste liquid, putting the desulfurization waste liquid into a beaker, adding the zinc acetate solution obtained in the step a into the desulfurization waste liquid, and putting the mixture on a constant-temperature heating magnetic stirrer to stir and mix for 30min to obtain a mixed liquid;
c. c, dropwise adding glacial acetic acid into the mixed solution obtained in the step b to adjust the pH value to be 7-9, and stirring the mixed solution on a magnetic stirrer for 10min to obtain a mixed solution;
d. d, covering a preservative film on the opening of the beaker filled with the mixed solution obtained in the step c, putting the beaker into a water bath kettle, heating to 70-90 ℃, keeping the temperature for 2-6h, taking out the beaker, and cooling the mixed solution to room temperature;
e. d, washing the solution obtained in the step d with deionized water, and then carrying out suction filtration on the precipitate by using a circulating water type vacuum pump;
f. e, putting the precipitate obtained in the step e into a vacuum drying oven, and keeping the temperature of the vacuum drying oven at 100 ℃ for 4-8 hours to obtain zinc sulfide powder with the purity of 99%;
g. selecting a graphite mold with the inner diameter of 20mm, lining a layer of graphite paper on the inner wall of the mold, weighing 2g of zinc sulfide powder obtained in the step e, putting the mold into a vacuum hot pressing furnace, pumping to the vacuum of 10Pa, heating to 800-plus-material temperature of 900 ℃ at the speed of 25 ℃/min, applying the pressure of 40MPa, preserving heat for 2h, naturally cooling the grinding tool to the room temperature, and taking out a zinc sulfide ceramic sample;
h. and g, coarse grinding the ceramic sample obtained in the step g by using sand paper, and polishing the sample by using a polishing machine to obtain the zinc sulfide ceramic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010904989.4A CN111995399A (en) | 2020-09-01 | 2020-09-01 | Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010904989.4A CN111995399A (en) | 2020-09-01 | 2020-09-01 | Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111995399A true CN111995399A (en) | 2020-11-27 |
Family
ID=73466192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010904989.4A Pending CN111995399A (en) | 2020-09-01 | 2020-09-01 | Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111995399A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778520A (en) * | 1987-03-26 | 1988-10-18 | University Of Waterloo | Process for leaching zinc from partially desulfurized zinc concentrates by sulfuric acid |
| CN106521631A (en) * | 2016-11-08 | 2017-03-22 | 清远先导材料有限公司 | Preparation method of polycrystal zinc sulfide |
| CN107500342A (en) * | 2017-09-22 | 2017-12-22 | 昌吉学院 | A kind of method that zinc sulphide is prepared using coking of coal desulfurization waste liquor |
| 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 |
| CN109052330A (en) * | 2018-09-12 | 2018-12-21 | 昌吉学院 | A method of sulphur simple substance is prepared using coking of coal desulfurization waste liquor |
| CN109264765A (en) * | 2018-09-12 | 2019-01-25 | 昌吉学院 | A method of copper sulfide is prepared using coking of coal desulfurization waste liquor |
-
2020
- 2020-09-01 CN CN202010904989.4A patent/CN111995399A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778520A (en) * | 1987-03-26 | 1988-10-18 | University Of Waterloo | Process for leaching zinc from partially desulfurized zinc concentrates by sulfuric acid |
| CN106521631A (en) * | 2016-11-08 | 2017-03-22 | 清远先导材料有限公司 | Preparation method of polycrystal zinc sulfide |
| CN107500342A (en) * | 2017-09-22 | 2017-12-22 | 昌吉学院 | A kind of method that zinc sulphide is prepared using coking of coal desulfurization waste liquor |
| CN109052330A (en) * | 2018-09-12 | 2018-12-21 | 昌吉学院 | A method of sulphur simple substance is prepared using coking of coal desulfurization waste liquor |
| CN109264765A (en) * | 2018-09-12 | 2019-01-25 | 昌吉学院 | A method of copper sulfide is prepared using coking of coal desulfurization waste liquor |
| 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 |
|---|
| 张深基: "《纺织厂电气控制技术》", 30 June 1997, 中国纺织出版社 * |
| 金春江等: "湿化学法从脱硫废液中合成高纯度ZnS及Zn5(OH)6(CO3)2", 《化工新型材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102674357A (en) | Method for synthesizing high-purity silicon carbide raw material for growing silicon carbide single crystals | |
| CN110044971B (en) | Gas-sensitive material, preparation method and application thereof in gas-sensitive sensor | |
| CA1145919A (en) | METHOD FOR PRODUCING POWDER OF .alpha.-SILICON NITRIDE | |
| CN102730690A (en) | Al4SiC4 material synthetic method | |
| CN109704778A (en) | A kind of SiBCN ceramics and preparation method thereof | |
| EP0238338B1 (en) | Process for producing alpha-sialon powder | |
| CN111995399A (en) | Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid | |
| CN107265495A (en) | Non-template method prepares zinc sulphide microballoon | |
| CN102659106A (en) | Pressureless sintering method for synthesizing high-purity Ti3SiC2 powder | |
| Hou et al. | Oxidation kinetics of aluminum nitride at different oxidizing atmosphere | |
| Liu et al. | Fabrication of β-sialon powder from kaolin | |
| CN103695954B (en) | A kind of method being prepared vanadous oxide by vanadate Direct Electrolysis | |
| CN105506735A (en) | Carbon material structural part for polycrystalline silicon ingots and preparation method of carbon material structural part | |
| CN110054212B (en) | Compound NH4GaS2And preparation method and application thereof | |
| CN102211937B (en) | Method for synthesizing high-purity aluminum silicon carbon superfine powder | |
| CN109796477B (en) | Preparation method of rare earth ion doped metal-organic framework fluorescent material | |
| Qin et al. | Role of the vapour phases in the formation mechanism of 15R-SiAlON in FexSiy-Si3N4-Al2O3 composites at 1800° C | |
| SU1054331A1 (en) | Batch for making refractory products | |
| CN109293368B (en) | Preparation method of aluminum nitride powder | |
| CN100457684C (en) | Synthetic preparation method of A1N ceramic powder | |
| WO2020057095A1 (en) | Method for preparing silicon carbide powder by using induction furnace | |
| JPS6355108A (en) | Aluminum nitride powder and production thereof | |
| CN110511032A (en) | A kind of sintering method improving nitride combined silicon carbide material against oxidative performance | |
| CN103896324B (en) | A kind of method utilizing blast furnace dust to prepare nano zine oxide | |
| CN103922752A (en) | Method for preparing beta-SiAlON multiphase material by using fly ash |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201127 |