CN100390067C - Purification process of high-purity plasma crystal zinc sulphide powder - Google Patents
Purification process of high-purity plasma crystal zinc sulphide powder Download PDFInfo
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- CN100390067C CN100390067C CNB2006100422174A CN200610042217A CN100390067C CN 100390067 C CN100390067 C CN 100390067C CN B2006100422174 A CNB2006100422174 A CN B2006100422174A CN 200610042217 A CN200610042217 A CN 200610042217A CN 100390067 C CN100390067 C CN 100390067C
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Abstract
The present invention discloses a purifying technological method for high-purity plasma crystal zinc sulphide powder. In the technology, domestic fluorescence level zinc sulphide powder is used as a basic raw material; after the basic raw material is sieved, tested and ground, the basic raw material enters a reaction vessel; a neutralization reagent is added to the reaction vessel to remove acid radicals and chlorine radicals; after the basic raw material and the neutralization reagent are washed by water, dehydrated and dried, the mixture enters a reduction furnace to remove oxides and enters a high-temperature oven to lead powder to be crystallized again; the surfaces of particles are flattened, and the specific surface areas of the particles are reduced; at last, the particles are cooled, mixed, sieved and packed at the drying atmosphere, and the high-purity plasma crystal zinc sulphide powder is obtained. The produced high-purity zinc sulphide powder has the advantages of high purity, few contained acid radicals, uniform particles and smooth surface, and generates no waste slag or waste gas in the reaction course; a small amount of waste water is easily treated; the produced high-purity zinc sulphide powder has no pollution to the environment; after trial by users, the produced high-purity zinc sulphide powder can completely reach the technical requirements of model number products and have a wide development perspective in the high-tech field.
Description
Technical field
The present invention relates to a kind of purification process of high-purity plasma crystal zinc sulphide powder, belong to chemical technology field.
Background technology
Usually the zinc sulphide production technique is divided into three kinds, and a kind of is homogeneous precipitation method; Second kind is gas phase and established law; The third is a hydrogen sulfide precipitation method.The difference of technology causes yield and quality different, and impurity is poisoned different with quantity of three wastes, and purposes and development prospect are also different, first kind of homogeneous precipitation method, because complicated operation, reasons such as quality instability and cost height have not re-used; Second kind of gas phase and established law, adopt sulphur and zinc powder in high-temperature kettle, to gasify, under catalyst action the reaction and become highly purified zinc sulphide to be wafer or crystal block shape, the characteristics of this technology are that processing condition are more easy to control, the product purity height, its shortcoming is, single batch yields poorly, and needs high-voltage high-temperature equipment, and cost is higher, product only is applicable to Coating Materials, and purposes is less.Therefore, manufacturer is few both at home and abroad; The third hydrogen sulfide precipitation method, the zinc sulphide of this explained hereafter is the particulate state powder.At present, domestic and international most zinc sulphide all adopts this method to make, the explained hereafter method is as follows: adopting high pure zinc oxide and sulfuric acid is raw material, after zinc oxide dissolves in dilute sulphuric acid, get solution of zinc sulfate, in solution, add refining reagent and remove most of metal ion, feed the stink damp precursor reactant again and obtain the zinc sulphide precipitation, remove byproduct sulfuric acid through washing, get the higher zinc sulphide product of purity after dehydration, the drying then.The zinc sulphide powder outward appearance of this explained hereafter is white or pale yellow powder, purity is higher, can reach 97%, the granularity particle diameter is concentrated relatively, and 3～5um scope particle diameter accounts for 60%, metal ion content is lower, be generally below the 1.0PPm, processing condition are easy to control, need not to become privileged construction equipment, cost is lower, is easy to industrialization production.This end-use is wider, be mainly used in color TV, monochrome television colour picture tube, typotron, the effective fluorescent material of monochrome presentation and photic, electricity causes, electroluminescent material, also can produce crystal simultaneously, cold pressing, the hot pressing Coating Materials.Therefore this explained hereafter is the main zinc sulphide powder production technique that adopts both at home and abroad at present.Though this explained hereafter zinc sulphide purposes is wider, but because hydrolysis in by product sulfuric acid that is produced in the technology and the washing, oxidation in the drying, reason such as particle surface is coarse in the precipitation makes this product in the relevant industry of high-tech, as defence and military, electronic information, the requirement that can not touch the mark of fields such as optical coating, at the demand of above defective and association area, positive more highly purified zinc sulphide powder of development all both at home and abroad.
Abroad when producing high-purity zinc sulphide; the main employing in the secondary sedimentation of fluorescence level zinc sulphide production technique improved reactivity, and neutralisation is removed acid group and refining metal ion, the methods such as gas shield drying removed; improve zinc sulphide purity, reduce acid group content and metal ion content.The zinc sulphide powder purity of this class methods gained can reach 99%, and through after the methods such as reduction dewaters, purity can reach 99.99% again, but the desired equipment precision instrument of this method standard height, adopt gathered the tetrafluoro material more, causes amount of investment big, cost increases, and corresponding selling price improves.At present, the fluorescence level zinc sulphide powder technology of domestic production, it mainly is the technology of introducing from Japan the eighties, the part major equipment adopts daily output equipment, production process route and equipment and external basically identical, quality product is also basic identical, and therefore, the fluorescence level zinc sulphide of being produced can not satisfy the technical requirement of high-tech association area equally.If adopt foreign technology to improve zinc sulphide purity, then must change existing equipment material, increase simultaneously follow-up reduction equipment such as dewater again, since domestic at present also less to the consumption of high purity zinc sulphide, take aforesaid method to drop into substantial contribution and be used for reforming equipment, improve production cost, also improper concerning enterprise, therefore, manufacturing enterprise is to the research and development of high purity zinc sulphide and think little of, and causes the production of domestic high purity zinc sulphide also to belong to blank.
High-purity zinc sulphide of the existing scale production of China is because purity only is 97%, it is higher to contain acid group, reasons such as particle surface is coarse, do not reach in advanced optics and the electron trade specialty products to the technical requirement of material, because domestic understanding to this product is later, it is blank that the development of product also belongs at home, production to the high purity zinc sulphide powder, foreign study exploitation at present concentrates on and further improves purity, improve yield, cut down the consumption of energy, reduce environmental pollution, reduce production costs, improve automatization control and production efficiency.
Summary of the invention
The purification process that the purpose of this invention is to provide a kind of product purity height, contain that acid group is lower, uniform particles and surfacing, production process does not have waste residue waste gas, free of contamination high-purity plasma crystal zinc sulphide powder.
For achieving the above object, technical scheme of the present invention is: the purification process of high-purity plasma crystal zinc sulphide powder, it is characterized in that: described purification process adopts fluorescence level zinc sulphide powder as basic raw material, and described processing method comprises following seven process:
(1) raw material screening
1) by powder shifter the particle of 2～3.5 μ m in the raw material zinc sulphide powder is sifted out and continue to employ;
2) will in the oxidation aluminium pot with behind the agate ball mixed grinding, return in the powder shifter and sieve greater than the particle of 3.5 μ m, and sift out the particle of particle diameter 2～3.5 μ m and continue to employ;
(2) Cl is removed in secondary sedimentation
-And SO
4 2-
1) removes Cl
-: the zinc sulphide powder after the screening is put into reactor, add a certain amount of high-purity deionization hot water and ammonia solution, stir and left standstill 60～120 minutes after 30～90 minutes, upper clear supernate is discharged, add the stirring of deionization hot water again and left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, after above-mentioned several times cleaning, get the wash water sample after the cleaning, with the silver nitrate solution check, this moment contained Cl
-Less than 20ppm;
2) remove SO
4 2-: removing Cl
-After slip in add 1000～2000 liters of the thiourea solutions of certain temperature and concentration, stir and left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, adding the stirring of deionization hot water again left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, after cleaning through several times, get the wash water sample after the cleaning, survey its SO
4 2-Content, contained SO at this moment
4 2-Less than 0.15%, the materials pump is input in the centrifuge then;
(3) dewatered drying
Slip enters water extracter carry out centrifuge dehydration after, send into and carry out drying in the loft drier, adopt steam drying, temperature is 120 ℃, after dry 12 hours, water ratio takes out cooling less than 2.0%;
(4) ammonia catalytic dehydration and deoxygenation
Dried zinc sulphide powder packed into seal in the reduction furnace, feed the reducing gas ammonia, be incubated 60～120 minutes after being heated to 260～800 ℃, stop heating and continue ventilation, after reaching room temperature, the zinc sulphide powder cooling comes out of the stove, acid group is less than 0.1% in the zinc sulphide powder, and oxide compound is less than 0.1%, and water ratio is less than 0.8%;
(5) high temperature solid-state method recrystallization
The zinc sulphide powder powder that reduction furnace is come out of the stove is packed in the protection stove that is placed with sulphur and sealing, feeds hydrogen and protects, and is heated to 600～1200 ℃; at high temperature smoked 80～150 minutes, blowing out, high temperature is come out of the stove; send into next procedure, this process makes specific surface area be reduced to 5.78～10m
2/ g;
(6) dry cooling
The product that high temperature is come out of the stove enters in the environment that accommodates dried nitrogen immediately, carries out reduction protection, and sealing is cooled to room temperature.
(7) batch mixing, sieve powder, packing
In the dried and clean air, the high-purity zinc sulphide powder of many stoves packed into and mix in the mixer, sieve through sub-sieve again, select the zinc sulphide powder powder of 2.5～3.5 μ m particle diameters and after packing, put in storage, promptly obtain high-purity zinc sulphide powder.
Beneficial effect: the present invention adopts above technical scheme, has the following advantages:
(1), the pointed impurity of progressively removing.
1) in raw material, adds a certain amount of ammonia solution, stir after washing, can remove the dechlorination root;
2) remove Cl
-The back adds a certain amount of thiourea solution again in slip, stir after washing, can remove SO
4 2-Removed the unprecipitated heavy metal ion of part simultaneously, as Fe
2+, Ni
2+, Mn
2+Deng, again through dehydration, oven dry.
(2), multiple operation is united purification.
1) employing can be removed O
2-The reducing gas ammonia, in moderate oven, put into powder zinc sulphide, feed ammonia through filtration drying, smoke at a certain temperature, remove oxide compound and moisture;
2) powder of packing in the warm stove feeds nitrogen, at high temperature be incubated certain hour after, specific surface area will decline to a great extent;
3) adopt mechanical means particle diameter is excessive, the later stage product had the particle of considerable influence grinds, sub-sieve;
4) powder contacts with air and can absorb moisture content and oxygen part when high temperature is come out of the stove, and therefore utilizes the gas shield falling temperature method, promptly feeds exsiccant hydrogen in the pyritous powder, makes powder reduce to room temperature, obtains high purity zinc sulphide product.
(3), flow process is for be interrupted producing, and is easy to realize industrialization.
(4), equipment adopts anticorrosion, anti-pollution material to manufacture more.
(5), production environment is required very strict, adopt stage purification to reach standard.Product is extremely tight to dust, metal, nonmetallic impurity content requirement, produces the environment of product and need ask dust content at 100,000/m
2Below, and used water quality is necessary for ionized water, according to environmental requirement, the sewage that produces handled reaches emission standard, thereby reach free of contamination purpose.
(6), environment is not produced pollution.In processing method of the present invention, do not produce waste residue, shielding gas is converted into innocuous gas basically in High Temperature Furnaces Heating Apparatus, therefore also do not have waste gas and produce; Discharge contained SO in the waste water
4 2-, CL
-And the content of neutralization reagent is lower, reaches the pollution exhaust criteria of country after handling through Waste Water Treatment, therefore can not produce environmental pollution aborning.
The processing method that the present invention adopts is compared with traditional processing method, the high purity zinc sulphide powder of being produced, and it is low to have solved fluorescence level zinc sulphide powder purity, acid ion content height, the coarse technical barrier of particle surface has the product purity height, it is lower to contain acid group, uniform particles and surfacing, and do not produce waste residue and waste gas in the reaction, a small amount of waste water is easy to handle, environmentally safe, its purity can reach 99.9%, and acid group is reduced to 0.02%, and specific surface area is reduced to 5.78～10m
2/ g after the user is on probation, can reach the technical requirements of type product fully, and the present invention has vast potential for future development in high-tech area.
Following table is the technical indicator standard of fluorescence level zinc sulphide, two kinds of materials of high purity zinc sulphide:
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Embodiment: as shown in the figure, the purification process of high-purity plasma crystal zinc sulphide powder comprises following seven process altogether:
1, raw material screening
1) by powder shifter the raw material zinc sulphide powder is screened, the particle of particle diameter between 2～3.5 μ m sifts out to be continued to employ;
2) particle diameter is returned in the powder shifter and sieves in the oxidation aluminium pot with behind the agate ball mixed grinding greater than the particle of 3.5 μ m, sift out the particle of particle diameter between 2～3.5 μ m and continue to employ;
(2) Cl is removed in secondary sedimentation
-And SO
4 2-
1) removes Cl
-: the zinc sulphide powder after the screening is put into reactor, add a certain amount of high-purity deionization hot water and ammonia solution, stir and left standstill 60 minutes after 30 minutes, upper clear supernate is discharged, add the stirring of deionization hot water again and left standstill 60 minutes after 30 minutes, discharge upper clear supernate, after cleaning through several times, get the wash water sample after the cleaning, check Cl with silver nitrate solution
-Content, this moment contained Cl
-Less than 20ppm; 2) remove SO
4 2-: removing Cl
-After slip in add 1500 liters of the thiourea solutions of certain temperature and concentration, stirs and left standstill 60 minutes after 30 minutes, the discharge upper clear supernate, add the stirring of deionization hot water again and left standstill 60 minutes after 30 minutes, discharge upper clear supernate, after cleaning through several times, get the wash water sample after the cleaning, survey its SO
4 2-Content, contained SO at this moment
4 2-Less than 0.15%, the materials pump is input in the centrifuge then;
Detected result is as follows:
| Main content | Metal content | SO 4 2-Content | Cl -Content | Water content | Oxide compound | Medium particle diameter (D50) | Specific surface area BET |
| 97.3％ | 1.0ppm | 0.15％ | 20ppm | 2.0％ | 0.45％ | 3.8±1.0μm | 38.3m 2/g |
3 dewatered dryings
Slip enters water extracter carry out centrifuge dehydration after, send into again and carry out drying in the loft drier, adopt steam drying, temperature is 120 ℃, after dry 12 hours, water ratio takes out cooling less than 2.0%;
4, ammonia catalytic dehydration and deoxygenation
Dried zinc sulphide powder packed into to be sealed in the reduction furnace, feeds ammonia and reduces, be heated to 400 ℃ after insulation 60 minutes, stop heating and continue ventilation, come out of the stove after the zinc sulphide powder cooling reaches room temperature, acid group is less than 0.1% in the zinc sulphide powder, oxide compound is less than 0.1%, and water ratio is less than 0.8%;
By test, analysis indexes is as follows:
| Main content | Metal content | SO 4 2-Content | Cl -Content | Water content | Oxide compound | Medium particle diameter (D50) | Specific surface area BET |
| 98.8％ | 1.0ppm | 0.10％ | 20ppm | 0.8％ | 0.1％ | 3.8±1.0μm | 37.0m 2/g |
5, high temperature solid-state method recrystallization
The zinc sulphide powder powder that reduction furnace is come out of the stove is packed in the protection stove that is placed with sulphur and sealing, feeds hydrogen and protects, and is heated to 800 ℃, smoked 80 minutes, and blowing out, high temperature is come out of the stove, and sends into next procedure, and this process makes specific surface area be reduced to 5.78m
2/ g;
Test result is as follows:
| Main content | Metal content | SO 4 2-Content | Cl -Content | Water content | Oxide compound | Medium particle diameter (D50) | Specific surface area BET |
| 99.5％ | 1.0ppm | 0.02％ | 20ppm | 0.1％ | 0.05％ | 3.0±0.5μm | 5.78m 2/g |
6, dry cooling
The product that high temperature is come out of the stove enters in the environment that accommodates dried nitrogen immediately, carries out reduction protection, and sealing is cooled to room temperature;
7, batch mixing, sieve powder, packing
The high-purity zinc sulphide powder that to repeatedly produce in the air of dried and clean is packed into and is mixed in the mixer, sieves through sub-sieve again, selects the zinc sulphide powder powder of 2.5～3.5 μ m particle diameters and puts in storage after packing, and promptly obtains high-purity zinc sulphide powder product.
Claims (1)
1. the purification process of high-purity plasma crystal zinc sulphide powder is characterized in that: described purification process adopts fluorescence level zinc sulphide powder as basic raw material, and described processing method comprises following seven process:
(1) raw material screening
1) by powder shifter the particle of 2～3.5 μ m in the raw material zinc sulphide powder is sifted out and continue to employ;
2) will in the oxidation aluminium pot with behind the agate ball mixed grinding, return in the powder shifter and sieve greater than the particle of 3.5 μ m, and sift out the particle of particle diameter 2～3.5 μ m and continue to employ;
(2) Cl is removed in secondary sedimentation
-And SO
4 2-
1) removes Cl
-: the zinc sulphide powder after the screening is put into reactor, add a certain amount of high-purity deionization hot water and ammonia solution, stir and left standstill 60～120 minutes after 30～90 minutes, upper clear supernate is discharged, add the stirring of deionization hot water again and left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, after above-mentioned several times cleaning, get the wash water sample after the cleaning, with the silver nitrate solution check, this moment contained Cl
-Less than 20ppm;
2) remove SO
4 2-: removing Cl
-After slip in add 1000～2000 liters of the thiourea solutions of certain temperature and concentration, stir and left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, adding the stirring of deionization hot water again left standstill 60～120 minutes after 30～90 minutes, discharge upper clear supernate, after cleaning through several times, get the wash water sample after the cleaning, survey its SO
4 2-Content, contained SO at this moment
4 2-Less than 0.15%, the materials pump is input in the centrifuge then;
(3) dewatered drying
Slip enters water extracter carry out centrifuge dehydration after, send into and carry out drying in the loft drier, adopt steam drying, temperature is 120 ℃, after dry 12 hours, water ratio takes out cooling less than 2.0%;
(4) ammonia catalytic dehydration and deoxygenation
Dried zinc sulphide powder packed into seal in the reduction furnace, feed the reducing gas ammonia, be incubated 60～120 minutes after being heated to 260～800 ℃, stop heating and continue ventilation, after reaching room temperature, the zinc sulphide powder cooling comes out of the stove, acid group is less than 0.1% in the zinc sulphide powder, and oxide compound is less than 0.1%, and water ratio is less than 0.8%;
(5) high temperature solid-state method recrystallization
The zinc sulphide powder powder that reduction furnace is come out of the stove is packed in the protection stove that is placed with sulphur and sealing, feeds hydrogen and protects, and is heated to 600～1200 ℃; at high temperature smoked 80～150 minutes, blowing out, high temperature is come out of the stove; send into next procedure, this process makes specific surface area be reduced to 5.78～10m
2/ g;
(6) dry cooling
The product that high temperature is come out of the stove enters in the environment that accommodates dried nitrogen immediately, carries out reduction protection, and sealing is cooled to room temperature;
(7) batch mixing, sieve powder, packing
In the dried and clean air, the high-purity zinc sulphide powder of many stoves packed into and mix in the mixer, sieve through sub-sieve again, select the zinc sulphide powder powder of 2.5～3.5 μ m particle diameters and after packing, put in storage, promptly obtain high-purity zinc sulphide powder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100422174A CN100390067C (en) | 2006-01-23 | 2006-01-23 | Purification process of high-purity plasma crystal zinc sulphide powder |
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|---|---|---|---|
| CNB2006100422174A CN100390067C (en) | 2006-01-23 | 2006-01-23 | Purification process of high-purity plasma crystal zinc sulphide powder |
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|---|---|
| CN1803626A CN1803626A (en) | 2006-07-19 |
| CN100390067C true CN100390067C (en) | 2008-05-28 |
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|---|---|---|---|
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591102A (en) * | 2015-02-06 | 2015-05-06 | 张家港汇普光学材料有限公司 | Sulfuric acid recovery system for zinc sulfide preparation by optical infrared imaging |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214710A (en) * | 1978-10-20 | 1980-07-29 | United States Borax & Chemical Corporation | Froth flotation of zinc sulfide |
| DE19844546C1 (en) * | 1998-09-29 | 2000-05-18 | Metallgesellschaft Ag | Production of zinc sulfide, useful in hydrometallurgical recovery of zinc, involves filtering and washing precipitate obtained from residual impure zinc sulfate electrolyte and impure sodium sulfide solution from barium sulfate production |
-
2006
- 2006-01-23 CN CNB2006100422174A patent/CN100390067C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214710A (en) * | 1978-10-20 | 1980-07-29 | United States Borax & Chemical Corporation | Froth flotation of zinc sulfide |
| DE19844546C1 (en) * | 1998-09-29 | 2000-05-18 | Metallgesellschaft Ag | Production of zinc sulfide, useful in hydrometallurgical recovery of zinc, involves filtering and washing precipitate obtained from residual impure zinc sulfate electrolyte and impure sodium sulfide solution from barium sulfate production |
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|---|---|
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