CN219701136U - High-efficient carrier gas sublimation crystallization system - Google Patents
High-efficient carrier gas sublimation crystallization system Download PDFInfo
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- CN219701136U CN219701136U CN202321000633.3U CN202321000633U CN219701136U CN 219701136 U CN219701136 U CN 219701136U CN 202321000633 U CN202321000633 U CN 202321000633U CN 219701136 U CN219701136 U CN 219701136U
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- 239000012159 carrier gas Substances 0.000 title claims abstract description 117
- 238000000859 sublimation Methods 0.000 title claims abstract description 78
- 230000008022 sublimation Effects 0.000 title claims abstract description 78
- 238000002425 crystallisation Methods 0.000 title claims abstract description 34
- 230000008025 crystallization Effects 0.000 title claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 83
- 239000012535 impurity Substances 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 239000003507 refrigerant Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims description 56
- 239000002245 particle Substances 0.000 claims description 31
- 238000001816 cooling Methods 0.000 claims description 15
- 239000002826 coolant Substances 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 30
- 238000012546 transfer Methods 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 30
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 239000001569 carbon dioxide Substances 0.000 description 15
- 230000005494 condensation Effects 0.000 description 15
- 238000009833 condensation Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 15
- 230000009286 beneficial effect Effects 0.000 description 9
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- 239000000428 dust Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- BHNHHSOHWZKFOX-UHFFFAOYSA-N 2-methyl-1H-indole Chemical compound C1=CC=C2NC(C)=CC2=C1 BHNHHSOHWZKFOX-UHFFFAOYSA-N 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- VEWLDLAARDMXSB-UHFFFAOYSA-N ethenyl sulfate;hydron Chemical compound OS(=O)(=O)OC=C VEWLDLAARDMXSB-UHFFFAOYSA-N 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- ZHDTXTDHBRADLM-UHFFFAOYSA-N hydron;2,3,4,5-tetrahydropyridin-6-amine;chloride Chemical compound Cl.NC1=NCCCC1 ZHDTXTDHBRADLM-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
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Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model relates to the technical field of fine chemical separation and purification, and discloses a high-efficiency carrier gas sublimation crystallization system which comprises a sublimation unit, a impurity removal unit, a desublimation unit, a carrier gas circulation unit and a refrigerant circulation unit which are communicated through pipelines, wherein a carrier gas heating device is communicated between an outlet of the carrier gas circulation unit and an inlet of the sublimation unit through a pipeline, and the outlet of the carrier gas circulation unit is communicated with the inlet pipeline of the desublimation unit through the refrigerant circulation unit; the desublimation unit comprises a desublimation device connected in series in one or more stages. The scheme adopts the sublimation mode of directly mixing the sublimated gas and the refrigerant, avoids the problems that the heat transfer efficiency is low, the heat transfer is affected by the adhesion of the sublimated material to the heat transfer surface, the product caking and the discharging are difficult and the like when the refrigerant indirectly cools the sublimated gas, and can control the sublimation temperature of each level of the sublimation device according to the different sublimation characteristics of impurities and products by arranging one-level or multi-level series-connected sublimation devices, enrich the impurities and the products in different sublimation devices, further remove impurities and improve the purity of the products.
Description
Technical Field
The utility model relates to the technical field of fine chemical separation and purification, in particular to a high-efficiency carrier gas sublimation crystallization system.
Background
At present, substances to be purified such as 4, 4-diaminodiphenyl ether, 2-methylindole, salicylic acid, metal carbonyl and the like have larger vapor partial pressure below the melting point, and meanwhile, the purification of substances with larger vapor partial pressure difference between the contained impurities and the target purification substances is often completed in a sublimation crystallization system according to sublimation and desublimation characteristics of the substances. According to the sublimation crystallization purification device system of the vinyl sulfate disclosed in the prior art CN216170061U, the sublimation crystallization purification device system is adopted, the vinyl sulfate solid powder is directly heated and sublimated in a sublimator to be converted into a gaseous state, then impurities such as solid salts carried in the gas are subjected to gas-solid separation through a cyclone separator, purified sublimated gas is obtained, and the sublimated gas is subjected to sublimation crystallization, so that the high-purity vinyl sulfate crystal is obtained. However, the following technical problems still exist in the prior art:
(1) In the prior art, the removal of impurities is only completed in a sublimation stage, specifically, after the raw materials are sublimated by heating, the non-sublimated solid impurities are removed by a cyclone separator; however, impurities in the mixed gas formed by combining the sublimated gas and the carrier gas cannot be removed, so that the purity of the product is reduced;
(2) In the prior art, a sublimation unit adopts a traditional kettle-type sublimator, so that the granularity requirement on materials per se is high, some large and fast materials can enter a system after being treated by the outside, the application range is narrow, and the sublimation efficiency is low;
(3) In the prior art, the condensation effect is limited, so that part of sublimated gas enters a carrier gas system along with carrier gas and is removed by a pulse dust collector, waste of raw materials is caused, and the product yield is reduced;
(4) In the prior art, the desublimation part adopts an indirect desublimation mode, crystals are directly condensed and crystallized on the inner wall of a container, and after long-time operation, the crystals are easy to deposit on a condensation surface, so that the subsequent heat transfer effect is poor, and the desublimation device cannot normally operate.
Disclosure of Invention
The utility model aims to provide a high-efficiency carrier gas sublimation crystallization system, which solves the technical problems that the sublimation efficiency is low, the application range of the system is limited, impurities mixed in the sublimated gas cannot be thoroughly removed, the sublimation efficiency is low, and a sublimator cannot operate for a long time in the prior art.
In order to achieve the above purpose, the utility model adopts the following technical scheme: the high-efficiency carrier gas sublimation crystallization system comprises a sublimation unit, a impurity removal unit, a desublimation unit, a carrier gas circulation unit and a refrigerant circulation unit which are communicated through pipelines, wherein a carrier gas heating device is communicated between an outlet of the carrier gas circulation unit and an inlet of the sublimation unit through a pipeline, and the outlet of the carrier gas circulation unit is communicated with the inlet pipeline of the desublimation unit through a refrigerant circulation unit; the desublimation unit comprises a desublimation device connected in series in one or more stages.
The principle and the advantages of the scheme are as follows:
1. compared with the prior art that impurities mixed in sublimated gas cannot be thoroughly removed to reduce the quality of products, the method can control the desublimation temperature of each level of desublimation device according to the desublimation characteristics of the impurities and the products by arranging the one-level or multi-level series connection desublimation devices, so that the impurities and the products are desublimated and enriched in different desublimation devices, further separation of the impurities is realized, and the products with higher purity are obtained.
2. In the scheme, circulating carrier gas enters a carrier gas unit and is redistributed, a part of the carrier gas enters a sublimation unit after being heated by a carrier gas heating device, and the carrier gas and sublimated gas of raw materials are combined into mixed gas to assist the sublimated gas to enter a desublimation unit for condensation and crystallization; the other part of the sublimated gas enters a desublimation unit after being cooled by a refrigerant circulation unit, and is opposite to the mixed gas, so that the condensation speed of the sublimated gas in the mixed gas is increased, and the sublimated gas is fully condensed; effectively avoiding the raw material waste caused by the fact that partial sublimated gas is discharged along with carrier gas due to limited desublimation effect of the existing equipment. In addition, by adopting the direct desublimation mode, the problems of low condensation efficiency, difficult heat transfer, product caking and discharging and the like caused by indirect desublimation, which are caused by the fact that desublimation materials adhere to a heat transfer surface, are avoided.
3. This scheme is through setting up edulcoration unit between sublimation unit and desublimation unit, is convenient for get rid of the non-sublimated solid particle (including non-sublimated impurity and non-sublimated coarse grain raw materials) that mix with in the sublimating gas, is convenient for promote impurity removal efficiency and sublimation crystallization in the chemicals and obtain the product fineness, promotes the product quality.
4. The one-stage or multistage series-connected desublimation device is arranged in the scheme, is suitable for the condition that impurities are condensed and crystallized before or after products, and can separate products and impurities with different desublimation characteristics, so that the application range of the system is effectively widened, and the cost of purchasing multiple sets of equipment for processing different raw materials by enterprises is reduced.
Preferably, the refrigerant circulation unit comprises a circulation compressor, a liquefier and a liquid cache tank which are communicated through pipelines, and an outlet of the liquid cache tank is communicated with the desublimation device through pipelines.
The beneficial effects are that: according to the scheme, carrier gas is compressed and cooled into low-temperature liquid through the circulating compressor and the liquefier and stored in the liquid cache tank, then the carrier gas is introduced into the desublimation device in the low-temperature liquid state to be opposite to the mixed gas, the sublimated gas is condensed by utilizing the evaporation heat absorption of the low-temperature liquid, and the condensation and crystallization of the sublimated gas in the mixed gas are realized. The scheme is particularly suitable for the conditions of easily sublimating raw materials, small carrier gas consumption, small condensation temperature difference and the like.
Preferably, the refrigerant circulation unit comprises a circulation compressor and a liquid cache tank which are communicated through pipelines, and the liquid cache tank is communicated with the desublimation device through pipelines; the bottom of the liquid cache tank is provided with a liquid outlet, the side surface of the upper part is provided with a liquid inlet, a pipeline between the liquid outlet and the liquid inlet is communicated with a liquefier, and the liquefier is positioned outside the liquid cache tank; and a spraying part is further arranged in the liquid cache tank, and the spraying part is communicated with a freezing medium storage tank outside the liquid cache tank.
The beneficial effects are that: in the scheme, carrier gas enters a liquid cache tank after passing through a circulating compressor, and is cooled into a low-temperature liquid state through an external freezing medium (such as frozen brine) sprayed out by a spraying part; the liquefier is arranged beside the liquid cache tank, so that less part of carrier gas which enters the liquid cache tank and is not condensed and liquefied is circularly liquefied into the liquid cache tank through the liquefier; then the liquid medium enters a desublimation device in a low-temperature state, and is opposite to the mixed gas to realize condensation and crystallization of the sublimated gas. The scheme is particularly suitable for the conditions of low raw material sublimation rate, large carrier gas consumption, large condensation temperature difference and the like.
Preferably, the desublimation unit comprises a three-stage desublimation device communicated by pipelines, and is a first-stage desublimation device, a second-stage desublimation device and a third-stage desublimation device which are sequentially arranged along the flowing direction of the mixed gas, wherein the first-stage desublimation device, the second-stage desublimation device and the third-stage desublimation device are respectively provided with a mixed gas inlet, a mixed gas outlet, a cooling medium inlet and a crystallization outlet, the mixed gas inlet of the first-stage desublimation device is communicated with an outlet pipeline of the impurity removal unit, the mixed gas outlet of the first-stage desublimation device is communicated with a mixed gas inlet pipeline of the second-stage desublimation device, the mixed gas outlet of the second-stage desublimation device is communicated with a mixed gas inlet pipeline of the third-stage desublimation device, and the mixed gas outlet of the third-stage desublimation device is communicated with an inlet pipeline of the carrier gas circulation unit; the cooling medium inlet of the primary desublimation device, the cooling medium inlet of the secondary desublimation device and the cooling medium inlet of the tertiary desublimation device are all communicated with the outlet pipeline of the liquid cache tank.
The beneficial effects are that: according to the scheme, the three-stage sublimating device communicated by the sequential pipelines is arranged, so that raw material sublimated gas and impurity sublimated gas in the mixed gas can be condensed and crystallized in sequence according to different sublimating characteristics, impurities and products can be effectively separated, and the purity of the products is improved; and this scheme sets up tertiary desublimation ware, the raw materials in the fully condensed gas mixture of being convenient for effectively reduces the raw materials volume that gets into carrier gas circulation unit along with the carrier gas, reduces the raw materials extravagant, promotes the product yield.
Preferably, the sublimation unit is internally provided with a particle size classifier positioned at the upper part and a pulverizer positioned at the lower part, the outer wall of the sublimation unit is provided with a carrier gas inlet communicated with the pulverizer and a mixed gas outlet communicated with the particle size classifier, the carrier gas inlet is communicated with a carrier gas heating device pipeline, and the mixed gas outlet is communicated with an inlet pipeline of the impurity removal unit.
The beneficial effects are that: in the scheme, after the massive materials are crushed by a crusher, the massive materials are quickly sublimated to form mixed gas in the presence of heated carrier gas, the mixed gas is wrapped with non-sublimated finer particle impurities and coarser particle materials to enter a particle size classifier, and under the classification effect of the particle size classifier, the finer particle impurities enter a impurity removing unit along with the mixed gas to remove the finer particle impurities; the coarser particle materials fall back to the pulverizer under the action of the particle size classifier to be continuously pulverized and sublimated.
The sublimation unit in this scheme is specifically a flash dryer. The sublimation unit of the scheme is different from a traditional kettle-type sublimator, a flash evaporation dryer is adopted as the sublimation unit, a pulverizer is arranged at the lower part of the sublimation unit, massive materials can be pulverized, particles are thinned, the contact area of carrier gas and the materials is increased, mass transfer is improved, and sublimation rate is accelerated; the upper part is provided with a particle size classifier, so that large-particle substances or sublimated residues which are not sublimated can be sublimated continuously, and the material utilization rate is improved.
Preferably, the particle size classifier is a classification ring or classification wheel.
Preferably, the pulverizer is an air jet pulverizer or a mechanical pulverizing device.
The beneficial effects are that: according to the scheme, the pulverizer is adopted to make the material particles finer, so that the contact area of the material and the heating carrier gas is increased, and the mass transfer and sublimation efficiency is improved; the size of the required material granularity can be adjusted at any time by adopting the granularity classifier, so that the non-sublimated material is fully sublimated, and the material utilization rate and the product yield are improved.
Preferably, a feeding hole is formed in the middle of the sublimation unit, and the feeding hole is communicated with a spiral pushing device.
The beneficial effects are that: through setting up spiral blevile of push in this scheme, the spiral feeding of the material of being convenient for, the material blocks up the feed inlet when avoiding the feeding when controlling material feed quantity, realizes the continuous feeding of material.
Preferably, the carrier gas circulation unit comprises a circulating carrier gas buffer tank, a circulating fan and a circulating carrier gas distribution tank which are communicated through pipelines; the inlet of the circulating gas-carrying buffer tank is communicated with a mixed gas outlet pipeline of the three-stage desublimation device; the circulating carrier gas distribution tank is provided with a heating outlet and a cooling outlet, a heating filter is communicated between the heating outlet and the carrier gas heating device through a pipeline, and a cooling filter is communicated between the cooling outlet and the circulating compressor through a pipeline.
The beneficial effects are that: according to the scheme, the carrier gas in the carrier gas circulation unit is reasonably distributed to the heating sublimation stage and the cooling desublimation stage by arranging the carrier gas distribution tank, so that the carrier gas utilization rate is improved; in addition, a heating filter and a cooling filter are respectively additionally arranged in front of the carrier gas heating device and the refrigerant circulating unit, so that mechanical impurities in carrier gas used for heating the sublimation stage and cooling the sublimation stage are conveniently removed, and the difficulty in removing the impurities in materials is avoided when the mechanical impurities enter the sublimation unit and the sublimation unit along with the carrier gas.
Preferably, the circulating gas-carrying buffer tank is also communicated with a gas-carrying storage tank.
The beneficial effects are that: according to the scheme, the carrier gas storage tank is arranged, so that carrier gas can be conveniently supplemented for the carrier gas circulation system.
Drawings
FIG. 1 is a schematic diagram of a high-efficiency carrier gas sublimation crystallization system in example 1 of the present utility model.
Fig. 2 is a schematic diagram of the structure of a sublimation unit in embodiment 1 of the present utility model.
Fig. 3 is a schematic structural diagram of a high-efficiency carrier gas sublimation crystallization system in embodiment 2 of the present utility model.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: sublimation unit 1, jet mill 11, particle size classifier 12, spiral pusher 13, impurity removal unit 2, desublimation unit 3, primary desublimation unit 31, secondary desublimation unit 32, tertiary desublimation unit 33, carrier gas circulation unit 4, circulating carrier gas buffer tank 41, circulating fan 42, circulating carrier gas distribution tank 43, heating filter 44, carrier gas heating device 45, carrier gas storage tank 47, refrigerant circulation unit 5, circulating compressor 51, liquefier 52, liquid buffer tank 53, shower portion 531, cooling filter 54, freezing medium storage tank 55.
Example 1
This embodiment is basically as shown in fig. 1: a high-efficiency carrier gas sublimation crystallization system comprises a sublimation unit 1, a impurity removal unit 2, a desublimation unit 3, a carrier gas circulation unit 4 and a refrigerant circulation unit 5 which are communicated through pipelines.
The carrier gas circulation unit 4 comprises a circulating carrier gas buffer tank 41, a circulating fan 42 and a circulating carrier gas distribution tank 43 which are communicated through pipelines; the circulating carrier gas buffer tank 41 is also in pipe communication with a carrier gas reservoir 47 for replenishing carrier gas circulating in the system. The circulating carrier gas distributing tank 43 is provided with a heating outlet and a cooling outlet, the heating outlet of the circulating carrier gas distributing tank 43 is in pipeline communication with the sublimation unit 1, and a heating filter 44 and a carrier gas heating device 45 are sequentially communicated on a connecting pipeline, wherein the carrier gas heating device 45 is specifically a carrier gas heater in the embodiment. A cooling outlet of the circulating carrier gas distributing tank 43 is communicated with a refrigerant circulating unit 5 through a pipeline between the desublimation unit 3, and the refrigerant circulating unit 5 comprises a circulating compressor 51, a liquefier 52 and a liquid buffer tank 53 which are communicated through a sequential pipeline; a cooling filter 54 is communicated between the circulation compressor 51 and the cooling outlet of the circulation carrier gas distribution tank 43 to purify impurities in the carrier gas circulating into the desublimation unit 3, and effectively prevent the impurities in the carrier gas from affecting the product quality. In this embodiment, the carrier gas is any one of carbon dioxide, nitrogen, air and helium, and in this embodiment, the carrier gas is specifically carbon dioxide.
As shown in fig. 2, in this embodiment, the sublimation unit 1 is specifically a flash evaporation dryer, and a pulverizer located at a lower portion and a particle size classifier 12 located at an upper portion are disposed in the sublimation unit 1, where the pulverizer is an airflow pulverizer 11 or a mechanical pulverizing device, and this embodiment is specifically the airflow pulverizer 11; the particle sizer 12 is a sizing ring or sizing wheel, in this embodiment the particle sizer 12 is specifically a sizing wheel. The outer wall of the sublimation unit 1 is provided with a carrier gas inlet communicated with the jet mill 11, a mixed gas outlet communicated with the particle size classifier 12 and a feed inlet, the carrier gas inlet is communicated with a carrier gas heating device 45 pipeline, and the mixed gas outlet is communicated with an inlet pipeline of the impurity removal unit 2; the feed inlet is positioned in the middle of the sublimation unit 1, and is communicated with a spiral pushing device 13. In this embodiment, the jet mill 11 is specifically a pulverizing rotor mill, which pulverizes the material particles to be finer, increases the contact area between the material particles and the heated carrier gas, and is beneficial to sublimation.
In this embodiment, the impurity removing unit 2 is specifically a cyclone, and an outlet of the impurity removing unit 2 is communicated with the desublimation unit 3.
As shown in fig. 1, the desublimation unit 3 includes a desublimation device with one or more stages connected in series, and in this embodiment, the desublimation unit 3 specifically includes a three-stage desublimation device with pipes connected, and a first-stage desublimation device 31, a second-stage desublimation device 32, and a three-stage desublimation device 33 are sequentially arranged along the flow direction of the mixture gas. The primary desublimation device 31, the secondary desublimation device 32 and the tertiary desublimation device 33 are respectively provided with a mixed gas inlet, a mixed gas outlet, a cooling medium inlet and a crystallization outlet, the mixed gas inlet of the primary desublimation device 31 is communicated with the outlet pipeline of the impurity removal unit 2, the mixed gas outlet of the primary desublimation device 31 is communicated with the mixed gas inlet pipeline of the secondary desublimation device 32, the mixed gas outlet of the secondary desublimation device 32 is communicated with the mixed gas inlet pipeline of the tertiary desublimation device 33, and the mixed gas outlet of the tertiary desublimation device 33 is communicated with the inlet pipeline of the circulating carrier buffer tank 41. The cooling medium inlet of the primary desublimation device 31, the cooling medium inlet of the secondary desublimation device 32 and the cooling medium inlet of the tertiary desublimation device 33 are communicated with the outlet pipeline of the liquid buffer tank 53, and the communication pipelines are provided with control valves (not shown in the figure).
The specific implementation process is as follows:
the carbon dioxide in the carrier gas circulation unit 4 forms heating carrier gas under the action of the heating filter 44 and the carrier gas heater, the heating carrier gas enters the sublimation unit 1, and the materials crushed by the crushing rotor mill are heated, so that the materials sublimate and form mixed gas with the carrier gas, and the mixed gas is conveyed into the cyclone dust collector of the impurity removal unit 2 to complete dust removal. The specific process is as follows: materials to be treated, such as 4, 4-diaminodiphenyl ether, 2-methylindole, salicylic acid, metal carbonyl and the like, are sent into a sublimation unit 1 by a spiral pushing device 13, crushed into fine particles by a crushing rotor mill, products in the fine particles sublimate after the fine particles are contacted with heated carrier gas to form mixed gas containing carrier gas, sublimated gas and non-sublimated particles, the mixed gas is subjected to grading treatment by a particle size classifier 12, and coarser particle materials fall back to a jet mill 11 to be continuously crushed and sublimated; the finer particle materials which cannot sublimate enter the cyclone dust collector along with the mixed gas, are removed under the action of the cyclone dust collector, and the mixed gas with the finer particle materials removed enters the desublimation unit 3 for condensation and crystallization.
In this embodiment, the cooling medium for condensation is liquid carbon dioxide, that is, the carbon dioxide in the carrier gas circulation unit 4 is distributed into the refrigerant circulation unit 5 under the action of the circulating carrier gas distribution tank 43, and forms liquefied carbon dioxide under the action of the cooling filter 54, the circulating compressor 51 and the liquefier 52 in sequence, the liquefied carbon dioxide temporarily exists in the liquid buffer tank 53, and then enters the primary desublimator 31, the secondary desublimator 32 and the tertiary desublimator 33 to be directly opposite-flushed and mixed with the mixed gas according to the requirement, so as to realize condensation crystallization of the sublimated gas. The flow of liquid carbon dioxide entering each level of desublimation devices is controlled by adjusting the control valve, so that sublimated gases with different components in the mixed gas are condensed and crystallized in different desublimation devices, separation between products with similar sublimation and desublimation characteristics and impurities is realized, and the purity of the products is effectively improved.
The carrier gas discharged from the mixed gas outlet of the three-stage desublimator 33 enters the circulating carrier buffer tank 41, awaiting recirculation.
In the embodiment, the low-temperature liquid carbon dioxide is used as a cooling medium, and the sublimation gas is condensed by utilizing the evaporation heat absorption of the low-temperature carbon dioxide, so that the method is particularly suitable for sublimation crystallization of materials under the conditions of easy sublimation of raw materials, small carrier gas consumption, small condensation temperature difference and the like.
Example 2
The present embodiment is basically the same as embodiment 1, except that, as shown in fig. 3, the refrigerant circulation unit 5 includes a circulation compressor 51 and a liquid buffer tank 53 in pipe communication, the liquid buffer tank 53 being in pipe communication with all of the primary desublimator 31, the secondary desublimator 32 and the tertiary desublimator 33; the bottom of the liquid cache tank 53 is provided with a liquid outlet, the side surface of the upper part is provided with a liquid inlet, a pipeline between the liquid outlet and the liquid inlet is communicated with a liquefier 52, and the liquefier 52 is positioned outside the liquid cache tank 53; the liquid buffer tank 53 is also provided with a spraying part 531, and the spraying part 531 is communicated with the freezing medium storage tank 55 outside the liquid buffer tank 53.
In this embodiment, the freezing medium storage tank 55 is filled with a freezing medium, specifically, frozen brine, which is sprayed from the spraying part 531, and cools the gaseous carbon dioxide delivered from the circulating compressor 51 into the liquid buffer tank 53 into low-temperature liquid carbon dioxide, and the low-temperature liquid carbon dioxide enters the sublimating device for condensing and crystallizing sublimating gas; liquefier 52 may liquefy a small portion of the uncooled carbon dioxide.
The sensible heat of gaseous carbon dioxide is utilized in the embodiment, so that condensation and crystallization of sublimate gas are accelerated. The embodiment is particularly suitable for the conditions that raw materials are not easy to sublimate, the consumption of carrier gas required by raw material sublimation is large, the condensation temperature difference is large, and the like.
The foregoing is merely exemplary of the present utility model, and specific technical solutions and/or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present utility model, and these should also be regarded as the protection scope of the present utility model, which does not affect the effect of the implementation of the present utility model and the practical applicability of the patent. The protection scope of the present utility model is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (10)
1. A high-efficiency carrier gas sublimation crystallization system is characterized in that: the device comprises a sublimation unit, a impurity removal unit, a desublimation unit, a carrier gas circulation unit and a refrigerant circulation unit which are communicated through pipelines, wherein a carrier gas heating device is communicated between an outlet of the carrier gas circulation unit and an inlet of the sublimation unit through a pipeline; the outlet of the refrigerant circulation unit is communicated with the inlet pipeline of the desublimation unit; the desublimation unit comprises a desublimation device connected in series in one or more stages.
2. A high efficiency carrier gas sublimation crystallization system as defined in claim 1, wherein: the refrigerant circulation unit comprises a circulation compressor, a liquefier and a liquid cache tank which are communicated through pipelines, and an outlet of the liquid cache tank is communicated with the desublimation device through pipelines.
3. A high efficiency carrier gas sublimation crystallization system as defined in claim 1, wherein: the refrigerant circulating unit comprises a circulating compressor and a liquid cache tank which are communicated through pipelines, and the liquid cache tank is communicated with the desublimation device through pipelines; the bottom of the liquid cache tank is provided with a liquid outlet, the side surface of the upper part is provided with a liquid inlet, a pipeline between the liquid outlet and the liquid inlet is communicated with a liquefier, and the liquefier is positioned outside the liquid cache tank; the liquid inlet extends into the liquid cache tank and is provided with a spraying part.
4. A high efficiency carrier gas sublimation crystallization system according to claim 2 or 3, wherein: the desublimation unit comprises a three-stage desublimation device communicated by pipelines, and is sequentially provided with a first-stage desublimation device, a second-stage desublimation device and a third-stage desublimation device along the flowing direction of the mixed gas, wherein the first-stage desublimation device, the second-stage desublimation device and the third-stage desublimation device are respectively provided with a mixed gas inlet, a mixed gas outlet, a cooling medium inlet and a crystallization outlet, the mixed gas inlet of the first-stage desublimation device is communicated with an outlet pipeline of the impurity removal unit, the mixed gas outlet of the first-stage desublimation device is communicated with a mixed gas inlet pipeline of the second-stage desublimation device, the mixed gas outlet of the second-stage desublimation device is communicated with a mixed gas inlet pipeline of the third-stage desublimation device, and the mixed gas outlet of the third-stage desublimation device is communicated with an inlet pipeline of the carrier gas circulation unit; the cooling medium inlet of the primary desublimation device, the cooling medium inlet of the secondary desublimation device and the cooling medium inlet of the tertiary desublimation device are all communicated with the outlet pipeline of the liquid cache tank.
5. A high efficiency carrier gas sublimation crystallization system as defined in claim 4, wherein: the sublimation unit is internally provided with a particle size classifier positioned at the upper part and a pulverizer positioned at the lower part, the outer wall of the sublimation unit is provided with a carrier gas inlet communicated with the pulverizer and a mixed gas outlet communicated with the particle size classifier, the carrier gas inlet is communicated with a carrier gas heating device pipeline, and the mixed gas outlet is communicated with an inlet pipeline of the impurity removal unit.
6. A high efficiency carrier gas sublimation crystallization system as defined in claim 5, wherein: the particle size classifier is a classification ring or classification wheel.
7. A high efficiency carrier gas sublimation crystallization system as defined in claim 6, wherein: the pulverizer is an air flow pulverizer or a mechanical pulverizing device.
8. A high efficiency carrier gas sublimation crystallization system as defined in claim 7, wherein: the sublimation unit middle part is equipped with the feed inlet, the feed inlet intercommunication has spiral blevile of push.
9. A high efficiency carrier gas sublimation crystallization system as defined in claim 8, wherein: the carrier gas circulation unit comprises a circulating carrier gas buffer tank, a circulating fan and a circulating carrier gas distribution tank which are communicated through pipelines; the inlet of the circulating gas-carrying buffer tank is communicated with a mixed gas outlet pipeline of the three-stage desublimation device; the circulating carrier gas distribution tank is provided with a heating outlet and a cooling outlet, a heating filter is communicated between the heating outlet and the carrier gas heating device through a pipeline, and a cooling filter is communicated between the cooling outlet and the circulating compressor through a pipeline.
10. A high efficiency carrier gas sublimation crystallization system as set forth in claim 9, wherein: the circulating gas-carrying buffer tank is also communicated with a gas-carrying storage tank.
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