CN108793235A - A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid - Google Patents
A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid Download PDFInfo
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- CN108793235A CN108793235A CN201811102948.2A CN201811102948A CN108793235A CN 108793235 A CN108793235 A CN 108793235A CN 201811102948 A CN201811102948 A CN 201811102948A CN 108793235 A CN108793235 A CN 108793235A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to a kind of methods preparing vulcanized lead using ammonia process of desulfurization waste liquid, this method is by raw material desulfurization waste liquor and lead acetate through filtering, the functionalization vulcanized lead product for stirring, heating, refiltering, obtaining high added value, this method can obtain the vulcanization lead material of different-shape by different control conditions, can finally turn waste into wealth.The vulcanized lead powder that the method obtains through the invention can be used for luminescent material, anti-fake material, Coating Materials, electroluminescent powder, nonlinear optical material, photoelectric conversion material etc. raw material, in photoelectric field, commonly used in the exploitation of photodetector material, Nano lead sulfide illuminator has the characteristics such as response is fast, can work at room temperature.This method saving cost, simple for process, the period is short, environmental-friendly, low energy consumption, production efficiency is high, raw material sources enrich, are easy to industrialization.
Description
Technical field:
The present invention relates to one kind using desulfurization waste liquor, lead acetate as starting material, by filtering, stirring, heats, refilters
A series of flows prepare vulcanized lead.
Background technology:
China is one using coal as the country of main energy sources, with the rapid development of industry, the SO that coal burning generates2
Have become the major pollutants of In The Atmosphere Over China pollution.From 2002, China carried out large-scale SO in power industry2It administers
Engineering.With the beginning that power plant desulfurization is administered, large quantities of foreign countries' flue gas desulfurization techniques are introduced into the country by different desulfurization companies,
Mostly limestone-gypsum method among these.With the large-scale use of flue gas desulfurization coal industry at home, other cigarettes
Desulfurization method is also gradually used, is realized, including seawater method, ammonia process, magnesium processes, Dual alkali etc., among these, ammonia process just by
More and more extensive concern.Ammonia flue gas desulfurization technique is the SO done using ammonia in absorbent removing flue gas2Technique.The seventies
Just, Japan starts to develop ammonia desulfurizing process and succeed in succession with states such as Italy.But due to Technological Economy etc.
Reason is applied less in the world.Into after the nineties, with advances in technology and the transformation to ammonia process of desulfurization idea, amino are de-
The application of sulphur technology is in the trend gradually risen.
Currently, the most of coking coal chemical industry enterprises in Xinjiang region take wet method ammonia desulfurizing process technology.In desulfurization
Cheng Dangzhong, after salt content reaches certain value, desulfuration efficiency substantially reduces, and doctor solution becomes desulfurization waste liquor.At this point, enterprise needs to add
Desulfurization can just be continued by entering new ammonia source and discharging partial desulfurization waste liquid.Using the above method, the desulfurization waste liquor of coal chemical enterprise does not have
Deep exploitation is obtained, many coal chemical enterprises are sprayed at water on dump as coal blending.Although this method solves desulfurization
The place to go of waste liquid, surface seems that waste liquid discharge is less, but does not tackle the problem at its root actually.Cause environment secondary
Pollution wastes the raw material of industry, increases enterprise's production cost.The invention of desulfurization waste liquor recycling treatment technology is reaching section
While energy emission reduction, moreover it is possible to the sulphur in desulfurization waste liquor be carried out recycling, can be that domestic enterprise bring preferable economy to imitate
Benefit.
Specifically, the principal element for influencing the removing of coal chemical industry enterprises exhaust gas is two kinds of ammonium thiocyanate, ATS (Ammonium thiosulphate) salt
Content is more than 250mg/L or more in doctor solution, and coal chemical industry enterprises generally take recrystallization extraction secondary salt at present, and will extraction
Desulfurization waste liquor after secondary salt, which is sprayed on dump, to be recycled, and the secondary salt added value that can be extracted in this way is low, in former doctor solution
Sulfide content reduced by only 30%, cannot reach the requirement of enterprise.And the present invention is handled desulfurization waste liquor and is sent out using hydrothermal synthesis
Method can not only prepare the high zinc sulfide powder of added value, but also former doctor solution sulfide content is made about to reduce 60%, can
It is continued cycling through as doctor solution and utilizes progress secondary desulfuration.Circular economy production, environmental protection life may be implemented in coal chemical industry enterprises in this way
Production can also be that enterprise brings economic benefit.
For vulcanized lead powder body material, in order to reduce its production cost.The present invention uses the preparation with industrialization potential
Technique, the theory to turn waste into wealth have been prepared with blocky and flower-shaped powder body material.The material is to prepare luminescent material, the sun
It can utilize and the good matrix of environment protection type energy storage material, infrared detector material, there is wide application prospect in recent years.
Invention content
Present invention aims at provide a kind of method preparing vulcanized lead using ammonia process of desulfurization waste liquid, this method is by former material
Expect desulfurization waste liquor and lead acetate Pb (CH3COO)2·3H2O through filtering, the flows such as stirring, heat, refilter and be made, by this hair
The vulcanized lead powder that bright the method obtains is for luminescent material, anti-fake material, Coating Materials, electroluminescent powder, nonlinear optical
Material, photoelectric conversion material etc. raw material are learned, in photoelectric field, is commonly used in the exploitation of photodetector material, nano-sulfur
Change lead illuminator and has the characteristics such as response is fast, can work at room temperature.In photocatalysis field, photohole, quantum can be generated
Dimensional effect, causing energy level change, energy gap to broaden makes the enhancing of its redox ability, for a kind of catalysis material, has
Excellent photocatalytic semiconductor characteristic.PbS quantum application field is more extensive, especially in biomarker and diagnosis, shines two
In terms of pole pipe, laser, infrared detector, ion selectivity sensor and single electron diode.
A kind of method preparing vulcanized lead using ammonia process sulphur waste liquid of the present invention, follows these steps to carry out:
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after continuing and stirring 10min, are used
Ammonium hydroxide adjusts the pH of solution between 4-7;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
12h-16h is kept the temperature after to 80 DEG C -160 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture after obtaining step d is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 4h-6h at 105 DEG C of temperature obtains the vulcanized lead of different-shape
Powder.
Solution ph in step c is adjusted to 4 or 7, generates the sample of different-shape.
A kind of method preparing vulcanized lead using ammonia process of desulfurization waste liquid of the present invention, this method is given up by desulfurization of raw material
Liquid and lead acetate Pb (CH3COO)2·3H2O through filtering, the flows such as stirring, heat, refilter and be made, chemical formula PbS, wherein
Desulfurization waste liquor (mL):Lead acetate (g)=1:0.01098.
A kind of method preparing vulcanized lead using ammonia process of desulfurization waste liquid of the present invention, compared with prior art, essence
Property feature is:
1) it is method that sulphur source prepares vulcanized lead to realize for the first time with coal chemical industry enterprises desulfurization waste liquor;
2) the desulfurization waste liquor secondary pollution of coking of coal enterprise is solved the problems, such as, preparing for PbS powder is more environmentally-friendly, low cost,
It is simple for process, provide possibility for coking of coal enterprise Green environmental protection production;
3) for coking of coal enterprise, to illustrate for producing the coke-oven plant of 1,000,000 tons of coke per year, the desulfurization generated daily is useless
Liquid measure is 30-40 tons, annual to generate 3,000,000-400 ten thousand tons of desulfurization waste liquor, and year processing desulfurization waste liquor at least needs 900,000 yuan.And this hair
The method that bright coking of coal desulfurization waste liquor prepares vulcanized lead meets this demand of coking of coal enterprise market, not only can be by supernatant
Liquid recycles, and can prepare high value added product vulcanized lead.
Description of the drawings
Fig. 1 is material X-ray diffraction spectrogram of the present invention, PbS materials when wherein a is pH=7, PbS when b is pH=4
Material;
Fig. 2 is the X-ray energy spectrogram of the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of material of the present invention, and wherein a is block-like PbS materials (pH=7), and b is flower-shaped PbS
Material (pH=4).
Specific implementation mode:
Embodiment 1
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 7 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
12h is kept the temperature after to 160 DEG C, then cooled to room temperature, obtained mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 4h at 105 DEG C of temperature obtains the sulphur of 0.419g bulk morphologies
Change lead powder body.
Embodiment 2
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 7 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
16h is kept the temperature after to 140 DEG C, then cooled to room temperature, obtained mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 5h at 105 DEG C of temperature obtains the sulphur of 0.420g bulk morphologies
Change lead powder body.
Embodiment 3
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 6 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
13h is kept the temperature after to 120 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, the dry 6h at 105 DEG C of temperature, obtains that 0.415g is existing blocky to be had again
The vulcanized lead powder of floriform appearance.
Embodiment 4
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 5 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
14h is kept the temperature after to 100 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, the dry 6h at 105 DEG C of temperature, obtains that 0.390g is existing blocky to be had again
The vulcanized lead powder of floriform appearance.
Embodiment 5
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 7 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
15h is kept the temperature after to 80 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 5h at 105 DEG C of temperature obtains the sulphur of 0.391g bulk morphologies
Change lead powder body.
Embodiment 6
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 4 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
12h-16h is kept the temperature after to 160 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 4h at 105 DEG C of temperature obtains the sulphur of 0.417g floriform appearances
Change lead powder body.
Embodiment 7
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 4 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
12h is kept the temperature after to 140 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 4h at 105 DEG C of temperature obtains the sulphur of 0.421g floriform appearances
Change lead powder body.
Embodiment 8
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 5 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
13h is kept the temperature after to 120 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, the dry 5h at 105 DEG C of temperature, obtains that 0.410g is existing blocky to be had again
The vulcanized lead powder of floriform appearance.
Embodiment 9
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 6 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
14h is kept the temperature after to 100 DEG C, then cooled to room temperature, obtains mixture;
E, the solidliquid mixture after step d reactions is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, the dry 6h at 105 DEG C of temperature, obtains that 0.415g is existing blocky to be had again
The vulcanized lead powder of floriform appearance.
Embodiment 10
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, after persistently stirring 10min, use ammonia
The pH value of solution is adjusted to 4 by water;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80%, heating
16h is kept the temperature after to 80 DEG C, then cooled to room temperature, obtains mixture;
E, the solidliquid mixture after step d reactions is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 6h at 105 DEG C of temperature obtains the sulphur of 0.398g floriform appearances
Change lead powder body.
Embodiment 11
Any one vulcanized lead of embodiment 1-10 is chosen, is surveyed through X-ray energy spectrometer (EDS) and X-ray diffraction spectrogram (XRD)
Examination, is PbS Crystal material.
Claims (2)
1. a kind of method preparing vulcanized lead using ammonia process of desulfurization waste liquid, it is characterised in that follow these steps to carry out:
A, desulfurization waste liquor is spare with 0.45 micron of filtering with microporous membrane;
B, the lead acetate powder for weighing 0.002mol adds in 40mL distilled water, and stirring is to being completely dissolved;
C, the obtained filtrates of step a are added dropwise in the acetic acid lead solution of step b, it, will with ammonium hydroxide after persistently stirring 10min
The pH of solution is adjusted between 4-7;
D, the solution that step c is obtained is placed in the reaction kettle of stainless steel and carries out hydro-thermal reaction, compactedness 80% is warming up to 80
12h-16h is kept the temperature after DEG C -160 DEG C, then cooled to room temperature, obtains mixture;
E, the mixture that step d is obtained is filtered, washed again, obtains vulcanized lead sample;
F, the sample for obtaining e is as in baking oven, and the dry 4h-6h at 105 DEG C of temperature obtains the vulcanization lead powder of different-shape
Body.
2. the method according to claim 1 for preparing vulcanized lead using ammonia process of desulfurization waste liquid, it is characterised in that in step c
PH is adjusted to 4 or 7.
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CN111995399A (en) * | 2020-09-01 | 2020-11-27 | 昌吉学院 | Method for preparing zinc sulfide ceramic material by using coal coking desulfurization waste liquid |
CN112479247A (en) * | 2020-12-16 | 2021-03-12 | 昌吉学院 | Method for preparing lead sulfide by using industrial desulfurization waste liquid |
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