CN209752879U - Molecular sieve reaction kettle rapid cooling process device - Google Patents
Molecular sieve reaction kettle rapid cooling process device Download PDFInfo
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- CN209752879U CN209752879U CN201822194417.2U CN201822194417U CN209752879U CN 209752879 U CN209752879 U CN 209752879U CN 201822194417 U CN201822194417 U CN 201822194417U CN 209752879 U CN209752879 U CN 209752879U
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- molecular sieve
- cooling
- mother liquor
- reaction kettle
- buffer tube
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- 238000001816 cooling Methods 0.000 title claims abstract description 140
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 74
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000012452 mother liquor Substances 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000000498 cooling water Substances 0.000 claims description 22
- 238000009833 condensation Methods 0.000 claims description 21
- 230000005494 condensation Effects 0.000 claims description 21
- 238000004804 winding Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000000463 material Substances 0.000 description 23
- 238000000926 separation method Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model provides a molecular sieve reation kettle rapid cooling process units, a serial communication port, include: the system comprises a deionized water tank, a molecular sieve reaction kettle, a mother liquor steam condenser and a mother liquor collecting tank; the deionized water tank and the mother liquor steam condenser are directly connected with the top of the molecular sieve reaction kettle; injecting high-heat mother liquor steam in the molecular sieve reaction kettle into a mother liquor steam condenser through a pipeline for primary cooling, condensing and liquefying, and conveying the liquefied mother liquor to the mother liquor collecting tank through a liquid discharge pipeline; and after high-heat mother liquor steam in the molecular sieve reaction kettle is exhausted, opening an ion water tank, injecting deionized water at room temperature into the molecular sieve reaction kettle through a pipeline, and carrying out secondary cooling on the molecular sieve reaction kettle.
Description
Technical Field
The utility model relates to a molecular sieve reation kettle rapid cooling process units, in particular to molecular sieve reation kettle rapid cooling and high temperature mother liquor steam condensation separation process units belongs to the technical field of molecular sieve material production process equipment.
Background
Molecular sieve materials represented by SAPO-34, SSZ-13, SSZ-33 and the like need to be synthesized at a higher crystallization temperature (generally more than or equal to 160 ℃), and the problems of material cooling and molecular sieve mother liquor separation after the crystallization reaction are difficult to realize in the industrial production of the molecular sieves. For a large molecular sieve reaction kettle, natural cooling needs a long time, changes such as crystal transformation of a molecular sieve product and the like are easily caused in a long-time cooling process, and the generation of a pure-phase target product is not facilitated. And the cooled molecular sieve product is mixed with the mother liquor, and the burden of the subsequent procedures such as product separation, molecular sieve washing and the like is still serious.
At present, most of cooling systems of reaction kettles adopt a mode of embedding cooling pipes into the reaction kettles to cool materials. Several reactor cooling systems are disclosed by researchers, wherein patent cn201320512531.x reports a reactor cooling structure, which comprises a reactor, a cooling tank and a cooling pipe. Realize the device cooling through the cooling tube that encircles in reation kettle, cooling tube upper portion is connected to the reation kettle top, the sub-unit connection cooling bath, and the cooling bath bottom has the water inlet, and the lateral wall is fixed with the delivery port. The cooling device has a simple design structure and low manufacturing cost, and can be used for cooling materials in the reaction kettle after the reaction is finished. Patent CN201720540262.6 reports a reation kettle cooling device, and the device is including setting up at inside cooling coil of reation kettle and setting up the cooler bin in reation kettle outside, and the cooler bin links to each other with refrigeration plant, and for cooling coil in the reation kettle provides cooling medium, have simple to operate, cooling rate is fast, characteristics such as cooling effect is good. In order to improve the cooling efficiency of the reaction kettle, patent CN201620047853.5 reports an automatic control device for cooling water in the reaction kettle, which adjusts the flow rate of the cooling water in the cooling coil through a PLC module of a temperature transmitter on the reaction kettle, so as to realize the automatic control of the cooling process of the reaction kettle. The design of the cooling coil can effectively reduce the temperature of materials in the reaction kettle, but for the molecular sieve material gel with high viscosity and the product thereof, the compact cooling coil is not beneficial to stirring the materials, and the cooling coil is easy to gather the materials and difficult to clean and remove, so that the batch difference of the products is large.
For preventing the influence that cooling coil mixes the material in to reation kettle, patent CN201621394548.X has reported a cauldron outer refrigerated device, takes high temperature material out through the oil pump with reation kettle exit linkage, and high temperature material cools down through the outer condenser of reation kettle, and the material after the cooling is sent back to reation kettle in, and then realizes the rapid cooling of material. However, for the molecular sieve product materials with higher viscosity and higher density, the circulating cooling mode outside the kettle needs to consume huge electric energy, has higher requirement on an oil pump, is easy to generate the problems of condenser blockage, difficult cleaning and the like, and is not suitable for the production of the molecular sieve products.
patent CN201620163155.1 adopts the method of the conduction oil in the outside jacket of cooling reation kettle to carry out the cooling of the inside material of reation kettle, need not special equipment component, does not influence the stirring state of material in the reation kettle, nevertheless needs the cooling water earlier to the conduction oil cooling, and the conduction oil after the cooling is the aftercooling material, and cooling efficiency is not high, and cooling time is longer. Patent No. cn201310256777.x reports a device for heating, chilling and cooling a reaction kettle by using the same heat carrier, which comprises a reaction kettle jacket, a pump, a heating device, a heat carrier tank, a cooling device and a heat carrier cold tank, thereby forming a heating unit, a chilling unit and a cooling unit. The quick switching of the cold and hot circulation of the heat-conducting medium in the jacket of the reaction kettle is realized through the switching valve, the cooling efficiency of the materials in the reaction kettle is improved, but for a large molecular sieve crystallization reaction kettle, the cooling time for cooling the high-temperature materials is still longer. The heat-conducting medium needs refrigeration and power circulation, the production operation intensity and the preparation cost of the molecular sieve product are increased, and the operation burden of the subsequent washing and other procedures of the product is not reduced.
In summary, the cooling mode of the reaction kettle at present mainly includes two cooling modes, namely cooling of a coil pipe inside the reaction kettle and cooling of a jacket medium circulation of the reaction kettle. Aiming at large-scale high-temperature molecular sieve reaction kettles, the product has high viscosity, high temperature and heavy mass, and the two material cooling methods have lower cooling efficiency and higher requirements on temperature resistance and pressure resistance of cooling equipment, so that the cooling cost and the cooling effect are poor.
SUMMERY OF THE UTILITY MODEL
the main purpose of the utility model is to provide a molecular sieve reaction kettle rapid cooling process unit.
The process device comprises:
The system comprises a deionized water tank, a molecular sieve reaction kettle, a mother liquor steam condenser and a mother liquor collecting tank; the deionized water tank and the mother liquor steam condenser are directly connected with the top of the molecular sieve reaction kettle; injecting high-heat mother liquor steam in the molecular sieve reaction kettle into a mother liquor steam condenser through a pipeline for primary cooling, condensing and liquefying, and conveying the liquefied mother liquor to the mother liquor collecting tank through a liquid discharge pipeline;
And after high-heat mother liquor steam in the molecular sieve reaction kettle is exhausted, opening an ionized water tank to inject ionized water at room temperature into the molecular sieve reaction kettle through a pipeline, and carrying out secondary cooling on the molecular sieve reaction kettle.
in one embodiment, the mother liquor vapor condenser has a cavity with an open top, the cavity is divided into a condensation area and a liquid collecting area, an exhaust buffer tube is arranged in the cavity, and the exhaust buffer tube extends to the open top of the cavity to communicate with the outside atmosphere.
in one embodiment, the condensation area is located at an upper cavity section of the mother liquid vapor condenser, the liquid collection area is located at a lower cavity section of the mother liquid vapor condenser, the exhaust buffer tube is located at the condensation area, and cooling coils are arranged on the inner wall and the outer wall of the exhaust buffer tube in a surrounding manner.
In one embodiment, the bottom of the liquid collecting region is provided with a liquid outlet.
In one embodiment, the cooling coil is spirally wound on the exhaust buffer tube, the winding direction of the cooling coil is the same as the cyclone direction of the mother liquor steam in the mother liquor steam condenser, and the cooling coil is provided with a cooling coil cooling water outlet and a cooling coil cooling water inlet.
In one embodiment, a cooling jacket is installed outside the cavity and correspondingly arranged in the condensation area, and the cooling jacket is provided with a jacket cooling water inlet and a jacket cooling water outlet.
In one embodiment of the present invention, the first and second electrodes are,
the cooling coil passes through the exhaust buffer tube, passes through the exhaust buffer tube after passing down along the axis of the exhaust buffer tube, is coiled outside the exhaust buffer tube, and passes through the exhaust buffer tube after reaching the bottom end of the exhaust buffer tube, passes through the exhaust buffer tube again, and passes through the exhaust buffer tube after passing upward for a certain distance along the axis of the exhaust buffer tube.
In one embodiment, the cooling coil wound around the outside of the exhaust buffer tube is a thick tube, the cooling coil located inside the exhaust buffer tube is a thin tube, and the thick tube and the thin tube are connected by a tapered section.
In one embodiment, the diameter of the thick tube is 2 times the diameter of the thin tube.
In one embodiment, the bottom of the exhaust buffer tube is connected with a detachable inverted cone-shaped shrinkage tube, and the diameter of a bottom thin opening of the inverted cone-shaped shrinkage tube is one half of that of a top thick opening.
To sum up, the utility model discloses following beneficial effect has: the molecular sieve reaction kettle is cooled once by discharging high-heat mother liquor steam, so that the cooling speed is high, and the operation is convenient. The mother liquor steam condenser with the water-cooled cyclone cooling structure is designed, so that the condensation efficiency is improved, the volume of the device is reduced, the environmental protection in the production process of the molecular sieve is facilitated, the template agent content in the product can be greatly reduced by pre-separating partial mother liquor, the burden of subsequent procedures such as molecular sieve washing and the like is remarkably reduced, and the wastewater discharge is reduced. The secondary cooling of the molecular sieve reaction kettle is realized by washing the products in the reaction kettle with room-temperature deionized water, the cooling speed is high, the operation is simple, the corrosion effect of molecular sieve materials on process conveying pipelines is weakened, the product quality is improved, and the generation cost is reduced. In addition, the molecular sieve reaction kettle does not need a cooling coil pipe design, so that high-viscosity materials can be mixed and cleaned in the kettle conveniently, and the stability of the product batch is ensured.
Drawings
FIG. 1 is a schematic view of a molecular sieve reaction kettle rapid cooling process device according to an embodiment of the present invention;
Fig. 2 is a schematic diagram of a mother liquor vapor condenser according to an embodiment of the present invention.
Wherein the reference numerals are:
In the figure: 1. a deionized water tank; 2. a molecular sieve reaction kettle; 3. a mother liquor steam condenser; 4. a mother liquor collection tank; 5. a liquid collection area; 6. a cooling jacket; 7. a shrink tube; 8. an exhaust buffer tube; 9. a diameter-changing section; 10. a cooling coil; 11. a cooling water outlet; 12. a cooling coil cooling water inlet; 13. an exhaust port; 14. a cooling coil cooling water outlet; 15. a mother liquor vapor inlet; 16. a condensation zone; 17. a cooling water inlet; 18. and a liquid discharge port.
Detailed Description
The detailed description and technical contents of the present invention are described below with reference to the drawings:
As shown in fig. 1, a molecular sieve reaction kettle rapid cooling process device comprises a deionized water tank 1, a mother liquor steam condenser 3 and a mother liquor collecting tank 4, wherein the deionized water tank 1 is directly connected with a feed inlet at the top of a molecular sieve reaction kettle 2, and deionized water is injected into the molecular sieve reaction kettle through a metering pump (not shown) on a conveying pipeline; the mother liquor steam condenser 3 is directly connected with an exhaust port 13 at the top of the molecular sieve reaction kettle 2, the exhaust amount is controlled by a valve (not shown) on an exhaust pipeline, a liquid discharge pipeline at the bottom of the mother liquor steam condenser 3 is connected to a feed port (not shown) at the top of the mother liquor collecting tank 4, and the mother liquor is conveyed to the mother liquor collecting tank 4 by an alkali-resistant infusion pump (not shown) on the liquid discharge pipeline; the mother liquor collection tank 4 has a cooling jacket and a stirring paddle for short-term storage of mother liquor or pretreatment of mother liquor.
A mother liquid steam condenser shown in figure 2 is a water-cooled cyclone cooling structure and has a cavity with an open top, and the cavity comprises a condensation zone 16 and a liquid collecting zone 5. An exhaust buffer tube 8 is disposed within the cavity and the exhaust buffer tube 8 extends to the top opening of the cavity to communicate with the outside atmosphere.
The condensation area 16 is provided with a condenser jacket 6 and a cooling coil 10; the condensation zone 16 is located at the upper section of the cavity of the mother liquor steam condenser 3, the liquid collection zone 5 is located at the lower section of the cavity of the mother liquor steam condenser 3, the exhaust buffer tube 8 is located at the condensation zone 16, and the cooling coils 10 are arranged on the inner wall and the outer wall of the exhaust buffer tube 8 in a surrounding manner. The cooling coil 10 is spirally wound on the exhaust buffer tube 8, the winding direction of the cooling coil 10 is the same as the mother liquid steam cyclone direction in the mother liquid steam condenser, and the cooling coil 10 is provided with a cooling coil cooling water outlet 14 and a cooling coil cooling water inlet 12. And a cooling jacket 6 is arranged on the outer side of the cavity and correspondingly arranged in the condensation area 16, and the cooling jacket is provided with a cooling water inlet 17 and a cooling water outlet 11.
The cooling coil 10 passes through the exhaust buffer tube 8, down the axis of the exhaust buffer tube 8 and then out of the exhaust buffer tube 8 and is coiled around the outside of the exhaust buffer tube 8 until the cooling coil 10 reaches the bottom end of the exhaust buffer tube 8 and then passes into the exhaust buffer tube 8 again and up the axis of the exhaust buffer tube 8 a distance before passing out of the exhaust buffer tube 8. The cooling water enters the cooling coil 10 from the cooling coil cooling water inlet 12 and is discharged from the cooling coil cooling water outlet 14 along the winding direction of the cooling coil 10.
The cooling coil wound around the outside of the exhaust buffer tube 8 is a thick tube, the cooling coil located inside the exhaust buffer tube 8 is a thin tube, and the thick tube and the thin tube are connected by a tapered section.
The diameter of the thick pipe is 2 times of that of the thin pipe, the thick pipe is coiled on the outer wall of the exhaust buffer pipe 8 along the cyclone direction of the mother liquor steam to form a main body of a cooling coil pipe 10, and the spiral cooling coil pipe 10 guides the mother liquor steam to carry out cyclone condensation. The distance between the cooling coil 10 and the inner wall of the cooling jacket 6 is similar to the diameter of the cooling coil. The 8 bottoms of exhaust buffer tube are connected detachable back taper shrink tube 7, and the diameter of the thin mouthful of 7 bottoms of shrink tube is the half of the thick mouthful in shrink tube top, prevents effectively that mother liquor from volatilizing along exhaust buffer tube 8 in collecting liquid district 5. The bottom of the liquid collecting area 5 is provided with a liquid outlet 18.
After the crystallization reaction in the molecular sieve reaction kettle 2 is finished, high-heat mother liquor steam is discharged into the mother liquor steam condenser 3 from the exhaust port 13 at the top of the molecular sieve reaction kettle 2. High fever mother liquor steam gets into mother liquor steam condenser 3 and carries out whirlwind condensation liquefaction along cooling coil 10 winding direction by mother liquor steam entry 15, and the mother liquor gathering after the liquefaction is in mother liquor steam condenser 3's collecting space 5, and the positive upper portion in collecting space 5 is the shrink tube 7 and the exhaust buffer tube 8 the same with external atmosphere, guarantees that liquid steam condenser 3 internal pressure is balanced. The cooled liquefied mother liquor is discharged through a liquid outlet 18 at the bottom of the liquid collecting area 5, enters a mother liquor collecting tank 4 to wait for the subsequent treatment of the mother liquor, and the primary cooling process of the molecular sieve reaction kettle 2 is completed. And when the pressure in the molecular sieve reaction kettle 2 is reduced to or close to the atmospheric pressure, opening a water feeding valve of the deionized water tank 1, introducing deionized water into the molecular sieve reaction kettle 2, carrying out secondary cooling, and introducing steam generated by the secondary cooling into the mother liquor steam condenser 3 again for cyclone condensation. And when the internal temperature of the molecular sieve reaction kettle 2 reaches the target temperature, finishing the temperature reduction process of the reaction kettle, and synchronously finishing the mother liquor separation and the primary washing process of the molecular sieve products.
In conclusion, according to the molecular sieve reaction kettle rapid cooling and high-temperature mother liquor steam condensation separation process device, high-temperature mother liquor steam in the molecular sieve reaction kettle is discharged and enters the mother liquor steam condenser to be subjected to cyclone condensation liquefaction, the liquefied mother liquor is conveyed to the mother liquor collecting tank 4 with cooling and heat preservation functions, and primary cooling and partial mother liquor separation of the molecular sieve reaction kettle are completed; after the high-heat mother liquor steam of the molecular sieve reaction kettle is exhausted, room-temperature deionized water in the deionized water tank enters the molecular sieve reaction kettle to finish secondary cooling of the molecular sieve reaction kettle and primary washing of a molecular sieve product.
Claims (10)
1. A molecular sieve reation kettle rapid cooling process units, its characterized in that includes:
The system comprises a deionized water tank, a molecular sieve reaction kettle, a mother liquor steam condenser and a mother liquor collecting tank; the deionized water tank and the mother liquor steam condenser are directly connected with the top of the molecular sieve reaction kettle; injecting high-heat mother liquor steam in the molecular sieve reaction kettle into the mother liquor steam condenser through a pipeline for primary cooling, condensing and liquefying, and conveying the liquefied mother liquor to the mother liquor collecting tank through a liquid discharge pipeline;
And after high-heat mother liquor steam in the molecular sieve reaction kettle is exhausted, opening a deionized water tank, injecting deionized water at room temperature into the molecular sieve reaction kettle through a pipeline, and carrying out secondary cooling on the molecular sieve reaction kettle.
2. The molecular sieve reaction kettle rapid cooling process device as claimed in claim 1, wherein the mother liquor steam condenser is provided with a cavity with an open top, the cavity is divided into a condensation area and a liquid collecting area, an exhaust buffer tube is arranged in the cavity, and the exhaust buffer tube extends to the open top of the cavity and is communicated with the outside atmosphere.
3. the molecular sieve reaction kettle rapid cooling process device as claimed in claim 2, wherein the condensation zone is located at the upper cavity section of the mother liquid steam condenser, the liquid collection zone is located at the lower cavity section of the mother liquid steam condenser, the exhaust buffer tube is located at the condensation zone, and cooling coils are arranged on the inner wall and the outer wall of the exhaust buffer tube in a surrounding manner.
4. the molecular sieve reaction kettle rapid cooling process device as claimed in claim 3, wherein a liquid outlet is arranged at the bottom of the liquid collecting area.
5. The molecular sieve reactor rapid cooling process device according to claim 3, wherein the cooling coil is spirally wound on the exhaust buffer tube, the winding direction of the cooling coil is the same as the mother liquor steam cyclone direction in the mother liquor steam condenser, and a cooling coil cooling water outlet and a cooling coil cooling water inlet are arranged on the cooling coil.
6. The molecular sieve reaction kettle rapid cooling process device as claimed in claim 3, wherein a cooling jacket is installed outside the cavity, the cooling jacket is correspondingly arranged in the condensation zone, and the cooling jacket is provided with a jacket cooling water inlet and a cooling water outlet.
7. The molecular sieve reaction kettle rapid cooling process device of claim 5,
The cooling coil passes through the exhaust buffer tube, passes through the exhaust buffer tube after passing down along the axis of the exhaust buffer tube, is coiled outside the exhaust buffer tube, and passes through the exhaust buffer tube after reaching the bottom end of the exhaust buffer tube, passes through the exhaust buffer tube again, and passes through the exhaust buffer tube after passing upward for a certain distance along the axis of the exhaust buffer tube.
8. the molecular sieve reactor rapid cooling process device according to claim 7, wherein the cooling coil wound outside the exhaust buffer tube is a thick tube, the cooling coil located inside the exhaust buffer tube is a thin tube, and the thick tube and the thin tube are connected by a reducer section.
9. The molecular sieve reactor rapid cooling process device of claim 8, wherein the diameter of the thick pipe is 2 times of the diameter of the thin pipe.
10. The molecular sieve reaction kettle rapid cooling process device as claimed in claim 2, wherein the bottom of the exhaust buffer tube is connected with a detachable inverted cone-shaped shrinkage tube, and the diameter of a bottom small opening of the inverted cone-shaped shrinkage tube is one half of that of a top large opening.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201822194417.2U CN209752879U (en) | 2018-12-25 | 2018-12-25 | Molecular sieve reaction kettle rapid cooling process device |
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| CN201822194417.2U CN209752879U (en) | 2018-12-25 | 2018-12-25 | Molecular sieve reaction kettle rapid cooling process device |
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| CN209752879U true CN209752879U (en) | 2019-12-10 |
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| CN201822194417.2U Active CN209752879U (en) | 2018-12-25 | 2018-12-25 | Molecular sieve reaction kettle rapid cooling process device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110935189A (en) * | 2019-12-12 | 2020-03-31 | 东莞市泰丰空调制冷设备有限公司 | Condensate water collecting device for steam condensation and using method thereof |
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2018
- 2018-12-25 CN CN201822194417.2U patent/CN209752879U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110935189A (en) * | 2019-12-12 | 2020-03-31 | 东莞市泰丰空调制冷设备有限公司 | Condensate water collecting device for steam condensation and using method thereof |
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