CN102092779B - Method for producing high-purity zinc sulfide and co-producing acetic acid and sodium chloride by using sodium hydrosulfite filter residues - Google Patents
Method for producing high-purity zinc sulfide and co-producing acetic acid and sodium chloride by using sodium hydrosulfite filter residues Download PDFInfo
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- CN102092779B CN102092779B CN2010102753676A CN201010275367A CN102092779B CN 102092779 B CN102092779 B CN 102092779B CN 2010102753676 A CN2010102753676 A CN 2010102753676A CN 201010275367 A CN201010275367 A CN 201010275367A CN 102092779 B CN102092779 B CN 102092779B
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Abstract
The invention provides a method for producing high-pure zinc sulfide and co-producing acetic acid and sodium chloride by using sodium hydrosulfite filter residues. The method is as follows: reacting the sodium hydrosulfite filter residues with hydrogen chloride so as to obtain a mixture liquid containing zinc chloride; filtering to obtain a zinc chloride containing solution, a sodium acetate solution and a hydrogen sulfide solution; carrying out a reaction on the zinc chloride-containing solution, sodium acetate solution and hydrogen sulfide solution in a pure substance mass ratio of zinc chloride to sodium acetate to hydrogen sulfide so as to obtain a zinc sulfide-containing precipitate, the mixture of sodium acetate and hydrogen sulfide; filtering the mixture of zinc sulfide-containing precipitate, sodium acetate and hydrogen sulfide to obtain zinc sulfide filter cakes and a solution containing acetic acid and sodium chloride; washing, drying and smashing the zinc sulfide filter cakes so as to obtain a zinc sulfide powder product; carrying out reduced pressure distillation on the solution containing acetic acid and sodium chloride, wherein the acetic acid is evaporated and escaped in a form of acetic acid gas; carrying out condensation rectification to obtain pure high-concentration acetic acid, wherein the residual is a sodium chloride solution after the acetic acid is evaporated and escaped; continuously distilling the sodium chloride solution so as to obtain a saturated or supersaturated sodium chloride solution, cooling so as to precipitate out sodium chloride crystals; and filtering the sodium chloride crystals in the filter to obtain the sodium chloride product.
Description
Technical field
The present invention relates to the technical field of the improvement and the utilization of waste residue, particularly a kind ofly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue.
Background technology
Vat powder is being commonly called as of V-Brite B (Sodium Hydrosulfite), is a kind of strong reductant, is widely used in weaving, printing and dyeing industry; Make dyeing auxiliaries and SYNTHETIC OPTICAL WHITNER; Also be medicine industry simultaneously, the raw material of synthetic dyestuff also is applied to copperplate printing and analytical reagent etc.
In recent years, market is vigorous to the increasing demand of vat powder, growth is very fast.Particularly weaving, printing and dyeing industry grow steadily to the vat powder demand, and 10～15% ascensional range is all arranged every year.In addition, be accompanied by the production exploitation of domestic high-grade newsprinting paper, the raising of kaolin quality, this potential vat powder market slowly highlights, and market potential is also in quick increase.At present, the total consumption of international insurance powder is 500,000 tons/year; China's 07 annual export volume is 8～100,000 tons/year; 08 annual export volume is 12～150,000 tons; 09 annual export volume is near 200,000 tons; Export volume obviously increases, and is maximum in the world vat powder export State.And domestic consumption is greatly about 20～250,000 tons/year.
The working method of vat powder mainly contains zinc powder method, sodium formate method and amalgamation process.At present, it mainly is preceding two kinds for what use in the industry.Wherein, the three wastes of sodium amalgam method production technique are handled and labour protection requires comparatively strictness, and power consumption is higher, in industry, seldom is used.The sodium formate method production technology is ripe, and flow process is brief, and the waste water generation is few, but product purity is lower, less stable; And zinc powder method mature production technology, product purity are high, good stability, are the main working methods of using in the industry.
It is that use purity is the sulfur dioxide gas processing zinc powder aqueous suspension more than 99% that the zinc powder method is produced vat powder; Generate the SODIUM HYDROSULPHITE zinc solution; Add sodium hydroxide then and carry out replacement(metathesis)reaction; Generate V-Brite B and zinc hydroxide deposition, obtain containing V-Brite B after the filtering separation and contain the sedimentary waste residue of zinc hydroxide.Filtrating is saltoutd with strong brine, again through filter, separate, after the dehydration, with washing with alcohol, drying and must V-Brite B.Thereby the production process of vat powder has been discharged the filter cake waste residue that contains zinc hydroxide in a large number through press filtration.The zinc hydroxide waste residue is a kind of strong alkaline substance, piles up the white dust that corrosion and alkaline curing all very seriously, the especially wind in soil are kicked up if do not handle and makes us especially suffocating.At present, commonly used treatment process is for recycling with zinc hydroxide waste residue oxygenerating zinc or metallic zinc.Its purposes is comparatively single, can not consume the increase that is accompanied by the vat powder turnout far away and the zinc powder waste residue that increases day by day.
In addition, zinc sulphide is a kind of two, six important compound semiconductors; Zinc sulfide nano-material is because of its outstanding physical property, and is wide like band gap, high refractive index; High transmission rate is in visible-range; Caused that people pay close attention to greatly, at optics, fields such as electronics and opto-electronic device have great potential.Zinc sulphide has good fluorescent effect and electroluminescent function; Nano-zinc sulfide has more unique photovoltaic effect; Demonstrate the performance of many excellences in fields such as electricity, magnetics, optics, mechanics and catalysis; Therefore the research of nano-zinc sulfide has caused more people's attention, and especially Bhargava in 1994 has reported the nanometer ZnS of handling through surface passivation: Mn fluorescent material at high temperature not only has the external quantum efficiency up to 18%, and its fluorescence lifetime has shortened 5 one magnitude; And luminescent properties had very big variation, and more a new way has been opened up in the application of ZnS in material.Zinc sulphide already can be used for making pigment and glass, luminescent powder, rubber, plastics, the luminous paint of white etc.For this reason, seek new; The working method of zinc sulphide has great economic implications.
Summary of the invention
The objective of the invention is to; Provide a kind of and produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue; This method turns waste into wealth; Effectively the zinc hydroxide in the vat powder filter residue is converted into zinc sulphide and coproduction by acetic acid and the sodium-chlor that has than the large economy meaning, fully excavates and utilized vat powder filter residue potential economic worth, also new approach is provided for the comprehensive utilization of vat powder filter residue and improvement.
Technical scheme of the present invention is following: a kind ofly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue, said vat powder filter residue is produced vat powder gained filter residue for the zinc powder method, comprises following concrete steps,
Steps A: the content of zinc hydroxide in the filter residue of conversion vat powder, and, be configured to suspension liquid with the pulverizing of vat powder filter residue, dispose dilute hydrochloric acid solution simultaneously;
Step B: is 1 with steps A gained suspension liquid and dilute hydrochloric acid solution according to zinc hydroxide and hydrogenchloride pure substance mass ratio: 0.54-0.94 puts in first corrosion-resistant reactor (1) successively, reacts under stirring, and obtains containing the mixed solution of zinc chloride;
Step C: the mixed solution that step B gained is contained zinc chloride filters through first strainer (2), obtains the clarifying filtrating that contains zinc chloride;
Step D: the clarifying filtrating that contains zinc chloride is reacted with an amount of zinc hydroxide in second corrosion-resistant reactor (3), removes impurity, and makes the muriate in the solution all be converted into zinc chloride, filters through second strainer (4) and has obtained purified liquor zinci chloridi;
Step e: be purified liquor zinci chloridi and sodium-acetate and hydrogen sulfide solution 1 according to the ratio of zinc chloride, sodium-acetate and hydrogen sulfide pure substance quality again: 1.01-1.41: 0.05-0.45 together sends into reactor drum (5), and reaction generates the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor under stirring slowly;
Step F: the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor is filtered through the 3rd strainer (6), obtain the zinc sulphide filter cake, contain the solution of acetic acid and sodium-chlor;
Step G: the zinc sulphide filter cake is pulverized through washing machine (7) washing drying, kibbler (8), obtains zinc sulphide powder product (9);
Step H: the solution that contains acetic acid and sodium-chlor is sent into underpressure distillation in the underpressure distillation device (10); Acetic acid is overflowed with the form evaporation of acetic gas; After prolong (11) cooling, obtain aqueous acetic acid, the gained aqueous acetic acid obtains purified height acetic acid (12) through rectifying;
Step I: after acetic acid was overflowed with the form evaporation of acetic gas, the remaining sodium chloride solution that is in the underpressure distillation device (10) continued distillation again and is sodium chloride saturated solution or sodium-chlor supersaturated solution; Cooling; Sodium chloride crystal is separated out, filter, obtain sodium-chlor product (14) through strainer (13).
Of the present inventionly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue, its chemical principle is:
Zn(OH)
2+2HCl＝＝＝＝＝ZnCl
2+H
2O
ZnCl
2+H
2S+2CH
3COONa ZnS+2CH
3COOH+2NaCl
The invention has the beneficial effects as follows: according to the inventionly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue; Effectively the zinc hydroxide in the vat powder filter residue is converted into zinc sulphide and coproduction by acetic acid and the sodium-chlor that has than the large economy meaning; Fully excavate and utilized vat powder filter residue potential economic worth, also new approach is provided for the comprehensive utilization of vat powder filter residue and improvement.Simultaneously, this method is simple to operate, and the facility investment expense is low, and by product is few, is suitable for applying.
Description of drawings
Fig. 1 produces the process flow sheet of high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method for according to the invention with the vat powder filter residue, wherein,
(1)---first corrosion-resistant reactor, (2)---first strainer, (3)---second corrosion-resistant reactor, (4)---second strainer; (5)---reactor drum, (6)---the 3rd strainer, (7)---washing machine, (8)---kibbler; (9)---zinc sulphide powder product, (10)---underpressure distillation device, (11)---prolong; (12)---purified height acetic acid, (13)---strainer, (14)---sodium-chlor product.
Embodiment
Embodiment 1
With reference to Fig. 1; A kind ofly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue, said vat powder filter residue is that the zinc powder method is produced vat powder gained filter residue, weighing 495kg vat powder; The content of zinc hydroxide is 297kg in the filter residue of conversion vat powder; And, be configured to suspension liquid with the pulverizing of vat powder filter residue, dispose dilute hydrochloric acid solution simultaneously; Is successively to put in first corrosion-resistant reactor (1) at 1: 0.74 gained suspension liquid and dilute hydrochloric acid solution according to zinc hydroxide and hydrogenchloride pure substance mass ratio, reacts under stirring, and obtains containing the mixed solution of zinc chloride; The mixed solution that gained is contained zinc chloride filters through first strainer (2), obtains the clarifying filtrating that contains zinc chloride; The clarifying filtrating that contains zinc chloride is reacted with an amount of zinc hydroxide in second corrosion-resistant reactor (3); Remove impurity; And make the muriate in the solution all be converted into zinc chloride; Filter through second strainer (4) and obtained purified liquor zinci chloridi, the pure substance quality of the zinc chloride that it contains is 408kg; Is purified liquor zinci chloridi and sodium-acetate and hydrogen sulfide solution together to send into reactor drum (5) at 1: 1.21: 0.25 according to the ratio of zinc chloride, sodium-acetate and hydrogen sulfide pure substance quality, and reaction generates the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor under stirring slowly; The mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor is filtered through the 3rd strainer (6), obtain zinc sulphide filter cake and the solution that contains acetic acid and sodium-chlor; The zinc sulphide filter cake is pulverized through washing machine (7) washing drying, kibbler (8), obtains zinc sulphide powder product (9), and the zinc sulphide pure substance quality that it contains is 297kg; The solution that contains acetic acid and sodium-chlor is sent into underpressure distillation in the underpressure distillation device (10); Acetic acid is overflowed with the form evaporation of acetic gas; After prolong (11) cooling, obtain aqueous acetic acid; The gained aqueous acetic acid obtains purified height acetic acid (12) through rectifying, and the acetic acid pure substance quality that it contains is 360kg; After acetic acid is overflowed with the form evaporation of acetic gas; The remaining sodium chloride solution that is in the underpressure distillation device (10) continues distillation again and is sodium chloride saturated solution or sodium-chlor supersaturated solution, cooling; Sodium chloride crystal is separated out; Filter through strainer (13), obtain sodium-chlor product (14), the sodium-chlor pure substance quality that it contains is 348kg.
Embodiment 2
With reference to Fig. 1; A kind ofly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue, said vat powder filter residue is that the zinc powder method is produced vat powder gained filter residue, weighing 495kg vat powder; The content of zinc hydroxide is 297kg in the filter residue of conversion vat powder; And, be configured to suspension liquid with the pulverizing of vat powder filter residue, dispose dilute hydrochloric acid solution simultaneously; Is successively to put in first corrosion-resistant reactor (1) at 1: 0.94 gained suspension liquid and dilute hydrochloric acid solution according to zinc hydroxide and hydrogenchloride pure substance mass ratio, reacts under stirring, and obtains containing the mixed solution of zinc chloride; The mixed solution that gained is contained zinc chloride filters through first strainer (2), obtains the clarifying filtrating that contains zinc chloride; The clarifying filtrating that contains zinc chloride is reacted with an amount of zinc hydroxide in second corrosion-resistant reactor (3), removes impurity, and makes the muriate in the solution all be converted into zinc chloride, filters through second strainer (4) and has obtained purified liquor zinci chloridi; Is purified liquor zinci chloridi and sodium-acetate and hydrogen sulfide solution together to send into reactor drum (5) at 1: 1.41: 0.45 according to the ratio of zinc chloride, sodium-acetate and hydrogen sulfide pure substance quality, and reaction generates the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor under stirring slowly; The mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor is filtered through the 3rd strainer (6), obtain zinc sulphide filter cake and the solution that contains acetic acid and sodium-chlor; The zinc sulphide filter cake is pulverized through washing machine (7) washing drying, kibbler (8), obtains zinc sulphide powder product (9), and the zinc sulphide pure substance quality that it contains is 297kg; The solution that contains acetic acid and sodium-chlor is sent into underpressure distillation in the underpressure distillation device (10); Acetic acid is overflowed with the form evaporation of acetic gas; After prolong (11) cooling, obtain aqueous acetic acid; The gained aqueous acetic acid obtains purified height acetic acid (12) through rectifying, and the acetic acid pure substance quality that it contains is 360kg; After acetic acid is overflowed with the form evaporation of acetic gas; The remaining sodium chloride solution that is in the underpressure distillation device (10) continues distillation again and is sodium chloride saturated solution or sodium-chlor supersaturated solution, cooling; Sodium chloride crystal is separated out; Filter through strainer (13), obtain sodium-chlor product (14), the sodium-chlor pure substance quality that it contains is 348kg.
Embodiment 3
With reference to Fig. 1; A kind ofly produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue, said vat powder filter residue is that the zinc powder method is produced vat powder gained filter residue, weighing 495kg vat powder; The content of zinc hydroxide is 297kg in the filter residue of conversion vat powder; And, be configured to suspension liquid with the pulverizing of vat powder filter residue, dispose dilute hydrochloric acid solution simultaneously; Is successively to put in first corrosion-resistant reactor (1) at 1: 0.54 gained suspension liquid and dilute hydrochloric acid solution according to zinc hydroxide and hydrogenchloride pure substance mass ratio, reacts under stirring, and obtains containing the mixed solution of zinc chloride; The mixed solution that gained is contained zinc chloride filters through first strainer (2), obtains the clarifying filtrating that contains zinc chloride; The clarifying filtrating that contains zinc chloride is reacted with an amount of zinc hydroxide in second corrosion-resistant reactor (3); Remove impurity; And make the muriate in the solution all be converted into zinc chloride; Filter through second strainer (4) and obtained purified liquor zinci chloridi, the zinc chloride pure substance quality that it contains is 298.80kg; Is purified liquor zinci chloridi and sodium-acetate and hydrogen sulfide solution together to send into reactor drum (5) at 1: 1.01: 0.05 according to the ratio of zinc chloride, sodium-acetate and hydrogen sulfide pure substance quality, and reaction generates the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor under stirring slowly; The mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor is filtered through the 3rd strainer (6), obtain zinc sulphide filter cake and the solution that contains acetic acid and sodium-chlor; The zinc sulphide filter cake is pulverized through washing machine (7) washing drying, kibbler (8), obtains zinc sulphide powder product (9), and the zinc sulphide pure substance quality that it contains is .42.63kg; The solution that contains acetic acid and sodium-chlor is sent into underpressure distillation in the underpressure distillation device (10); Acetic acid is overflowed with the form evaporation of acetic gas; After prolong (11) cooling, obtain aqueous acetic acid; The gained aqueous acetic acid obtains purified height acetic acid (12) through rectifying, and the acetic acid pure substance quality that it contains is 52.74kg; After acetic acid is overflowed with the form evaporation of acetic gas; The remaining sodium chloride solution that is in the underpressure distillation device (10) continues distillation again and is sodium chloride saturated solution or sodium-chlor supersaturated solution, cooling; Sodium chloride crystal is separated out; Filter through strainer (13), obtain sodium-chlor product (14), the sodium-chlor pure substance quality that it contains is 50.97kg.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries method.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (1)
1. produce high-purity zinc sulphide coproduction by acetic acid and sodium-chlor method with the vat powder filter residue for one kind, said vat powder filter residue is produced vat powder gained filter residue for the zinc powder method, it is characterized in that, comprises following concrete steps,
Steps A: the content of zinc hydroxide in the filter residue of conversion vat powder, and, be configured to suspension liquid with the pulverizing of vat powder filter residue, dispose dilute hydrochloric acid solution simultaneously;
Step B: is 1 with steps A gained suspension liquid and dilute hydrochloric acid solution according to zinc hydroxide and hydrogenchloride pure substance mass ratio: 0.54-0.94 puts in first corrosion-resistant reactor (1) successively, reacts under stirring, and obtains containing the mixed solution of zinc chloride;
Step C: the mixed solution that step B gained is contained zinc chloride filters through first strainer (2), obtains the clarifying filtrating that contains zinc chloride;
Step D: the clarifying filtrating that contains zinc chloride is reacted with an amount of zinc hydroxide in second corrosion-resistant reactor (3), removes impurity, and makes the muriate in the solution all be converted into zinc chloride, filters through second strainer (4) and has obtained purified liquor zinci chloridi;
Step e: be purified liquor zinci chloridi and sodium-acetate and hydrogen sulfide solution 1 according to the ratio of zinc chloride, sodium-acetate and hydrogen sulfide pure substance quality again: 1.01-1.41: 0.05-0.45 together sends into reactor drum (5), and reaction generates the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor under stirring slowly;
Step F: the mixture of Containing Sulfur zinc deposition, acetic acid and sodium-chlor is filtered through the 3rd strainer (6), obtain the zinc sulphide filter cake, contain the solution of acetic acid and sodium-chlor;
Step G: the zinc sulphide filter cake is pulverized through washing machine (7) washing drying, kibbler (8), obtains zinc sulphide powder product (9);
Step H: the solution that contains acetic acid and sodium-chlor is sent into underpressure distillation in the underpressure distillation device (10); Acetic acid is overflowed with the form evaporation of acetic gas; After prolong (11) cooling, obtain aqueous acetic acid, the gained aqueous acetic acid obtains purified height acetic acid (12) through rectifying;
Step I: after acetic acid was overflowed with the form evaporation of acetic gas, the remaining sodium chloride solution that is in the underpressure distillation device (10) continued distillation again and is sodium chloride saturated solution or sodium-chlor supersaturated solution; Cooling; Sodium chloride crystal is separated out, filter, obtain sodium-chlor product (14) through strainer (13).
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| CN2010102753676A CN102092779B (en) | 2010-09-06 | 2010-09-06 | Method for producing high-purity zinc sulfide and co-producing acetic acid and sodium chloride by using sodium hydrosulfite filter residues |
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| CN2010102753676A CN102092779B (en) | 2010-09-06 | 2010-09-06 | Method for producing high-purity zinc sulfide and co-producing acetic acid and sodium chloride by using sodium hydrosulfite filter residues |
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| CN102092779B true CN102092779B (en) | 2012-07-04 |
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| CN110304639B (en) * | 2019-07-10 | 2022-04-08 | 浙江宏达化学制品有限公司 | Purification method of sodium o-sulfonate benzaldehyde byproduct salt |
| CN114262108B (en) * | 2020-09-16 | 2024-03-19 | 上海医药工业研究院 | Treatment method of wastewater containing hydrochloric acid and acetic acid |
| CN113979583B (en) * | 2021-11-04 | 2023-09-22 | 武汉瑞阳化工有限公司 | Treatment method of acid wastewater generated in process of synthesizing 1-fluoronaphthalene |
| CN114230078B (en) * | 2021-12-21 | 2023-09-22 | 武汉瑞阳化工有限公司 | Comprehensive utilization method of acid wastewater generated in production of 1-fluoronaphthalene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107218A (en) * | 1986-10-16 | 1988-04-27 | 广东省汕头大学 | Produce the novel process of zinc oxide by the vat powder filter residue |
| CN1069297A (en) * | 1991-08-02 | 1993-02-24 | 北京矿冶研究总院 | Method for producing zinc powder from zinc-containing material by leaching electrolysis method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107218A (en) * | 1986-10-16 | 1988-04-27 | 广东省汕头大学 | Produce the novel process of zinc oxide by the vat powder filter residue |
| CN1069297A (en) * | 1991-08-02 | 1993-02-24 | 北京矿冶研究总院 | Method for producing zinc powder from zinc-containing material by leaching electrolysis method |
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