CN108004413A - Powdery acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof - Google Patents

Powdery acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof Download PDF

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Publication number
CN108004413A
CN108004413A CN201711208385.0A CN201711208385A CN108004413A CN 108004413 A CN108004413 A CN 108004413A CN 201711208385 A CN201711208385 A CN 201711208385A CN 108004413 A CN108004413 A CN 108004413A
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China
Prior art keywords
cigarette ash
white cigarette
lead salt
salt stabilizer
parts
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CN201711208385.0A
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Chinese (zh)
Inventor
王永斌
王怡霖
吴斌
周涛
黄建芬
吴克富
周俊涛
张红
许素敏
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Northwest Research Institute of Mining and Metallurgy
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Northwest Research Institute of Mining and Metallurgy
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Priority to CN201711208385.0A priority Critical patent/CN108004413A/en
Publication of CN108004413A publication Critical patent/CN108004413A/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/02—Working-up flue dust
    • 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
    • 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
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a powdery acid-leaching modified white smoke ash composite lead salt stabilizer, which is characterized in that: white soot collected by electric dust collection and generated in the copper smelting process is used as a raw material, soluble metal ions are removed by leaching with water and sulfuric acid, insoluble metal substances are converted into basic sulfate, and a powdery product is obtained by 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

A kind of acidleach of powdery is modified white cigarette ash complex lead salt stabilizer and preparation method thereof
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 powdery 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 is to be synthesized to be made with sulfuric acid with lead oxide, or using nitric acid and Lead button reacts to obtain plumbi nitras, then obtains lead sulfate precipitation thing with sulfuric acid reaction, after washed plus in caustic soda and is made.Prepared 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 suction human body is toxic.Composite lead heat stabilizer is Employ symbiosis reaction technology by three salt, disalt and metallic soap in 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 produces, thing phase composition fluctuation is big, it is difficult to there is unified processing method, is particularly leaching valuable metal Tailings in still contain soluble metal and poisonous and hazardous heavy non-ferrous metal element, directly discharge can cause environmental pollution, only It can have a great influence 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 powdery 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 powdery is modified white cigarette ash complex lead salt stabilizer, it is characterised in that：The warp produced using copper weld pool process The gather dust white cigarette ash of collection of electricity is raw material, goes out neutralization reaction through hot dipping, its water and sulfuric acid leaching slough soluble metal ion, together When insoluble metal object is changed into alkali sulfate, through drying, crush obtained powder product.
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, the fineness of materials of the complex lead salt stabilizer is below 0.075mm.
Preferably, a kind of acidleach of powdery is modified the preparation method of white cigarette ash complex lead salt stabilizer, comprises the following steps：
（1）Water, white cigarette ash, glacial acetic acid and the concentrated sulfuric acid through electric collection of gathering dust produced using copper weld pool process are sequentially added instead Answer in groove, 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 leached into solution, at the same time will Insoluble metal object is changed into alkali sulfate in white cigarette ash；Wherein：The parts by weight of various material amounts are：3-5 parts of water, white cigarette ash 1 part, 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 the copper wherein contained, zinc are recycled in more solito processing；
（3）The filter residue that filtering washing obtains is dried at 100-110 DEG C, it is below 0.075mm to be then crushed to fineness of materials, Obtain powder product.
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 producing.
Beneficial effects of the present invention are：
（1）The present invention is directed to the recycling of white cigarette lime-ash, it extracts the same of valuable metal in white cigarette ash in water and sulfuric acid 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, properties of product are good, suitable for industrial metaplasia Production.
（3）The catalyst for using glacial acetic acid 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 component in leaching process, glacial acetic acid dosage is white cigarette ash quality 0.2-2%。
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention.
Embodiment
Embodiment 1：
（1）Experiment raw material：White cigarette ash raw material gathers dust product for the Copper making electricity of the copper smelting plant of silver Nonferrous Metals Group company, its White cigarette ash composition sees attached list 1.
（2）Preparation method：First by water and white cigarette ash according to solid-to-liquid ratio 1:3 ratio is added in leaching tanks, is added and is accounted for The glacial acetic acid of white cigarette ash mass ratio 0.2%, slurry is tuned into the case where rotating speed is the frame type stirring of 90r/min；Then add account for it is white 10% sulfuric acid of cigarette ash mass ratio, is heated with stirring to 60 DEG C, Leach reaction 5h；Slurry is filtered again, is washed, makes leachate Separated with leached mud, obtained leachate, which is conventionally handled, recycles the valuable metals such as the copper wherein contained, zinc.Finally will The filter residue that filtering washing obtains is dried at 100 DEG C, and it is below 0.075mm to be then crushed to fineness of materials, that is, obtains powdery production Product.
（3）Product analysis：Powder product appearance is white or taupe powder, without detailed mechanical admixture；Lead content（With oxygen Change lead meter）69.2%, sulfur trioxide content 12.5%, 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 2：
（1）Experiment raw material：White cigarette ash raw material gathers dust product for the Copper making electricity of the copper smelting plant of silver Nonferrous Metals Group company, its White cigarette ash composition sees attached list 1.
（2）Preparation method：First by water and white cigarette ash according to solid-to-liquid ratio 1:6 ratio is added in leaching tanks, is added and is accounted for The glacial acetic acid of white cigarette ash mass ratio 2%, slurry is tuned into the case where rotating speed is the frame type stirring of 120r/min；Then add account for it is white 50% sulfuric acid of cigarette ash mass ratio, is heated with stirring to 90 DEG C, Leach reaction 2h；Slurry is filtered again, is washed, makes leachate Separated with leached mud, obtained leachate, which is conventionally handled, recycles the valuable metals such as the copper wherein contained, zinc.Finally will The filter residue that filtering washing obtains is dried at 110 DEG C, and it is below 0.075mm to be then crushed to fineness of materials, that is, obtains powdery production Product.
（3）Product analysis：Powder product appearance is white or taupe powder, without detailed mechanical admixture；Lead content（With oxygen Change lead meter）72.2%, sulfur trioxide content 14.2%, 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：White cigarette ash raw material gathers dust product for the Copper making electricity of the copper smelting plant of silver Nonferrous Metals Group company, its White cigarette ash composition sees attached list 1.
（2）Preparation method：First by water and white cigarette ash according to solid-to-liquid ratio 1:4 ratio is added in leaching tanks, is added and is accounted for The glacial acetic acid of white cigarette ash mass ratio 1.0%, stirs in the case where rotating speed is the frame type stirring of 120r/min and is tuned into slurry；Then add again Enter to account for 25% sulfuric acid of white cigarette ash mass ratio, be heated with stirring to 80 DEG C, Leach reaction 3h；Slurry is filtered again, is washed, is made Leachate and leached mud separation, obtained leachate, which is conventionally handled, recycles the valuable metals such as the copper wherein contained, zinc. Finally the filter residue that filtering washing obtains is dried at 105 DEG C, it is below 0.075mm to be then crushed to fineness of materials, that is, is obtained Powder product.
（3）Product analysis：Powder product appearance is white or taupe powder, without detailed mechanical admixture；Lead content（With oxygen Change lead meter）70.8%, sulfur trioxide content 13.2%, 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.

Claims (6)

1. a kind of acidleach of powdery is modified white cigarette ash complex lead salt stabilizer, it is characterised in that：Produced using copper weld pool process White cigarette ash through electric collection of gathering dust is raw material, goes out neutralization reaction through hot dipping, its water and sulfuric acid leaching slough soluble metal ion, Insoluble metal object is changed into alkali sulfate at the same time, through drying, crushes obtained powder product.
2. a kind of acidleach of powdery 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 powdery according to claim 1 or 2 is modified white cigarette ash complex lead salt stabilizer, its feature exists In：The fineness of materials of the complex lead salt stabilizer is below 0.075mm.
4. a kind of acidleach of powdery according to any of the above-described claim is modified the preparation of white cigarette ash complex lead salt stabilizer Method, it is characterised 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 produced using copper weld pool process are sequentially added instead Answer in groove, 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 leached into solution, at the same time will Insoluble metal object is changed into alkali sulfate in white cigarette ash；Wherein：The parts by weight of various material amounts are：3-5 parts of water, white cigarette ash 1 part, 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 the copper wherein contained, zinc are recycled in more solito processing；
（3）The filter residue that filtering washing obtains is dried at 100-110 DEG C, it is below 0.075mm to be then crushed to fineness of materials, Obtain powder product.
5. a kind of acidleach of powdery according to claim 4 is modified the preparation method of white cigarette ash complex lead salt stabilizer, its 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.
CN201711208385.0A 2017-11-27 2017-11-27 Powdery acid-leaching modified white smoke ash composite lead salt stabilizer and preparation method thereof Pending CN108004413A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0492817A (en) * 1990-08-06 1992-03-25 Sakai Chem Ind Co Ltd Massive tribasic lead sulfate
CN1222537A (en) * 1997-06-26 1999-07-14 天津市红星化工厂 Composite microcrystal tribasic lead sulfate and its preparation
CN101307158A (en) * 2008-07-09 2008-11-19 重庆太岳科技有限公司 Process for preparing nano-base lead salt

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0492817A (en) * 1990-08-06 1992-03-25 Sakai Chem Ind Co Ltd Massive tribasic lead sulfate
CN1222537A (en) * 1997-06-26 1999-07-14 天津市红星化工厂 Composite microcrystal tribasic lead sulfate and its preparation
CN101307158A (en) * 2008-07-09 2008-11-19 重庆太岳科技有限公司 Process for preparing nano-base lead salt

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
曹学增: "三盐基硫酸铅的生产工艺条件研究", 《山东化工》 *
罗金凤 等: "从铅废渣制取三盐基硫酸铅的研究进展", 《化工科技》 *

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Application publication date: 20180508