CN110817811A - Preparation method of high-purity selenium powder with uniform particle size distribution - Google Patents
Preparation method of high-purity selenium powder with uniform particle size distribution Download PDFInfo
- Publication number
- CN110817811A CN110817811A CN201911275840.8A CN201911275840A CN110817811A CN 110817811 A CN110817811 A CN 110817811A CN 201911275840 A CN201911275840 A CN 201911275840A CN 110817811 A CN110817811 A CN 110817811A
- Authority
- CN
- China
- Prior art keywords
- particle size
- size distribution
- selenium powder
- acid
- uniform particle
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Photoreceptors In Electrophotography (AREA)
Abstract
The invention discloses a preparation method of high-purity selenium powder with uniform particle size distribution by an environment-friendly and efficient separation process, which comprises the steps of dissolving raw material crude selenium by acid, stirring and reacting for 50-70 min at 30-50 ℃, cooling to room temperature, and carrying out solid-liquid separation to obtain filter residue a; drying the filter residue a and dissolving the filter residue in Na2SO3Reacting in the solution at 90-100 ℃ for 1-5 h, cooling to room temperature, and carrying out solid-liquid separation to obtain a filtrate b; dropwise adding acid into the filtrate b to react to obtain a material c; and (4) carrying out solid-liquid separation on the material c, and washing insoluble substances to obtain the high-purity selenium powder with uniform target object particle size distribution. The purity of the selenium powder prepared by the method can reach 99.9 percent, the selenium powder has uniform particle size distribution, high purity and little pollution; the required equipment is simple, the process is simple, the pollution is low, and the production efficiency of the selenium powder is improved.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a preparation method of high-purity selenium powder with uniform particle size distribution.
Background
Selenium is a typical rare-earth element in group VI A of the periodic Table of elements and has properties similar to those of sulfur. The high-purity selenium is mainly used in electronic industry such as phototube and solar battery, and the pigment industry uses a large amount of selenium due to the stability of selenium-containing pigment to light, heat and chemical action, and can also be used for copying machine, glass decolouring, metallurgical additive and the like. The selenium powder can make the glass colored purple or light red, and is a good coloring agent and decoloring agent. Since the activity ratio of selenium powder is high, selenium powder is often used as a raw material in most application processes in order to improve efficiency. The main preparation method of the selenium powder at present is a mechanical crushing mode, and the method has low working efficiency, high energy consumption, introduction of impurities, influence on product purity and the like.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity selenium powder with uniform particle size distribution.
The invention aims to realize that the preparation method of the high-purity selenium powder with uniform particle size distribution comprises the steps of pretreatment, main reaction, acid reaction and post-treatment, and specifically comprises the following steps:
A. pretreatment: dissolving raw material crude selenium with acid, stirring and reacting at 30-50 ℃ for 50-70 min, cooling to room temperature, and carrying out solid-liquid separation to obtain filter residue a;
B. main reaction: drying the filter residue a and dissolving the filter residue in Na2SO3Reacting in the solution at 90-100 ℃ for 1-5 h, cooling to room temperature, and carrying out solid-liquid separation to obtain a filtrate b;
C. acid reaction: dropwise adding acid into the filtrate b to react to obtain a material c;
D. and (3) post-treatment: and (4) carrying out solid-liquid separation on the material c, and washing insoluble substances to obtain the high-purity selenium powder with uniform target object particle size distribution.
The purity of the selenium powder prepared by the method can reach 99.9 percent, the selenium powder has uniform particle size distribution, high purity and little pollution; the required equipment is simple, the process is simple, the pollution is low, and the production efficiency of the selenium powder is improved.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
The preparation method of the high-purity selenium powder with uniform particle size distribution comprises the steps of pretreatment, main reaction, acid reaction and post-treatment, and specifically comprises the following steps:
A. pretreatment: dissolving raw material crude selenium with acid, stirring and reacting at 30-50 ℃ for 50-70 min, cooling to room temperature, and carrying out solid-liquid separation to obtain filter residue a;
B. main reaction: drying the filter residue a and dissolving the filter residue in Na2SO3Reacting in the solution at 90-100 ℃ for 1-5 h, cooling to room temperature, and carrying out solid-liquid separation to obtain a filtrate b;
C. acid reaction: dropwise adding acid into the filtrate b to react to obtain a material c;
D. and (3) post-treatment: and (4) carrying out solid-liquid separation on the material c, and washing insoluble substances to obtain the high-purity selenium powder with uniform target object particle size distribution.
The acid in the step A is one or more of sulfuric acid, nitric acid and hydrochloric acid.
The concentration of the acid is 30-100 g/L.
The temperature for acid dissolution in step A is less than 100 ℃.
In step B, Na2SO3The concentration of the solution is 200-400 g/L.
The acid in the step C is sulfuric acid.
The concentration of the acid is 100-300 g/L.
And C, the acid reaction time in the step C is 1-3 h, and the pH value is controlled to be 1-3.
And C, dropwise adding at a constant speed, wherein the dropwise adding speed is 10-50 ml/min.
And D, washing for 3-5 times by using deionized water, wherein the pH value is 6.5-7.5.
The invention is further illustrated by the following specific examples:
example 1
300ml of 50g/L H was taken2SO4Dissolving 200g of crude selenium, and stirring and reacting for 1h at 40 ℃; filtering after the solution is cooled, carrying out solid-liquid separation, and drying filter residue at 80 ℃. Dissolving 100g of dried filter residue in 400mL of 250g/L Na2SO3In solution, the reaction was carried out at 95 ℃ for 1 hour. And cooling to room temperature, carrying out suction filtration, transferring the filtrate into a round-bottom flask, dropwise adding 200g/L sulfuric acid at the speed of 30mL/min, adjusting the pH of the solution to 1, reacting for 1h at 60 ℃, carrying out suction filtration, washing with deionized water for 3 times until the pH is neutral, and thus obtaining the high-purity selenium powder.
Example 2
300ml of 40g/L H was taken2SO4Dissolving 200g of crude selenium, and stirring and reacting for 2 hours at the temperature of 30 ℃; after the solution is cooled, the solution is filtered, solid-liquid separation is carried out, and filter residue is dried at 90 ℃. Dissolving 100g of dried filter residue in 400mL of 210g/L Na2SO3In solution, the reaction was carried out at 90 ℃ for 2 h. And cooling to room temperature, carrying out suction filtration, transferring the filtrate to a round-bottom flask, adding 150g/L sulfuric acid, dropwise adding at the speed of 40mL/min, adjusting the pH of the solution to 2, reacting at 50 ℃ for 2h, carrying out suction filtration, and washing with deionized water for 3 times until the pH is neutral to obtain the high-purity selenium powder.
Example 3
300ml of 70g/L H was taken2SO4Dissolving 200g of crude selenium, and stirring and reacting for 3 hours at 50 ℃; after the solution is cooled, the solution is filtered, solid-liquid separation is carried out, and filter residue is dried at the temperature of 100 ℃. Dissolving 100g of dried filter residue in 400mL of 300g/L Na2SO3In solution, the reaction was carried out at 96 ℃ for 4 hours. And cooling to room temperature, carrying out suction filtration, transferring the filtrate to a round-bottom flask, adding 100g/L sulfuric acid, dropwise adding at the speed of 50mL/min, adjusting the pH of the solution to 3, reacting at 60 ℃ for 3 hours, carrying out suction filtration, and washing with deionized water for 3 times until the pH is neutral to obtain the high-purity selenium powder.
Claims (10)
1. The preparation method of the high-purity selenium powder with uniform particle size distribution is characterized by comprising the steps of pretreatment, main reaction, acid reaction and post-treatment, and specifically comprises the following steps:
A. pretreatment: dissolving raw material crude selenium with acid, stirring and reacting at 30-50 ℃ for 50-70 min, cooling to room temperature, and carrying out solid-liquid separation to obtain filter residue a;
B. main reaction: drying the filter residue a and dissolving the filter residue in Na2SO3Reacting in the solution at 90-100 ℃ for 1-5 h, cooling to room temperature, and carrying out solid-liquid separation to obtain a filtrate b;
C. acid reaction: dropwise adding acid into the filtrate b to react to obtain a material c;
D. and (3) post-treatment: and (4) carrying out solid-liquid separation on the material c, and washing insoluble substances to obtain the high-purity selenium powder with uniform target object particle size distribution.
2. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1, wherein the acid in step A is one or more of sulfuric acid, nitric acid and hydrochloric acid.
3. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1 or 2, wherein the concentration of the acid is 30-100 g/L.
4. The method for preparing high purity selenium powder with uniform particle size distribution as claimed in claim 1, wherein the temperature of acid dissolution in step a is less than 100 ℃.
5. The method for preparing high purity selenium powder with uniform particle size distribution as claimed in claim 1, wherein Na is added in step B2SO3The concentration of the solution is 200-400 g/L.
6. The method for preparing high purity selenium powder with uniform particle size distribution as claimed in claim 1, wherein said acid in step C is sulfuric acid.
7. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1 or 6, wherein the concentration of the acid is 100-300 g/L.
8. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1, wherein the acid reaction time in step C is 1-3 h, and the pH value is controlled to be 1-3.
9. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1, wherein the dropwise addition in the step C is carried out at a constant speed, and the dropwise addition rate is 10-50 ml/min.
10. The method for preparing high-purity selenium powder with uniform particle size distribution according to claim 1, wherein the washing in step D is washing with deionized water for 3-5 times, and the pH value is 6.5-7.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911275840.8A CN110817811A (en) | 2019-12-12 | 2019-12-12 | Preparation method of high-purity selenium powder with uniform particle size distribution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911275840.8A CN110817811A (en) | 2019-12-12 | 2019-12-12 | Preparation method of high-purity selenium powder with uniform particle size distribution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110817811A true CN110817811A (en) | 2020-02-21 |
Family
ID=69545047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911275840.8A Pending CN110817811A (en) | 2019-12-12 | 2019-12-12 | Preparation method of high-purity selenium powder with uniform particle size distribution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110817811A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715859A (en) * | 2022-04-25 | 2022-07-08 | 昆明冶金研究院有限公司 | Method for preparing 3N selenium from selenium slag |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB698228A (en) * | 1951-06-09 | 1953-10-07 | Gold Und Silber Scheideanstale | Production of pure selenium |
| US3966889A (en) * | 1973-07-31 | 1976-06-29 | Asahi Glass Co., Ltd. | Process for the recovery of selenium from waste gas |
| JPS57179004A (en) * | 1981-04-28 | 1982-11-04 | Asahi Glass Co Ltd | Refining method for metallic selenium |
| WO1989012700A1 (en) * | 1988-06-17 | 1989-12-28 | Fmc Technologies Limited | Recovery of high purity selenium from ores, scrubber sludges, anode slime deposits and scrap |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN102363522A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Technology for extracting selenium from low-grade selenium-containing material |
| CN102583264A (en) * | 2012-02-03 | 2012-07-18 | 昆明冶金研究院 | Method for leaching selenium in acid mud by using sodium sulfite |
| CN103723692A (en) * | 2013-12-13 | 2014-04-16 | 金川集团股份有限公司 | Method for separating and extracting selenium from copper smelting wet process dust collection acid mud |
| CN104743526A (en) * | 2015-03-27 | 2015-07-01 | 大冶有色金属有限责任公司 | Refining process of crude selenium |
| CN106853959A (en) * | 2016-09-19 | 2017-06-16 | 三门峡市有色金属质量科学研究所 | A kind of method that use impure selenium wet method prepares high purity selenium |
-
2019
- 2019-12-12 CN CN201911275840.8A patent/CN110817811A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB698228A (en) * | 1951-06-09 | 1953-10-07 | Gold Und Silber Scheideanstale | Production of pure selenium |
| US3966889A (en) * | 1973-07-31 | 1976-06-29 | Asahi Glass Co., Ltd. | Process for the recovery of selenium from waste gas |
| JPS57179004A (en) * | 1981-04-28 | 1982-11-04 | Asahi Glass Co Ltd | Refining method for metallic selenium |
| WO1989012700A1 (en) * | 1988-06-17 | 1989-12-28 | Fmc Technologies Limited | Recovery of high purity selenium from ores, scrubber sludges, anode slime deposits and scrap |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN102363522A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Technology for extracting selenium from low-grade selenium-containing material |
| CN102583264A (en) * | 2012-02-03 | 2012-07-18 | 昆明冶金研究院 | Method for leaching selenium in acid mud by using sodium sulfite |
| CN103723692A (en) * | 2013-12-13 | 2014-04-16 | 金川集团股份有限公司 | Method for separating and extracting selenium from copper smelting wet process dust collection acid mud |
| CN104743526A (en) * | 2015-03-27 | 2015-07-01 | 大冶有色金属有限责任公司 | Refining process of crude selenium |
| CN106853959A (en) * | 2016-09-19 | 2017-06-16 | 三门峡市有色金属质量科学研究所 | A kind of method that use impure selenium wet method prepares high purity selenium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715859A (en) * | 2022-04-25 | 2022-07-08 | 昆明冶金研究院有限公司 | Method for preparing 3N selenium from selenium slag |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792187B (en) | Method for producing feed grade ferrous sulfate monohydrate from titanium pigment waste acid condensed slag | |
| CN108110357A (en) | A kind of method that valuable metal is recycled from positive material of waste lithium iron phosphate | |
| CN113428882B (en) | Method for preparing battery-grade lithium carbonate from spodumene | |
| CN103449517B (en) | Method for preparing white arsenic from arsenic-containing dust in evaporation-free manner | |
| CN102925718B (en) | Composite sodium salt for producing sodium stannate from cassiterite concentrate and application of composite sodium salt | |
| CN102603000A (en) | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material | |
| CN104084598A (en) | Production method for solar cell high-density monodisperse silver powder | |
| CN102923764A (en) | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner | |
| CN101007656A (en) | Waste molybdenum nickel cobalt catalyst utilization method for environmental protection | |
| CN109809440B (en) | Method for preparing high-purity lithium chloride, high-purity lithium formate and high-purity lithium carbonate | |
| CN101708835A (en) | Production method of high-purity zinc phosphate | |
| CN103387266B (en) | Method for direct production of ultra-pure manganese sulfate by non-carbon reduction of manganese dioxide | |
| CN109896546B (en) | Preparation method of ammonium tungsten bronze nanorod | |
| CN104129814B (en) | A kind of method that is raw material production ammonium meta-vanadate with oil hydrogenation spent catalyst | |
| CN110817811A (en) | Preparation method of high-purity selenium powder with uniform particle size distribution | |
| CN108394931B (en) | Method for preparing 3BS (3-beta-butyl benzene) by utilizing acid leaching lead mud | |
| CN107602422B (en) | Preparation method of cleaning type product 1,6, 1,7 mixed clevuric acid | |
| CN110453091B (en) | Method for preparing high-purity cobalt solution from cobalt alloy waste | |
| CN104495803A (en) | Purification method of natural microcrystalline graphite | |
| CN103058162A (en) | Preparation method for electronic grade high-purity copper pyrophosphate | |
| CN102766171B (en) | Modified humic acid and application thereof in reducing roasting by manganese oxide ore pyrogenic method | |
| CN116199270B (en) | Treatment process for reducing wastewater in cobalt oxide production process | |
| CN102153148B (en) | Method for preparing iron oxide red | |
| CN108502911B (en) | Barite purifying and whitening agent and purifying and whitening method thereof | |
| CN114572954B (en) | Method for preparing battery grade ferric phosphate by using pyrite cinder |
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: 20200221 |