CN114669076B - Micro-melt crystallization and falling film crystallization combined material purification system and method - Google Patents
Micro-melt crystallization and falling film crystallization combined material purification system and method Download PDFInfo
- Publication number
- CN114669076B CN114669076B CN202210325041.2A CN202210325041A CN114669076B CN 114669076 B CN114669076 B CN 114669076B CN 202210325041 A CN202210325041 A CN 202210325041A CN 114669076 B CN114669076 B CN 114669076B
- Authority
- CN
- China
- Prior art keywords
- crystallization
- micro
- melt
- falling film
- crystallizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/06—Jet mills
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of material crystallization, and particularly discloses a material purification system and a method combining micro-melt crystallization and falling film crystallization, wherein the purification system comprises a micro-melt crystallizer and a falling film crystallizer, the micro-melt crystallizer comprises a crystallization cavity and a crystallization crushing cavity, a crystal scraping mechanism for scraping crystallization on the inner wall of the crystallization cavity is arranged in the crystallization cavity, a contraction section, a throat section and an expansion section are sequentially arranged in the crystallization crushing cavity according to the material flow direction, and a crushing piece is arranged in the crystallization crushing cavity; the purification method adopts the purification system to purify the materials. According to the invention, primary crystallization is carried out through the micro-melt crystallizer to obtain the micro-melt, micro-particle crystallization is obtained after solid-liquid separation of the micro-melt, little or no mother liquor is wrapped by the micro-particle crystallization, secondary crystallization is carried out through the falling film crystallizer after the micro-particle crystallization is melted to obtain a high-purity material, and the purity of the micro-particle crystallization is higher, so that the crystallization time of the falling film crystallizer is shortened, and the material purification efficiency is improved.
Description
Technical Field
The invention relates to the technical field of material crystallization, in particular to a material purification system and method combining micro-melt crystallization and falling film crystallization.
Background
The crystallization technology is one of the technologies having an important role in the separation and purification process of products, and the crystallization process is generally classified into four types, namely solution crystallization, melt crystallization, precipitation crystallization and sublimation crystallization. Falling film crystallization, which is one of melt crystallization, is a crystallization process in which separation is achieved according to difference in freezing point between separated substances. The falling film crystallizer is one of key equipment for realizing melt crystallization, has the advantages of capability of separating out a high-purity product, low operation temperature, low pollution, energy conservation and the like, and is widely applied to refining and purifying products in the fields of petroleum, chemical engineering, medicines and the like.
In the actual production process, if the purity (concentration) of a target product contained in a liquid material to be separated and purified is low, multiple melting crystallization is required, so that if a single falling film crystallizer is used, the crystallization time is long, the material purification efficiency is low, subsequent process steps can be suspended to wait for crystallization products, and the industrial continuous production is not facilitated; and if a plurality of falling film crystallizers are utilized, the equipment investment cost is high, and the cost reduction of enterprises is not facilitated.
In order to solve the problems, a suspension crystallizer can be additionally arranged before the falling film crystallizer, and the suspension crystallizer is used for carrying out primary crystallization on the liquid material. However, the crystallization particles obtained by the suspension crystallizer are large, more mother liquor is wrapped in the suspension crystallizer, the crystallization purity is relatively low, the falling film crystallizer still needs to be repeatedly crystallized for many times, the required time is still long, and the purification efficiency is still low.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention provides a material purification system and method combining micro-melt crystallization and falling film crystallization, which is used to solve the problem of low purification efficiency in the purification of low-purity materials in the prior art.
In order to achieve the above and other related objects, the present invention provides a material purification system combining micro-melt crystallization and falling film crystallization, including a falling film crystallizer and a micro-melt crystallizer, wherein the micro-melt crystallizer is located in front of the falling film crystallizer according to a material purification sequence, the micro-melt crystallizer includes a crystallization cavity for crystallization and a crystallization crushing cavity for crushing crystallization, the crystallization crushing cavity is communicated with the crystallization cavity, a crystal scraping mechanism for scraping crystallization on an inner wall of the crystallization cavity is disposed in the crystallization cavity, a contraction section, a throat section and an expansion section are sequentially disposed in the crystallization crushing cavity according to a material flow direction, and a crushing member is disposed in the crystallization crushing cavity.
The material purification system combining micro-melt crystallization and falling film crystallization has the following beneficial effects:
the micro-melt crystallizer is provided with the contraction section, the throat section and the expansion section in the crystallization crushing cavity, when a liquid material (from the crystallization cavity and containing large-particle crystals) flows through the contraction section, the flow area of the liquid material is reduced, the flow rate of the liquid material is increased, the liquid material impacts on the crushing piece, and the large-particle crystals in the liquid material are crushed into micro-particle crystals under the action of the crushing piece, so that the crystals are crushed, a molten fluid (namely a micro-melt) containing the micro-particle crystals is further obtained, the formation of the large-particle crystals wrapped with a mother solution is avoided, and the purity of the micro-particle crystals is higher than that of the large-particle crystals.
Optionally, the crushing member is located in the expanding section and includes a support grid, and a side wall of the support grid facing the throat section is provided with a plurality of spikes for crushing crystals.
In this scheme, refine out the structure of broken piece, support the net and support the spike on the net and can collide with the large granule crystallization in the liquid material to make the large granule crystallization broken under the impact effect, form the microparticle crystallization, release the mother liquor of parcel in the large granule crystallization. In addition, the meshes of the supporting grid are larger than the grain size of large-grain crystals, so that the crystals are prevented from blocking the supporting grid.
Optionally, the crushing member is located in the throat section, and the crushing member includes a rotating shaft rotatably connected in the crystallization crushing cavity, and a plurality of turbine blades are fixedly connected to the rotating shaft.
In this scheme, refine out the structure of broken piece, change epaxial turbine blade and take place to rotate under liquid material's impact to exert the shearing force to the large granule crystallization in the liquid material, and then make the large granule crystallization broken, form the microparticle crystallization, release the mother liquor of parcel in the large granule crystallization.
Optionally, the crushing piece is located throat portion and expansion section, and the crushing piece that is located throat portion is including rotating the pivot of connecting in the broken intracavity of crystallization, a plurality of turbine blades of fixedly connected with in the pivot, and the crushing piece that is located expansion section includes the support grid, supports the grid orientation be equipped with a plurality of spikes that are used for broken crystallization on a lateral wall of throat portion.
In the scheme, the crushing piece is positioned in the throat section, and the turbine blade rotates under the impact action of the liquid material, so that the shearing force is applied to large-particle crystals in the liquid material, the large-particle crystals can be crushed to form micro-particle crystals, and the blockage of the throat section by the large-particle crystals can be avoided; and the crushing piece positioned in the expansion section can crush the large-particle crystals into micro-particle crystals by impacting the large-particle crystals on the supporting grids and the spikes, so that the crushing effect of the large-particle crystals is ensured.
Optionally, the micro-melt crystallizer comprises a shell, the inner space of the shell forms the crystallization cavity, the crystal scraping mechanism comprises a stirring shaft, stirring blades and a connecting rod are arranged on the stirring shaft, and a scraping wafer used for scraping crystals on the inner wall of the crystallization cavity is arranged at one end, far away from the stirring shaft, of the connecting rod.
In this scheme, the utilization is scraped the crystallization that the wafer formed on with crystallization intracavity wall and is scraped down, avoids the crystallization to pile up on the inner wall of crystallization chamber, ensures to get into to contain the large granule crystallization in the liquid material of broken intracavity of crystallization, and then ensures the output of microparticle crystallization.
Optionally, the micro-melt crystallizer comprises a plurality of crystallization tubes, the inner space of each crystallization tube forms the crystallization cavity and the crystallization crushing cavity, the crystal scraping mechanism comprises a crystal scraping grid and a driving component used for driving the crystal scraping grid to slide in a reciprocating mode, and the crystal scraping grid is attached to the inner wall of the crystallization cavity.
In this scheme, the crystallization that the crystallization net formed on with crystallization intracavity wall is scraped to the utilization, avoids the crystallization to pile up on the inner wall of crystallization chamber, ensures to get into to contain the large granule crystallization in the liquid material of the broken intracavity of crystallization, and then ensures the output of microparticle crystallization.
Optionally, the driving assembly comprises a cross rod, a disc and a rotating rod, one end of the cross rod is hinged to the crystal scraping grid, the other end of the cross rod is connected with the disc in an eccentric rotating mode, the rotating rod is connected with the side wall of the crystallization cavity in a sealing and rotating mode, and one end, far away from the disc, of the rotating rod extends out of the crystallization tube.
In this embodiment, rotate the bull stick and can drive the disc and rotate, because the one end and the eccentric rotation of disc of horizontal pole are connected, and the other end of horizontal pole with scrape brilliant net hinge, consequently, the horizontal pole is pulled under the drive of disc and is scraped brilliant net along the reciprocal slip of axial in broken chamber of crystallization to the realization is scraped crystalline.
Optionally, a separating mechanism and a heating mechanism are further arranged between the micro-melt crystallizer and the falling film crystallizer according to the material purification sequence.
In the scheme, the micro-melt (containing micro-particle crystals) obtained by the micro-melt crystallizer is subjected to solid-liquid separation under the action of the separation mechanism to obtain the micro-particle crystals, and the micro-particle crystals form a molten material under the heating of the heating mechanism and are sent into the falling film crystallizer to be subjected to secondary crystallization.
Optionally, the purification system further comprises a filtrate tank, the filtrate tank is communicated with a return pipe, and one end of the return pipe, which is far away from the filtrate tank, is communicated with the crystallization cavity of the micro-melt crystallizer.
In the scheme, after solid-liquid separation of the micro-melt is realized by the separation mechanism, the filtrate flows into the filtrate tank and then flows into the crystallization cavity of the micro-melt crystallizer through the backflow pipe to be crystallized again, so that a target product in the material is crystallized in the micro-melt crystallizer as much as possible, and the waste is reduced.
The invention also provides a material purification method combining micro-melt crystallization and falling film crystallization, and the material purification system combining micro-melt crystallization and falling film crystallization is adopted for material purification.
The material purification method combining micro-melt crystallization and falling film crystallization has the following beneficial effects:
in the invention, the micro-melt is obtained by primary crystallization through the micro-melt crystallizer in the material purification system combining micro-melt crystallization and falling film crystallization, and micro-particle crystallization is obtained after solid-liquid separation of the micro-melt, so that large-particle crystallization wrapped with mother liquor is avoided, and the purity of the micro-particle crystallization is higher than that of crystallization obtained through a traditional suspension crystallizer, so that the crystallization time of the micro-particle crystallization in the falling film crystallizer after melting can be effectively shortened, the material purification efficiency is further improved, and the purity of a crystallization product obtained through the falling film crystallizer is more than 99.99%.
Drawings
Fig. 1 is a schematic structural diagram of a material purification system combining micro-melt crystallization and falling film crystallization according to example 1 of the present invention;
FIG. 2 is a longitudinal sectional view of a micro-melt mold according to example 1 of the present invention;
FIG. 3 isbase:Sub>A sectional view taken along the line A-A in FIG. 2 (the stirring vanes are not shown);
FIG. 4 is an enlarged schematic illustration of the tapping pipe from FIG. 2;
FIG. 5 is a partial sectional axial view of the tapping pipe according to example 2 of the invention;
FIG. 6 is a left side view of the turbine blade of FIG. 5;
FIG. 7 is a partial cross-sectional axial view of a tapping pipe according to example 3 of the present invention;
fig. 8 is a schematic structural diagram of a material purification system combining micro-melt crystallization and falling film crystallization according to example 4 of the present invention;
FIG. 9 is a longitudinal cross-sectional view of a micro-melt mold in accordance with example 4 of the present invention;
fig. 10 is an enlarged schematic view of a in fig. 9.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should also be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations of the invention described above will occur to those skilled in the art. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Reference numerals in the drawings of the specification include: the device comprises a micro-melt crystallizer 1, a separation mechanism 2, a filtrate tank 3, a heating mechanism 4, a falling-film crystallizer 5, a mother liquor tank 6, a residual liquor tank 7, a product tank 8, a shell 9, a crystallization cavity 10, a discharge pipe 11, a crystallization crushing cavity 12, a contraction section 121, a throat section 122, an expansion section 123, a liquid inlet pipe 13, a seed crystal feeding pipe 14, a stirring shaft 15, a driving motor 16, a stirring blade 17, a connecting rod 18, an arc-shaped plate 19, a scraping wafer 20, a crushing piece 21, a supporting grid 211, a spike 212, a rotating shaft 213, a falling-off prevention piece 2131, a turbine blade 214, a supporting rod 215, a cylinder 216, a cooling and heating medium cavity channel 22, a cooling and heating medium inlet pipe 23, a cooling and heating medium outlet pipe 24, a backflow pipe 25, a crystallization pipe 26, a scraping crystal grid 27, a cross rod 28, a disc 29, a rotating rod 30, a cylinder 31 and a sleeve 32.
Example 1
As shown in fig. 1 (arrows in fig. 1 indicate the flow direction of the material), the present embodiment provides a material high-efficiency purification system, which includes a micro-melt crystallizer 1, a separation mechanism 2, a filtrate tank 3, a heating mechanism 4, a falling film crystallizer 5, a mother liquor tank 6, a residual liquor tank 7 and a product tank 8. Referring to fig. 2 and 3, the micro-melt crystallizer 1 comprises a shell 9, a crystallization cavity 10 for crystallization is formed in the inner space of the shell 9, a discharge pipe 11 is communicated with the bottom of the crystallization cavity 10, and a crystallization crushing cavity 12 for crushing crystallization is formed in the inner space of the discharge pipe 11.
The top of the crystallization cavity 10 is communicated with a liquid inlet pipe 13 and a seed crystal feeding pipe 14, and the seed crystal feeding pipe 14 is provided with two valves for controlling the on-off of the seed crystal feeding pipe 14. Be equipped with in the crystallization chamber 10 and be used for striking off the brilliant mechanism of scraping of crystallization on the crystallization chamber 10 inner wall, scrape brilliant mechanism and include (mixing) shaft 15, casing 9 is stretched out on the top of (mixing) shaft 15, and (mixing) shaft 15 is connected with the sealed rotation of the roof of casing 9, and the top of casing 9 is passed through bolt fixed mounting and is used for driving (mixing) shaft 15 pivoted driving motor 16. The welding has stirring leaf 17 and connecting rod 18 on the (mixing) shaft 15, and the one end that connecting rod 18 kept away from (mixing) shaft 15 is equipped with and is used for striking off crystalline wafer 20 of scraping on the crystallization chamber 10 inner wall, and specifically, the one end welding that connecting rod 18 kept away from (mixing) shaft 15 has arc 19, and it scrapes wafer 20 to bond on the arc 19, and in this embodiment, it adopts rubber materials to make to scrape wafer 20.
The crystallization crushing cavity 12 is internally provided with a contraction section 121, a throat section 122 and an expansion section 123 in sequence according to the material flowing direction, the crushing members 21 (the number of the crushing members 21 can be multiple, in the embodiment, the number of the crushing members 21 is one) are arranged in the crystallization crushing cavity 12, the crushing members 21 are positioned in the expansion section 123, specifically, as shown in fig. 4, each crushing member 21 comprises a supporting grid 211, the supporting grid 211 is welded on the inner wall of the expansion section 123, a plurality of spikes 212 for crushing crystals are welded on the left side wall of the supporting grid 211, and the spikes 212 are conical. The side length of the meshes of the supporting grid 211 is more than one centimeter, so that the supporting grid 211 is prevented from being blocked by crystallization.
A cooling and heating medium channel 22 is formed in the peripheral side wall of the shell 9, a cooling and heating medium inlet pipe 23 is communicated with the bottom end of the cooling and heating medium channel 22, and a cooling and heating medium outlet pipe 24 is communicated with the top end of the cooling and heating medium channel 22.
One end of the discharge pipe 11, which is far away from the micro-melt crystallizer 1, is communicated with a feed inlet of the separation mechanism 2, and in this embodiment, the separation mechanism 2 adopts a centrifuge in the prior art to realize solid-liquid separation. The liquid outlet of the centrifuge is communicated with the top end of the filtrate tank 3 through a pipeline, so that the filtrate is stored in the filtrate tank 3. The bottom of the filtrate tank 3 is communicated with a return pipe 25, one end of the return pipe 25, which is far away from the filtrate tank 3, is communicated with the liquid inlet pipe 13, and the return pipe 25 is provided with a valve for controlling the on-off of the return pipe 25 and a liquid pump for conveying filtrate. The discharge port of the heating mechanism 4 is communicated with the feed port of the falling film crystallizer 5 through a pipeline, in this embodiment, the heating mechanism 4 adopts a heating kettle in the prior art to heat the microparticles subjected to solid-liquid separation to crystallize, so that the microparticles are crystallized to form a molten material.
The bottom intercommunication of falling film crystallizer 5 has ejection of compact house steward, and the one end that falling film crystallizer 5 was kept away from to ejection of compact house steward has three ejection of compact branch pipes through four-way pipe joint intercommunication, and three ejection of compact branch pipes communicate respectively with the top intercommunication of mother liquor jar 6, fluid residue jar 7 and product jar 8, and all install the valve that is used for controlling ejection of compact branch pipe break-make on three ejection of compact branch pipes. In addition, in another embodiment, the discharge header is communicated with a return pipe, and one end of the return pipe, which is far away from the discharge header, is communicated with a pipeline between the heating kettle and the falling film crystallizer 5, so that the molten material entering the falling film crystallizer 5 can be repeatedly subjected to melt crystallization, and more target products in the molten material can be crystallized as much as possible.
The embodiment also provides a material purification method combining micro-melt crystallization and falling film crystallization, which adopts the material purification system combining micro-melt crystallization and falling film crystallization to purify materials, and specifically comprises the following steps:
s1, crude purification: the liquid material flows into the crystallization cavity 10 through the liquid inlet pipe 13, the cooling medium in the cooling medium channel 22 in the peripheral side wall of the shell 9 heats or cools the peripheral side wall of the shell 9 in advance, and the temperature is controlled at the freezing point temperature of the target product, so that the target product in the liquid material entering the crystallization cavity 10 starts to crystallize. In the crystallization process, the stirring shaft 15 rotates slowly, the stirring blade 17 and the connecting rod 18 rotate along with the stirring shaft 15, and the scraping wafers 20 on the arc-shaped plate 19 rotate along with the rotation, so that crystals formed on the inner wall of the crystallization cavity 10 are scraped, crystal particles scraped by the scraping wafers 20 are large, and mother liquor (impurities) is wrapped in large-particle crystals. Under the stirring of the stirring blades 17, large-particle crystals are suspended in the liquid material and flow with the liquid material into the discharge pipe 11, i.e. into the crystal-crushing chamber 12. After flowing into the crystallization crushing cavity 12, the liquid material flows through the contraction section 121, then flows through the throat section 122 and the expansion section 123, when the liquid material flows through the contraction section 121, the flow area of the liquid material is reduced, the flow rate of the liquid material is increased, after the liquid material flows into the expansion section 123, the liquid material impacts on the crushing piece 21, and large-particle crystals in the liquid material are crushed into micro-particle crystals under the action of the spikes 212 and the supporting grids 211, so that the crystals are crushed, further, a molten fluid (micro-melt) containing the micro-particle crystals is obtained, and primary crystallization is completed. And then, the micro-melt enters a centrifuge to realize solid-liquid separation, so that micro-particle crystals and filtrate are obtained, and the filtrate enters a filtrate tank 3 to be stored.
S2, fine purification: and (2) conveying the microparticle crystals obtained in the step (S1) to a heating kettle through a closed conveyor (such as a screw conveyor or a belt conveyor) (in the process, taking out part of the microparticle crystals, and adding the part of the microparticle crystals into a crystallization cavity 10 in batches through a seed crystal adding pipe 14), heating to obtain a molten material, and feeding the molten material into a falling film crystallizer 5 through a pipeline for secondary crystallization to obtain a crystallized product, wherein the purity of the crystallized product is more than 99.99%. In the process, the mother liquor flows into the mother liquor tank 6 through the discharge header pipe and the discharge branch pipe corresponding to the mother liquor tank 6, the sweating liquid flows into the residual liquor tank 7 through the discharge header pipe and the discharge branch pipe corresponding to the residual liquor tank 7, and the crystallized product (molten state) flows into the product tank 8 through the discharge header pipe and the discharge branch pipe corresponding to the product tank 8.
In the material purification system and method combining micro-melt crystallization and falling film crystallization in this embodiment, micro-particle crystallization can be obtained through the micro-melt crystallizer 1, the mother liquor content in the molten material entering the falling film crystallizer 5 is reduced, the purity of the molten material entering the falling film crystallizer 5 is improved, the crystallization time of the falling film crystallizer 5 is shortened, and the material purification efficiency is effectively improved.
Example 2
The present embodiment is different from the first embodiment only in that: the crushing member 21 in this embodiment is different from the crushing member 21 in embodiment 1, as shown in fig. 5 and 6, the crushing member 21 in this embodiment is located in the throat section 122, the crushing member 21 includes a rotating shaft 213 rotatably connected in the crystal crushing cavity 12, specifically, a support rod 215 is welded on the inner wall of the contraction section 121, a cylinder 216 is welded on the bottom end of the support rod 215, the left end of the rotating shaft 213 is coaxially and rotatably connected with the cylinder 216, and an anti-slip member 2131 for preventing the rotating shaft 213 from disengaging from the cylinder 216 is further welded on the rotating shaft 213. The rotating shaft 213 is welded with a plurality of turbine blades 214, in this embodiment, the number of the turbine blades 214 is eight, and each four turbine blades 214 form a group.
In this embodiment, the liquid material containing large-particle crystals flows into the crystal crushing cavity 12 from the crystallization cavity 10, and the flow velocity of the liquid material increases after flowing through the constriction section 121, so that the flow velocity of the liquid material in the throat section 122 is relatively high, the liquid material impacts on the turbine blade 214, the turbine blade 214 drives the rotating shaft 213 to rotate, and the rotating turbine blade 214 applies a shearing force to the large-particle crystals in the liquid material, so that the large-particle crystals are crushed to form micro-particle crystals, and the mother liquor wrapped in the large-particle crystals is released. Moreover, the rotating turbine blades 214 apply shear forces to the liquid material, which can effectively prevent large particle crystals from clogging the throat section 122.
Example 3
The present embodiment differs from embodiment 1 only in that: the crushing member 21 in this embodiment is different from the crushing member 21 in embodiment 1, as shown in fig. 7, in this embodiment, the crushing member 21 is located in the throat section 122 and the expanding section 123, the crushing member 21 located in the throat section 122 includes a rotating shaft 213 rotatably connected in the crystal crushing cavity 12, specifically, a strut 215 is welded on the inner wall of the contracting section 121, a cylinder 216 is welded on the bottom end of the strut 215, the left end of the rotating shaft 213 is coaxially and rotatably connected with the cylinder 216, and an anti-falling member 2131 for preventing the rotating shaft 213 from falling off the cylinder 216 is welded on the rotating shaft 213. A plurality of turbine blades 214 are welded on the rotating shaft 213, in this embodiment, the number of the turbine blades 214 is eight, and every four turbine blades 214 form a group; the crushing member 21 in the expanding section 123 comprises a supporting grid 211, the supporting grid 211 is welded on the inner wall of the expanding section 123, a plurality of spikes 212 for crushing crystals are welded on the left side wall of the supporting grid 211, and the spikes 212 are in a conical shape. The side length of the meshes of the supporting grid 211 is more than one centimeter, so that the supporting grid 211 is prevented from being blocked by crystallization.
In this embodiment, the liquid material containing large-particle crystals flows into the crystal crushing cavity 12 from the crystallization cavity 10, and the flow velocity of the liquid material after flowing through the constriction section 121 is increased, so that the flow velocity of the liquid material in the throat section 122 is high, the liquid material impacts on the turbine blade 214, the turbine blade 214 drives the rotating shaft 213 to rotate, the rotating turbine blade 214 applies a shearing force to the large-particle crystals in the liquid material, so that the large-particle crystals are crushed to form micro-particle crystals, the mother liquid wrapped in the large-particle crystals is released, and the primary crushing is completed. In the process, part of large-particle crystals may not be crushed, so that the part of large-particle crystals impact on the supporting grid 211 and the spikes 212 along with the liquid material to realize secondary crushing, ensure the crushing effect of the large-particle crystals, reduce the amount of the large-particle crystals which are not crushed, and further improve the purity of the molten material.
Example 4
The present embodiment is different from embodiment 1 in that: the micro-melt crystallizer 1 in this embodiment is different from the micro-melt crystallizer 1 in embodiment 1, as shown in fig. 8, 9 and 10, the micro-melt crystallizer 1 in this embodiment includes a housing 9, a plurality of crystallization tubes 26 are disposed in the housing 9, in this embodiment, the number of the crystallization tubes 26 is three (it should be noted that, after reading the present invention, a person skilled in the art can design an appropriate number of crystallization tubes 26 in the housing 9 according to actual production requirements), and the internal space of each crystallization tube 26 forms a crystallization cavity 10 and a crystallization crushing cavity 12.
Be equipped with in the crystallization chamber 10 and be used for striking off the brilliant mechanism of scraping of crystallization on the crystallization chamber 10 inner wall, scrape brilliant mechanism including scraping brilliant net 27 and be used for the drive to scrape the drive assembly of brilliant net 27 horizontal slip, scrape the setting of the inner wall of brilliant net 27 laminating in crystallization chamber 10. The drive assembly comprises a cross rod 28, a disc 29 and a rotating rod 30, the right end of the cross rod 28 is hinged to the crystal scraping grid 27, the left end of the cross rod 28 is connected with the disc 29 in an eccentric rotating mode, specifically, a cylinder 31 in an eccentric arrangement is welded on the disc 29, a sleeve 32 is welded at the left end of the cross rod 28, and the sleeve 32 is sleeved on the cylinder 31. The rotating rod 30 is connected with the side wall of the crystallization chamber 10 in a sealing and rotating way, and one end of the rotating rod 30, which is far away from the disc 29, extends out of the crystallization tube 26, and in addition, the rotating rod 30 is positioned outside the shell 9.
Since the number of the crystallization tubes 26 is three, the number of the rotation levers 30 is also three, and the rotation levers 30 may be driven by a worker manually or by a motor. In this embodiment, a motor is selected to drive the rotating rods 30 to rotate, and the number of the motors is one, specifically, the output end of each motor is coaxially and fixedly connected with a driving shaft, each rotating rod 30 is coaxially and fixedly connected with a driven tooth, and the driving shaft is coaxially and fixedly connected with a driving tooth engaged with the driven tooth, so that the three rotating rods 30 are driven to rotate simultaneously through the engagement of the driving tooth and the driven tooth.
In this embodiment, the structure of the crystal crushing chamber 12 is the same as that of the crystal crushing chamber 12 in any one of embodiments 1 to 3, and the structure of the crystal crushing chamber 12 in this embodiment is the same as that of the crystal crushing chamber 12 in embodiment 1. In addition, in the present embodiment, the crystal crushing chamber 12 is located outside the housing 9.
The right end of the crystallization pipe 26 is communicated with a feed inlet of a centrifuge, the left end of the crystallization pipe 26 is communicated with a liquid inlet pipe 13, the liquid inlet pipe 13 is communicated with a seed crystal feeding pipe 14, and valves for controlling the on-off of the seed crystal feeding pipe 14 are installed on the seed crystal feeding pipe 14. The arrangement of the return pipe is the same as that of the return pipe in embodiment 1.
A cooling and heating medium inlet pipe 23 and a cooling and heating medium outlet pipe 24 are communicated with the inside of the casing 9 so as to input the cooling and heating medium into the inside of the casing 9, thereby controlling the crystallization temperature.
When the liquid material crystallization device is used, liquid materials flow into the crystallization pipe 26, and the crystallization temperature is controlled in advance by the cooling and heating medium in the shell 9, so that the liquid materials are crystallized on the inner wall of the crystallization cavity 10 every 4-6 min, a worker starts the motor for 30-50 s, the rotating rod 30 is driven by the motor to rotate, the disc 29 is driven to rotate, the cross rod 28 is driven to move left and right, the cross rod 28 drives the crystal scraping mesh 27 to slide left and right in a reciprocating mode, crystals on the inner wall of the crystallization cavity 10 are scraped, the scraped crystal particles are large, large-particle crystals flow into the crystallization crushing cavity 12 along with the liquid materials rightward, and after the liquid materials are accelerated, the crushing piece 21 is used for crushing large-particle crystals in the liquid materials, and therefore molten fluid (micro-melt) containing micro-particle crystals is obtained. Further, since the crystal crushing chamber 12 is outside the housing 9 and does not exchange heat with the cooling/heating medium, the inner wall of the crystal crushing chamber 12 is hardly crystallized.
In addition, after the motor stops working, the crystal scraping grids 27 stop sliding, so that the liquid materials are crystallized on the inner wall of the crystallization cavity 10.
In summary, in the present embodiment, the crystal scraping grid 27 intermittently reciprocates left and right to scrape the crystal on the inner wall of the crystallization chamber 10 to form a liquid material containing large-particle crystals, and then the liquid material flows into the crystallization crushing chamber 12, the flow rate of the liquid material increases, the large-particle crystals in the liquid material are crushed into fine-particle crystals by the crushing member 21, and a molten fluid (micro-melt) containing the fine-particle crystals is obtained, and then solid-liquid separation is performed by the centrifuge to obtain the fine-particle crystals. The microparticle crystallization forms a molten material under the heating action of the heating kettle, the molten material enters the falling film crystallizer 5 for secondary crystallization, and finally, a crystallization product with the purity of 99.99 percent is obtained. In addition, since the purity of the microparticle crystals is higher than that of the large-particle crystals, the present embodiment can effectively shorten the crystallization time of the falling film crystallizer 5, thereby improving the purification efficiency of the material. In addition, this embodiment is particularly useful for the purification of low-purity liquid material, effectively improves the purification efficiency of low-purity liquid material.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A material purification system combining micro-melt crystallization and falling film crystallization comprises a falling film crystallizer, and is characterized in that: still include little melt crystallizer, according to the material purification order, little melt crystallizer is located before the falling liquid film crystallizer, little melt crystallizer is including the broken chamber of crystallization that is used for the crystallization and is used for broken crystallization, broken chamber of crystallization and crystallization chamber intercommunication, and the crystallization intracavity is equipped with and is used for striking off the crystalline mechanism of scraping of crystallization intracavity wall on, and broken intracavity of crystallization is equipped with contraction section, larynx section and expansion segment according to material flow direction in proper order, the broken intracavity of crystallization is equipped with broken piece.
2. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: the crushing piece is positioned in the expansion section and comprises a supporting grid, and a plurality of spikes for crushing crystals are arranged on one side wall of the supporting grid, which faces the throat section.
3. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: the crushing piece is located the throat section, and the crushing piece is including rotating the pivot of connecting in the broken intracavity of crystallization, a plurality of turbine blades of fixedly connected with in the pivot.
4. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: the crushing piece is located throat portion and expansion section, and the crushing piece that is located throat portion is including rotating the pivot of connecting in the broken intracavity of crystallization, a plurality of turbine blades of fixedly connected with in the pivot, and the crushing piece that is located expansion section is including supporting the net, supports the net orientation be equipped with a plurality of spikes that are used for broken crystallization on a lateral wall of throat portion.
5. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: the micro-melt crystallizer comprises a shell, the inner space of the shell forms the crystallization cavity, the crystal scraping mechanism comprises a stirring shaft, a stirring blade and a connecting rod are arranged on the stirring shaft, and a scraping wafer used for scraping crystals on the inner wall of the crystallization cavity is arranged at one end, far away from the stirring shaft, of the connecting rod.
6. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: the micro-melt crystallizer comprises a plurality of crystallization tubes, the inner space of each crystallization tube forms a crystallization cavity and a crystallization crushing cavity, the crystal scraping mechanism comprises a crystal scraping grid and a driving component used for driving the crystal scraping grid to slide in a reciprocating mode, and the crystal scraping grid is attached to the inner wall of the crystallization cavity.
7. The system for purification of materials in combination with micro-melt crystallization and falling film crystallization of claim 6, wherein: the drive assembly comprises a cross rod, a disc and a rotating rod, one end of the cross rod is hinged to the crystal scraping grid, the other end of the cross rod is connected with the disc in an eccentric rotating mode, the rotating rod is connected with the side wall of the crystallization cavity in a sealing rotating mode, and one end, far away from the disc, of the rotating rod extends out of the crystallization tube.
8. A system for purification of materials in combination with micro-melt crystallization and falling film crystallization according to claim 1, wherein: according to the material purification sequence, a separation mechanism and a heating mechanism are also arranged between the micro-melt crystallizer and the falling film crystallizer.
9. A combined micro-melt crystallization and falling film crystallization material purification system according to claim 8, characterized in that: the purification system further comprises a filtrate tank, the filtrate tank is communicated with a backflow pipe, and one end, far away from the filtrate tank, of the backflow pipe is communicated with a crystallization cavity of the micro-melt crystallizer.
10. A material purification method combining micro-melt crystallization and falling film crystallization is characterized in that: material purification using a combined micro-melt crystallization and falling film crystallization material purification system according to any one of claims 1 to 9.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210325041.2A CN114669076B (en) | 2022-03-30 | 2022-03-30 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
| PCT/CN2022/124042 WO2023184924A1 (en) | 2022-03-30 | 2022-10-09 | Material purification system and method combining micro-melt crystallization and falling film crystallization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210325041.2A CN114669076B (en) | 2022-03-30 | 2022-03-30 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114669076A CN114669076A (en) | 2022-06-28 |
| CN114669076B true CN114669076B (en) | 2023-03-28 |
Family
ID=82076083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210325041.2A Active CN114669076B (en) | 2022-03-30 | 2022-03-30 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN114669076B (en) |
| WO (1) | WO2023184924A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114669076B (en) * | 2022-03-30 | 2023-03-28 | 上海东庚化工技术有限公司 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
| CN115554722B (en) * | 2022-12-05 | 2023-03-24 | 利安隆（天津）制药有限公司 | Vitamin K2 bulk drug purification reaction system |
| CN117138726A (en) * | 2023-10-26 | 2023-12-01 | 河南中锆新材料有限公司 | Reducing agent adding device for improving reaction efficiency, smelting furnace and zirconia preparation process |
| CN117959753B (en) * | 2024-04-02 | 2024-06-14 | 河北惠尔信新材料股份有限公司 | Crystallization device for manufacturing high-grade ferrous sulfate heptahydrate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3801285A (en) * | 1968-09-04 | 1974-04-02 | E Meisenburg | Apparatus for receiving crystals |
| CN104174181A (en) * | 2014-05-14 | 2014-12-03 | 重庆紫光化工股份有限公司 | Separation and purification system of organic synthesis feed liquid and separation and purification method thereof |
| CN109045743A (en) * | 2018-08-29 | 2018-12-21 | 江苏德邦工程有限公司 | The novel double down film melting crystallizer of one kind and its substance separating technology |
| CN215249601U (en) * | 2021-01-21 | 2021-12-21 | 青海盐湖工业股份有限公司 | Crystallization system |
| CN113912124A (en) * | 2021-10-29 | 2022-01-11 | 沈阳工业大学 | Purification method for micronization of ammonium paratungstate particles |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6256496B2 (en) * | 2015-03-06 | 2018-01-10 | Ｊｆｅスチール株式会社 | Crystallizer and crystallization method |
| CN112225635B (en) * | 2020-11-03 | 2022-09-23 | 中国石油化工股份有限公司 | Device, method and application for crystallization and separation of paraxylene |
| CN213912428U (en) * | 2020-11-30 | 2021-08-10 | 荆州市凯文生物科技有限公司 | Crystallization kettle anti-clogging device |
| CN114669076B (en) * | 2022-03-30 | 2023-03-28 | 上海东庚化工技术有限公司 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
-
2022
- 2022-03-30 CN CN202210325041.2A patent/CN114669076B/en active Active
- 2022-10-09 WO PCT/CN2022/124042 patent/WO2023184924A1/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3801285A (en) * | 1968-09-04 | 1974-04-02 | E Meisenburg | Apparatus for receiving crystals |
| CN104174181A (en) * | 2014-05-14 | 2014-12-03 | 重庆紫光化工股份有限公司 | Separation and purification system of organic synthesis feed liquid and separation and purification method thereof |
| CN109045743A (en) * | 2018-08-29 | 2018-12-21 | 江苏德邦工程有限公司 | The novel double down film melting crystallizer of one kind and its substance separating technology |
| CN215249601U (en) * | 2021-01-21 | 2021-12-21 | 青海盐湖工业股份有限公司 | Crystallization system |
| CN113912124A (en) * | 2021-10-29 | 2022-01-11 | 沈阳工业大学 | Purification method for micronization of ammonium paratungstate particles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114669076A (en) | 2022-06-28 |
| WO2023184924A1 (en) | 2023-10-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114669076B (en) | Micro-melt crystallization and falling film crystallization combined material purification system and method | |
| CN102356055B (en) | Methods and apparatus for production of natural l-menthol | |
| CN108939599A (en) | A kind of self-loopa crystallizer and multistage continuous crystallisation process | |
| CN108554796B (en) | Sand and stone screening box for building with cooling function | |
| CN112225635B (en) | Device, method and application for crystallization and separation of paraxylene | |
| CN112774244B (en) | Scraper type surface crystallizer | |
| CN105233522B (en) | A kind of freezing and crystallizing device | |
| CN211932436U (en) | Efficient crystallized honey feeding and melting system | |
| CN106048262A (en) | Purifying method and purifying apparatus for gallium | |
| CN217141575U (en) | Micro-melt crystallizer | |
| CN214344537U (en) | Multistage condensation crystallization purification device | |
| CN217511207U (en) | Solidification crystallization device for producing sulfamic acid by recrystallization method | |
| CN205145656U (en) | Crystal scrubber | |
| CN215315716U (en) | Prilling granulator is used in tubular product processing with screening mechanism | |
| CN112626349B (en) | Continuous crystallization and purification device and crystallization and purification method for scattered metal | |
| CN212067795U (en) | A recrystallization device for piperic acid is synthetic | |
| CN108837548A (en) | A kind of medical science exploitation drug evaporated crystallization device | |
| CN208626655U (en) | A kind of crystallization apparatus | |
| CN214051557U (en) | Melting device for high-efficiency co-crystallization production | |
| CN110973320A (en) | Efficient freezing and concentrating method suitable for food serous fluid | |
| CN206762364U (en) | A kind of sandstone mud separator | |
| CN116139526B (en) | High-efficient betaine crystallization device | |
| CN111520975A (en) | Industrial salt drying system and method | |
| CN214810861U (en) | Retort for bioseparation purification | |
| CN219272204U (en) | Purification device is used in heparin sodium production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |