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 PDFInfo
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- 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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- C01G21/14—Carbonates
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- B01D29/03—Filters 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D29/96—Filters 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
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- B01D29/01—Filters 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
- B01D29/03—Filters 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
- B01D2029/033—Filters 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
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Abstract
本发明涉及一种用于含铅化合物中提纯碳酸铅的装置，包括反应釜、溶液循环装置、底座、中空三通管道和结晶滤网，所述的底座上设有溶液循环装置，溶液循环装置的上方设有反应釜，反应釜通过中空三通管道和溶液循环装置相连，所述的结晶滤网位于溶液循环装置内。本发明结构简单、设计合理，使用稀硝酸（HNO3）浸取，并用双氧水（H2O2）的工艺，能获得纯度较高的超细碳酸铅结晶，从而解决不同批次碳酸铅催化活性差异的问题，使用钩型提手拿取沉淀方便操作，同时节约实验开销，采用循环管道使反应物充分接触反应，提高实验的精度和可操作性，具有很好的普及应用前景。
The invention relates to a device for purifying lead carbonate from lead-containing compounds, comprising a reaction kettle, a solution circulation device, a base, a hollow three-way pipe and a crystallization filter, the base is provided with a solution circulation device, a solution circulation device A reactor is arranged above the reactor, and the reactor is connected to the solution circulation device through a hollow three-way pipe, and the crystallization filter is located in the solution circulation device. The invention is simple in structure and reasonable in design, and can obtain ultrafine lead carbonate crystals with high purity by using dilute nitric acid (HNO 3 ) leaching and hydrogen peroxide (H 2 O 2 ) technology, thereby solving the catalytic activity of different batches of lead carbonate. For the problem of differences, it is convenient to use the hook-shaped handle to pick up the sediment, and at the same time save the cost of the experiment, and use the circulation pipeline to make the reactants fully contact and react, improve the accuracy and operability of the experiment, and have a good prospect for popularization and application.
Description
技术领域technical field
本发明涉及一种用于含铅化合物中提纯碳酸铅的装置，尤其涉及一种用于废铅膏回收过程中将脱硫完的含铅化合物中提纯碳酸铅的装置。The invention relates to a device for purifying lead carbonate from lead-containing compounds, in particular to a device for purifying lead carbonate from desulfurized lead-containing compounds in the recycling process of waste lead plaster.
背景技术Background technique
目前，蓄电池废铅膏的数量庞大，如若直接掩埋处理，其中的重金属离子将对土壤产生破坏，污染生态；同时由蓄电池废铅膏中提取出来的碳酸铅具有较大的回收利用价值,应用领域广泛。At present, there is a huge amount of waste battery lead paste. If it is directly buried, the heavy metal ions in it will damage the soil and pollute the ecology; at the same time, the lead carbonate extracted from the waste lead paste of battery has a great recycling value. Application fields widely.
例如，在固体推进剂中广泛采用碳酸铅为燃烧催化剂,但是失水碳酸铅为块状固体,需经过粉碎、水洗、研磨、过筛后才能应用, 另外,使用过程中发现，不同厂家，不同批次的碳酸铅的催化活性差异很大，因此研究适宜的合成方法，通过严格控制工艺条件, 直接获得超细碳酸铅。解决不同批次碳酸铅的催化活性差异的问题具有重要的意义。For example, lead carbonate is widely used as a combustion catalyst in solid propellants, but dehydrated lead carbonate is a massive solid that can only be applied after crushing, washing, grinding, and sieving. In addition, it was found during use that different manufacturers have different The catalytic activity of batches of lead carbonate varies greatly. Therefore, suitable synthesis methods are studied, and ultrafine lead carbonate can be directly obtained by strictly controlling the process conditions. It is of great significance to solve the problem of the difference in catalytic activity of different batches of lead carbonate.
另外现如今采用的固液分离装置为旋液分离器，市价昂贵，如果能改进提纯碳酸铅过程中的固液分离方式，不仅减少了成本，同时提升了实验的可操作性。In addition, the solid-liquid separation device currently used is a hydrocyclone, which is expensive in the market. If the solid-liquid separation method in the process of purifying lead carbonate can be improved, it will not only reduce the cost, but also improve the operability of the experiment.
发明内容Contents of the invention
本发明的目的在于：针对现有技术的缺陷，提出了一种结构简单、设计合理的用于含铅化合物中提纯碳酸铅的装置，可以解决实验室制备超细碳酸铅装置较贵和搅拌桨难以清洗的问题，而且可以利用溶液循环电泵将反应液体循环过滤得到充分沉淀，提高实验的精度和可操作性。The object of the invention is: aim at the defect of prior art, propose a kind of simple in structure, the device that is used for purifying lead carbonate in lead-containing compound rationally, can solve laboratory preparation superfine lead carbonate device expensive and agitating paddle It is difficult to clean the problem, and the solution circulation electric pump can be used to circulate and filter the reaction liquid to obtain sufficient precipitation, which improves the accuracy and operability of the experiment.
本发明所采用的技术方案是：一种用于含铅化合物中提纯碳酸铅的装置，包括反应釜、溶液循环装置、底座、中空三通管道和结晶滤网，所述的底座上设有溶液循环装置，溶液循环装置的上方设有反应釜，反应釜通过中空三通管道和溶液循环装置相连，所述的结晶滤网位于溶液循环装置内；所述的反应釜直壁圆筒形结构，反应釜内设有过滤网、搅拌器和搅拌器电机，将废铅膏（碳酸铅、二氧化铅、氧化铅等含铅化合物）固体置于过滤网上，向反应釜中加入稀硝酸(HNO3)和双氧水（H2O2），使其与废铅膏固体反应，利用搅拌器电机驱动搅拌器的叶片，加快溶液流动，获得含Pb2+的溶液；同时，将搅拌器设置在过滤网下方为了使搅拌器叶片和废铅膏固体分离，从而保护搅拌器的叶片不受损坏。The technical solution adopted in the present invention is: a device for purifying lead carbonate in lead-containing compounds, including a reaction kettle, a solution circulation device, a base, a hollow three-way pipeline and a crystallization filter, and the base is provided with a solution Circulation device, a reaction kettle is provided above the solution circulation device, and the reaction kettle is connected to the solution circulation device through a hollow tee pipe, and the crystallization filter is located in the solution circulation device; the straight wall cylindrical structure of the reaction kettle, The reaction kettle is equipped with a filter screen, agitator and agitator motor. Put the solid waste lead paste (lead carbonate, lead dioxide, lead oxide and other lead-containing compounds) on the filter screen, and add dilute nitric acid (HNO 3 ) and hydrogen peroxide (H 2 O 2 ) to make it react with waste lead paste solids, use the stirrer motor to drive the blades of the stirrer, speed up the flow of the solution, and obtain a solution containing Pb 2+ ; at the same time, set the stirrer on the filter The bottom is to separate the agitator blades from the waste lead paste solids, so as to protect the agitator blades from damage.
在本发明中：所述的中空三通管道的一个通道与反应釜的侧壁相连，另一通道与下方的溶液循环装置相连，第三个通道的开口于空气中，其中含Pb2+的溶液从反应釜内侧壁的中空三通管道的一个入口进入，通过竖直的中空三通管道流入下方溶液循环装置，在中空三通管道内配合上部为弧形结构的钩形提手，钩形提手下方设置有结晶滤网；从中空三通管道置于空气中的开口，向其中加入碳酸钠（Na2CO3），碳酸钠（Na2CO3）落在结晶滤网上，进入溶液循环装置的含Pb2+的溶液在管道中循环，连续接触结晶滤网上的碳酸钠（Na2CO3），使之产生碳酸铅沉淀，得到碳酸铅结晶。In the present invention: one passage of the hollow tee pipe is connected with the side wall of the reaction kettle, another passage is connected with the solution circulation device below, and the opening of the third passage is in the air, wherein Pb 2+ The solution enters from an inlet of the hollow three-way pipe on the inner wall of the reactor, and flows into the solution circulation device below through the vertical hollow three-way pipe. There is a crystallization filter under the handle; add sodium carbonate (Na 2 CO 3 ) into it from the opening of the hollow three-way pipe placed in the air, and the sodium carbonate (Na 2 CO 3 ) falls on the crystallization filter and enters the solution circulation The solution containing Pb 2+ in the device circulates in the pipeline, and continuously contacts the sodium carbonate (Na 2 CO 3 ) on the crystallization filter to cause lead carbonate to precipitate and obtain lead carbonate crystals.
在本发明中：所述的溶液循环装置包括溶液循环电泵和循环管道，含Pb2+的溶液从中空三通管道中进入溶液循环装置，在溶液循环电泵的驱动下，在循环管道中呈顺时针方向循环流动，其流动方向与结晶滤网的上表面相垂直，指向结晶滤网的下方；在循环过程中，含Pb2+的溶液与结晶滤网上的碳酸钠（Na2CO3）固体充分反应，不断生成碳酸铅沉淀，结晶于结晶滤网上；所述的循环管道内设有供结晶滤网放置的台阶，处于循环管道的截面处；在溶液循环装置中，循环管道采用圆形管道循环的设计，溶液在循环的过程中更加充分反应，使溶液来回不断的触碰结晶滤网，将沉淀充分打在滤网上，获得沉淀碳酸铅。In the present invention: the solution circulation device includes a solution circulation electric pump and a circulation pipeline, the solution containing Pb enters the solution circulation device from the hollow three - way pipeline, and under the drive of the solution circulation electric pump, in the circulation pipeline It circulates in a clockwise direction, and its flow direction is perpendicular to the upper surface of the crystallization filter, pointing to the bottom of the crystallization filter; during the circulation process, the solution containing Pb 2+ and the sodium carbonate (Na 2 CO 3 ) The solid fully reacts, continuously generates lead carbonate precipitates, and crystallizes on the crystallization filter; the circulation pipeline is provided with a step for placing the crystallization filter, which is at the cross section of the circulation pipeline; in the solution circulation device, the circulation pipeline adopts a circular With the design of circular pipeline circulation, the solution reacts more fully during the circulation process, so that the solution continuously touches the crystallization filter back and forth, and the precipitate is fully hit on the filter to obtain precipitated lead carbonate.
在本发明中：与中空三通管道配合的钩形提手采用弯型手柄设计，与结晶滤网相连配合，便可直接拿出超细PbCO3产物，结晶滤网与循环管道不必紧密贴合，防止沉淀过多时，拿出会有液体渗出；所述的循环管道的左下方设有一排液口，当反应到析不出产物碳酸铅时（即循环管道中的溶液中Pb2+已完全沉淀为碳酸铅结晶），便可以通过排液口将其排出。In the present invention: the hook-shaped handle matched with the hollow tee pipe adopts a curved handle design, and is connected with the crystallization filter to directly take out the ultra-fine PbCO 3 product, and the crystallization filter and the circulation pipeline do not need to be closely attached , when preventing too much precipitation, there will be liquid oozing out; the lower left side of the circulation pipeline is provided with a liquid outlet, when the reaction is to separate out the product lead carbonate (that is, the Pb in the solution in the circulation pipeline has already Completely precipitated as lead carbonate crystals), it can be discharged through the drain port.
采用上述技术方案后，本发明的有益效果为：本发明结构简单、设计合理，使用稀硝酸（HNO3）浸取，并用双氧水（H2O2）的工艺，能获得纯度较高的超细碳酸铅结晶，从而解决不同批次碳酸铅催化活性差异的问题，使用钩型提手拿取沉淀方便操作，同时节约实验开销，采用循环管道使反应物充分接触反应，提高实验的精度和可操作性，具有很好的普及应用前景。After adopting the above-mentioned technical scheme, the beneficial effects of the present invention are: the present invention has simple structure and reasonable design, and can obtain high-purity ultra- fine Lead carbonate is crystallized to solve the problem of differences in the catalytic activity of different batches of lead carbonate. It is convenient to use the hook-shaped handle to pick up the precipitate, and at the same time save the cost of the experiment. The circulation pipeline is used to make the reactants fully contact and react, which improves the accuracy and operability of the experiment. It has a good prospect of popularization and application.
附图说明Description of drawings
图1为本发明的结构示意图；Fig. 1 is a structural representation of the present invention;
图2为本发明另一结构示意图；Fig. 2 is another structural representation of the present invention;
图3为本发明中反应釜的内部示意图；Fig. 3 is the internal schematic diagram of reactor among the present invention;
图4为本发明中的中空三通管道的连接示意图；Fig. 4 is the connection schematic diagram of hollow tee pipe among the present invention;
图5为本发明的钩形提手与结晶滤网结合示意图。Fig. 5 is a schematic diagram of the combination of the hook-shaped handle and the crystallization filter of the present invention.
图中：1.过滤网；2.搅拌器；3.搅拌器电机；4.反应釜；5.钩形提手；6.中空三通管道；7.结晶滤网；8.溶液循环电泵；9.循环管道；10.底座；11.排液口；12.溶液循环装置。In the figure: 1. filter screen; 2. agitator; 3. agitator motor; 4. reaction kettle; 5. hook handle; 6. hollow tee pipe; 7. crystallization filter; 8. solution circulation electric pump ; 9. Circulation pipeline; 10. Base; 11. Drain port; 12. Solution circulation device.
具体实施方式Detailed ways
下面将结合附图对本发明作进一步的说明。The present invention will be further described below in conjunction with the accompanying drawings.
由图1-5可见，一种用于含铅化合物中提纯碳酸铅的装置，包括反应釜4、溶液循环装置12、底座10、中空三通管道6和结晶滤网7，所述的底座10上设有溶液循环装置12，溶液循环装置12的上方设有反应釜4，反应釜4通过中空三通管道6和溶液循环装置12相连，所述的结晶滤网7位于溶液循环装置12内；所述的反应釜4直壁圆筒形结构，反应釜4内设有过滤网1、搅拌器2和搅拌器电机3，将废铅膏（碳酸铅、二氧化铅、氧化铅等含铅化合物）固体置于过滤网1上，向反应釜4中加入稀硝酸(HNO3)和双氧水（H2O2），使其与废铅膏固体反应，利用搅拌器电机3驱动搅拌器2的叶片，加快溶液流动，获得含Pb2+的溶液；同时，将搅拌器2设置在过滤网1下方为了使搅拌器2的叶片和废铅膏固体分离，从而保护搅拌器2的叶片不受损坏。As can be seen from Figures 1-5, a device for purifying lead carbonate in lead-containing compounds includes a reaction kettle 4, a solution circulation device 12, a base 10, a hollow tee pipe 6 and a crystallization filter screen 7, and the base 10 A solution circulation device 12 is arranged on it, and a reactor 4 is arranged above the solution circulation device 12. The reactor 4 is connected to the solution circulation device 12 through a hollow three-way pipeline 6, and the crystallization filter screen 7 is located in the solution circulation device 12; Described reaction kettle 4 straight wall cylindrical structures, are provided with filter screen 1, agitator 2 and agitator motor 3 in the reaction kettle 4, lead-containing compounds such as waste lead plaster (lead carbonate, lead dioxide, plumbous oxide) ) solid on the filter screen 1, add dilute nitric acid (HNO 3 ) and hydrogen peroxide (H 2 O 2 ) into the reaction kettle 4 to make it react with the waste lead plaster solid, and use the stirrer motor 3 to drive the blade of the stirrer 2 , to speed up the flow of the solution to obtain a solution containing Pb 2+ ; at the same time, the agitator 2 is arranged below the filter screen 1 in order to separate the blades of the agitator 2 from the waste lead paste solids, thereby protecting the blades of the agitator 2 from damage.
所述的中空三通管道6的一个通道与反应釜4的侧壁相连，另一通道与下方的溶液循环装置12相连，第三个通道的开口于空气中，其中含Pb2+的溶液从反应釜4内侧壁的中空三通管道6的一个入口进入，通过竖直的中空三通管道6流入下方溶液循环装置12，在中空三通管道6内配合上部为弧形结构的钩形提手5，钩形提手5下方设置有结晶滤网7；从中空三通管道6置于空气中的开口，向其中加入碳酸钠（Na2CO3），碳酸钠（Na2CO3）落在结晶滤网7上，进入溶液循环装置12的含Pb2+的溶液在管道中循环，连续接触结晶滤网7上的碳酸钠（Na2CO3），使之产生碳酸铅沉淀，得到碳酸铅结晶。A passage of the described hollow three-way pipe 6 is connected with the side wall of the reaction kettle 4, another passage is connected with the solution circulation device 12 below, and the opening of the third passage is in the air, wherein the solution containing Pb 2+ from One entrance of the hollow three-way pipe 6 on the inner wall of the reaction kettle 4 enters, and flows into the lower solution circulation device 12 through the vertical hollow three-way pipe 6, and the upper part of the hollow three-way pipe 6 is equipped with a hook-shaped handle with an arc structure 5. There is a crystallization filter 7 under the hook handle 5; from the opening of the hollow three-way pipe 6 placed in the air, add sodium carbonate (Na 2 CO 3 ) into it, and the sodium carbonate (Na 2 CO 3 ) falls on the On the crystallization filter 7, the solution containing Pb 2+ that enters the solution circulation device 12 circulates in the pipeline, and continuously contacts the sodium carbonate (Na 2 CO 3 ) on the crystallization filter 7 to cause lead carbonate to precipitate to obtain lead carbonate crystallization.
所述的溶液循环装置12包括溶液循环电泵8和循环管道9，含Pb2+的溶液从中空三通管道6中进入溶液循环装置12，在溶液循环电泵8的驱动下，在循环管道9中呈顺时针方向循环流动，其流动方向与结晶滤网7的上表面相垂直，指向结晶滤网7的下方；在循环过程中，含Pb2+的溶液与结晶滤网7上的碳酸钠（Na2CO3）固体充分反应，不断生成碳酸铅沉淀，结晶于结晶滤网7上；所述的循环管道9内设有供结晶滤网7放置的台阶，处于循环管道9的截面处；在溶液循环装置12中，循环管道9采用圆形管道循环的设计，溶液在循环的过程中更加充分反应，使溶液来回不断的触碰结晶滤网7，将沉淀充分打在结晶滤网7上，获得沉淀碳酸铅。Described solution circulation device 12 comprises solution circulation electric pump 8 and circulation pipe 9, and the solution containing Pb enters solution circulation device 12 from hollow tee pipe 6, under the drive of solution circulation electric pump 8, in circulation pipe In 9, it circulates in a clockwise direction, and its flow direction is perpendicular to the upper surface of the crystallization filter screen 7, pointing to the bottom of the crystallization filter screen 7; The sodium (Na 2 CO 3 ) solid fully reacts to continuously generate lead carbonate precipitates, which crystallize on the crystallization filter 7; the circulation pipeline 9 is provided with a step for placing the crystallization filter 7, which is at the cross section of the circulation pipeline 9 ; In the solution circulation device 12, the circulation pipeline 9 adopts the design of circular pipeline circulation, and the solution reacts more fully in the process of circulation, so that the solution continuously touches the crystallization filter screen 7 back and forth, and the precipitation is fully hit on the crystallization filter screen 7 On, precipitated lead carbonate is obtained.
与中空三通管道6配合的钩形提手5采用弯型手柄设计，与结晶滤网7相连配合，便可直接拿出超细PbCO3产物，结晶滤网7与循环管道9不必紧密贴合，防止沉淀过多时，拿出会有液体渗出；所述的循环管道9的左下方设有一排液口11，当反应到析不出产物碳酸铅时（即循环管道中的溶液中Pb2+已完全沉淀为碳酸铅结晶），便可以通过排液口11将其排出。The hook-shaped handle 5 matched with the hollow three-way pipe 6 adopts a curved handle design, and is connected with the crystallization filter 7 to directly take out the ultrafine PbCO 3 product, and the crystallization filter 7 and the circulation pipe 9 do not need to be closely attached , when preventing too much precipitation, take out and have liquid to ooze out; The lower left side of described circulation pipe 9 is provided with a liquid outlet 11, when reacting to not separating out product plumbous carbonate (that is, in the solution in the circulation pipe Pb 2 + has been completely precipitated as lead carbonate crystals), it can be discharged through the drain port 11.
如图4所示，含Pb2+的溶液从上方反应釜4中经由中空三通管道6流入下方溶液循环装置12中，最终使Pb2+沉淀于结晶滤网上。As shown in Figure 4, the solution containing Pb 2+ flows from the upper reactor 4 through the hollow three-way pipe 6 into the lower solution circulation device 12, and finally the Pb 2+ is precipitated on the crystallization filter.
在反应釜4中发生的主要反应方程式为：The main reaction equation that takes place in reactor 4 is:
2HNO3（稀）+2PbO=2Pb(NO3)2+H2O； PbCO3+2HNO3=Pb（NO3)2+H2O+CO2；2HNO 3 (dilute)+2PbO=2Pb(NO 3 ) 2 +H 2 O; PbCO 3 +2HNO 3 =Pb(NO 3 ) 2 +H 2 O+CO 2 ;
H2O2+PbO2+2HNO3=Pb(NO3)2+2H2O+O2；H 2 O 2 +PbO 2 +2HNO 3 =Pb(NO 3 ) 2 +2H 2 O+O 2 ;
Pb3(CO3)2(OH)2+6HNO3=3Pb(NO3)2+3H2O+2CO2；Pb 3 (CO 3 ) 2 (OH) 2 +6HNO 3 =3Pb(NO 3 ) 2 +3H 2 O+2CO 2 ;
在这一系列反应发生后，得到的二价铅溶液流向中空三通管道6，通过结晶滤网7，在循环管道9处不断循环，此时向中空三通管道6上方通口加碳酸钠固体或溶液使二价铅溶液与碳酸钠发生反应，主要反应方程式为：After this series of reactions took place, the divalent lead solution obtained flows to the hollow tee pipe 6, passes through the crystallization filter screen 7, and circulates continuously at the circulation pipe 9. Or the solution makes divalent lead solution react with sodium carbonate, and the main reaction equation is:
Pb(NO3)2+Na2CO3=PbCO3+2NaNO3，之后，获得的提纯后的PbCO3固体被拦截在结晶滤网7处，溶液通过循环管道9不断充分反应，达到一定程度，将钩形提手5从中空三通管道6拿出，得到提纯后的超细碳酸铅。Pb(NO 3 ) 2 +Na 2 CO 3 =PbCO 3 +2NaNO 3 , after that, the obtained purified PbCO 3 solid is intercepted at the crystallization filter 7, and the solution is fully reacted continuously through the circulation pipeline 9 to a certain extent, The hook-shaped handle 5 is taken out from the hollow tee pipe 6 to obtain the purified ultrafine lead carbonate.
以上对本发明的具体实施方式进行了描述，但本发明并不限于以上描述。对于本领域的技术人员而言，任何对本技术方案的同等修改和替代都是在本发明的范围之中。因此，在不脱离本发明的精神和范围下所作的均等变换和修改，都应涵盖在本发明的范围内。The specific embodiments of the present invention have been described above, but the present invention is not limited to the above description. For those skilled in the art, any equivalent modifications and substitutions to the technical solutions are within the scope of the present invention. Therefore, equivalent changes and modifications made without departing from the spirit and scope of the present invention shall fall within the scope of the present invention.
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