CN210683240U - Cadmium sulfide production system for manufacturing thin-film solar chips - Google Patents
Cadmium sulfide production system for manufacturing thin-film solar chips Download PDFInfo
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- CN210683240U CN210683240U CN201921634519.XU CN201921634519U CN210683240U CN 210683240 U CN210683240 U CN 210683240U CN 201921634519 U CN201921634519 U CN 201921634519U CN 210683240 U CN210683240 U CN 210683240U
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Abstract
The utility model discloses a cadmium sulfide production system for manufacturing thin-film solar chips, which comprises a cadmium sulfate reaction kettle, a filter, a standing barrel, a cadmium sulfate heater and a cadmium sulfide reaction kettle which are sequentially communicated through a pipeline; the top of the cadmium sulfide reaction kettle is provided with an air hole, a hydrogen sulfide gas pipe is assembled in the air hole, and the hydrogen sulfide gas pipe is introduced into the bottom of the cadmium sulfide reaction kettle. The production system has simple structure, low production cost and high efficiency; the production method directly adopts cadmium ingots, and the raw materials are convenient to use; the cadmium sulfide is high in purity (the purity can reach 99.99%) and is uniform yellow powder, and the cadmium sulfide is suitable for industrial production of enterprises.
Description
Technical Field
The utility model relates to a chemical material preparation field, concretely relates to a production system for thin-film solar chip makes cadmium sulfide.
Background
Cadmium sulfide (CdS) is a typical II-IV group semiconductor compound, the forbidden band width of the CdS is 2.42eV at room temperature, the CdS has excellent photoelectric conversion characteristics and luminescence performance, when the particle size of the CdS is smaller than the wave radius of an exciton of 6nm, an obvious quantum size effect can be shown, and meanwhile, an absorption edge and a blue shift of a fluorescence peak can appear. These excellent properties of cadmium sulfide have led to their wide use in light emitting diodes, solar cells, nonlinear optics, and the like.
In the existing cadmium sulfide production system, the structure is complex, heating treatment is required when a cadmium sulfate intermediate product is prepared in the generation method, the energy consumption is high, cadmium powder is generally adopted for reaction, a cadmium raw material needs to be processed and utilized, the production cost is high, the purity of the prepared cadmium sulfide is low, and the consumption requirement of consumers is not met.
SUMMERY OF THE UTILITY MODEL
Aiming at the problems in the prior art, the utility model aims to provide a production system of cadmium sulfide for manufacturing thin-film solar chips, which has simple structure, low production cost and high efficiency; the production method directly adopts cadmium ingots, and the raw materials are convenient to use; the cadmium sulfide is high in purity (the purity can reach 99.99%) and is uniform yellow powder, and the cadmium sulfide is suitable for industrial production of enterprises.
In order to achieve the above purpose, the present invention adopts the following technical solution.
A production system of cadmium sulfide for manufacturing a thin film solar chip comprises: the cadmium sulfate reaction kettle, the filter, the standing barrel, the cadmium sulfate heater and the cadmium sulfide reaction kettle are sequentially communicated through a pipeline; the top of the cadmium sulfide reaction kettle is provided with an air hole, a hydrogen sulfide gas pipe is assembled in the air hole, and the hydrogen sulfide gas pipe is introduced into the bottom of the cadmium sulfide reaction kettle.
Preferably, the cadmium sulfide reaction kettle further comprises a washing barrel, and a discharge hole of the cadmium sulfide reaction kettle is communicated with a feed hole of the washing barrel.
Preferably, the washing machine further comprises a dehydrator, and the discharge port of the washing barrel is communicated with the feeding port of the dehydrator.
Preferably, the drying device further comprises a drying box, and the drying box is used for drying the materials discharged from the dehydrator.
Preferably, the cadmium sulfate reaction kettle further comprises a pump, the pump is arranged on a pipeline between the cadmium sulfate reaction kettle and the filter, and the pump is used for conveying materials in the cadmium sulfate reaction kettle into the filter.
(II) a production method of cadmium sulfide for manufacturing a thin-film solar chip comprises the following steps:
step 1, firstly adding water into a cadmium sulfate reaction kettle, then adding concentrated sulfuric acid while stirring, and diluting the concentrated sulfuric acid to obtain dilute sulfuric acid; adding cadmium ingots into the dilute sulfuric acid, then adding a nitric acid solution in batches, and adjusting the pH value to obtain a cadmium sulfate solution;
step 2, filtering the cadmium sulfate solution by using a filter, and standing the filtered solution by using a standing barrel to obtain a purified cadmium sulfate solution;
and 3, heating the cadmium sulfate solution by using a heater, introducing the heated cadmium sulfate solution into a cadmium sulfide reaction kettle, and introducing hydrogen sulfide gas into the cadmium sulfide reaction kettle to obtain cadmium sulfide.
Preferably, in step 1, the ratio of the water, the concentrated sulfuric acid, the cadmium ingot and the nitric acid solution is (100-: (10-15) L: (80-120) kg: 6.5L.
Preferably, in step 1, the concentration of the concentrated sulfuric acid is not less than 70%, and the concentration of the nitric acid solution is not less than 20%.
Further preferably, in step 1, the ratio of the water, the concentrated sulfuric acid, the cadmium ingot and the nitric acid solution is 120 kg: 12.5L: 100 kg: 6.5L.
Preferably, in step 1, the pH is adjusted to 6-7.
Preferably, in step 1, the adding of the nitric acid solution in batches is performed in 9 times, wherein 2.5L is added for the first time, 500mL is added for the second time after 1 hour, and then 500mL is added every 30 min.
Preferably, in step 2, the standing is still for 22-26 hours.
Preferably, in step 3, the heating is carried out to 40-50 ℃.
Preferably, in the step 3, the introduction rate of the hydrogen sulfide gas is 2.5-5.5L/min, and when the concentration of cadmium ions in the cadmium sulfide reaction kettle is less than 15-18g/L, the introduction of the hydrogen sulfide is stopped.
Preferably, step 4 is further included after step 3, and the cadmium sulfide is sequentially washed, dehydrated, dried and cooled to obtain pure cadmium sulfide.
Further preferably, step 4 specifically comprises: washing cadmium sulfide with 70-90 deg.C warm water for 6-8 times until pH is 6-7; and dehydrating by using a dehydrator, drying by using an oven, and cooling to room temperature to obtain the pure cadmium sulfide.
Preferably, the drying temperature is 110-130 ℃, and the drying time is 46-50 hours.
Compared with the prior art, the beneficial effects of the utility model are that:
the production system of the cadmium sulfide for manufacturing the thin-film solar chip has simple structure, low production cost, high production efficiency and low energy consumption, and the obtained cadmium sulfide has high purity (the purity can reach 99.99 percent) and is suitable for industrial production of enterprises; the cadmium ingot is directly adopted, and the raw materials are convenient to use; and the method has the advantages of no need of additional heating, low energy consumption, full reaction, high production efficiency, simple production method and easy operation and implementation.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a diagram of a system for producing cadmium sulfide for manufacturing thin film solar chips according to the present invention;
in the figure: 1 cadmium sulfate reaction kettle; 2, a filter; 3, standing the barrel; 4 cadmium sulfate heater; 5, a cadmium sulfide reaction kettle; 501 a hydrogen sulfide gas pipe; 6, washing the barrel; 7, a dehydrator; 8 pumps.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Referring to fig. 1, according to an embodiment of the present disclosure, a system for producing cadmium sulfide for manufacturing thin film solar chips includes: the cadmium sulfate reaction kettle 1, the filter 2, the standing barrel 3, the cadmium sulfate heater 4 and the cadmium sulfide reaction kettle 5 are sequentially communicated through a pipeline; the top of the cadmium sulfide reaction kettle 5 is provided with an air hole, a hydrogen sulfide gas pipe 501 is arranged in the air hole, and the hydrogen sulfide gas pipe 501 is introduced into the bottom of the cadmium sulfide reaction kettle 5.
In the above examples, water, concentrated sulfuric acid, cadmium ingot, and nitric acid solution (HNO) were mixed3) Respectively put into cadmium sulfate reaction to react to generate cadmium sulfate solution (CdSO)4) And hydrogen (H)2) Nitrogen dioxide (NO)2) And oxygen (O)2) The generated gas can be directly discharged or recycled. The generated cadmium sulfate solution is treated by a filter 2 and a standing barrel 3, so that cadmium ingots which are not completely reacted and impurities which are insoluble in the sulfuric acid solution are removed, and the purity of cadmium sulfate is improved; wherein, the discharge hole at the bottom of the side wall of the standing barrel 3 is close to the barrel bottom as much as possible and keeps a certain distance with the barrel bottom, so that the cadmium sulfate and the impurities can be fully separated, and the cadmium sulfate solution can be ensured to fully flow out. The purified cadmium sulfate solution is heated by a cadmium sulfate heater 4 and then enters a cadmium sulfide reaction kettle 5, and hydrogen sulfide gas is introduced into the bottom of the cadmium sulfide reaction kettle 5, so that cadmium sulfate and hydrogen sulfide can fully react to generate cadmium sulfide precipitate. The utility model discloses a production system for cadmium sulfide that thin-film solar chip made simple structure, low in production cost, production efficiency is high, and the power consumption is low, and the purity of the cadmium sulfide of gained is high, is applicable to enterprise's industrial production.
Referring to fig. 1, according to an embodiment of the present invention, the apparatus further comprises a washing tub 6, wherein the discharge port of the cadmium sulfide reaction kettle 5 is communicated with the feed port of the washing tub 6.
In the above examples, impurities such as sulfuric acid remain in the cadmium sulfide produced, and the cadmium sulfide is put into the washing tub 6 and repeatedly washed with warm water until it becomes neutral, thereby removing impurities such as sulfuric acid and improving the purity of the cadmium sulfide.
Referring to fig. 1, according to an embodiment of the present invention, the washing machine further includes a dewatering machine 7, and the discharge port of the washing tub 6 is communicated with the feeding port of the dewatering machine 7.
In the above examples, the cadmium sulfide after washing was dehydrated by the dehydrator 7 to remove water.
According to the utility model discloses an embodiment still includes the drying cabinet, the drying cabinet is used for right the material that hydroextractor 7 came out carries out the drying.
In the above embodiment, the dehydrated cadmium sulfide is dried to further reduce the water content, so that the purified cadmium sulfide is convenient to store and transport.
Referring to fig. 1, according to an embodiment of the present invention, the cadmium sulfate reactor further comprises a pump 8, the pump 8 is disposed on the pipeline between the cadmium sulfate reactor 1 and the filter 2, and the pump 8 is used for conveying the materials in the cadmium sulfate reactor 1 to the filter 2.
In the above embodiment, the cadmium sulfide solution generated in the cadmium sulfate reaction kettle 1 is sent into the filter 2 through the pump 8, so that the working efficiency is improved.
Example 1
A production method of cadmium sulfide for manufacturing a thin film solar chip comprises the following steps:
step 1, adding 120kg of water into a cadmium sulfate reaction kettle, and then adding 12.5L of concentrated sulfuric acid (H) while stirring2SO4) Diluting concentrated sulfuric acid to obtain dilute sulfuric acid; adding 100kg of cadmium (Cd) ingot into the dilute sulfuric acid, adding a nitric acid solution for 9 times, adding 2.5L of the nitric acid solution for the first time, adding 500mL of the nitric acid solution for the second time after 1 hour, and adding 500mL of the nitric acid solution for 7 times and every 30 min; adjusting pH to 7 to obtain cadmium sulfate solution (CdSO)4) (ii) a Wherein the concentration of the concentrated sulfuric acid is not less than 70%, and the concentration of the nitric acid solution is not less than 20%. The reaction formula of each raw material in the cadmium sulfate reaction kettle is as follows: 2HNO3+Cd+H2SO4＝CdSO4+2H2↑+2NO2↑+O2↑。
And 2, filtering the cadmium sulfate solution by using a filter, and standing the filtered solution for 24 hours by using a standing barrel to obtain the purified cadmium sulfate solution.
And 3, heating the cadmium sulfate solution to 45 ℃ by adopting a heater, introducing the heated cadmium sulfate solution into a cadmium sulfide reaction kettle, introducing hydrogen sulfide gas into the cadmium sulfide reaction kettle at a rate of 4L/min, and stopping introducing the hydrogen sulfide when the concentration of cadmium ions in the cadmium sulfide reaction kettle is less than 16.5g/L to obtain the cadmium sulfide. Wherein, the reaction formula in the cadmium sulfide reaction kettle is as follows: cdso4+H2S＝CdS↓+H2SO4。
And 4, washing the cadmium sulfide for 7 times by using warm water at the temperature of 80 ℃, washing until the pH value is 6, dehydrating by using a dehydrator, drying for 48 hours at the temperature of 120 ℃ by using an oven, cooling to room temperature, sealing and packaging to obtain the pure cadmium sulfide.
Example 2
A production method of cadmium sulfide for manufacturing a thin film solar chip comprises the following steps:
step 1, adding 100kg of water into a cadmium sulfate reaction kettle, adding 10L of concentrated sulfuric acid while stirring, and diluting the concentrated sulfuric acid to obtain dilute sulfuric acid; adding 80kg of cadmium ingot into the dilute sulfuric acid, adding a nitric acid solution for 9 times, adding 2.5L of the nitric acid solution for the first time, adding 500mL of the nitric acid solution for the second time after 1 hour, and then adding 500mL of the nitric acid solution for 7 times and every 30 min; adjusting the pH value to 7 to obtain a cadmium sulfate solution; wherein the concentration of the concentrated sulfuric acid is not less than 70%, and the concentration of the nitric acid solution is not less than 20%.
And 2, filtering the cadmium sulfate solution by using a filter, and standing the filtered solution for 22 hours by using a standing barrel to obtain the purified cadmium sulfate solution.
And 3, heating the cadmium sulfate solution to 46 ℃ by adopting a heater, introducing the heated cadmium sulfate solution into a cadmium sulfide reaction kettle, introducing hydrogen sulfide gas into the cadmium sulfide reaction kettle at a rate of 5.5L/min, and stopping introducing the hydrogen sulfide when the concentration of cadmium ions in the cadmium sulfide reaction kettle is less than 15g/L to obtain the cadmium sulfide.
And 4, washing the cadmium sulfide for 8 times by adopting warm water at 70 ℃, washing until the pH value is 6, dehydrating by adopting a dehydrator, drying for 50 hours at 110 ℃ by adopting an oven, cooling to room temperature, sealing and packaging to obtain the pure cadmium sulfide.
Example 3
A production method of cadmium sulfide for manufacturing a thin film solar chip comprises the following steps:
step 1, adding 140kg of water into a cadmium sulfate reaction kettle, adding 15L of concentrated sulfuric acid while stirring, and diluting the concentrated sulfuric acid to obtain dilute sulfuric acid; adding 120kg of cadmium ingot into the dilute sulfuric acid, adding a nitric acid solution for 9 times, adding 2.5L of the nitric acid solution for the first time, adding 500mL of the nitric acid solution for the second time after 1 hour, and then adding 500mL of the nitric acid solution for 7 times and every 30 min; adjusting the pH value to 6.5 to obtain a cadmium sulfate solution; wherein the concentration of the concentrated sulfuric acid is not less than 70%, and the concentration of the nitric acid solution is not less than 20%.
And 2, filtering the cadmium sulfate solution by using a filter, and standing the filtered solution for 26 hours by using a standing barrel to obtain the purified cadmium sulfate solution.
And 3, heating the cadmium sulfate solution to 40 ℃ by adopting a heater, introducing the heated cadmium sulfate solution into a cadmium sulfide reaction kettle, introducing hydrogen sulfide gas into the cadmium sulfide reaction kettle at a rate of 2.5L/min, and stopping introducing the hydrogen sulfide when the concentration of cadmium ions in the cadmium sulfide reaction kettle is less than 18g/L to obtain the cadmium sulfide.
And 4, washing the cadmium sulfide for 6 times by adopting warm water at 90 ℃, washing until the pH value is 6.5, dehydrating by adopting a dehydrator, drying for 46 hours at 130 ℃ by adopting an oven, cooling to room temperature, sealing and packaging to obtain the pure cadmium sulfide.
Example 4
A production method of cadmium sulfide for manufacturing a thin film solar chip comprises the following steps:
step 1, adding 120kg of water into a cadmium sulfate reaction kettle, adding 14L of concentrated sulfuric acid while stirring, and diluting the concentrated sulfuric acid to obtain dilute sulfuric acid; adding 110kg of cadmium ingot into the dilute sulfuric acid, adding a nitric acid solution for 9 times, adding 2.5L of the nitric acid solution for the first time, adding 500mL of the nitric acid solution for the second time after 1 hour, and then adding 500mL of the nitric acid solution for 7 times and every 30 min; adjusting the pH value to 6 to obtain a cadmium sulfate solution; wherein the concentration of the concentrated sulfuric acid is not less than 70%, and the concentration of the nitric acid solution is not less than 20%.
And 2, filtering the cadmium sulfate solution by using a filter, and standing the filtered solution for 25 hours by using a standing barrel to obtain the purified cadmium sulfate solution.
And 3, heating the cadmium sulfate solution to 50 ℃ by adopting a heater, introducing the heated cadmium sulfate solution into a cadmium sulfide reaction kettle, introducing hydrogen sulfide gas into the cadmium sulfide reaction kettle at a rate of 3.5L/min, and stopping introducing the hydrogen sulfide when the concentration of cadmium ions in the cadmium sulfide reaction kettle is less than 16.5g/L to obtain the cadmium sulfide.
And 4, washing the cadmium sulfide with warm water at the temperature of 80 ℃ for 8 times until the pH value is 7, dehydrating with a dehydrator, drying for 47 hours at the temperature of 120 ℃ with an oven, cooling to room temperature, sealing and packaging to obtain the pure cadmium sulfide.
In the above embodiment, in step 1, when the cadmium sulfate solution is prepared, the cadmium ingot is adopted, the cadmium ingot does not need to be processed into cadmium powder, and the raw materials are convenient to use; the heat released by diluting the concentrated sulfuric acid is utilized to ensure that the nitric acid solution, cadmium and sulfuric acid react to generate cadmium sulfate without additional heating, so that the energy consumption is low and the production cost is low; the nitric acid solution can be used as a reactant to participate in the reaction and can also be used as a catalyst to promote the reaction in the reaction, so that the reaction efficiency is improved, and the nitric acid solution is added in batches, so that the reaction can be fully carried out. In the step 2, the cadmium sulfate solution is filtered and kept stand, so that incompletely reacted cadmium ingots in the cadmium sulfate solution and impurities insoluble in the sulfuric acid solution can be effectively removed, and the purity of cadmium sulfate is improved. In the step 3, the cadmium sulfate solution is heated and then reacts with the hydrogen sulfide to generate cadmium sulfide precipitate, the cadmium sulfide precipitate is favorably smoothly reacted with the hydrogen sulfide by the way of heating firstly, and the reaction efficiency is improved. And 4, finally, repeatedly washing the prepared cadmium sulfide with water to remove acidic substances, and dehydrating and drying the cadmium sulfide to obtain the cadmium sulfide with the purity of 99.99 percent.
Although the invention has been described in detail in this specification with reference to specific embodiments and illustrative embodiments, it will be apparent to those skilled in the art that certain changes and modifications can be made therein without departing from the scope of the invention. Therefore, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. A system for producing cadmium sulfide for thin film solar chip fabrication, comprising: the cadmium sulfate reaction kettle (1), the filter (2), the standing barrel (3), the cadmium sulfate heater (4) and the cadmium sulfide reaction kettle (5) are communicated in sequence through pipelines; the top of the cadmium sulfide reaction kettle (5) is provided with an air hole, a hydrogen sulfide gas pipe (501) is assembled in the air hole, and the hydrogen sulfide gas pipe (501) is introduced into the bottom of the cadmium sulfide reaction kettle (5).
2. The production system of cadmium sulfide for manufacturing thin-film solar chips as claimed in claim 1, further comprising a washing barrel (6), wherein the discharge port of the cadmium sulfide reaction kettle (5) is communicated with the feed port of the washing barrel (6).
3. The production system of cadmium sulfide for manufacturing thin-film solar chips as defined in claim 2, further comprising a dehydrator (7), wherein the outlet of the washing barrel (6) is communicated with the inlet of the dehydrator (7).
4. The production system of cadmium sulfide for manufacturing thin film solar chips as claimed in claim 3, further comprising a drying oven for drying the material from the dehydrator (7).
5. The production system of cadmium sulfide for manufacturing thin film solar chips as claimed in claim 4, further comprising a pump (8), wherein the pump (8) is arranged on a pipeline between the cadmium sulfate reaction kettle (1) and the filter (2), and the pump (8) is used for conveying materials in the cadmium sulfate reaction kettle (1) to the filter (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921634519.XU CN210683240U (en) | 2019-09-27 | 2019-09-27 | Cadmium sulfide production system for manufacturing thin-film solar chips |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921634519.XU CN210683240U (en) | 2019-09-27 | 2019-09-27 | Cadmium sulfide production system for manufacturing thin-film solar chips |
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| CN210683240U true CN210683240U (en) | 2020-06-05 |
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| CN201921634519.XU Expired - Fee Related CN210683240U (en) | 2019-09-27 | 2019-09-27 | Cadmium sulfide production system for manufacturing thin-film solar chips |
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