CN109019669A - A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature - Google Patents
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature Download PDFInfo
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- CN109019669A CN109019669A CN201811057474.4A CN201811057474A CN109019669A CN 109019669 A CN109019669 A CN 109019669A CN 201811057474 A CN201811057474 A CN 201811057474A CN 109019669 A CN109019669 A CN 109019669A
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- waste liquor
- zinc sulphide
- desulfurization waste
- room temperature
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The present invention relates to zinc sulphide preparation fields, specifically disclose a kind of method for preparing zinc sulphide using improved desulfurization waste liquor room temperature, and this method is raw material using coking of coal coal gas, through supercooling, are passed through desulfurizing tower, spray ammonium hydroxide, obtain improved desulfurization waste liquor.It after concentration, imports in reactor tank, soluble zinc salt is added, obtains zinc sulphide after stirring, centrifugation, filtering, drying.The present invention does not need that catalyst is added using the method that improved desulfurization waste liquor room temperature prepares zinc sulphide, saves the spending of enterprise's purchase catalyst；And the hydrogen sulfide in coal gas is directly converted the sulphion for the divalent that is negative and the sulphur hydrogen radical ion of negative one valence by the present invention, it can avoid the generation of other sulfur-bearing secondary salts, to simplify the later period to the correlation step of desulfurization waste liquor salt extraction, while alleviating corrosion of the doctor solution for pipeline in pipeline.
Description
Technical field
It is specifically a kind of to prepare zinc sulphide using improved desulfurization waste liquor room temperature the present invention relates to zinc sulphide preparation field
Method.
Background technique
Coking of coal enterprise is in the selection of sulfur method at present, can be divided into two kinds: dry desulfurization and wet desulphurization.Dry method is de-
Sulphur is mainly used in small-sized coke-oven plant or other need the place of deep desulfuration.Wet desulphurization includes monoethanolamine method, ammonia sulphur
Joint washing method, vacuum potassium carbonate method, HPF method, PDS and rubber method, modified ADA method etc. have the advantages such as treating capacity is big, application
Most wide is HPF method.Hydrogen sulfide (H in coking of coal coal gas2S) content of gas reaches 4-10g/m3, stink damp, which is known from experience, corrodes coal
Gas cleaning equipment and storage conveying equipment.After HPF method absorbs coal gas with doctor solution, concentrated ammonia liquor and catalyst are added, later
It is passed through compressed air, sulphur is produced by regenerator, sulfur melting kettle etc. later, doctor solution recycles after regenerator.But with
The progress of reaction, generate a large amount of secondary salts in doctor solution.Correlative study shows the secondary salt meeting corrosion pipeline of higher concentration, simultaneously
Reduce desulfuration efficiency.It takes the enterprise of HPF method desulfurization to need certain interval of time that corresponding catalyst is added at present, therefore increases
The spending of enterprise's purchase catalyst.
Zinc sulphide is a kind of very important direct band-gap semicondictor, has maximum forbidden band in II-VI compounds of group
Width, it has the function of excellent fluorescent effect and electroluminescent, is widely used in luminous, Flied emission, fuel cell, too
Sun can convert, the degradation of organic matter, nonlinear optical device and light emitting diode etc., moreover it is possible to release from methanol solution
Hydrogen has potential value to the development and application of hydrogen energy source, also has in optical material, catalyst, electronic controller etc. wide
General application prospect.Due to its ir transmissivity with higher, can be used as infra-red material window, kinescope anti-reflection coating and
Light phase modulation etc., while being also commonly used for luminescence generated by light and electroluminescent material.As photochemical catalyst, labyrinth
Nano material, especially three-dimensional structure possess biggish specific surface area and preferable Surface Permeability, are easily achieved high energy
Transfer efficiency and big light-gathering ability, there is good application prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing zinc sulphide using improved desulfurization waste liquor room temperature, to solve
The problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme:
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；
(3) mixture a is stirred, centrifugal treating, obtains mixture b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 70-110 DEG C to get zinc sulphide is arrived.
As a further solution of the present invention: in step (1), the mass concentration of ammonium hydroxide is 3-17%.
As a further solution of the present invention: in step (2), the soluble zinc salt is zinc sulfate, zinc nitrate or second
Sour zinc.
As a further solution of the present invention: in step (2), the purity 399.0% of the soluble zinc salt.
As a further solution of the present invention: in step (2), the mass ratio of improved desulfurization waste liquor and soluble zinc salt is
1:0.001-0.01。
As a further solution of the present invention: in step (3), mixing time 1-2h, mixing speed 100-500r/
min。
As a further solution of the present invention: step (5) dries zinc sulphide sample under the conditions of 90 DEG C to get arriving
Zinc sulphide.
Compared with prior art, the beneficial effects of the present invention are:
1. the present invention does not need that catalyst is added using the method that improved desulfurization waste liquor room temperature prepares zinc sulphide, enterprise is saved
The spending for buying catalyst can effectively solve to take HPF method desulfurization that certain interval of time addition catalyst is needed to cause to pay wages
Larger problem.
2. the present invention directly by coal gas hydrogen sulfide conversion be negative divalent sulphion and negative one valence sulphur hydrogen radical from
Son can avoid the generation of other sulfur-bearing secondary salts, to simplify the later period to the correlation step of desulfurization waste liquor salt extraction, while alleviate pipe
Corrosion of the doctor solution for pipeline in road can solve current desulfurization waste liquor and prepare that zinc sulphide processing step is complicated, takes off in pipeline
Sulphur liquid for pipeline seriously corroded the problem of.
Detailed description of the invention
Fig. 1 is the XRD spectrum of zinc sulphide prepared by the embodiment of the present invention 3.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 3%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc sulfate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.001；
(3) mixture a is stirred, centrifugal treating, mixing time 1h, mixing speed 100r/min obtains mixture
b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 70 DEG C to get zinc sulphide is arrived.
Embodiment 2
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 17%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc nitrate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.01；
(3) mixture a is stirred, centrifugal treating, mixing time 2h, mixing speed 500r/min obtains mixture
b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 110 DEG C to get zinc sulphide is arrived.
Embodiment 3
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 10%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc acetate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.005；
(3) mixture a is stirred, centrifugal treating, mixing time 1.5h, mixing speed 250r/min is mixed
Object b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 90 DEG C to get zinc sulphide is arrived.
Embodiment 4
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 5%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc sulfate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.002；
(3) mixture a is stirred, centrifugal treating, mixing time 1.2h, mixing speed 150r/min is mixed
Object b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 80 DEG C to get zinc sulphide is arrived.
Embodiment 5
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 8%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc nitrate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.007；
(3) mixture a is stirred, centrifugal treating, mixing time 1.7h, mixing speed 350r/min is mixed
Object b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 100 DEG C to get zinc sulphide is arrived.
Embodiment 6
A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature, comprising the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；The mass concentration of ammonium hydroxide is 12%；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；The soluble zinc salt is zinc acetate.The purity 399.0% of the soluble zinc salt.Improved desulfurization waste liquor with
The mass ratio of soluble zinc salt is 1:0.004；
(3) mixture a is stirred, centrifugal treating, mixing time 1.6h, mixing speed 420r/min is mixed
Object b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 102 DEG C to get zinc sulphide is arrived.
Experimental example
The zinc sulphide that embodiment 3 is prepared is tested by powder x-ray diffraction (XRD), and XRD spectrum is shown in Fig. 1, it was demonstrated that real
It applies the zinc sulphide that example 3 is prepared and is free of other impurities.
It should be strongly noted that innovative point of the invention is: not needing that catalyst is added, save enterprise and buy catalyst
Spending；Hydrogen sulfide in coal gas is directly converted to the sulphion for the divalent that is negative and the sulphur hydrogen radical ion of negative one valence, is avoided
The generation of other sulfur-bearing secondary salts simplifies the later period to the correlation step of desulfurization waste liquor salt extraction, mitigates in pipeline doctor solution for pipeline
Corrosion.It can effectively solve that the enterprise of HPF method desulfurization is taken to need certain interval of time that corresponding catalyst is added at present, increase
The problem of having added the spending of enterprise's purchase catalyst, can also solve current desulfurization waste liquor and prepare zinc sulphide processing step complexity, pipe
In road doctor solution for pipeline seriously corroded the problem of.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (7)
1. a kind of method for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which comprises the following steps:
(1) coking of coal coal gas is passed through desulfurization tower bottom after cooling tower cooler, ammonium hydroxide is passed through under desulfurizing tower top spray
Come, obtains improved desulfurization waste liquor；
(2) improved desulfurization waste liquor is passed through in reactor tank, and a certain amount of soluble zinc salt is added, mixed after mixing
Close object a；
(3) mixture a is stirred, centrifugal treating, obtains mixture b；
(4) mixture b is filtered processing, obtains zinc sulphide sample；
(5) zinc sulphide sample is dried under the conditions of 70-110 DEG C to get zinc sulphide is arrived.
2. the method according to claim 1 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which is characterized in that step
Suddenly in (1), the mass concentration of ammonium hydroxide is 3-17%.
3. the method according to claim 1 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which is characterized in that step
Suddenly in (2), the soluble zinc salt is zinc sulfate, zinc nitrate or zinc acetate.
4. the method according to claim 3 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which is characterized in that step
Suddenly in (2), the purity 399.0% of the soluble zinc salt.
5. the method according to claim 1 to 4 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, feature
It is, in step (2), the mass ratio of improved desulfurization waste liquor and soluble zinc salt is 1:0.001-0.01.
6. the method according to claim 5 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which is characterized in that step
Suddenly in (3), mixing time 1-2h, mixing speed 100-500r/min.
7. the method according to claim 6 for preparing zinc sulphide using improved desulfurization waste liquor room temperature, which is characterized in that step
Suddenly (5) dry zinc sulphide sample under the conditions of 90 DEG C to get zinc sulphide is arrived.
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| CN201811057474.4A CN109019669A (en) | 2018-09-11 | 2018-09-11 | A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature |
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| CN201811057474.4A CN109019669A (en) | 2018-09-11 | 2018-09-11 | A method of zinc sulphide is prepared using improved desulfurization waste liquor room temperature |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB347799A (en) * | 1930-02-24 | 1931-05-07 | St Joseph Lead Co | Process for making zinc sulphide |
| CN1821082A (en) * | 2006-03-07 | 2006-08-23 | 上海大学 | Process for preparing nano zinc sulfide |
| CN104402040A (en) * | 2014-11-18 | 2015-03-11 | 辽宁石化职业技术学院 | Preparation method of high-purity zinc sulfide |
| CN104479762A (en) * | 2014-11-26 | 2015-04-01 | 北京首钢国际工程技术有限公司 | Coke oven gas desulfuration alkali washing process |
| CN107500342A (en) * | 2017-09-22 | 2017-12-22 | 昌吉学院 | A kind of method that zinc sulphide is prepared using coking of coal desulfurization waste liquor |
-
2018
- 2018-09-11 CN CN201811057474.4A patent/CN109019669A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB347799A (en) * | 1930-02-24 | 1931-05-07 | St Joseph Lead Co | Process for making zinc sulphide |
| CN1821082A (en) * | 2006-03-07 | 2006-08-23 | 上海大学 | Process for preparing nano zinc sulfide |
| CN104402040A (en) * | 2014-11-18 | 2015-03-11 | 辽宁石化职业技术学院 | Preparation method of high-purity zinc sulfide |
| CN104479762A (en) * | 2014-11-26 | 2015-04-01 | 北京首钢国际工程技术有限公司 | Coke oven gas desulfuration alkali washing process |
| CN107500342A (en) * | 2017-09-22 | 2017-12-22 | 昌吉学院 | A kind of method that zinc sulphide is prepared using coking of coal desulfurization waste liquor |
Non-Patent Citations (1)
| Title |
|---|
| 王永刚等主编: "《煤化工工艺学》", 30 September 2014, 中国矿业大学出版社 * |
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