CN107117647B - A kind of device for purifying ceruse in lead-containing compounds - Google Patents

A kind of device for purifying ceruse in lead-containing compounds Download PDF

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Publication number
CN107117647B
CN107117647B CN201710362048.0A CN201710362048A CN107117647B CN 107117647 B CN107117647 B CN 107117647B CN 201710362048 A CN201710362048 A CN 201710362048A CN 107117647 B CN107117647 B CN 107117647B
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Prior art keywords
solution
ceruse
crystallization
reaction kettle
strainer
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CN107117647A (en
Inventor
吴梦陵
许金亮
张珑
吴衍文
王鑫
甘子瑞
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Jiangsu Jiangchuan Machinery Manufacturing Co ltd
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Nanjing Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G21/00Compounds of lead
    • C01G21/14Carbonates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/03Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/96Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor in which the filtering elements are moved between filtering operations; Particular measures for removing or replacing the filtering elements; Transport systems for filters
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06DMEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/03Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
    • B01D2029/033Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting bar screens
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to a kind of devices for purifying ceruse in lead-containing compounds, including reaction kettle, solution circulating device, pedestal, hollow three-way pipeline and crystallization strainer, the pedestal is equipped with solution circulating device, the top of solution circulating device is equipped with reaction kettle, reaction kettle is connected by hollow three-way pipeline with solution circulating device, and the crystallization strainer is located in solution circulating device.The configuration of the present invention is simple, reasonable design, use dust technology(HNO3)Leaching, is used in combination hydrogen peroxide(H2O2)Technique, the higher ultra-fine ceruse crystallization of purity can be obtained, to solve the problems, such as different batches ceruse catalytic activity difference, it is conveniently operated using hook handle precipitation of taking, save experiment expense simultaneously, so that reactant is come into full contact with reaction using circulating line, improve the precision and operability of experiment, there is good popularization and application foreground.

Description

A kind of device for purifying ceruse in lead-containing compounds
Technical field
The present invention relates to a kind of devices for purifying ceruse in lead-containing compounds, more particularly to one kind being used for scrap lead cream The device of ceruse will be purified in removal process in the complete lead-containing compounds of desulfurization.
Background technology
Currently, the substantial amounts of waste accumulator lead plaster, if directly burial processing, heavy metal ion therein will be to soil Generate destruction, pollution ecology;By the ceruse extracted in waste accumulator lead plaster there is larger recycling to be worth simultaneously, Application field is extensive.
For example, widely used ceruse is combustion catalyst in solid propellant, but dehydration ceruse is blocky solid Body, need to by crushing, wash, be ground up, sieved after could apply, in addition, use during find, different manufacturers, different batches Ceruse catalytic activity difference it is very big, therefore study suitable synthetic method, by strictly controlling process conditions, directly Obtain ultra-fine ceruse.Solve the problems, such as that the catalytic activity difference of different batches ceruse has great importance.
In addition for the equipment for separating liquid from solid nowadays used for cyclone hydraulic separators, market price is expensive, if purification carbonic acid can be improved Solid-liquid separation method during lead not only reduces cost, while improving the operability of experiment.
Invention content
It is an object of the invention to:In view of the drawbacks of the prior art, it is proposed that a kind of simple structure and reasonable design is used for The device that ceruse is purified in lead-containing compounds can solve laboratory and prepare that ultra-fine ceruse device is more expensive to be difficult to agitating paddle The problem of cleaning, and solution cycle electric pump can be utilized fully to be precipitated reaction liquid circulating filtration, improve experiment Precision and operability.
The technical solution adopted in the present invention is:A kind of device for purifying ceruse in lead-containing compounds, including it is anti- Kettle, solution circulating device, pedestal, hollow three-way pipeline and crystallization strainer are answered, the pedestal is equipped with solution circulating device, molten The top of liquid circulating device is equipped with reaction kettle, and reaction kettle is connected by hollow three-way pipeline with solution circulating device, the knot Brilliant strainer is located in solution circulating device;The reaction kettle straight wall is columnar structured, and filter screen, blender are equipped in reaction kettle And agitator motor, by scrap lead cream(The lead-containing compounds such as ceruse, brown lead oxide, lead oxide)Solid is placed on filter screen, to Dust technology (HNO is added in reaction kettle3) and hydrogen peroxide(H2O2), make itself and scrap lead cream solid reaction, driven using agitator motor The blade of blender accelerates solution flowing, obtains and contain Pb2+Solution;Meanwhile blender being arranged below filter screen in order to make Mixing arm and the separation of scrap lead cream solid, to protect the blade of blender without damage.
In the present invention:One channel of the hollow three-way pipeline is connected with the side wall of reaction kettle, another channel with The solution circulating device of lower section is connected, and third channel is opened in air, wherein containing Pb2+Solution from reaction kettle madial wall An entrance of hollow three-way pipeline enter, lower section solution circulating device is flowed by vertical hollow three-way pipeline, in Cooperation top is the hook-type handle of arcuate structure in empty three-way pipeline, and crystallization strainer is provided with below hook-type handle;From hollow three It threads a pipe the opening being placed in air, sodium carbonate is added thereto(Na2CO3), sodium carbonate(Na2CO3)It falls on crystallization strainer, Contain Pb into solution circulating device2+Solution recycle in the duct, continuously contact with crystallization strainer on sodium carbonate(Na2CO3), It is allowed to generate ceruse precipitation, obtains ceruse crystallization.
In the present invention:The solution circulating device includes solution cycle electric pump and circulating line, contains Pb2+Solution from Enter solution circulating device in hollow three-way pipeline, under the driving that solution recycles electric pump, in side clockwise in circulating line To circulating, flow direction and the upper surface of crystallization strainer are perpendicular, are directed toward the lower section of crystallization strainer;In cyclic process In, contain Pb2+Solution with crystallization strainer on sodium carbonate(Na2CO3)Solid fully reacts, and is continuously generated ceruse precipitation, knot Crystalline substance is on crystallization strainer;It is equipped with the step placed for crystallization strainer in the circulating line, is at the section of circulating line; In solution circulating device, circulating line uses the design of circular pipe cycle, solution more fully anti-during cycle It answers, making solution, constantly touching crystallizes strainer back and forth, and precipitation is fully beaten on strainer, precipitating lead carbonates are obtained.
In the present invention:Curved handle design is used with the hook-type handle of hollow three-way pipeline cooperation, with crystallization strainer phase Even coordinate, can directly take out ultra-fine PbCO3Product, crystallization strainer need not be fitted closely with circulating line, prevent precipitation excessive When, it takes out and has liquid exudation;The lower left of the circulating line is equipped with a leakage fluid dram, and product carbonic acid can not be analysed when being reacted to When lead(Pb in solution i.e. in circulating line2+It has been precipitated as ceruse crystallization completely), can be discharged it by leakage fluid dram.
After adopting the above technical scheme, beneficial effects of the present invention are:The configuration of the present invention is simple, reasonable design, use are dilute Nitric acid(HNO3)Leaching, is used in combination hydrogen peroxide(H2O2)Technique, the higher ultra-fine ceruse crystallization of purity can be obtained, to solve The problem of different batches ceruse catalytic activity difference, is conveniently operated using hook handle precipitation of taking, while saving experiment and opening Pin, makes reactant come into full contact with reaction, improves the precision and operability of experiment using circulating line, has universal well answer Use foreground.
Description of the drawings
Fig. 1 is the structural diagram of the present invention;
Fig. 2 is another structural schematic diagram of the present invention;
Fig. 3 is the schematic internal view of reaction kettle in the present invention;
Fig. 4 is the connection diagram of the hollow three-way pipeline in the present invention;
Fig. 5 is the hook-type handle and crystallization strainer combination schematic diagram of the present invention.
In figure:1. filter screen;2. blender;3. agitator motor;4. reaction kettle;5. hook-type handle;6. hollow three-way pipe Road;7. crystallizing strainer;8. solution recycles electric pump;9. circulating line;10. pedestal;11. leakage fluid dram;12. solution circulating device.
Specific implementation mode
Below in conjunction with attached drawing, the present invention is further illustrated.
By Fig. 1-5 as it can be seen that a kind of device for purifying ceruse in lead-containing compounds, including reaction kettle 4, solution recycle Device 12, pedestal 10, hollow three-way pipeline 6 and crystallization strainer 7, the pedestal 10 are equipped with solution circulating device 12, solution The top of circulator 12 is equipped with reaction kettle 4, and reaction kettle 4 is connected by hollow three-way pipeline 6 with solution circulating device 12, described Crystallization strainer 7 be located in solution circulating device 12;4 straight wall of reaction kettle is columnar structured, and filtering is equipped in reaction kettle 4 Net 1, blender 2 and agitator motor 3, by scrap lead cream(The lead-containing compounds such as ceruse, brown lead oxide, lead oxide)Solid is placed in On filter screen 1, dust technology (HNO is added into reaction kettle 43) and hydrogen peroxide(H2O2), make itself and scrap lead cream solid reaction, utilize Agitator motor 3 drives the blade of blender 2, accelerates solution flowing, obtains and contain Pb2+Solution;Meanwhile blender 2 being arranged In order to make blade and the separation of scrap lead cream solid of blender 2 below filter screen 1, to protect the blade of blender 2 not to be damaged It is bad.
One channel of the hollow three-way pipeline 6 is connected with the side wall of reaction kettle 4, the solution in another channel and lower section Circulator 12 is connected, and third channel is opened in air, wherein containing Pb2+Solution from the hollow of 4 madial wall of reaction kettle One entrance of three-way pipeline 6 enters, and lower section solution circulating device 12 is flowed by vertical hollow three-way pipeline 6, hollow Cooperation top is the hook-type handle 5 of arcuate structure in three-way pipeline 6, and 5 lower section of hook-type handle is provided with crystallization strainer 7;From hollow Three-way pipeline 6 is placed in the opening in air, and sodium carbonate is added thereto(Na2CO3), sodium carbonate(Na2CO3)It falls in crystallization strainer 7 On, contain Pb into solution circulating device 122+Solution recycle in the duct, continuously contact with crystallization strainer 7 on sodium carbonate (Na2CO3), it is allowed to generate ceruse precipitation, obtains ceruse crystallization.
The solution circulating device 12 includes solution cycle electric pump 8 and circulating line 9, contains Pb2+Solution from hollow three It threads a pipe and enters solution circulating device 12 in 6, under the driving that solution recycles electric pump 8, in clockwise in circulating line 9 It circulates, flow direction and the upper surface of crystallization strainer 7 are perpendicular, are directed toward the lower section of crystallization strainer 7;In cyclic process In, contain Pb2+Solution with crystallization strainer 7 on sodium carbonate(Na2CO3)Solid fully reacts, and is continuously generated ceruse precipitation, knot Crystalline substance is on crystallization strainer 7;The step placed for crystallization strainer 7 is equipped in the circulating line 9, cutting in circulating line 9 At face;In solution circulating device 12, circulating line 9 using circular pipe cycle design, solution during cycle more Add abundant reaction, making solution, constantly touching crystallizes strainer 7 back and forth, and precipitation is fully beaten on crystallization strainer 7, obtains and precipitates carbon Lead plumbate.
Curved handle design is used with the hook-type handle 5 that hollow three-way pipeline 6 coordinates, be connected cooperation with crystallization strainer 7, just Ultra-fine PbCO can directly be taken out3Product, crystallization strainer 7 need not be fitted closely with circulating line 9, when preventing from precipitating excessive, be taken out Have liquid exudation;The lower left of the circulating line 9 be equipped with a leakage fluid dram 11, when be reacted to can not analyse product ceruse when (Pb in solution i.e. in circulating line2+It has been precipitated as ceruse crystallization completely), can be discharged it by leakage fluid dram 11.
As shown in figure 4, containing Pb2+Solution from top reaction kettle 4 via hollow three-way pipeline 6 flow into lower section solution recycle In device 12, finally make Pb2+It is deposited on crystallization strainer.
The key reaction equation occurred in reaction kettle 4 is:
2HNO3(It is dilute)+2PbO=2Pb(NO3)2+H2O; PbCO3+2HNO3=Pb(NO3)2+H2O+CO2
H2O2+PbO2+2HNO3=Pb(NO3)2+2H2O+O2
Pb3(CO3)2(OH)2+6HNO3=3Pb(NO3)2+3H2O+2CO2
After the generation of this series reaction, obtained divalent lead solution flows to hollow three-way pipeline 6, by crystallizing strainer 7, It is constantly recycled at circulating line 9, adds sodium carbonate solid or solution to keep divalent lead molten to 6 top port of hollow three-way pipeline at this time Liquid reacts with sodium carbonate, and key reaction equation is:
Pb(NO3)2+Na2CO3=PbCO3+2NaNO3, later, the PbCO after the purification of acquisition3Solid is intercepted at crystallization filter At net 7, solution is reached a certain level by the constantly fully reaction of circulating line 9, hook-type handle 5 is taken from hollow three-way pipeline 6 Go out, the ultra-fine ceruse after being purified.
The specific implementation mode of the present invention is described above, but the present invention is not limited to above description.For this For the technical staff in field, any equal modification and replacement to the technical program is all within the scope of the invention.Cause This, without departing from the spirit and scope of the invention made by impartial conversion and modification, all should be contained within the scope of the invention.

Claims (5)

1. a kind of device for purifying ceruse in lead-containing compounds, it is characterised in that:Including reaction kettle, solution cycle dress Set, pedestal, hollow three-way pipeline and crystallization strainer, the pedestal be equipped with solution circulating device, solution circulating device it is upper Side is equipped with reaction kettle, and reaction kettle is connected by hollow three-way pipeline with solution circulating device, and the crystallization strainer is located at solution In circulator;One channel of the hollow three-way pipeline is connected with the side wall of reaction kettle, another channel and lower section it is molten Liquid circulating device is connected, and third channel is opened in air;It is located at the channel in air in the hollow three-way pipeline Interior to be equipped with hook-type handle, the top of hook-type handle is arcuate structure, and lower end is connected with crystallization strainer.
2. a kind of device for purifying ceruse in lead-containing compounds according to claim 1, it is characterised in that:It is described Reaction kettle in be equipped with filter screen, blender and agitator motor, filter screen is located at the top of blender, and agitator motor is located at The lower section of blender, to drive the blade of blender to rotate.
3. a kind of device for purifying ceruse in lead-containing compounds according to claim 2, it is characterised in that:It is described Reaction kettle straight wall it is columnar structured.
4. a kind of device for purifying ceruse in lead-containing compounds according to claim 1, it is characterised in that:Institute The solution circulating device stated includes solution cycle electric pump and circulating line, and the circulating line uses the knot of circular pipe cycle Structure ensures abundant reaction of solution during cycle, the step placed for crystallization strainer is equipped in the circulating line.
5. a kind of device for purifying ceruse in lead-containing compounds according to claim 4, it is characterised in that:Institute The lower left for the circulating line stated is equipped with a leakage fluid dram, and the product of final reaction is discharged by leakage fluid dram.
CN201710362048.0A 2017-05-22 2017-05-22 A kind of device for purifying ceruse in lead-containing compounds Active CN107117647B (en)

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CN114082377B (en) * 2021-09-27 2023-07-14 天能集团(濮阳)再生资源有限公司 Device and method for producing lead oxide by using waste lead-acid storage battery
CN114408978B (en) * 2022-03-07 2024-08-23 科立鑫(珠海)新能源有限公司 Process for preparing battery-grade manganese sulfate by utilizing manganese in cobalt raw material

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GB1468052A (en) * 1974-11-25 1977-03-23 Gen Electric Co Ltd Crystals and their manufacture
CN105561883A (en) * 2015-12-17 2016-05-11 北方华锦化学工业集团有限公司 Online switching feeding system of loop reactor
CN105797430B (en) * 2016-05-24 2019-03-05 河南银金达彩印股份有限公司 A kind of efficiently organic recycling design purification device and technique
CN106435194A (en) * 2016-09-30 2017-02-22 刘振 Efficient desulfurization technology for waste lead-acid cell lead plaster
CN106587142B (en) * 2016-11-23 2017-12-29 超威电源有限公司 A kind of method that 4BS is prepared using waste lead acid battery lead cream

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Effective date of registration: 20201229

Address after: 224217 in the government building of WuLie Town, Dongtai City, Yancheng City, Jiangsu Province

Patentee after: Collective assets management company of township enterprises in WuLie Town, Dongtai City

Address before: No. 101, Nanxu Avenue, Zhenjiang City, Jiangsu Province, 212000

Patentee before: JIANGSU HUIZHI INTELLECTUAL PROPERTY SERVICES Co.,Ltd.

Effective date of registration: 20201229

Address after: No. 101, Nanxu Avenue, Zhenjiang City, Jiangsu Province, 212000

Patentee after: JIANGSU HUIZHI INTELLECTUAL PROPERTY SERVICES Co.,Ltd.

Address before: 1 No. 211167 Jiangsu city of Nanjing province Jiangning Science Park Hongjing Road

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Effective date of registration: 20240716

Address after: 224000, Group 6, Lianyi Community Town, Wulie Town, Dongtai City, Yancheng City, Jiangsu Province (within Dongtai Daquan Zinc Products Factory)

Patentee after: Jiangsu Jiangchuan Machinery Manufacturing Co.,Ltd.

Country or region after: China

Address before: 224217 in the government building of WuLie Town, Dongtai City, Yancheng City, Jiangsu Province

Patentee before: Collective assets management company of township enterprises in WuLie Town, Dongtai City

Country or region before: China