CN108084490A - Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof - Google Patents
Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof Download PDFInfo
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- CN108084490A CN108084490A CN201711206743.4A CN201711206743A CN108084490A CN 108084490 A CN108084490 A CN 108084490A CN 201711206743 A CN201711206743 A CN 201711206743A CN 108084490 A CN108084490 A CN 108084490A
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- lead salt
- white cigarette
- cigarette ash
- complex lead
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C01G21/20—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a pasty acid-leaching modified white soot composite lead salt stabilizer, which is a powdery product obtained by leaching water and sulfuric acid to remove soluble metal ions and simultaneously converting insoluble metal substances into basic sulfate by taking white soot generated in the copper smelting process and collected by electric dust collection as a raw material, drying and crushing; the raw materials used in the invention adopt industrial waste slag, the raw materials are wide in source and low in price, the preparation method is simple and reasonable to operate, poisoning caused by lead dust in production and use is avoided, the product performance is good, and the method is suitable for industrial production.
Description
Technical field
The present invention relates to slag comprehensive utilization of resources field, it is steady to be modified white cigarette ash complex lead salt for a kind of specifically acidleach of pulpous state
Determine agent and preparation method thereof.
Background technology
Lead salt stabilizer has monomer and compound two major class, and lead salt is substantially used in the polyvinyl chloride plastic material products in China
Stabilizer makees main stabilizer.The lead sulfate tribasic of monomer be synthesized with lead oxide with sulfuric acid be made or using nitric acid and
Plumbi nitras is obtained by the reaction in lead button, then obtains lead sulfate precipitation object with sulfuric acid reaction, after washed plus in caustic soda and is made.It prepared
It needing to consume purity higher oxidation leady raw materials or lead button in journey, cost is higher, and dust is big in use, and metering numbers are more,
Measurement error easily occurs, influences greatly, there is pollution to section quality, dust sucking human body is toxic.Composite lead heat stabilizer is
Symbiosis reaction technology is employed by three salt, disalt and metallic soap in the reaction system with the crystallite dimension of nascent state and various lubrications
Agent is mixed, and operation is more complicated, and product cost is higher.
White cigarette ash is in the fusion process of copper smelting by pyrometallurgy, the ash-laden gas of sulfonium and two benches generation of blowing is being made, through excess enthalpy
After heat boiler, roto-clone, induced-draft fan and cottrell, what is obtained contains the white of a variety of valuable metals such as a large amount of copper, zinc, lead
Color cigarette ash.The cigarette ash is rich in there is a variety of valuable metals such as copper, lead, zinc, arsenic, bismuth, antimony, indium, for this rich in valuable metal
Flue dust, current most of method of comprehensive utilization leach the soluble metals such as copper and the zinc in white cigarette ash with water logging and dilute sulfuric acid, then
Leachate and leached mud are handled respectively using different methods.But due to being influenced by raw material, process, process conditions, copper
The cigarette ash complicated component that melting generates, object phase composition fluctuation is big, it is difficult to there is unified processing method, is particularly leaching valuable metal
Tailings in still containing soluble metal and poisonous and hazardous heavy non-ferrous metal element, directly discharge can cause environmental pollution, only
It can be affected as danger wastes stockpiling disposal to environmental protection.
The content of the invention
A kind of acidleach the object of the present invention is to provide pulpous state is modified white cigarette ash complex lead salt stabilizer and preparation method thereof.
In order to meet above-mentioned purpose, the technical solution that the present invention takes is：
A kind of acidleach of pulpous state is modified white cigarette ash complex lead salt stabilizer, using the generation of copper weld pool process through electric collection of gathering dust
White cigarette ash goes out neutralization reaction for raw material, through hot dipping, and water and sulfuric acid leaching slough soluble metal ion, while by insoluble gold
Belong to object and be changed into alkali sulfate, filtered, washing, the mixture and vacuum for adding in warmed-up dioctyl ester and linolenic acid
Evaporation obtains pasty products.
Preferably, the parts by weight of various material amounts are in the complex lead salt stabilizer：3-5 parts of water, 1 part of white cigarette ash,
0.002-0.02 parts of glacial acetic acid, 0.1-0.5 parts of the concentrated sulfuric acid.
Preferably, complex lead salt stabilizer is by being pre-heated to 60-90 DEG C of dioctyl ester and linolenic acid mixture, making
By water, mutually modification is transferred to oil phase to alkali formula complex lead salt product, by being evaporated in vacuo obtained pasty products.
Preferably, a kind of acidleach of pulpous state is modified the preparation method of white cigarette ash complex lead salt stabilizer, which is characterized in that bag
Include following steps：
（1）Water, white cigarette ash, glacial acetic acid and the concentrated sulfuric acid through electric collection of gathering dust generated using copper weld pool process are sequentially added instead
It answers in slot, then carrying out heating in stirring leaches neutralization reaction, and the extraction temperature is 60-90 DEG C, extraction time 2-5h,
Mechanical agitation speed is 90-120r/min；Water and sulfuric acid soluble metal ion in white cigarette ash is made to be leached into solution, simultaneously will
Insoluble metal object is changed into alkali sulfate in white cigarette ash；Wherein：The mass fraction of various material amounts is：3-5 parts of water, white cigarette
1 part of ash, 0.002-0.02 parts of glacial acetic acid, 0.1-0.5 parts of the concentrated sulfuric acid；
（2）After Leach reaction, slurry is filtered, is washed, separates leachate and leached mud, obtained leachate by
The valuable metals such as copper, the zinc that more solito processing recycling wherein contains；What is obtained crosses the alkali formula that filter residue is aqueous 20-30%
Complex lead salt product；
（3）The alkali formula complex lead salt product of above-mentioned aqueous 20-30% is sent into heating mixer, 60-90 DEG C is heated to, is stirring
Under conditions of mix rotating speed is 90-120r/min, warmed-up to 60-90 DEG C of dioctyl ester and linolenic acid mixing is added portionwise
Object is stirred 10-30min, and making alkali formula complex lead salt product, mutually modification is transferred to oil phase by water；
（4）The alkali formula complex lead salt product for being modified as oil phase is sent into and is evaporated in vacuo, removes moisture through being evaporated in vacuo, vacuum degree is
2000Pa-500Pa, vacuum evaporation time are 1-3h to get pasty products.
Preferably, the step（1）The solid-to-liquid ratio of middle raw material is 1：3-6.
Preferably, the step（1）Middle leaching process ventilation, prevents arsenic hydride from generating.
Preferably, the step（3）Dioctyl ester and linolenic acid mixture in dioctyl ester and linolenic acid ratio be 1:
1, dosage accounts for the 10-50% of alkali formula complex lead salt product quality.
Beneficial effects of the present invention are：
（1）The present invention be directed to white cigarette lime-ash recycling, in water and sulfuric acid extract white cigarette ash in valuable metal it is same
When, by being processed further that complex lead salt stabilizer has been prepared, in the complex lead salt stabilizer containing tribasic lead sulfate,
The plurality of active ingredients such as lead silicate, other basic metal sulfate, amorphous silicic acid and silicates, have excellent heat resistance and
Electrical insulating property, available for opaque or translucent polrvinyl chloride product such as hard tube, hardboard, injection moulding polrvinyl chloride product, electricity
The processing and manufacturing of device cable insulation material etc..
（2）Raw material used employs industrial waste slag in the present invention, and raw material sources are inexpensive extensively, its preparation method operation
Advantages of simple avoids production and neutralizes the poisoning caused by lead powder dirt in use, and properties of product are good, suitable for industrial metaplasia
Production.
（3）The catalyst that glacial acetic acid is used to be converted as lead salt in white cigarette ash in technical solution of the present invention, makes in white cigarette ash
Oxidation lead composition be completely converted into tribasic lead sulfate ingredient in leaching process, glacial acetic acid dosage is white cigarette ash quality
0.2-2%。
（4）The alkali formula complex lead salt of production is produced using the mixture of dioctyl ester and linolenic acid in technical solution of the present invention
Product carry out surface modification, change the physicochemical properties of powder surface and assign its new function, with meet modern new material,
The needs of the development of new techniques of new process.Meanwhile significantly inhibit and alleviate the complex lead salt stabilizer product in production and
Environmental pollution caused by use has good application prospect.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific embodiment
Embodiment 1：
（1）Experiment raw material：Comprehensive flue dust is received using the smelting products of copper ore electricity of the copper smelting plant of silver Nonferrous Metals Group company（White cigarette
Ash）For raw material, white cigarette ash composition is to be shown in Table 1.
（2）Preparation method：
A, by water and white cigarette ash according to solid-to-liquid ratio 1:3 ratios are added in leaching tanks, add dosage is about white cigarette ash quantity 0.2%
Dense acetic acid, stirring be tuned into slurry；Then sulfuric acid is added under stiring, and sulphuric acid is the 10% of white cigarette ash.Speed of agitator is
60r/min, heating temperature are 60 DEG C, Leach reaction 5h；
B, slurry is filtered, washed, separate leachate and leached mud.Obtained leachate is conventionally handled back
Receive the valuable metals such as copper, the zinc wherein contained.The obtained alkali formula complex lead salt product crossed filter residue and be aqueous 30%.
C, aqueous 30% alkali formula complex lead salt is sent into special heating mixer, 60 DEG C is heated to, in speed of agitator
Under conditions of 90r/min, warmed-up to 60 DEG C of dioctyl ester and linolenic acid mixture is added portionwise, is stirred 10-
30min, making alkali formula complex lead salt product, mutually modification is transferred to oil phase by water.Dioctyl ester and linolenic acid ratio are 1 in mixture:1,
Its dosage accounts for the 10% of alkali formula complex lead salt product quality.
D, the alkali formula complex lead salt product for being modified as oil phase is sent into and be evaporated in vacuo, moisture, vacuum are removed through being evaporated in vacuo
It spends for 2000Pa, it is 3h to get pasty products to be evaporated in vacuo the time.
（3）Product analysis：
Product appearance is white or taupe pasty products, without detailed mechanical admixture.Contents of Main Components is（%）：Lead content（With
Lead oxide meter）62.2%, sulfur trioxide content 11.3%, heating loss≤0.5%, residue on sieve（0.075mm）≤0.5%.In product
Contents of Main Components sees attached list 1.
Embodiment 2：
（1）Experiment raw material：Comprehensive flue dust is received using the smelting products of copper ore electricity of the copper smelting plant of silver Nonferrous Metals Group company（White cigarette
Ash）For raw material, white cigarette ash composition is to be shown in Table 1.
（2）Preparation method：
A, by water and white cigarette ash according to liquid-solid ratio 1:6 ratios are added in leaching tanks, add dosage is about white cigarette ash quantity 2%
Dense acetic acid, stirring are tuned into slurry；Then sulfuric acid is added under stiring, and sulphuric acid is the 50% of white cigarette ash.Speed of agitator is
120r/min, heating temperature are 90 DEG C, Leach reaction 2h；
B, slurry is filtered, washed, separate leachate and leached mud.Obtained leachate is conventionally handled back
Receive the valuable metals such as copper, the zinc wherein contained.The obtained alkali formula complex lead salt product crossed filter residue and be aqueous 20%.
C, aqueous 20% alkali formula complex lead salt is sent into special heating mixer, 90 DEG C is heated to, in speed of agitator
Under conditions of 120r/min, warmed-up to 90 DEG C of dioctyl ester and linolenic acid mixture is added portionwise, is stirred 10-
30min, making alkali formula complex lead salt product, mutually modification is transferred to oil phase by water.Dioctyl ester and linolenic acid ratio are 1 in mixture:1,
Its dosage accounts for the 50% of alkali formula complex lead salt product quality.
D, the alkali formula complex lead salt product for being modified as oil phase is sent into and be evaporated in vacuo, moisture, vacuum are removed through being evaporated in vacuo
It spends for 500Pa, it is 1h to get pasty products to be evaporated in vacuo the time.
（3）Product analysis：
Product appearance is white or taupe pasty products, without detailed mechanical admixture.Contents of Main Components is（%）：Lead content（With
Lead oxide meter）31.1%, sulfur trioxide content 5.7%, heating loss≤0.5%, residue on sieve（0.075mm）≤0.5%.It is main in product
Component content is wanted to see attached list 1.
Embodiment 3：
（1）Experiment raw material：Comprehensive flue dust is received using the smelting products of copper ore electricity of the copper smelting plant of silver Nonferrous Metals Group company（White cigarette
Ash）For raw material, white cigarette ash composition is to be shown in Table 1.
（2）Preparation method：
A, by water and white cigarette ash according to solid-to-liquid ratio 1:4 ratios are added in leaching tanks, add dosage is about white cigarette ash quantity 1%
Dense acetic acid, stirring are tuned into slurry；Then sulfuric acid is added under stiring, and sulphuric acid is the 20% of white cigarette ash.Speed of agitator is
120r/min, heating temperature are 80 DEG C, Leach reaction 5h；
B, slurry is filtered, washed, separate leachate and leached mud.Obtained leachate is conventionally handled back
Receive the valuable metals such as copper, the zinc wherein contained.The obtained alkali formula complex lead salt product crossed filter residue and be aqueous 26%.
C, aqueous 26% alkali formula complex lead salt is sent into special heating mixer, 80 DEG C is heated to, in speed of agitator
Under conditions of 120r/min, warmed-up to 70 DEG C of dioctyl ester and linolenic acid mixture is added portionwise, is stirred
20min, making alkali formula complex lead salt product, mutually modification is transferred to oil phase by water.Dioctyl ester and linolenic acid ratio are 1 in mixture:1,
Its dosage accounts for the 25% of alkali formula complex lead salt product quality.
D, the alkali formula complex lead salt product for being modified as oil phase is sent into and be evaporated in vacuo, moisture, vacuum are removed through being evaporated in vacuo
It spends for 1000Pa, it is 2h to get pasty products to be evaporated in vacuo the time.
（3）Product analysis：
Product appearance is white or taupe pasty products, without detailed mechanical admixture.Contents of Main Components is（%）：Lead content（With
Lead oxide meter）46.7%, sulfur trioxide content 8.47%, heating loss≤0.5%, residue on sieve（0.075mm）≤0.5%.In product
Contents of Main Components sees attached list 1.
Claims (7)
1. a kind of acidleach of pulpous state is modified white cigarette ash complex lead salt stabilizer, it is characterised in that：It is generated using copper weld pool process
White cigarette ash through electric collection of gathering dust is raw material, goes out neutralization reaction through hot dipping, and water and sulfuric acid leaching slough soluble metal ion,
Insoluble metal object is changed into alkali sulfate simultaneously, filtered, washing adds in warmed-up dioctyl ester and linolenic acid
Mixture and vacuum evaporation obtain pasty products.
2. a kind of acidleach of pulpous state according to claim 1 is modified white cigarette ash complex lead salt stabilizer, it is characterised in that：Institute
The parts by weight for stating various material amounts in complex lead salt stabilizer are：3-5 parts of water, 1 part of white cigarette ash, glacial acetic acid 0.002-0.02
Part, 0.1-0.5 parts of the concentrated sulfuric acid.
3. a kind of acidleach of pulpous state according to claim 1 or 2 is modified white cigarette ash complex lead salt stabilizer, feature exists
In：Complex lead salt stabilizer is by being pre-heated to 60-90 DEG C of dioctyl ester and linolenic acid mixture, making alkali formula complex lead salt
By water, mutually modification is transferred to oil phase to product, by being evaporated in vacuo obtained pasty products.
4. a kind of acidleach of pulpous state according to any of the above-described claim is modified the preparation of white cigarette ash complex lead salt stabilizer
Method, which is characterized in that comprise the following steps：
（1）Water, white cigarette ash, glacial acetic acid and the concentrated sulfuric acid through electric collection of gathering dust generated using copper weld pool process are sequentially added instead
It answers in slot, then carrying out heating in stirring leaches neutralization reaction, and the extraction temperature is 60-90 DEG C, extraction time 2-5h,
Mechanical agitation speed is 90-120r/min；Water and sulfuric acid soluble metal ion in white cigarette ash is made to be leached into solution, simultaneously will
Insoluble metal object is changed into alkali sulfate in white cigarette ash；Wherein：The mass fraction of various material amounts is：3-5 parts of water, white cigarette
1 part of ash, 0.002-0.02 parts of glacial acetic acid, 0.1-0.5 parts of the concentrated sulfuric acid；
（2）After Leach reaction, slurry is filtered, is washed, separates leachate and leached mud, obtained leachate by
The valuable metals such as copper, the zinc that more solito processing recycling wherein contains；What is obtained crosses the alkali formula that filter residue is aqueous 20-30%
Complex lead salt product；
（3）The alkali formula complex lead salt product of above-mentioned aqueous 20-30% is sent into heating mixer, 60-90 DEG C is heated to, is stirring
Under conditions of mix rotating speed is 90-120r/min, warmed-up to 60-90 DEG C of dioctyl ester and linolenic acid mixing is added portionwise
Object is stirred 10-30min, and making alkali formula complex lead salt product, mutually modification is transferred to oil phase by water；
（4）The alkali formula complex lead salt product for being modified as oil phase is sent into and is evaporated in vacuo, removes moisture through being evaporated in vacuo, vacuum degree is
2000Pa-500Pa, vacuum evaporation time are 1-3h to get pasty products.
5. a kind of acidleach of powdery according to claim 4 is modified the preparation method of white cigarette ash complex lead salt stabilizer,
It is characterized in that：The step（1）The solid-to-liquid ratio of middle raw material is 1：3-6.
6. a kind of acidleach of powdery according to claim 4 or 5 is modified the preparation method of white cigarette ash complex lead salt stabilizer,
It is characterized in that：The step（1）Middle leaching process ventilation.
7. a kind of acidleach of powdery according to claim 4 is modified the preparation method of white cigarette ash complex lead salt stabilizer,
It is characterized in that：The step（3）Dioctyl ester and linolenic acid mixture in dioctyl ester and linolenic acid ratio be 1:1, it uses
Amount accounts for the 10-50% of alkali formula complex lead salt product quality.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711206743.4A CN108084490A (en) | 2017-11-27 | 2017-11-27 | Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711206743.4A CN108084490A (en) | 2017-11-27 | 2017-11-27 | Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof |
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| CN201711206743.4A Pending CN108084490A (en) | 2017-11-27 | 2017-11-27 | Pasty acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519729A (en) * | 2009-03-19 | 2009-09-02 | 金川集团有限公司 | Method for preparing tribasic lead sulfate by using ash of copper converter |
| CN102995452A (en) * | 2012-10-23 | 2013-03-27 | 合肥市安山涂层织物有限公司 | Polyvinyl chloride synthetic leather for gloves and manufacturing method thereof |
-
2017
- 2017-11-27 CN CN201711206743.4A patent/CN108084490A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519729A (en) * | 2009-03-19 | 2009-09-02 | 金川集团有限公司 | Method for preparing tribasic lead sulfate by using ash of copper converter |
| CN102995452A (en) * | 2012-10-23 | 2013-03-27 | 合肥市安山涂层织物有限公司 | Polyvinyl chloride synthetic leather for gloves and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 罗金凤等: "铅废渣制取三盐基硫酸铅的研究进展", 《化工科技》 * |
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