CN209735020U - High-acidity thermal crystalline substance continuous crystallization device - Google Patents
High-acidity thermal crystalline substance continuous crystallization device Download PDFInfo
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- CN209735020U CN209735020U CN201822090694.9U CN201822090694U CN209735020U CN 209735020 U CN209735020 U CN 209735020U CN 201822090694 U CN201822090694 U CN 201822090694U CN 209735020 U CN209735020 U CN 209735020U
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Abstract
A high-acidity thermal crystalline substance continuous crystallization device comprises a steam heater (1), a crystallizer (2), a high-efficiency concentration evaporator (3) and an automatic control system, wherein an axial liquid inlet pipe (4) is arranged at the lower part of the crystallizer, a coaxial guide pipe (5) extending to the top of the crystallizer is covered at the top of the liquid inlet pipe, the steam heater is connected to a feeding port of the axial liquid inlet pipe of the crystallizer through a liquid inlet pipeline (6), the crystallizer and the high-efficiency concentration evaporator are connected through a section of straight pipe (7), and a crystal separation discharging port (10) is arranged at the bottom of the crystallizer; the top of the high-efficiency concentration evaporator is provided with a steam outlet (8) and a vacuum pump (11), and a material transferring circulation pipeline (9) is connected between the upper part of the high-efficiency concentration evaporator and the steam heater. The utility model discloses can realize the concentrated crystallization serialization of high acidity heat crystallinity material, can guarantee the stable in process, device high efficiency operation improves production efficiency, reduces workman intensity of labour, promotes the improvement product quality.
Description
Technical Field
The utility model relates to a chemical industry separation and purification technical field, concretely relates to high acidity heat crystallinity thing concentration crystallization device.
Background
The traditional DTB crystallization device is only suitable for the crystallization separation of cold crystallization physical substances, but not suitable for hot crystallization physical substances, because the traditional DTB crystallization device pumps hot saturated material liquid to a cooling zone to carry out cooling crystallization, and the hot crystallization physical substances cause the dissolution of product crystals through cooling, so that the expected effect is not achieved. The existing high-acidity concentrated crystallization of thermal crystalline substances is mostly intermittent concentrated crystallization, because when the temperature difference is not formed between an evaporator and a feed liquid of a crystallizer, the thermal saturated feed liquid is easy to crystallize in a steam heater to block pipelines, so that continuous heating and evaporation can not be carried out, continuous heating and crystallization can not be carried out, intermittent concentrated crystallization can only be carried out by integrally heating a crystallization kettle, automatic control is not easy to realize, the continuity of concentrated crystallization is difficult to realize, the efficiency of the crystallization process is low, the labor intensity of workers is high, and the problems of high quality fluctuation, unstable product quality and the like can be brought by human factors, the strong acidity of the feed liquid has high corrosivity on equipment, and the thermal crystalline substance crystallization separation technology needs to be improved.
Disclosure of Invention
The utility model discloses the purpose is to solve the problem that above-mentioned prior art exists, provides a high acidity heat crystallinity nature material continuous crystallization device to realize the concentrated crystallization serialization of high acidity heat crystallinity nature material, improve production efficiency, reduce workman intensity of labour, promote and improve the product quality.
The purpose of the utility model is realized through the following technical scheme:
A high-acidity thermal crystalline substance continuous crystallization device comprises a steam heater, a crystallizer, a high-efficiency concentration evaporator and an automatic control system, wherein an axial liquid inlet pipe is arranged at the lower part of the center of the crystallizer, a guide pipe which extends to the top of the crystallizer and has the same axis is covered at the top of the liquid inlet pipe, a liquid outlet of the steam heater is connected with a bottom feed inlet of the axial liquid inlet pipe of the crystallizer through a liquid inlet pipeline, a liquid outlet at the top of the crystallizer is connected with a liquid inlet at the bottom of the high-efficiency concentration evaporator through a section of straight pipe, and a crystal separation discharge port is arranged at the; the top of the high-efficiency concentration evaporator is provided with a steam outlet which is connected with a vacuum pump, and a material transferring circulation pipeline is connected between the upper part of the high-efficiency concentration evaporator and the steam heater; a liquid level meter and a thermometer are arranged on the crystallizer, a steam control valve is arranged at an air inlet of a steam pipeline of the steam heater, a raw material liquid feeding pump is arranged on a liquid inlet pipeline, and a circulating material transferring pump is arranged on a material transferring circulating pipeline; and the vacuum pump, the liquid level meter, the steam control valve, the thermometer, the raw material liquid feeding pump and the circulating material transferring pump are all connected with an automatic control system.
The utility model discloses be connected with the circulation line who takes the circulating pump between crystallizer lower part and high-efficient concentration evaporator upper portion. The exhaust port of the MVR vapor compression device is connected with the vapor heater through a vapor return pipeline. The steam heater, the crystallizer, the high-efficiency concentration evaporator, the straight pipe, the axial liquid inlet pipe, the flow guide pipe, the liquid inlet pipeline, the material transferring circulation pipeline and the circulation pipeline are all made of strong acid corrosion resistant materials, including but not limited to silicon carbide, G30, graphite and enamel. And the vacuum pump, the raw material liquid feeding pump and the circulating material transferring pump all adopt acid and alkali resistant pumps.
The utility model discloses the device during operation, open the vacuum pump evacuation earlier, make the whole equipment start work under vacuum state, open raw material liquid charge pump, make the feed liquid in the heater get into the crystallizer, control system control raw material liquid charge pump stops when the liquid level risees in the crystallizer and reaches the setting value, open circulation commentaries on classics material pump simultaneously, open the steam control valve simultaneously, steam gets into the heater, feed liquid heating heaies up in the heater for, the feed liquid of heating gets into the crystallizer from the feed liquor pipeline, start evaporating when the material temperature reaches the boiling point that the vacuum corresponds, the material feeds back to control system through the thermometer after reaching evaporating temperature, the steam control valve is closed promptly (when the material temperature is less than evaporating temperature, the steam control valve is automatic opening promptly). The straight pipe of connecting crystallizer and high-efficient concentrated evaporimeter has formed the necking down section between crystallizer and high-efficient concentrated evaporimeter, plays pressure control's effect, forms the boiling point difference through the liquid level difference in elevation, and the interior high fever feed liquid of crystallizer evaporates under the evaporimeter is vacuum state and forms tiny crystalline substance, and tiny crystalline substance sinks to the crystallizer gradually at the continuous increase in-process of gravity, through crystal settlement growth and thermal crystallization characteristic, further grows up in the higher crystallizer of temperature, forms better crystal. The temperature of the bottom of the crystallizer is higher than the temperature of the top of the crystallizer, the temperature of the evaporator is lower than the temperature of the top of the crystallizer, when feed liquid which is not crystallized rises to the high-efficiency concentration evaporator, the temperature of the feed liquid does not reach the condition of evaporative crystallization, the feed liquid returns to the steam heater through the feed transfer circulation pipeline and is heated, and the feed liquid forms closed circulation evaporative continuous crystallization among the evaporator, the steam heater and the crystallizer. The flow guide pipe can ensure that small crystal grains with small weight are lifted to the liquid level along the flow guide pipe along with the feed liquid while guiding the flow, and the crystal slowly grows to reach a certain weight and then sinks to the bottom of the crystallizer along the flow guide pipe. When the device is operated until the crystal amount in the crystallizer reaches the requirement, the crystal separation discharge port is opened through the control system to realize the crystal separation.
The utility model discloses according to hot crystal material attribute, adopt anti-DTB cold crystal material attribute to design, high-efficient concentrated evaporimeter passes through liquid level pressure device with the crystallizer and is the straight tube control promptly, makes the material temperature in the high-efficient concentrated evaporimeter be less than the material temperature in the crystallizer, provides the condition for hot crystal property material crystal growth. The utility model discloses in returning the feed liquid that the temperature reduces back to steam heater again, can avoid because the hot crystallization pipeline forms the problem of jam in the heater, realize the crystallization control of continuous concentration.
The utility model discloses can realize the concentrated crystallization serialization of high acidity heat crystallinity material, can guarantee the stable in process, device high efficiency operation improves production efficiency, reduces workman intensity of labour, promotes the improvement product quality.
Drawings
Fig. 1 is a schematic view of the present invention.
Detailed Description
the continuous crystallization device for high-acidity thermal crystalline substance shown in fig. 1 comprises a steam heater 1 for heating feed liquid, a crystallizer 2 connected with the steam heater, a high-efficiency concentration evaporator 3 positioned above the crystallizer and an automatic control system. Be provided with axial feed liquor pipe 4 in crystallizer center lower part, be covered with at the feed liquor pipe top and extend to the honeycomb duct 5 of the same axle center at the crystallizer top, steam heater 1's liquid outlet passes through inlet pipe 6 and connects in the bottom feed inlet 4a of crystallizer axial feed liquor pipe 4, the top liquid outlet of crystallizer 2 is connected through one section straight tube 7 with the inlet of high-efficient concentrated evaporimeter 3 bottom, and the effect of straight tube 7 is with evaporimeter and crystallizer intercommunication, control liquid level height to form the liquid boiling point difference of evaporimeter and crystallizer. A crystal separation discharge port 10 is arranged at the bottom of the crystallizer; a steam outlet 8 is formed in the top of the high-efficiency concentration evaporator 3, the steam outlet 8 is connected with a vacuum pump 11, and a material transferring circulation pipeline 9 is connected between the upper part of the high-efficiency concentration evaporator 3 and the steam heater 1; a liquid level meter 12 and a thermometer 14 are arranged on the crystallizer, a steam control valve 21 is arranged at the air inlet of a steam pipeline of the steam heater 1, a raw material liquid feeding pump 15 is arranged on the liquid inlet pipeline 6, and a circulating material transferring pump 16 is arranged on the material transferring circulating pipeline 9; and the vacuum pump 11, the liquid level meter 12, the steam control valve 21, the thermometer 14, the raw material liquid feeding pump 15 and the circulating material transferring pump 16 are all connected with an automatic control system.
the utility model discloses the device during operation opens vacuum pump 11 evacuation earlier, and the back begins to work under the whole equipment is inside to be in vacuum state. Starting a raw material liquid feeding pump 15 to enable the material liquid in a steam heater 1 to enter a crystallizer 2, when a liquid level meter 12 detects that the liquid level in the crystallizer rises to reach a set value, a control system controls the raw material liquid feeding pump to stop, at the moment, a circulating material transferring pump 16 is started, meanwhile, a steam control valve 21 is started, steam enters the steam heater to heat the material liquid in the steam heater, the heated material liquid enters the crystallizer from a liquid inlet pipeline, evaporation is started when the temperature of the material liquid reaches a boiling point corresponding to a vacuum degree, the material liquid is fed back to the control system through a thermometer 14 after reaching an evaporation temperature, the steam control valve 21 is closed, and when the temperature of the material liquid is lower than the evaporation temperature, the steam control valve is automatically. Under the action of vacuum negative pressure, the feed liquid continuously rises from the crystallizer along the straight pipe 7. Connect straight tube 7 of crystallizer and high-efficient concentrated evaporimeter to have formed the necking down section between crystallizer and high-efficient concentrated evaporimeter, be equivalent to a liquid level pressure differential device, form the liquid level difference of elevation between crystallizer and high-efficient concentrated evaporimeter through straight tube 7, thereby form the boiling point difference of feed liquid, it evaporates under high-efficient concentrated evaporimeter is vacuum state to make the interior high fever feed liquid of crystallizer form tiny crystalline substance, tiny crystalline substance is crescent at the in-process weight that continuous crystallization is grown, sink to the crystallizer bottom gradually under the action of gravity, and further grow up in the higher crystallizer of temperature, form better crystal. The temperature of the bottom of the crystallizer is higher than the temperature of the top of the crystallizer, the temperature of the evaporator is lower than the temperature of the top of the crystallizer, when the feed liquid which is not crystallized rises to the high-efficiency concentration evaporator, the temperature of the feed liquid can not reach the condition of evaporative crystallization, and the feed liquid is returned to the steam heater 1 by the circulating material transfer pump 16 through the material transfer circulating pipeline 9 to be heated, so that the feed liquid forms the evaporative continuous crystallization of closed circulation among the evaporator, the steam heater and the crystallizer. The flow guide pipe 5 can ensure that fine crystal grains with small weight are lifted to the liquid level along the flow guide pipe along with feed liquid while guiding the flow, and the crystal slowly grows to reach a certain weight and then sinks to the bottom of the crystallizer along the flow guide pipe. When the whole set of device works and operates until the crystal amount in the crystallizer reaches the required amount, the control system opens the crystal separation discharge port 10 to realize crystal separation, and the separated crystals (the separated crystals are the mixture of liquid and crystals at this time) are put into a centrifuge to remove the liquid, so that the required all-solid-state crystals are obtained.
The utility model discloses still be connected with the circulating line 17 of taking circulating pump 18 between crystallizer 2 lower part and high-efficient concentrated evaporimeter upper portion. When the granularity of the settled crystals in the crystallizer is too small and can not meet the required requirement, the mixed material of the small crystals and the liquid at the bottom of the crystallizer (the material at the bottom of the crystallizer is the mixture of the settled crystals and the feed liquid in the running process of the device) is pumped into the high-efficiency concentration evaporator 3 by the circulating pump and is returned to the steam heater 1 for heating and crystallization again through the material transferring and circulating pipeline 9. Except that the steam discharge port 8 at the top of the high-efficiency concentration evaporator 3 is connected with the vacuum pump 11, the rear end of the vacuum pump is also connected with the MVR steam compression device 19 through the exhaust pipeline 13, the exhaust port of the MVR steam compression device 19 is connected with the steam heater through the steam return pipeline 20, and hot steam compressed by the MVR steam compression device 19 can be returned to the steam heater 1 through the steam return pipeline 20, so that high efficiency and energy conservation are realized.
The utility model discloses a main part is like steam heater 1, crystallizer 2, high-efficient concentrated evaporimeter 3, straight tube 7, axial feed liquor pipe 4, honeycomb duct 5, feed liquor pipeline 6, commentaries on classics material circulating line 9, circulating line 17 etc. all adopt strong acid corrosion resistant's material preparation, like carborundum, G30, graphite, enamel etc.. The vacuum pump 11, the raw material liquid feeding pump 15 and the circulating material transferring pump 16 are all acid and alkali resistant pumps. The inner walls of all pipelines need to be smooth, and high-acidity thermal crystalline substance crystals are not easy to adhere.
The utility model discloses a steam heater, crystallizer, high-efficient concentrated evaporimeter, MVR vapor compression device all can adopt prior art equipment. The control system adopts a PLC control system.
Adopt the utility model discloses a production example that the device carries out stannous sulfate's concentrated crystallization is as follows:
The acidity of sulfuric acid is 35g/L, Sn2+ stannous sulfate solution with the concentration of 70g/L is used as original solution, when the working is started, the vacuum degree is set to be 0.05MPa through a PLC control system, and the temperature of an efficient concentration evaporator is set to be 70 ℃; starting a vacuum pump to vacuumize, starting a feed pump of the raw material liquid to enable the stannous sulfate liquid to enter a heater and a crystallizer, stopping the feed pump of the raw material liquid when the liquid level in the crystallizer rises to a designed value, and simultaneously starting a circulating material transferring pump to circulate, wherein the liquid level of the material in the crystallizer is controlled by a liquid level meter; at the moment, the steam control valve is opened to carry out heat exchange on the materials in the heater, the materials are evaporated when the temperature of the materials reaches the boiling point corresponding to the vacuum degree, the evaporation temperature of the materials is used as a feedback signal, and when the temperature of the materials is increased to the evaporation temperature by steam, the steam control valve is automatically closed. When the temperature of the material is lower than the evaporation temperature, the steam control valve is automatically opened; when the operation concentration is carried out until the acidity of sulfuric acid is 110g/L, continuous crystal separation is realized, and the separated crystals are put into a centrifugal machine to centrifugally remove liquid under the control of a control system to obtain stannous sulfate crystals.
Claims (6)
1. A high-acidity thermal crystalline substance continuous crystallization device is characterized by comprising a steam heater (1), a crystallizer (2), a high-efficiency concentration evaporator (3) and an automatic control system, wherein an axial liquid inlet pipe (4) is arranged at the lower part of the center of the crystallizer, a coaxial guide pipe (5) extending to the top of the crystallizer is covered at the top of the liquid inlet pipe, a liquid outlet of the steam heater (1) is connected with a bottom feeding hole (4a) of the axial liquid inlet pipe (4) of the crystallizer through a liquid inlet pipeline (6), a top liquid outlet of the crystallizer (2) is connected with a liquid inlet at the bottom of the high-efficiency concentration evaporator (3) through a section of straight pipe (7), and a crystal separation discharging hole (10) is formed at the bottom of the crystallizer; a steam outlet (8) is arranged at the top of the high-efficiency concentration evaporator (3), the steam outlet is connected with a vacuum pump (11), and a material transferring circulation pipeline (9) is connected between the upper part of the high-efficiency concentration evaporator (3) and the steam heater (1); a liquid level meter (12) and a thermometer (14) are arranged on the crystallizer, a steam control valve (21) is arranged at the air inlet of a steam pipeline of the steam heater (1), a raw material liquid feeding pump (15) is arranged on a liquid inlet pipeline (6), and a circulating material transferring pump (16) is arranged on a material transferring circulating pipeline (9); the vacuum pump (11), the liquid level meter (12), the steam control valve (21), the thermometer (14), the raw material liquid feeding pump (15) and the circulating material transferring pump (16) are all connected with an automatic control system.
2. The continuous crystallizing device of high acidity thermal crystalline substance according to claim 1, wherein a circulating line (17) with a circulating pump (18) is connected between the lower part of the crystallizer (2) and the upper part of the high efficiency concentration evaporator (3).
3. The continuous crystallization device for high acidity hot crystalline substance as claimed in claim 1 or 2, wherein the vapor discharge port (8) at the top of the high efficiency concentration evaporator (3) is connected to the MVR vapor compression device (19) through the exhaust line (13).
4. The apparatus for continuously crystallizing a highly acidic hot crystalline substance as claimed in claim 3, wherein the exhaust port of the MVR vapor compression device (19) is connected to the vapor heater (1) through a vapor return line (20).
5. The continuous crystallization device for high-acidity thermal crystalline substance according to claim 1, wherein the steam heater (1), the crystallizer (2), the high-efficiency concentration evaporator (3), the straight pipe (7), the axial liquid inlet pipe (4), the draft tube (5), the liquid inlet pipeline (6), the material transfer circulation pipeline (9) and the circulation pipeline (17) are all made of materials resistant to strong acid corrosion, including but not limited to silicon carbide, G30, graphite and enamel.
6. The apparatus for continuous crystallization of a highly acidic thermally crystalline substance as set forth in claim 1, wherein the vacuum pump (11), the raw material liquid feed pump (15), and the circulation transfer pump (16) are acid-base pumps.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201822090694.9U CN209735020U (en) | 2018-12-13 | 2018-12-13 | High-acidity thermal crystalline substance continuous crystallization device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201822090694.9U CN209735020U (en) | 2018-12-13 | 2018-12-13 | High-acidity thermal crystalline substance continuous crystallization device |
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| CN209735020U true CN209735020U (en) | 2019-12-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550274A (en) * | 2018-12-13 | 2019-04-02 | 云南锡业股份有限公司化工材料分公司 | A kind of highly acidity thermal crystalline substance continuous crystallisation device |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550274A (en) * | 2018-12-13 | 2019-04-02 | 云南锡业股份有限公司化工材料分公司 | A kind of highly acidity thermal crystalline substance continuous crystallisation device |
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