CN104651628A - A process of producing lead chloride from lead-containing glass of waste cathode-ray tubes - Google Patents
A process of producing lead chloride from lead-containing glass of waste cathode-ray tubes Download PDFInfo
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- CN104651628A CN104651628A CN201310581048.1A CN201310581048A CN104651628A CN 104651628 A CN104651628 A CN 104651628A CN 201310581048 A CN201310581048 A CN 201310581048A CN 104651628 A CN104651628 A CN 104651628A
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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
- 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
Abstract
The invention provides a process of producing lead chloride from lead-containing glass of waste cathode-ray tubes, aiming at the present situation that lead-containing glass of waste cathode-ray tubes at present in China is high in discarded quantity, short of high value-added resource utilization techniques and severe in environmental harm. The process is characterized in that: the lead-containing glass of the waste cathode-ray tubes is smashed and ground, a chlorinating agent is added, the mixture is granulated, a chlorination reaction is performed by atmosphere and temperature adjustment and control, and a product of the reaction is collected and subjected to purification to obtain a lead chloride product having purity of about 98%. The process is simple and convenient in operation, high in efficiency, low in cost, easily available in raw materials and good in quality of the produced lead chloride, and has a good industrialization application prospect. The left solid residue does not belong to hazardous waste by detection and can be directly used for production of building materials or buried. The lead concentration in exhaust in a production process meets the national emission standards in China.
Description
Technical field
The present invention relates to the method that lead chloride prepared by waste cathode-ray tube flint glass, the solid waste resource recovery belonging to environment protection and comprehensive utilization of resources field utilizes new technology, is particularly suitable for the various harmless treatment containing scrap lead and recycling utilization.
Background technology
Along with the development of plate of flat liquid crystal display and plasma display is with universal, legacy CRT display is substituted substantially.In China, have large quantities of waste computer every year, televisor is dropped, the plumbous oxide containing more than 20% massfraction in cone glass of cathode ray tubes wherein, the Leaching of its heavy metal lead has exceeded the regulation of country to danger wastes.Process discarded cone glass of cathode ray tubes how rationally, greenly, realize its resources circulation recycling, become people and be badly in need of solving.Because lead in cathode-ray tube glass is wrapped in the middle of silicon dioxide molecules, traditional treatment process is very limited to the recovering effect of lead.In recent years, in cone glass of cathode ray tubes recycling, Chinese scholars has carried out more research, and these methods mainly concentrate on lixiviation process, solidification method and as aspects such as material of construction recyclings.These methods have been employed to reclaim field with waste cathode-ray tube cone glass, but have that environmental risk is high, starting material are expensive and the deficiency such as lead recovery is low.Meanwhile, also have the new technology of some cone glass of cathode ray tubes process, comprise overcritical partition method, mechanical activation method and ultrasonic extraction etc., these methods as being separated or preprocessing means, are not yet applied mostly in actual production.
Dchlorine metallurgy technology at metallurgy industry comparative maturity, in solid waste field, this technology in flying dust, metal tail thing and slag valuable metal recovery in also apply to some extent.Chloride volatility process is applied to waste cathode-ray tube cone glass to reclaim lead wherein, there is many irreplaceable advantages, a kind of simple, novel method that cost is low, efficient, oligosaprobic can be provided for recovery plumbous in waste cathode-ray tube glass.
Summary of the invention
The present invention is directed to the present situation that current China waste cathode-ray tube flint glass learies is large, high added value application technology as the second resource is deficient, environmental hazard is serious, provide a set of discarded flint glass to produce the technique of lead chloride.It is characterized in that: cathode tube flint glass crushing and grinding will be discarded, add chlorizating agent granulation, under certain atmosphere and temperature condition, implement chlorination reaction, after collecting the purified process of product, obtain the lead chloride product that purity is about 98%.Concrete technology comprises following step:
1, pretreatment procedure: discarded cathode tube is broken into the fragment that diameter is less than 10mm, removes top coat, then below mechanical ball milling to 200 order, by powder at 105 DEG C dry 24 hours for subsequent use;
2, granulating working procedure: by above-mentioned powder and CaCl
2powder in mass ratio 1.8-2.0:1 ratio uniform mixing, by the tableting under pressure of mixture tabletting machine at 5.0MPa, the compressing tablet time kept for 30 seconds, made the cylindrical particle of diameter 1.0cm;
3, atmosphere regulation and control operation: above-mentioned particle is put into electrothermic type reactor, and reactor one end connects condenser, and condenser connects vacuum system, opens vacuum apparatus, makes system pressure remain on 600 ± 50Pa;
4, synthesis procedure: open electrothermic type reactor power supply, temperature of reactor is made to rise to 1000-1100 DEG C with the speed of 20 DEG C/min, keep 1.0 – 1.5 hours, at this moment the thick lead chloride powders obtained within the condenser, product in condenser is regularly discharged collection, obtain thick lead chloride product, simultaneously regular starting material supplementary new in electrothermic type reactor;
5, purification procedures: the above-mentioned thick lead chloride powder collected is placed in electrothermic type purification reactor, the pressure of keeping system is 600 ± 50Pa, under 650 DEG C of conditions, carry out purification process 0.5 hour, the lead chloride product purity now obtained is about 98.0%, can sell as industrial chemicals.
Above-mentioned technological operation is easy, and efficiency is high, and cost is low, mild condition, and starting material are cheap and easy to get, the lead chloride excellent product quality of production; Remaining solid residue does not belong to danger wastes after testing, can be directly used in and produces material of construction or carry out landfill; Concentration plumbous in tail gas in production process meets GB-25466-2010 emission standard.
Content of the present invention is set forth further below in conjunction with Figure of description and embodiment.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that lead chloride prepared by discarded cathode tube flint glass.
Fig. 2 is the relation of Heating temperature and plumbous rate of evaporation, and showing 1000-1100 DEG C is suitable service temperature.In this figure, the pressure of reactive system is 600 ± 50Pa, and the hold-time is 1h.
Fig. 3 is the XRD figure spectrum contrast of product before and after purification process, the effect of display purification process.The XRD figure spectrum of product after (a) purification process, the XRD figure spectrum of product before (b) purification process.
Embodiment
The invention will be further described for embodiment plan given below; but can not be interpreted as it is limiting the scope of the invention; some nonessential improvement and adjustment that person skilled in art makes the present invention according to foregoing, still belong to protection scope of the present invention.
Embodiment 1:
The technique of lead chloride produced by waste cathode-ray tube flint glass, specifically comprises the following steps:
According to the process flow sheet of Fig. 1, discarded cathode tube flint glass is broken into the fragment that diameter is less than 10mm, washes away the coating on surface by wet scrubbing and ultrasonic cleaning technique, then it is ground with mechanical attrition method, obtain 200 object powder, by powder dry 24h at 105 DEG C.By Powdered CaCl
2be 1:1.8 Homogeneous phase mixing with negative ray pipe powder with mass ratio, take 100g mixture and put into the tableting under pressure of tabletting machine at 5.0MPa, keep 30s, make the cylindrical particle of diameter 1.0cm.Particle is put into electrothermic type reactor, reactor one end connects condenser, and condenser connects vacuum system.Open vacuum apparatus, make system pressure remain on 620Pa; Open electrothermic type reactor power supply, temperature of reactor is risen to 1000 DEG C (Fig. 2), keep 2.0h, after reaction terminates, on prolong, be enriched lead chloride mixture 48.4g yellow powder.The above-mentioned thick lead chloride powder collected is placed in electrothermic type purification reactor, the pressure of keeping system is 600Pa, purification process 0.5h(Fig. 3 is carried out under 650 DEG C of conditions), now collect 19.0g white lead chloride powder within the condenser, purity is 98.6%.The tail gas that reaction produces passes into the HNO of 1mol/L
3middle purification, in the tail gas of final discharge after testing, plumbous concentration meets GB-25466-2010 emission standard.
Embodiment 2:
The technique of lead chloride produced by waste cathode-ray tube flint glass, specifically comprises the following steps:
According to the process flow sheet of Fig. 1, cathode tube is broken into the fragment that diameter is less than 10mm, washes away the coating on surface by wet scrubbing and ultrasonic cleaning technique, then it is ground with mechanical attrition method, obtain 200 object powder, by powder dry 24h at 105 DEG C.By Powdered CaCl
2be 1:1.9 Homogeneous phase mixing with negative ray pipe powder with mass ratio, take about 500g mixture and put into the tableting under pressure 30s of tabletting machine at 5.0MPa, make the cylindrical particle that diameter is 1.0cm.Above-mentioned particle is put into electrothermic type reactor, and reactor one end connects condenser, and condenser connects vacuum system.Open vacuum apparatus, make system pressure remain on 650Pa; Open electrothermic type reactor power supply, temperature of reactor is risen to 1000 DEG C (Fig. 2), keeps 1.0 hours, after reaction terminates, on prolong, be enriched lead chloride mixture 48.4g yellow powder.The above-mentioned thick lead chloride powder collected is placed in electrothermic type purification reactor, the pressure of keeping system is 600Pa, under 650 DEG C of conditions, carry out purification process 0.5 hour (Fig. 3), now collect 239g white lead chloride powder within the condenser, purity is 97.9%.The tail gas that reaction produces passes into the HNO of 1mol/L
3middle purification, in the tail gas of final discharge after testing, plumbous concentration meets GB-25466-2010 emission standard.
In above-mentioned example, the collection of described waste cathode-ray tube cone glass disassembles enterprise from waste and old electric electric equipment products.The invention is not restricted to above-described embodiment, summary of the invention all can be implemented, and has good effect.
Claims (2)
1. the technique of lead chloride produced by waste cathode-ray tube flint glass, specifically comprises the following steps:
(1) pretreatment procedure: discarded cathode tube is broken into the fragment that diameter is less than 10mm, removes top coat, then below mechanical ball milling to 200 order, by powder at 105 DEG C dry 24 hours for subsequent use;
(2) granulating working procedure: by above-mentioned powder and CaCl
2powder in mass ratio 1.8-2.0:1 ratio uniform mixing, by mixture tabletting machine at 5.0MPa pressure lower sheeting, the compressing tablet time kept for 30 seconds, made the cylindrical particle of diameter 1.0cm;
(3) atmosphere regulation and control operation: above-mentioned particle is put into electrothermic type reactor, and reactor one end connects condenser, and condenser connects vacuum system, opens vacuum apparatus, makes system pressure remain on 600 ± 50Pa;
(4) synthesis procedure: open electrothermic type reactor power supply, make temperature of reactor rise to 1000-1100 DEG C with the speed of 20 DEG C/min, then keep 1.0 – 1.5 hours, the thick lead chloride powders now obtained within the condenser.
(5) purification procedures: above-mentioned thick lead chloride powder is placed in electrothermic type purification reactor and carries out purifying, obtaining purity is about 98.0% lead chloride product.
2. produce the technique of lead chloride according to waste cathode-ray tube flint glass according to claim 1, it is characterized in that: in step (6), the pressure of purifier system is 600 ± 50Pa, and temperature is 650 DEG C, and the purification process time is 0.5 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310581048.1A CN104651628A (en) | 2013-11-18 | 2013-11-18 | A process of producing lead chloride from lead-containing glass of waste cathode-ray tubes |
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| CN201310581048.1A CN104651628A (en) | 2013-11-18 | 2013-11-18 | A process of producing lead chloride from lead-containing glass of waste cathode-ray tubes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607284A (en) * | 2014-12-31 | 2015-05-13 | 上海第二工业大学 | Mechanical activation and wet vulcanization treatment method of waste cathode ray tube cone glass |
| CN107385227A (en) * | 2017-07-25 | 2017-11-24 | 上海第二工业大学 | The mechanochemistry recovery method of lead in a kind of flint glass |
-
2013
- 2013-11-18 CN CN201310581048.1A patent/CN104651628A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607284A (en) * | 2014-12-31 | 2015-05-13 | 上海第二工业大学 | Mechanical activation and wet vulcanization treatment method of waste cathode ray tube cone glass |
| CN107385227A (en) * | 2017-07-25 | 2017-11-24 | 上海第二工业大学 | The mechanochemistry recovery method of lead in a kind of flint glass |
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Application publication date: 20150527 |
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