CN105460958A - Method for producing elemental mercury and zinc sulfate by using mercury-containing waste catalyst - Google Patents
Method for producing elemental mercury and zinc sulfate by using mercury-containing waste catalyst Download PDFInfo
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- CN105460958A CN105460958A CN201410538315.1A CN201410538315A CN105460958A CN 105460958 A CN105460958 A CN 105460958A CN 201410538315 A CN201410538315 A CN 201410538315A CN 105460958 A CN105460958 A CN 105460958A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for producing elemental mercury and zinc sulfate by using a mercury-containing waste catalyst, and relates to the technical field of three wastes treatment and utilization of organic industrial waste mercury catalysts. The method comprises the following steps: sending a waste mercury catalyst to a sealed distiller, distilling the catalyst, starting a power supply to heat the catalyst to 295-308DEG C in order to make mercury chloride directly sublimate to a gas, and cooling the gas to form liquid mercury chloride; reacting the liquid mercury chloride with a sodium sulfate solution according to a pure mass ratio of 1:0.29-0.85 to generate a mercury sulfate and sodium chloride mixed solution; carrying out sealed pumping filtration to obtain a filter cake mercury sulfate, diluting the filter cake with water, and reacting the diluted filter cake with zinc particles according to a pure mass ratio of 1:0.03-0.51 to generate a zinc sulfate and mercury solution; filtering the zinc sulfate and mercury solution to obtain a filter cake, washing the filter cake, dehydrating the washed filter cake, and packaging the dehydrated filter cake to obtain an elemental mercury product; and carrying out normal pressure distillation on the clarified zinc sulfate solution, cooling the obtained material, crystallizing the cooled material, and packaging the crystallized material to obtain a zinc sulfate crystal product. The method effectively prevents pollution of the waste mercury catalyst to environment, and generates high economic benefits for enterprises.
Description
Technical field
The present invention relates to organic industry to give up the disposal of three wastes of mercury catalyst and the technical field of utilization, particularly relate to a kind of method utilizing mercurous spent catalyst to produce Elemental Mercury and zinc sulfate.
Background technology
In the reaction with acetylene method synthesizing chloroethylene, the industrial Hg chloride content that uses is the high mercury catalyst of 10wt%, due to mercury chloride easy sublimation in reaction is carried out, can work the mischief to environment.People improve at the mercury catalyst of the method for seeking to acetylene method synthesizing chloroethylene, attempt to develop a kind of low mercury or non-mercury catalyst, make it under higher transformation efficiency and selectivity, there is the longer life-span, and the harm of environment is reached minimum, for the industrial applications of later low mercury or non-mercury catalyst is laid a good foundation.Prepared one at transformation efficiency, selectivity or all reasonable catalyzer mercury chloride on work-ing life by practice, its transformation efficiency reaches 97%, and selectivity reaches 98%, and mercury content is lower, belongs to the more promising catalyzer of one.But adopt this mercuric chleride catalyst, in the reaction with acetylene method synthesizing chloroethylene, the quantity discharged of mercurous spent catalyst is that product per ton discharges 0.002 ton, and useless mercury (mercury chloride) content of discharge is 2 ~ 7%;
One, reacted useless mercury not only effectively do not utilize, and can cause secondary pollution;
Two, mercury chloride can be used to produce the product such as Elemental Mercury and other salt, and mercury is generally used in scientific instrument (electro-kinetic instrument, operating device, thermometer, weather gauge) and mercury boiler, mercury air pump and mercury-vapour lamp, and its economic worth is high; The economic worth of the product such as zinc sulfate and sodium-chlor is also higher.
Summary of the invention
The mercurous spent catalyst that the present invention is intended to produce in the reaction to acetylene method synthesizing chloroethylene carries out the comprehensive regulation, provides a kind of method utilizing mercurous spent catalyst to produce Elemental Mercury and zinc sulfate.
For achieving the above object, the technical solution used in the present invention is as follows:
Useless mercury catalyst is obtained Elemental Mercury production zinc sulfate and sodium-chlor through following three steps:
The first step, sends into useless mercury catalyst in sealed distiller and distills, and starts power supply and heats to 295 ~ 308 DEG C and make mercury chloride be directly sublimed into gas, then be cooled to the mercury chloride of liquid;
Second step, reacts mercuric chloride solution obtained above and metabisulfite solution with pure mass ratio 1: 0.29 ~ 0.85, generates Mercury bisulfate and sodium-chlor mixing solutions; Then obtain filter cake Mercury bisulfate through closed suction filtration, react with pure mass ratio 1: 0.03 ~ 0.51 with zinc granule after dilute with water, generate the solution of zinc sulfate and mercury; Filtration obtains filter cake through washing, dewatering, be packaged to be Elemental Mercury product; Clarification solution of zinc sulfate through air distillation, cooling, crystallization, be packaged to be zinc sulfate crystal product;
3rd step, sends to sodium chloride solution obtained above in air distillation device and distills, enter water cooler when distillation temperature reaches sodium chloride saturated solution, obtains sodium chloride crystal product through cooling, crystallization.
Main chemical reactions formula of the present invention is:
HgCl
2+Na
2SO
4＝HgSO
4+2NaCl
HgSO
4+Zn＝ZnSO
4+Hg
Beneficial effect of the present invention is: one, is fully utilized by useless mercury catalyst, effectively prevent the pollution of useless mercury catalyst to sublimity; Its two, the Elemental Mercury produced and zinc chloride product serve many purposes, economic benefits.
Embodiment
Embodiment one
Useless mercury catalyst is obtained Elemental Mercury production zinc sulfate and sodium-chlor through following three steps:
The first step, the mercury catalyst that given up by 500Kg is sent in sealed distiller and is distilled, and starts power supply and heats to 295 ~ 308 DEG C and make mercury chloride be directly sublimed into gas, then be cooled to the mercury chloride of liquid;
Second step, reacts mercuric chloride solution obtained above and metabisulfite solution with pure mass ratio 1: 0.34, generates Mercury bisulfate and sodium-chlor mixing solutions; Then obtain filter cake Mercury bisulfate through closed suction filtration, react with pure mass ratio 1: 0.02 with zinc granule after dilute with water, generate the solution of zinc sulfate and mercury; Filtration obtains filter cake through washing, dewatering, be packaged to be Elemental Mercury product 1.6Kg; Clarification solution of zinc sulfate through air distillation, cooling, crystallization, be packaged to be zinc sulfate crystal product 1.2Kg;
3rd step, sends to sodium chloride solution obtained above in air distillation device and distills, enter water cooler when distillation temperature reaches sodium chloride saturated solution, obtains sodium chloride crystal product 16.5Kg through cooling, crystallization.
Embodiment two
Useless mercury catalyst is obtained Elemental Mercury production zinc sulfate and sodium-chlor through following three steps:
The first step, the mercury catalyst that given up by 500Kg is sent in sealed distiller and is distilled, and starts power supply and heats to 295 ~ 308 DEG C and make mercury chloride be directly sublimed into gas, then be cooled to the mercury chloride of liquid;
Second step, reacts mercuric chloride solution obtained above and metabisulfite solution with pure mass ratio 1: 0.54, generates Mercury bisulfate and sodium-chlor mixing solutions; Then obtain filter cake Mercury bisulfate through closed suction filtration, react with pure mass ratio 1: 0.22 with zinc granule after dilute with water, generate the solution of zinc sulfate and mercury; Filtration obtains filter cake through washing, dewatering, be packaged to be Elemental Mercury product 27.4Kg; Clarification solution of zinc sulfate through air distillation, cooling, crystallization, be packaged to be zinc sulfate crystal product 21.2Kg;
3rd step, sends to sodium chloride solution obtained above in air distillation device and distills, enter water cooler when distillation temperature reaches sodium chloride saturated solution, obtains sodium chloride crystal product 26.1Kg through cooling, crystallization.
Embodiment three
Useless mercury catalyst is obtained Elemental Mercury production zinc sulfate and sodium-chlor through following three steps:
The first step, the mercury catalyst that given up by 500Kg is sent in sealed distiller and is distilled, and starts power supply and heats to 295 ~ 308 DEG C and make mercury chloride be directly sublimed into gas, then be cooled to the mercury chloride of liquid;
Second step, reacts mercuric chloride solution obtained above and metabisulfite solution with pure mass ratio 1: 0.74, generates Mercury bisulfate and sodium-chlor mixing solutions; Then obtain filter cake Mercury bisulfate through closed suction filtration, react with pure mass ratio 1: 0.42 with zinc granule after dilute with water, generate the solution of zinc sulfate and mercury; Filtration obtains filter cake through washing, dewatering, be packaged to be Elemental Mercury product 71.6Kg; Clarification solution of zinc sulfate through air distillation, cooling, crystallization, be packaged to be zinc sulfate crystal product 55.4Kg;
3rd step, sends to sodium chloride solution obtained above in air distillation device and distills, enter water cooler when distillation temperature reaches sodium chloride saturated solution, obtains sodium chloride crystal product 35.8Kg through cooling, crystallization.
The above is only three preferred embodiments of the present invention, is not used for limiting the present invention, and its similar embodiments all, all should be covered by the protection domain of patent of the present invention.
Claims (1)
1. the method utilizing mercurous spent catalyst to produce Elemental Mercury and zinc sulfate, it is characterized in that: useless mercury catalyst is obtained Elemental Mercury production zinc sulfate and sodium-chlor through following three steps: the first step, useless mercury catalyst is sent in sealed distiller and distill, start power supply to heat to 295 ~ 308 DEG C and make mercury chloride be directly sublimed into gas, then be cooled to the mercury chloride of liquid; Second step, reacts mercuric chloride solution obtained above and metabisulfite solution with pure mass ratio 1: 0.29 ~ 0.85, generates Mercury bisulfate and sodium-chlor mixing solutions; Then obtain filter cake Mercury bisulfate through closed suction filtration, react with pure mass ratio 1: 0.03 ~ 0.51 with zinc granule after dilute with water, generate the solution of zinc sulfate and mercury; Filtration obtains filter cake through washing, dewatering, be packaged to be Elemental Mercury product; Clarification solution of zinc sulfate through air distillation, cooling, crystallization, be packaged to be zinc sulfate crystal product; 3rd step, sends to sodium chloride solution obtained above in air distillation device and distills, enter water cooler when distillation temperature reaches sodium chloride saturated solution, obtains sodium chloride crystal product through cooling, crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410538315.1A CN105460958A (en) | 2014-09-24 | 2014-09-24 | Method for producing elemental mercury and zinc sulfate by using mercury-containing waste catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410538315.1A CN105460958A (en) | 2014-09-24 | 2014-09-24 | Method for producing elemental mercury and zinc sulfate by using mercury-containing waste catalyst |
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| CN105460958A true CN105460958A (en) | 2016-04-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111809069A (en) * | 2020-06-30 | 2020-10-23 | 沈阳环境科学研究院 | Method for recovering waste mercury sulfate reagent |
-
2014
- 2014-09-24 CN CN201410538315.1A patent/CN105460958A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111809069A (en) * | 2020-06-30 | 2020-10-23 | 沈阳环境科学研究院 | Method for recovering waste mercury sulfate reagent |
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Application publication date: 20160406 |