CN103288123A - Method of preparing fine zinc sulfide through closed cycle - Google Patents

Method of preparing fine zinc sulfide through closed cycle Download PDF

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Publication number
CN103288123A
CN103288123A CN2013101671704A CN201310167170A CN103288123A CN 103288123 A CN103288123 A CN 103288123A CN 2013101671704 A CN2013101671704 A CN 2013101671704A CN 201310167170 A CN201310167170 A CN 201310167170A CN 103288123 A CN103288123 A CN 103288123A
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solution
znso
zinc sulphide
closed cycle
zinc sulfide
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CN103288123B (en
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陆巧芳
李中义
游贤德
魏宇生
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LUOYANG HONGYUAN CHEMICAL & ENGINEERING CO., LTD.
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LUOYANG SHENGMU METAL MATERIAL Co Ltd
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Abstract

The invention discloses a method of preparing fine zinc sulfide through closed cycle. The method comprises the following steps of: mixing ZnO solid powder with an H2SO4 solution, reacting to obtain a doped ZnSO4 solution, removing impurities from the doped ZnSO4 solution to obtain a pure ZnSO4 solution with impurity content smaller than 0.02%, reacting the pure ZnSO4 solution with a Na2S solution, filter pressing and separating the reaction products to obtain coarse solid zinc sulfide, filter pressing and separating the washed mixed solution of the coarse solid zinc sulfide, drying, roasting and highly crushing the extracted solid zinc sulfide to obtain fine zinc sulfide, mixing the separated out wastewater containing sodium sulfate and zinc sulfide with ZnO solid powder and the H2SO4 solution to realize closed cycle. The method disclosed by the invention is simple in technique, convenient to operate, low in investment cost, free of wastewater and waste gas emission, environment-friendly, capable of saving water resource and high in by-product yield.

Description

A kind of closed cycle prepares the method for meticulous zinc sulphide
Technical field
The invention belongs to the fine chemical technology field, relate to a kind of preparation method of zinc sulphide, especially relate to the method that a kind of closed cycle prepares meticulous zinc sulphide.
Background technology
Zinc sulphide easily disperses, be difficult for reuniting, white for neutrality, and has good optical character, the component of Chang Zuowei thermoset(ting)plastic, thermoplastics, reinforcing fiber glass, fire retardant, synthetic chloroprene rubber and dispersion agent is widely used in semi-conductor, pigment, photo-luminescent devices, solar cell, infrared detector, fiber optics communication etc.
In the prior art, zinc sulphide is produced and preparation adopts zink sulphide purification or hydrogen sulfide to feed the method for zinc solution reaction usually, complex manufacturing, because the oxygenizement in the insufficient and storage process of purification, separation, zinc sulphide powder contains a spot of sulfate radical usually, and the zinc sulphide transformation efficiency is about 50%, transformation efficiency is very low, particle is thick and particle diameter is inhomogeneous, more because hydrogen sulfide has hypertoxicity, makes to have huge potential safety hazard in the production; And " three wastes " quantity discharged is big, and is too serious to the harm that environment causes, and makes to produce to be difficult to development, and output is difficult to increase, and faces very serious sewage handling problem.
Chinese patent CN101205077A discloses a kind of method for preparing barium sulfate and zinc sulphide, and wherein the preparation of zinc sulphide is zinc oxide ZnO and the sulfuric acid H that adopts the zinc-containing ores calcining to make 2SO 4Reaction, reaction solution makes zinc sulfate ZnSO through purifying impurity 4Solution, pure zinc sulfate ZnSO then 4Solution and Sodium Sulphide Na 2The S reaction, reaction product obtains zinc sulphide through the press filtration separation.The zinc sulphide that this method makes is thick product, contains a small amount of sodium sulfate in the product, and purity is low, and price is low, and purposes is single, and is main as the raw material of smelting zinc.
Along with industrial expansion, the purposes of meticulous zinc sulphide in fields such as semi-conductor, pigment, photo-luminescent devices, solar cell, infrared detector, fiber optics communication is increasingly extensive, existing meticulous zinc sulphide can not be met the need of market, therefore, press for a kind of simple and easy to do, environment friendly and pollution-free meticulous zinc sulphide preparation method.
Summary of the invention
For addressing the above problem, the purpose of this invention is to provide the method that a kind of closed cycle prepares meticulous zinc sulphide, its raw materials cost is low, and technology is simple, and is easy to operate, waste water in the production process got back in the original production process reused, and realizes closed cycle.
For achieving the above object, the present invention adopts following technical scheme:
A kind of closed cycle prepares the method for meticulous zinc sulphide, and it may further comprise the steps:
Step 1, with ZnO pressed powder and H 2SO 4Solution mixes and adds in first reactor, wherein ZnO pressed powder and H 2SO 4Solution quality is than being 1:1.5～2.5, H 2SO 4Mass percent concentration is 20～25%, and after reacting 25～35min under 65～75 ℃ of temperature condition, the solution pH value is 5.0～5.5 behind the conditioned reaction, the ZnSO that obtains mixing 4Solution; Then, the ZnSO to mixing 4Solution carries out removal of impurities to be handled, and removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution obtain foreign matter content less than 0.02% pure ZnSO 4Solution;
Step 2, with the pure ZnSO that obtains in the step 1 4Solution and Na 2S solution adds in second reactor, wherein ZnSO 4Solution and Na 2S solution quality ratio is 2～2.5:1, Na 2The S mass percent concentration is 20～25%, and reaction product adopts pressure filter to carry out press filtration separation first time, obtains filter cake moisture and is not more than 30% and Na 2SO 4Content is not more than 5% solids crude zinc sulphide;
Step 3, in rinse bath, clean thick zinc sulphide with clear water, the solution specific gravity control after the cleaning between 0～0.2, Na wherein 2SO 4Content is less than 0.15%;
Mixed solution in step 4, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the solid zinc sulphide that extracts is dry under 100～110 ℃ of conditions of temperature, roast 30～50min under 745～755 ℃ of high temperature, carry out height with micronizer mill again and pulverize, obtaining granularity is the meticulous zinc sulphide products of 1000～1500 purposes;
After mixed solution in step 5, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the liquid that dialysis is come out, the waste water that namely contains quality percentage composition 0.7～1.7% sodium sulfate and quality percentage composition 0.75～0.85% zinc sulphide is sent in first reactor, with ZnO pressed powder and H 2SO 4Solution mixes, and realizes closed cycle.
Chemical equation
ZnO+H 2SO 4→ZnSO 4+H 2O
ZnSO 4+Na 2S→ZnS+Na 2SO 4
Above-mentioned closed cycle prepares in the method for meticulous zinc sulphide, and the ZnO pressed powder is with zinc ore or to contain the zinc waste material be raw material.
Described closed cycle prepares the method for meticulous zinc sulphide, in step 1, to the ZnSO that mixes 4Solution carries out the removal of impurities treatment step, with the ZnSO that mixes 4Solution is put into deblending slot, adds oxygenant H in deblending slot 2O 2Oxidation ZnSO 4Impurity iron in the solution; Again with the ZnSO after the removal of impurities 4Solution is put into displacing device, adds zinc powder, and under 85～95 ℃ of temperature and agitation condition, reaction 30～40min carries out filtering separation, removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution.
Described closed cycle prepares the method for meticulous zinc sulphide, in step 1, to the ZnSO that mixes 4Solution carries out the removal of impurities treatment step and carries out 1～3 time.
Described closed cycle prepares the method for meticulous zinc sulphide, in step 3, cleans thick zinc sulphide several times with 45～55 ℃ of clear water in rinse bath.
Because adopt aforesaid technical scheme, the present invention has following superiority:
This closed cycle prepares the method for meticulous zinc sulphide, its technology is simple, easy to operate, cost of investment is low, the crude zinc oxide materials wide material sources, require not strict to starting material, the waste water that produces in the zinc sulphide production process can be sent into the original production process, continue to utilize, realize no waste water, exhaust gas emission, environmentally friendly, the conserve water resource, byproduct yield height, the meticulous zinc sulphide quality product that the makes requirement that is up to state standards, economic benefit improves 10～20%, has solved waste water in the traditional processing technology, exhaust gas emission problem and waste water reclamation cost height, big drawback consumes energy.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Can be described in further detail the present invention with reference to the process flow sheet among Fig. 1 and following examples; But following examples only are illustrations, and the present invention is not limited to these embodiment.
Embodiment 1
Step 1, in first reactor, add clear water 150ml, under agitation add the 53ml massfraction and be 98% dense H 2SO 4Being mixed with mass percent concentration is 20% rare H 2SO 4Solution adds 50g crude zinc oxide materials (containing ZnO 85%), ZnO pressed powder and H again 2SO 4Solution quality is than being 1:2.25, and behind reaction 32min under 65 ℃ of temperature condition, the solution pH value is 5.0 behind the conditioned reaction, the ZnSO that obtains mixing 4Solution; Then, with the ZnSO that mixes 4Solution is put into deblending slot, adds oxygenant H in deblending slot 2O 2Oxidation ZnSO 4Impurity iron in the solution; Again with the ZnSO after the removal of impurities 4Solution is put into displacing device, adds zinc powder, and under 92 ℃ of temperature and agitation condition, reaction 30min carries out filtering separation, removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution through chemical examination, test, obtain foreign matter content less than 0.02% pure ZnSO 4Solution;
Step 2, with the pure ZnSO that obtains in the step 1 4Solution and 40.7g Na 2S solution adds in second reactor, wherein ZnSO 4Solution and Na 2The S solution quality is than being 2.06:1, Na 2The S mass percent concentration is 20%, and reaction generates ZnS 44.85g, Na 2SO 465.37g reaction product adopts pressure filter to carry out press filtration separation first time, obtains filter cake moisture and be 25% and Na 2SO 4Content is 4% solids crude zinc sulphide;
Step 3, clean thick zinc sulphide 3 times with clear water in rinse bath, the solution proportion after the cleaning is 0.15, wherein Na 2SO 4Content is less than 0.15%;
Mixed solution in step 4, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the solid zinc sulphide that extracts is dry under 100 ℃ of conditions of temperature, roast 50min under 750 ℃ of high temperature, carrying out height with micronizer mill again pulverizes, obtaining granularity is the meticulous zinc sulphide product of 1000～1500 purposes 44.7g, contains Na in the meticulous zinc sulphide 2SO 40.18g;
After mixed solution in step 5, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the liquid that dialysis is come out, the waste water that namely contains 1.5% sodium sulfate, 0.79% zinc sulphide is sent in first reactor, realizes closed cycle.
Embodiment 2
Step 1, in first reactor, add the waste water 150ml contain 1.5% sodium sulfate, 0.79% zinc sulphide, under agitation add the 53ml massfraction and be 98% dense H 2SO 4Being mixed with mass percent concentration is 20% rare H 2SO 4Solution adds 50g crude zinc oxide materials (containing ZnO 85%), ZnO pressed powder and H again 2SO 4Solution quality is than being 1:2.25, and behind reaction 28min under 70 ℃ of temperature condition, the solution pH value is 5.2 behind the conditioned reaction, the ZnSO that obtains mixing 4Solution; Then, with the ZnSO that mixes 4Solution is put into deblending slot, adds oxygenant H in deblending slot 2O 2Oxidation ZnSO 4Impurity iron in the solution; Again with the ZnSO after the removal of impurities 4Solution is put into displacing device, adds zinc powder, and under 85 ℃ of temperature and agitation condition, reaction 35min carries out filtering separation, removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution through chemical examination, test, obtain foreign matter content less than 0.02% pure ZnSO 4Solution;
Step 2, with the pure ZnSO that obtains in the step 1 4Solution and 40.7g Na 2S solution adds in second reactor, wherein ZnSO 4Solution and Na 2The S solution quality is than being 2.06:1, Na 2The S mass percent concentration is 20%, and reaction generates ZnS 44.84g, Na 2SO 475.40g reaction product adopts pressure filter to carry out press filtration separation first time, obtains filter cake moisture and be 25% and Na 2SO 4Content is 5% solids crude zinc sulphide;
Step 3, clean thick zinc sulphide 3 times with clear water in rinse bath, the solution proportion after the cleaning is 0.15, wherein Na 2SO 4Content is less than 0.15%;
Mixed solution in step 4, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the solid zinc sulphide that extracts is dry under 100 ℃ of conditions of temperature, roast 45min under 745 ℃ of high temperature, carrying out height with micronizer mill again pulverizes, obtaining granularity is the meticulous zinc sulphide product of 1000～1500 purposes 44.7g, contains Na in the meticulous zinc sulphide 2SO 40.18g;
After mixed solution in step 5, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the liquid that dialysis is come out, the waste water that namely contains 1.5% sodium sulfate, 0.79% zinc sulphide is sent in first reactor, realizes closed cycle, does not have discharging.
Per-cent among above-mentioned two embodiment refers to is mass percent.

Claims (5)

1. a closed cycle prepares the method for meticulous zinc sulphide, and it is characterized in that: it may further comprise the steps:
Step 1, with ZnO pressed powder and H 2SO 4Solution mixes and adds in first reactor, wherein ZnO pressed powder and H 2SO 4Solution quality is than being 1:1.5～2.5, H 2SO 4Mass percent concentration is 20～25%, and after reacting 25～35min under 65～75 ℃ of temperature condition, the solution pH value is 5.0～5.5 behind the conditioned reaction, the ZnSO that obtains mixing 4Solution; Then, the ZnSO to mixing 4Solution carries out removal of impurities to be handled, and removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution obtain foreign matter content less than 0.02% pure ZnSO 4Solution;
Step 2, with the pure ZnSO that obtains in the step 1 4Solution and Na 2S solution adds in second reactor, wherein ZnSO 4Solution and Na 2S solution quality ratio is 2～2.5:1, Na 2The S mass percent concentration is 20～25%, and reaction product adopts pressure filter to carry out press filtration separation first time, obtains filter cake moisture and is not more than 30% and Na 2SO 4Content is not more than 5% solids crude zinc sulphide;
Step 3, in rinse bath, clean thick zinc sulphide with clear water, the solution specific gravity control after the cleaning between 0～0.2, Na wherein 2SO 4Content is less than 0.15%;
Mixed solution in step 4, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the solid zinc sulphide that extracts is dry under 100～110 ℃ of conditions of temperature, roast 30～50min under 745～755 ℃ of high temperature, carry out height with micronizer mill again and pulverize, obtaining granularity is the meticulous zinc sulphide products of 1000～1500 purposes;
After mixed solution in step 5, the rinse bath adopts pressure filter to carry out the press filtration separation second time, the liquid that dialysis is come out, the waste water that namely contains quality percentage composition 0.7～1.7% sodium sulfate and quality percentage composition 0.75～0.85% zinc sulphide is sent in first reactor, with ZnO pressed powder and H 2SO 4Solution mixes, and realizes closed cycle.
2. closed cycle according to claim 1 prepares the method for meticulous zinc sulphide, it is characterized in that: the ZnO pressed powder is with zinc ore or to contain the zinc waste material be raw material.
3. closed cycle according to claim 1 prepares the method for meticulous zinc sulphide, it is characterized in that: in step 1, to the ZnSO that mixes 4Solution carries out the removal of impurities treatment step, with the ZnSO that mixes 4Solution is put into deblending slot, adds oxygenant H in deblending slot 2O 2Oxidation ZnSO 4Impurity iron in the solution; Again with the ZnSO after the removal of impurities 4Solution is put into displacing device, adds zinc powder, and under 85～95 ℃ of temperature and agitation condition, reaction 30～40min carries out filtering separation, removes ZnSO 4Impurity nickel, molybdenum, chromium, copper, lead and iron in the solution.
4. closed cycle according to claim 1 prepares the method for meticulous zinc sulphide, it is characterized in that: in step 1, to the ZnSO that mixes 4Solution carries out the removal of impurities treatment step and carries out 1～3 time.
5. closed cycle according to claim 1 prepares the method for meticulous zinc sulphide, it is characterized in that: in step 3, clean thick zinc sulphide several times with 45～55 ℃ of clear water in rinse bath.
CN201310167170.4A 2013-05-08 2013-05-08 Method of preparing fine zinc sulfide through closed cycle Expired - Fee Related CN103288123B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103964491A (en) * 2014-05-05 2014-08-06 潍坊大耀新材料有限公司 Method for preparing high-purity submicron ZnS powder
CN104003435A (en) * 2014-06-05 2014-08-27 张家港汇普光学材料有限公司 Method for reducing iron ion content in zinc sulfide
CN114314640A (en) * 2021-12-02 2022-04-12 广东鑫达新材料科技有限公司 Preparation method of zinc sulfide
EP3988503A1 (en) 2020-10-22 2022-04-27 Venator Germany GmbH Method for preparing zinc sulfide
CN116081680A (en) * 2023-03-01 2023-05-09 广西象州汇智纳米科技有限公司 Method for preparing pigment grade zinc sulfide by using byproduct sodium sulfide solution

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817518A (en) * 2006-03-10 2006-08-16 同济大学 Production of metal zinc powder from zinc dust and zinc dross
CN101205077A (en) * 2006-12-22 2008-06-25 洛阳市宏源钡盐化工研究所 Method for preparing barium sulfate and zinc sulfide
JP2010510953A (en) * 2006-12-01 2010-04-08 ザッハトレーベン ヒェミー ゲゼルシヤフト ミット ベシュレンクテル ハフツング Transparent zinc sulfide with high specific surface area
CN101798107A (en) * 2010-04-08 2010-08-11 洛阳师范学院 Method for preparing Q-state zinc sulfide nanoparticles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817518A (en) * 2006-03-10 2006-08-16 同济大学 Production of metal zinc powder from zinc dust and zinc dross
JP2010510953A (en) * 2006-12-01 2010-04-08 ザッハトレーベン ヒェミー ゲゼルシヤフト ミット ベシュレンクテル ハフツング Transparent zinc sulfide with high specific surface area
CN101205077A (en) * 2006-12-22 2008-06-25 洛阳市宏源钡盐化工研究所 Method for preparing barium sulfate and zinc sulfide
CN101798107A (en) * 2010-04-08 2010-08-11 洛阳师范学院 Method for preparing Q-state zinc sulfide nanoparticles

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103964491A (en) * 2014-05-05 2014-08-06 潍坊大耀新材料有限公司 Method for preparing high-purity submicron ZnS powder
CN104003435A (en) * 2014-06-05 2014-08-27 张家港汇普光学材料有限公司 Method for reducing iron ion content in zinc sulfide
CN104003435B (en) * 2014-06-05 2015-12-30 张家港汇普光学材料有限公司 A kind of method reducing iron ion content in zinc sulphide
EP3988503A1 (en) 2020-10-22 2022-04-27 Venator Germany GmbH Method for preparing zinc sulfide
WO2022083997A1 (en) 2020-10-22 2022-04-28 Venator Germany Gmbh Method for preparing zinc sulfide
CN114314640A (en) * 2021-12-02 2022-04-12 广东鑫达新材料科技有限公司 Preparation method of zinc sulfide
CN116081680A (en) * 2023-03-01 2023-05-09 广西象州汇智纳米科技有限公司 Method for preparing pigment grade zinc sulfide by using byproduct sodium sulfide solution

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