WO2023134233A1 - 一种连续型降膜熔融结晶器 - Google Patents

一种连续型降膜熔融结晶器 Download PDF

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Publication number
WO2023134233A1
WO2023134233A1 PCT/CN2022/124105 CN2022124105W WO2023134233A1 WO 2023134233 A1 WO2023134233 A1 WO 2023134233A1 CN 2022124105 W CN2022124105 W CN 2022124105W WO 2023134233 A1 WO2023134233 A1 WO 2023134233A1
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Prior art keywords
crystallization
tube
heat exchange
tubes
falling film
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PCT/CN2022/124105
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English (en)
French (fr)
Inventor
康小玲
梁勇军
丁永良
李明全
李博文
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上海东庚化工技术有限公司
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Publication of WO2023134233A1 publication Critical patent/WO2023134233A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0009—Crystallisation cooling by heat exchange by direct heat exchange with added cooling fluid

Definitions

  • the present application relates to the technical field of crystallization equipment, in particular to a continuous falling film melting crystallizer.
  • Crystallization is the process by which a substance forms crystals from a liquid (liquid or melt) or gaseous state. Crystallization is an important method for solid purification. It can separate high-purity products, and has the advantages of low energy consumption, safe operation, and wide application range (such as the separation and purification of azeotropes and heat-sensitive substances that cannot be separated by conventional separation methods), etc. .
  • Falling film crystallization is a new type of crystallization separation technology, which includes three steps of crystallization, sweating and melting.
  • the principle is: the material flows from top to bottom along the tube wall and crystallizes during the flow process, and the cooling medium flows along the other side of the tube wall, transferring heat with the material and cooling the material during the flow process.
  • Falling film melting crystallizer is a kind of equipment used in falling film crystallization process.
  • the existing falling film melting crystallizer generally uses a distributor to evenly distribute the material or cold and hot media on the inner and outer walls of the crystallization tube, and control the flow rate of the material or cold and hot media to make it flow downward in a film shape along the tube wall under the action of gravity.
  • the flow rate is relatively slow, the crystallization process takes a long time, and the crystallization tube is usually a round tube, the material or cold and hot media will tend to gather radially under the action of gravity, and the distribution of materials or cold and hot media is uneven.
  • the heat exchange area is reduced and the heat exchange efficiency is reduced.
  • the radial crystallization thickness of the crystallization tube is greater than the circumferential crystallization thickness, and the crystallization thickness of the upper part of the crystallization tube is greater than that of the lower part.
  • the uneven crystallization thickness further reduces the heat transfer efficiency and increases the crystallization and/or Or the melting time is not conducive to reducing energy consumption; moreover, the uneven crystallization layer causes the material to produce a top-down impact force, and the crystallization layer itself has gravity. Re-melting into the material will further increase the crystallization time and energy consumption. When large crystals fall, it will even cause the crystallization tube to be blocked, which will easily cause the crystals to wrap impurities. Moreover, the congested crystallization tube cannot discharge sweat smoothly during the sweating process.
  • the heat medium raises the crystallization temperature to slightly lower than the melting point of the product, and sweating liquid appears.
  • sweating liquid appears on the tube wall, it is easy to cause the crystals to fall and block the crystallization tube. On the one hand, it is not easy to discharge The sweating liquid affects the purity of the product. On the other hand, the crystals fall into the sweating liquid and partially melt and are discharged thereupon, which affects the product yield.
  • the object of the present invention is to provide a kind of falling film melting crystallizer, is used to solve the separation and purification of adopting existing falling film melting crystallizer, high energy consumption, uneven crystallization thickness, product The technical problems of low purity, low yield and poor production continuity.
  • the invention provides a falling film melting crystallizer, which includes a cylinder body, the top and bottom of the cylinder body are respectively provided with a feed inlet and a discharge port, and the inside of the cylinder body is sequentially provided with several layers of crystallizers from top to bottom.
  • the crystallization zone is provided with a number of crystallization tubes arranged vertically, and heat exchange tubes are set outside the crystallization tubes.
  • the crystallization tubes and heat exchange tubes in the adjacent crystallization zone correspond to each other and communicate with each other.
  • the crystallization tube on the upper layer and the crystallization tube on the lowermost layer are connected to the feed port and the discharge port respectively; the cylinder body is provided with a cold and heat medium inlet and outlet connected to the top of the heat exchange tube in each layer of crystallization area, so The lower part of the cylinder body is provided with a cooling and heating medium inlet and outlet communicating with the bottom end of the heat exchange tube located at the lowermost layer.
  • the working principle of this device is: when using the falling film melting crystallizer of the present invention to carry out crystallization, the cold medium medium is first passed into the heat exchange tube from the cold and heat medium inlet and outlet of the uppermost crystallization zone, and the material to be purified is fed into the heat exchange tube from the feed inlet. Through the crystallization tube, the material and the cooling medium exchange heat, cool down and then crystallize during the flow process. At the same time, during the crystallization process, new cooling medium can also be introduced into the heat exchange tube from the cooling and heating medium inlet and outlet set in the middle of the cylinder. , so as to improve the uniformity of heat exchange between the material to be purified and the cold medium in the upper and lower parts of the cylinder, thereby improving the uniformity of crystallization in the upper part and lower part.
  • the invention can improve the exchange between the material to be purified and the cold medium in the upper and lower parts of the cylinder by adding a cold and hot medium inlet and outlet in the middle of the cylinder. Thermal uniformity, thereby improving the uniformity of crystallization in the upper part of the cylinder and crystallization in the lower part.
  • a number of swirl film distributors are also provided in the cylinder, and the swirl film distributors are located between the liquid separator and the crystallization tubes in the uppermost crystallization zone, which correspond one-to-one to the crystallization tubes in the uppermost crystallization zone and communicate with each other.
  • the swirling membrane distributor is funnel-shaped, including a funnel body and a tubular part. The inner wall of the funnel body is provided with a number of spiral diversion grooves.
  • the swirl film distributor can swirl the material to distribute the film, and the spiral liquid separation tank set on the inner wall of the funnel can make the material swirl, so that the material enters the crystallization tube more evenly, and the swirl makes the material to be purified have a certain
  • the circumferential initial speed can reduce the radial aggregation tendency of the material and further improve the uniformity of crystallization.
  • the swirling flow method can also increase the film-forming speed of the material and shorten the crystallization time.
  • a ventilation pipe is provided in the tubular part of the swirl membrane distributor, a ventilation hole is provided on the upper part of the ventilation pipe, a diversion platform is provided at the top of the ventilation pipe, and the outer diameter of the ventilation pipe is smaller than the length of the bottom end of the diversion platform, specifically 3/1-1/2 of the length of the bottom end of the deflector, and the inner diameter of the ventilation pipe is smaller than the inner diameter of the tubular part, specifically 3/1-1/2 of the inner diameter of the tubular part.
  • the ventilation hole set on the upper part of the ventilation pipe is conducive to emptying the air in the uppermost crystallization tube.
  • the liquid material to be purified flowing from top to bottom is in countercurrent contact with the air flowing from bottom to top, and the gas-liquid two-phase countercurrent contact makes the material to be purified form Swirl flow ensures good film-forming effect and makes the material enter the crystallization tube more uniformly.
  • the deflector is conical or umbrella-shaped, and the conical or umbrella-shaped deflector can play a role in "splitting" the material, so that the material is evenly distributed on the inner wall of the tubular part and then flows evenly into the crystallization tube in the form of a film
  • the wall further improves the crystallization uniformity of the material.
  • a number of re-distribution membrane heads are also arranged in the cylinder, and the re-distribution membrane heads are installed at the junction of two crystallization tubes connected to each other in adjacent crystallization areas.
  • the distribution table is located at the top of the air duct, which is conical or umbrella-shaped, and the outer diameter of the air duct is smaller than the bottom length of the material redistribution table, specifically 3/1-1 of the bottom length of the material redistribution table /2; the inner diameter of the air guide tube is smaller than the inner diameter of the crystallization tube, specifically 3/1-1/2 of the inner diameter of the crystallization tube.
  • the air guide hole set on the upper part of the air guide tube is conducive to emptying the air in the crystallization tube in other crystallization areas.
  • the liquid material to be purified flowing from top to bottom is in countercurrent contact with the air flowing from bottom to top, and the gas-liquid two-phase countercurrent contact makes the material to be purified Form a swirling flow to ensure a good film-forming effect, so that the material is more evenly distributed on the inner wall of the crystallization tube in the rest of the crystallization area.
  • the cone-shaped or umbrella-shaped material redistribution table can play a role of "splitting" the material, so that the material is evenly distributed on the inner wall of the crystallization tube, and the crystallization uniformity of the material is improved.
  • the membrane redistribution head also includes several deflectors, all of which are distributed in a circle with the air guide tube as the central axis, and the guide vanes are arranged obliquely between the air guide tube and the crystallization tube, and the air guide tube passes through the guide plate fixed on the inner wall of the crystallization tube,
  • the deflector is in the shape of a triangular prism.
  • the deflector in contact with the inner wall of the crystallization tube plays a role of "splitting" the material to be purified, so that the material to be purified is evenly distributed on the inner wall of the crystallization tube, so that the heat exchange and cooling of the material to be purified are more uniform, and the crystallization uniformity of the material to be purified is improved;
  • a "V"-shaped bayonet which is wide at the top and narrow at the bottom, is formed between adjacent deflectors that are in contact with the inner wall of the crystallization tube. The bayonet can effectively support and hold the crystal to prevent the crystal from falling off.
  • a material distributor is also provided in the barrel, which communicates with the feed inlet, and the material distributor is used to divide the material to be purified.
  • the material distributor includes a material distribution pipe network and a liquid distribution head
  • the material distribution pipe network includes a first pipeline and a second pipeline, all the first pipelines are radially distributed around the feed inlet, and all the second pipelines
  • the feed inlet is distributed in a circular direction at the center, and the first pipeline and the second pipeline intersect and communicate with each other, and a liquid separator is arranged at the intersection of the first pipeline and the second pipeline, and the liquid separator is in the shape of an inverted funnel, and There are a number of spiral liquid separation tanks on the inner wall, and all liquid separation heads correspond to the crystallization tubes in the uppermost crystallization area.
  • the material to be purified can be divided through the first pipeline and the second pipeline, so that the material to be purified entering the liquid separator has a certain circumferential initial velocity, which is beneficial to reducing the radial aggregation tendency of the material to be purified.
  • a number of spiral liquid separation tanks set on the inner wall of the liquid separation head can make the material to be purified swirl, so that the material to be purified can enter the crystallization tube more uniformly, and the swirl can make the material to be purified have a certain circumferential initial speed, which can Reduce the radial aggregation tendency of materials and further improve the uniformity of crystallization.
  • the swirling method can also increase the film-forming speed of materials and shorten the crystallization time.
  • each layer of crystallization area is provided with a cold and hot medium deflector, and the cold and hot medium deflector is located below the inlet and outlet of the cold and hot medium. They are in one-to-one correspondence with the heat exchange tubes and communicate with each other.
  • the diversion holes set on the hot and cold medium deflector plate can divert the cold medium medium into a film, and then make the cold medium medium distribute and flow in the form of a film in the heat exchange tube, improving the heat exchange between the cold medium medium and the material to be purified Uniformity.
  • a filter screen is also provided in the cylinder, and the filter screen is provided between the discharge port and the crystallization tube in the lowermost crystallization zone.
  • the filter set between the discharge port and the crystallization tube in the lowermost crystallization area can prevent the crystals from falling and block the discharge pipe between the discharge port and the cylinder, and the filter screen can collect the material in the middle, and then melt it Re-crystallization is beneficial to increase the yield, which in turn is beneficial to the realization of continuous production.
  • bosses are uniformly arranged on the inner wall of the crystallization tube.
  • the axial height of the boss is 0.5-3 mm, preferably 0.5-1 mm. Since the thickness of the crystal is generally 1-2mm, if the height of the boss is too high, it is easy to make the material flow in a strand instead of a film, which is not conducive to improving the uniformity of the crystal; if the height of the boss is too low, it will have a shunting effect on the material Not obvious.
  • the upper part of the longitudinal section of the boss is in a shape with a narrow top and a wide bottom, such as a triangle or an arc.
  • the upper part of the longitudinal section is narrow in the upper part and the lower part is wide in the shape of the boss, which can play the role of "shunting" the material to be purified, so that the heat exchange and cooling of the material to be purified can be more uniform, and the crystallization uniformity of the material to be purified can be improved;
  • the upper part of the longitudinal section of the boss It is in the shape of a narrow top and a wide bottom. Therefore, a "V"-shaped bayonet with a wide top and a narrow bottom is formed between the left and right adjacent bosses. The bayonet can effectively support and hold the crystal to prevent the crystal from falling off.
  • the inner wall of the crystallization tube is provided with anti-slip lines, and the anti-slip lines protrude outward or are concave inward by 0.1-1 mm along the inner wall of the crystallization tube. Since the inner wall of the crystallization tube protrudes outward or is concave inward by 0.1-1mm, the anti-skid pattern can improve the gripping force between the crystal and the inner wall of the crystallization tube, preventing the crystal from falling off the wall of the crystallization tube.
  • the upper part of the barrel is provided with an overflow port, and excess material can be discharged out of the barrel through the overflow port 18 .
  • an overflow port is provided on the top of the barrel.
  • Fig. 1 is the longitudinal sectional structure schematic diagram of falling film melting crystallizer
  • Fig. 2 is the bottom view of material distribution pipe network
  • Fig. 3 is a partial enlarged view of A in Fig. 1;
  • Fig. 4 is a schematic diagram of a longitudinal section structure of a liquid dispenser
  • Figure 5 is a bottom view of the liquid dispenser head
  • Fig. 6 is the bottom view of the cooling and heating medium deflector
  • Fig. 7 is a schematic diagram of the longitudinal section structure of the cooling and heating medium deflector
  • Fig. 8 is a longitudinal sectional structural schematic diagram of the assembly structure of the cooling and heating medium guide plate, the crystallization tube and the cooling and heating medium guide tube;
  • Fig. 9 is a schematic diagram of a longitudinal section structure of a swirling membrane distributor
  • Fig. 10 is the bottom view of the swirl film distributor
  • Fig. 11 is a schematic diagram of the longitudinal section structure of the connection structure between the swirl film distributor and the crystallization tube;
  • Fig. 12 is a longitudinal sectional structural schematic diagram of the assembly structure of the redistribution membrane head and the crystallization tube;
  • Figure 13 is a top view of the redistribution film head
  • Figure 14 is a schematic structural view of the guide vane
  • Fig. 15 is a schematic diagram of the longitudinal section structure of the inner wall of the crystallization tube provided with bosses;
  • Fig. 16 is a schematic diagram of the shape of the longitudinal section of the boss
  • Fig. 17 is a schematic diagram of the longitudinal section structure of the inner wall of the crystallization tube provided with anti-slip lines;
  • Fig. 18 is a longitudinal sectional structural schematic diagram of the assembly structure in which the lower end of the liquid separator extends into the funnel body of the swirl film distributor;
  • Fig. 19 is a schematic diagram of the longitudinal section structure of the connection structure between the swirl membrane distributor and the crystallization tube in which the longitudinal section of the bottom inner wall of the tubular part is in a figure-eight shape;
  • Fig. 20 is a longitudinal sectional structural schematic diagram of another installation method of the cooling and heating medium deflector, the crystallization tube and the cooling and heating medium guide tube.
  • the falling film melting crystallizer shown in Figure 1 is used for the separation and purification of materials through the falling film crystallization process.
  • the falling film melting crystallizer of the embodiment of the present invention includes a cylinder body 1 .
  • the top of the barrel 1 is provided with a feed port 2 and an overflow port 16, and the feed port 2 is the entrance for the material to be purified to enter the interior of the barrel 1.
  • the bottom of the barrel 1 is provided with a discharge port 3, and the discharge port 3 is a passage for materials (such as mother liquor, sweating liquid, and purified final product) to be discharged from the barrel 1 .
  • the upper part of the outer wall of the cylinder body 1 is provided with an overflow port 18, and the overflow port 18 can discharge excess material out of the cylinder body.
  • a material distributor, an upper crystallization zone and a lower crystallization zone are sequentially arranged inside the barrel 1 from top to bottom.
  • Both the upper crystallization zone and the lower crystallization zone are provided with crystallization tubes 6 , heat exchange tubes 7 , cooling and heating medium inlets and outlets 17 and cooling and heating medium deflectors 5 .
  • the material distributor includes a material distribution pipe network
  • the feed port 2 communicates with the material distribution pipe network through the feed pipe
  • the material distribution pipe network includes several first pipes 410 and several second pipes.
  • the pipes 430, all the first pipes 410 are distributed radially around the feed inlet 2
  • all the second pipes 430 are annular pipes, and are distributed circumferentially around the feed inlet 2
  • all the first pipes 410 and The second pipes 430 intersect each other and communicate with each other.
  • a liquid distributor 420 is provided, and the liquid distributor 420 is in one-to-one correspondence with the crystallization tubes 6 .
  • the liquid-dispensing head 420 is in the shape of an inverted funnel, and the inner wall of the liquid-dispensing head 420 is provided with a number of liquid-dispensing grooves 421.
  • the liquid-separating grooves 421 are helical (the way of left-handed or right-handed can be selected according to the geographical location during specific implementation).
  • Setting the liquid separator 420 at the intersection of the first pipeline 410 and the second pipeline 430 is beneficial to make the material to be purified in the liquid distributor 420 have a certain circumferential initial velocity and reduce the radial aggregation tendency of the material to be purified.
  • a number of spiral liquid separation grooves 421 arranged on the inner side wall of the liquid separation head 420 can make the material to be purified be in a swirling flow mode, so that the material to be purified can enter the crystallization tube 6 more evenly.
  • the initial speed can reduce the radial aggregation tendency of the material to be purified and further improve the uniformity of crystallization.
  • the swirl method can also increase the film-forming speed of the material to be purified and shorten the crystallization time.
  • the two ends of all the crystallization tubes 6 are connected with the feed port 2 and the discharge port 3 respectively, and the outer side of the crystallization tube 6 is provided with a heat exchange tube 7, and the upper end and the lower end of the heat exchange tube 7 are connected with the adjacent cold and hot medium inlet and outlet respectively. 17 communicates, the crystallization tube 6 is fixed on the inner wall of the cylinder body 1 through the crystallization tube splint 12, and the crystallization tube splint 12 is provided with a through hole on the plate surface, and the aperture of the through hole is slightly larger than the outer diameter of the crystallization tube 6.
  • the crystallization tube 6 can be in the shape of a cylinder, a square column, a hollow triangular prism or a hollow polygon.
  • the new cold medium can be passed into the heat exchange tube through the added cold and hot medium inlet and outlet 17 in the middle of the cylinder 1
  • the uniformity of heat exchange during the crystallization process of the upper crystallization zone and the lower crystallization zone can be improved, thereby improving the crystal thickness uniformity of the upper crystallization layer and the lower crystallization layer.
  • impurities in the crystallization layer in the crystallization tube 6 of the lower crystallization area can be washed away, thereby improving the purity of the crystallization layer.
  • it also acts as a rinse during the sweating phase, improving the purity of the final product.
  • the cooling and heating medium guide plate 5 is arranged between the upper end of the heat exchange tube 7 and the cooling and heating medium inlet and outlet 17 adjacent thereto.
  • the hot and cold medium guide plate 5 is provided with a number of guide holes 51, and all the guide holes 51 correspond to the heat exchange tubes 7 one by one and communicate with each other. groove.
  • the hot and cold medium guide plate 5 can divert the flow of the cold medium, and then make the cold medium flow in a film shape along the inner wall of the heat exchange tube 7, so that the heat exchange between the material to be purified and the cold medium is more uniform, and the uniformity of crystallization is improved.
  • the cooling and heating medium guide plate 5 can also fix the heat exchange tube 7 and the crystallization tube 6 on the inner wall of the cylinder body 1 .
  • a membrane distributor is also provided in the cylinder body 1, and the membrane distributor includes several swirl membrane distributors 8, the swirl membrane distributor 8 is located directly below the liquid separator 420, and is installed on the At the top of the crystallization tube 6 , the swirl film distributor 8 corresponds to the liquid separator 420 and the crystallization tube 6 one by one.
  • the swirl membrane distributor 8 is funnel-shaped, including a funnel body 810 and a tubular part 820 connected to the lower end of the funnel body 810.
  • the inner wall of the funnel body 810 of the swirl membrane distributor 8 is provided with a spiral diversion groove 811 (can be determined according to the actual implementation. Select the left-handed or right-handed way according to the geographical location).
  • the swirl film distributor 8 is provided with a vent pipe 10 , and the vent pipe 10 is fixedly installed in the tubular part 820 of the swirl film distributor 8 through the connecting piece 19 .
  • a deflector 11 is provided on the top of the vent pipe 10, and the deflector 11 is conical or umbrella-shaped.
  • An air hole 101 is provided on the upper side wall of the air pipe 10 .
  • the length of the bottom end of the flow guide table 11 is less than the inner diameter of the tubular portion 820 of the swirl membrane distributor 8 , specifically 1/2-1/3 of the inner diameter of the tubular portion 820 of the swirl membrane distributor 8 .
  • the height of the deflector 11 is smaller than the height of the funnel body 810 of the swirl membrane distributor 8 , specifically 1/3-1/2 of the height of the funnel body 810 of the swirl membrane distributor 8 .
  • the cone-shaped or umbrella-shaped deflector 11 provided on the top of the ventilation pipe 10 can play a role of "splitting" the material, so that the material is evenly distributed on the inner wall of the tubular part 820, and flows evenly along the inner wall of the tubular part 820 to the upper layer in the form of a film
  • the crystallization tube 6 improves the crystallization uniformity of the material.
  • the ventilation hole 101 provided on the side wall of the upper part of the ventilation pipe 10 is conducive to emptying the air in the crystallization tube 6 through the exhaust passage 9, and the liquid material to be purified flowing from top to bottom is in countercurrent contact with the air flowing from bottom to top.
  • the phase countercurrent contact makes the material to be purified form a swirling flow to ensure a good film-forming effect, so that the material to be purified enters the crystallization tube 6 in the upper crystallization area more evenly.
  • each layer of crystallization area is also provided with a crystallization tube splint 12, and the crystallization tube splint 12 plate surface is provided with some through holes, and the diameter of the through hole is slightly greater than the outer diameter of the crystallization tube 6, and all through holes are respectively connected with
  • the crystallization tubes 6 are connected in one-to-one correspondence.
  • each layer of crystallization area is also provided with a heat exchange tube splint 14, and the heat exchange tube splint 14 is provided with a number of through holes on the plate surface, and the diameter of the through hole is slightly larger than the outer surface of the heat exchange tube 7. diameter, and all the through holes communicate with the heat exchange tubes 7 in one-to-one correspondence.
  • the crystallization tube 7 in the lower crystallization area is provided with a redistribution film head 13, and the redistribution film head 13 includes an air guide tube 1302 and a material redistribution platform 1301 arranged at the top of the air guide tube 1302,
  • the air guide tube 1302 is fixed on the inner wall of the crystallization tube 6 by a plurality of guide vanes 1303, and all the guide vanes take the air guide tube 1302 as the central axis and are distributed in a circle, and the guide vanes are arranged obliquely between the air guide tube 1302 and the crystallization tube 6,
  • the flow sheet 1303 is in the shape of a triangular prism
  • the material redistribution table 1301 is in the shape of a cone or an umbrella.
  • the cone-shaped or umbrella-shaped deflector 11 provided on the top of the ventilation pipe 10 can play a role of "splitting" the material, so that the material is evenly distributed on the deflector 1303, and flows along the deflector 1303 to the crystallization area of the lower layer
  • the inner wall of the crystallization tube 6, and the deflector 1303 in contact with the inner wall of the crystallization tube 6 can play a "splitting" effect on the material to be purified, so that the heat exchange and cooling of the material to be purified are more uniform, and the crystallization uniformity of the material to be purified is improved.
  • a V-shaped bayonet with a wide top and a narrow bottom is formed between adjacent deflectors 1303 that are in contact with the inner wall of the crystallization tube 6 .
  • the bayonet can effectively support and hold the crystals and prevent the crystals from falling off.
  • the air guide hole 13021 provided on the upper part of the air guide tube 1302 is conducive to emptying the air in the crystallization tube 6 through the exhaust channel 9, and the liquid material to be purified flowing from top to bottom is in countercurrent contact with the air flowing from bottom to top, and the gas-liquid two-phase counterflow
  • the contact makes the material to be purified form a swirling flow to ensure a good film-forming effect, so that the material to be purified is evenly distributed on the inner wall of the crystallization tube 6 in the lower crystallization area.
  • filter screen 15 is arranged between discharge port 3 and crystallization tube 6, and is sunken downwards.
  • the filter screen 15 can prevent the crystallization from falling and block the discharge pipe between the discharge port 3 and the cylinder body 1.
  • the filter screen 15 is sunken downwards to collect the material in the middle, and then crystallize again after melting, which is beneficial to improve the yield. rate, thus realizing continuous production.
  • the material to be purified is sent into the feed port 2, and the material to be purified enters the first pipeline 410 and the second pipeline 430 through the feed pipeline to realize split flow, and then enters the liquid distribution head set at the intersection of the first pipeline 410 and the second pipeline 430
  • the material to be purified entering the liquid separator 420 has a certain circumferential initial velocity, which can reduce the radial aggregation tendency of the material to be purified.
  • the spiral liquid separation tank 421 provided on the inner side wall of the splitter head 420 allows the material to be purified to enter the swirling flow membrane distributor 8 in a swirling flow.
  • the spiral diversion groove 811 provided on the inner wall of the funnel body 810 of the swirl film distributor 8 allows the material to be purified to enter the tubular part 820 in a swirling manner, and the conical or umbrella-shaped diversion at the upper end of the ventilation pipe 10 arranged in the tubular part 820 Platform 11 plays a role of "shunting" for the material to be purified, so that the material to be purified is evenly distributed on the inner wall of the tubular part 820, and the vent hole 101 provided on the top of the vent pipe 10 makes the air in the crystallization tube 6 empty through the exhaust channel 9, and makes the The material to be purified forms a swirling flow, ensuring a good film-forming effect, so that the material to be purified is evenly distributed on the inner wall of the tubular part 820, and flows along the inner wall of the tubular part 820 to the inner wall of the crystallization tube 6 in the form of a film.
  • the material to be purified enters the crystallization tube 6 in a swirling flow, and flows along the inner wall of the crystallization tube 6 in a film shape.
  • the cooling medium enters the heat exchange tube 7 from the cooling and heating medium inlet and outlet 17 provided on the upper part of the cylinder body 6 through the cooling and heating medium deflector 5 , and flows along the inner wall of the heat exchange tube 7 in a film shape.
  • the material to be purified transfers heat with the cold medium, cools down and then crystallizes. During this process, the temperature of the cooling medium gradually rises, and the temperature difference between it and the material gradually decreases.
  • the material gradually flows along the crystallization tube 6 of the upper crystallization zone to the junction of the two crystallization tubes 6 where the upper and lower crystallization zones are connected to each other.
  • the distribution table 1301 plays a role of "splitting" the material to be purified, so that the material to be purified is evenly distributed on the guide plate 1303, and flows along the guide plate 1303 to the inner wall of the crystallization tube 6 in the lower crystallization area.
  • the air in the crystallization tube 6 in the lower crystallization area is emptied through the air guide hole 13021 opened on the upper part of the air guide tube 1302, and the material to be purified forms a swirling flow.
  • the new cold medium is passed into the heat exchange tube 7 through the cold and hot medium inlet and outlet 17 set in the middle of the cylinder 1, and the material to be purified exchanges heat with the cold medium, cools down and then crystallizes.
  • the inner wall of the crystallization tube 6 is uniformly provided with several bosses 61, the axial height of the bosses 61 is 0.5-3mm, preferably 0.5-1mm,
  • the boss 61 is triangular or arc-shaped. Specifically, the boss 61 with a narrow top and a wide bottom in the longitudinal section acts as a "shunt" for the material to be purified, making the heat exchange and cooling of the material to be purified more uniform, and improving the crystallization uniformity of the material to be purified.
  • a "V"-shaped bayonet with a wide top and a narrow bottom is formed.
  • This bayonet can effectively support and hold the crystal to prevent the crystal from falling off. Since the thickness of the crystal is generally 1-2mm, if the boss If the height of 61 is too high, it is easy to make the material to be purified flow in strands instead of films, which is not conducive to improving the uniformity of crystallization. If the height of the boss 61 is too low, the diversion effect on the material is not obvious.
  • the inner wall of the crystallization tube 6 is also provided with anti-slip lines 62, and the anti-slip lines 62 protrude outward or inwardly 0.1-1mm along the inner wall of the crystallization tube 6, preferably 0.1-0.5mm.
  • the anti-slip pattern 62 can improve the grasping force between the crystal and the inner wall of the crystallization tube 6, and prevent the crystal from falling off from the wall of the crystallization tube 6.
  • the anti-slip pattern 62 can be star-shaped, wave-shaped, cross-shaped, etc., as long as the crystal can be made to produce concave-convex shape Just the structure.
  • the lower end of the liquid distribution head 420 extends into the funnel body 810 of the swirl film distribution head 8, and the radius of the bottom end of the liquid distribution head 420 is smaller than that of the swirl distribution film
  • the inner diameter of the bottom of the tubular part 820 of the swirl membrane distributor 8 gradually increases from top to bottom, that is, the longitudinal section of the inner wall of the bottom of the tubular part 820 is in a figure-eight shape. .
  • the longitudinal section of the inner wall at the bottom of the tubular part 820 is arranged in a figure-eight shape.
  • the cooling and heating medium guide plate 5 is arranged between the upper end of the heat exchange tube 7 and the cooling and heating medium inlet and outlet 17 adjacent thereto.
  • the hot and cold medium guide plate 5 is provided with a number of guide holes 51 , all of which correspond to the heat exchange tubes 7 one by one and communicate with each other.
  • the diameter of the guide holes 51 is slightly larger than the outer diameter of the heat exchange tube 7 .
  • the number of layers of the crystallization area can be adjusted according to actual production requirements.
  • the number of layers of the crystallization area can be adjusted to 3 layers according to the actual production situation.
  • Median inlet and outlet 17 the total length of the interconnected crystallization tubes of three layers is equal to the total length of the interconnected crystallization tubes when the crystallization region is two layers.

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Abstract

本发明提供一种连续型降膜熔融结晶器。所述降膜熔融结晶器包括筒体，所述筒体的顶部和底部分别设置有进料口和出料口，筒体内部从上至下依次设有若干层结晶区，结晶区均设有若干竖向设置的结晶管，结晶管外均套设有换热管，相邻结晶区的结晶管、换热管一一对应并相互连通，位于最上层的结晶管和位于最下层的结晶管分别与进料口和出料口相连通；筒体上设有与每层结晶区的换热管顶端相连通的冷热媒进出口，筒体的下部设有与位于最下层的换热管底端相连通的冷热媒进出口。本发明通过在筒体中部增设冷热媒进出口，能够改善筒体上部和下部的待提纯物料与冷媒介质之间的换热均匀性，进而改善筒体上部结晶和下部结晶的均匀性。

Description

一种连续型降膜熔融结晶器 技术领域
本申请涉及结晶设备技术领域，尤其涉及一种连续型降膜熔融结晶器。
背景技术
结晶是指物质从液态(液体或熔融体)或气态形成结晶的过程。结晶是固体提纯的重要方法，其能够分离出高纯度产品，具有能耗低、操作安全、适用范围广(如适用于常规分离方法无法分离的共沸物、热敏性物质等的分离提纯)等优点。
降膜结晶是一种新型的结晶分离技术，其包括结晶、发汗和熔融三个步骤。其原理为：物料沿管壁自上而下流动并在流动过程中结晶，冷却介质沿管壁的另一侧流动，在流动过程中与物料传热并使物料降温。
降膜熔融结晶器是一种用于降膜结晶工艺的设备。现有的降膜熔融结晶器普遍采用分布器将物料或冷热媒均匀分布到结晶管内外壁上，控制物料或者冷热媒流速使其在重力作用下沿管壁呈膜状向下流动，为保持良好的成膜效果，流速较为缓慢，结晶过程时间较长，并且结晶管通常采用圆管，物料或者冷热媒在重力作用下会呈径向聚集趋势，物料或冷热媒分布不均从而减少了换热面积，降低了换热效率，结晶管径向结晶厚度大于周向结晶厚度，且结晶管上部结晶厚度大于下部厚度，结晶厚度不均进一步降低了传热效率，增加了结晶和/或熔融时间，不利于降低能耗；再者，结晶层不均使物料产生自上而下的冲击力，且结晶层本身存在重力，二者的综合作用易使结晶自管壁脱落，使结晶重新熔化至物料中，进一步增加了结晶时间和能耗，大块结晶掉落时甚至会造成结晶管拥堵，易使结晶包裹杂质，并且，拥堵的结晶管在发汗过程中无法顺利排出发汗液，影响了产品纯度；此外，发汗过程中，热媒使结晶温度上升至略低于产品熔点时出现发汗液，发汗液出现在管壁时也易使结晶掉落，堵塞结晶管，一方面不易排出发汗液，影响产品纯度，另一方面结晶掉入发汗液后部分融化并随之排出，影响了产品收率。
综上，采用现有的降膜熔融结晶器进行分离提纯，能耗高，结晶厚度不均，产品纯度低，收率低，生产连续性差，限制了生产效率的提高。
发明内容
鉴于以上所述现有技术的缺点，本发明的目的在于提供一种降膜熔融结晶器，用于解决采用现有的降膜熔融结晶器进行分离提纯，能耗高，结晶厚度不均，产品纯度低，收率低，生产连续性差的技术问题。
本发明提供了一种降膜熔融结晶器，包括筒体，所述筒体的顶部和底部分别设置有进料口和出料口，所述筒体内部从上至下依次设有若干层结晶区，所述结晶区均设有若干竖向设置的结晶管，所述结晶管外均套设有换热管，相邻结晶区的结晶管、换热管一一对应并相互连通，位于最上层的结晶管和位于最下层的结晶管分别与进料口和出料口相连通；所述筒体上设有与每层结晶区的换热管顶端相连通的冷热媒进出口，所述筒体的下部设有 与位于最下层的换热管底端相连通的冷热媒进出口。
本装置的工作原理为：采用本发明的降膜熔融结晶器进行结晶时，先从最上层结晶区的冷热媒进出口将冷媒介质通入换热管中，从进料口将待提纯物料通入结晶管内，物料与冷媒介质在流动过程中换热、降温进而结晶，同时，在结晶过程中，还可以从筒体中部设置的冷热媒进出口向换热管内通入新的冷媒介质，从而改善筒体上部和下部的待提纯物料与冷媒介质之间的换热均匀性，进而改善上部结晶和下部结晶的均匀性。
本装置的有益效果为：与传统的降膜熔融结晶器相比，本发明通过在筒体中部增设冷热媒进出口，能够改善筒体上部和下部的待提纯物料与冷媒介质之间的换热均匀性，进而改善筒体上部结晶和下部结晶的均匀性。
可选地，筒体内还设置有若干旋流布膜器，旋流布膜器位于分液头与最上层结晶区的结晶管之间，其与最上层结晶区的结晶管一一对应且相互连通，旋流布膜器呈漏斗状，包括漏斗本体和管状部分，漏斗本体内壁开设有若干螺旋状导流槽。旋流布膜器能够对物料进行旋流布膜，漏斗本体内壁设置的螺旋状分液槽能够使物料呈旋流方式，使物料更均匀地进入结晶管，并且，旋流使待提纯物料具备一定的周向初始速度，能够降低物料的径向聚集趋势，进一步改善结晶均匀性，旋流方式还能够提高物料的成膜速度，缩短结晶时间。
可选地，旋流布膜器的管状部分内设置有通气管，所述通气管上部设置有通气孔，通气管顶端设置有导流台，通气管外径小于导流台底端长度，具体为导流台底端长度的3/1-1/2，通气管的内径小于所述管状部分内径，具体为管状部分内径的3/1-1/2。通气管上部设置的通气孔有利于将最上层的结晶管内空气排空，自上至下流动的液态待提纯物料与自下至上流动的空气逆流接触，气液两相逆流接触使待提纯物料形成旋流，保证良好的成膜效果，使物料更均匀地进入结晶管。
可选地，导流台呈锥形或伞状，锥形或伞状导流台能够对物料起到“分流”作用，使物料均匀分布于管状部分内壁进而以膜状形式均匀流动至结晶管内壁，进一步改善物料的结晶均匀性。
可选地，筒体内还设置有若干再布膜头，再布膜头安装于相邻结晶区相互连通的两结晶管的连接处，再布膜头包括物料再分布台和导气管，物料再分布台位于所述导气管的顶端，其呈锥形或伞状，且导气管外径小于所述物料再分布台的底端长度，具体为物料再分布台底端长度的3/1-1/2；导气管内径小于所述结晶管内径，具体为结晶管内径的3/1-1/2。导气管上部设置的导气孔有利于将其他结晶区的结晶管内空气排空，自上至下流动的液态待提纯物料与自下至上流动的空气逆流接触，气液两相逆流接触使待提纯物料形成旋流，保证良好的成膜效果，使物料更均匀的分布于其余结晶区的结晶管内壁。呈锥形或伞状物料再分布台能够对物料起到“分流”作用，使物料均匀分布于结晶管内壁，改善物料的结晶均匀性。
可选地，再布膜头还包括若干导流片，所有导流片以导气管为中心轴，呈圆周分布，导流片倾斜设置于导气管与结晶管之间，导气管通过导流片固定于结晶管的内壁，
导流片呈三棱柱状。与结晶管内壁接触的导流片对待提纯物料起到“分流”作用，使待提纯物料均匀分布于结晶管内壁，使待提纯物料换热、降温更均匀，改善待提纯物料的结晶均匀性；与结晶管内壁接触的相邻导流片之间形成上宽下窄类似“V”型的卡口，该卡口能够有效支撑并卡住结晶，防止结晶脱落。
可选地，筒体内还设置有物料分布器，其与进料口连通，物料分布器用于将待提纯物料进行分流。
可选地，物料分布器包括物料分布管网和分液头，物料分布管网包括第一管道和第二管道，所有第一管道以进料口为中心呈径向分布，所有第二管道以进料口为中心呈环向分布，且第一管道和第二管道相互交叉、相互连通，第一管道和第二管道的交叉点处设置有分液头，分液头呈倒置漏斗状，且内壁开设有若干螺旋状分液槽，所有分液头与最上层结晶区的结晶管一一对应。通过第一管道和第二管道能够对待提纯物料进行分流，使进入分液头内的待提纯物料具备一定的周向初速度，有利于降低待提纯物料的径向聚集趋势。分液头内壁设置的若干螺旋状分液槽能够使待提纯物料呈旋流方式，使待提纯物料更均匀地进入结晶管，并且，旋流使待提纯物料具备一定的周向初始速度，能够降低物料的径向聚集趋势，进一步改善结晶均匀性，旋流方式还能够提高物料的成膜速度，缩短结晶时间。
可选地，每层结晶区均设置有冷热媒导流板，冷热媒导流板位于冷热媒进出口的下方，冷热媒导流板上设置有若干导流孔，导流孔与换热管一一对应并相互连通。冷热媒导流板上设置的导流孔能够将冷媒介质进行导流布膜，进而使冷媒介质在换热管中呈膜状分布、流动，改善冷媒介质与待提纯物料之间的换热均匀性。
可选地，筒体内还设置有过滤网，过滤网设置于所述出料口与最下层结晶区的结晶管之间。出料口与最下层结晶区的结晶管之间设置的过滤网能够防止结晶掉落堵塞出料口与筒体之间的出料管道，并且，过滤网能够将物料收集到中部，进而融化后再次结晶，有利于提高收率，进而有利于实现连续化生产。
可选地，结晶管内壁均匀设置有若干凸台。
可选地，凸台的轴向高度为0.5-3mm，优选为0.5-1mm。由于结晶的厚度一般为1-2mm，若凸台的高度过高，易使物料呈股状而非膜状流动，不利于改善结晶均匀性；若凸台的高度过低，对物料的分流作用不明显。
可选地，凸台的纵向截面上部呈上窄下宽的形状，如三角形或弧形。纵向截面上部呈上窄下宽的形状的凸台能够对待提纯物料起到“分流”作用，使待提纯物料换热、降温更均匀，改善待提纯物料的结晶均匀性；凸台的纵向截面上部呈上窄下宽的形状，故而，左右相邻凸台之间形成上宽下窄类似“V”型的卡口，该卡口能够有效支撑并卡住结晶，防止结晶脱落。
可选地，结晶管内壁设置有防滑纹，防滑纹沿结晶管内壁向外突或向内凹0.1-1mm。由于沿结晶管内壁向外突或向内凹0.1-1mm，故而，防滑纹能够提高结晶与结晶管内壁壁面之间的抓臂力，防止结晶自结晶管管壁脱落。
可选地，筒体的上部设置有溢流口，通过溢流口18能够将过多的物料排出筒体。
可选地，筒体的顶部设置有溢气口。
附图说明
为了更清楚地说明本申请的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，对于本领域普通技术人员而言，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为降膜熔融结晶器的纵向剖面结构示意图；
图2为物料分布管网的仰视图；
图3为图1中A的局部放大图；
图4为分液头的纵向剖面结构示意图；
图5为分液头的仰视图；
图6为冷热媒导流板的仰视图；
图7为冷热媒导流板的纵向剖面结构示意图；
图8为冷热媒导流板与结晶管和冷热媒导流管的装配结构的纵向剖面结构示意图；
图9为旋流布膜器的纵向剖面结构示意图；
图10为旋流布膜器的仰视图；
图11为旋流布膜器与结晶管的连接结构的纵向剖面结构示意图；
图12为再布膜头与结晶管的装配结构的纵向剖面结构示意图；
图13为再布膜头的俯视图；
图14为导流片的结构示意图；
图15为设置有凸台的结晶管内壁的纵向剖面结构示意图；
图16为凸台的纵向剖面的形状示意图；
图17为设置有防滑纹的结晶管内壁的纵向剖面结构示意图；
图18为分液头下端伸入旋流布膜器的漏斗本体内的装配结构的纵向剖面结构示意图；
图19为管状部分底部内壁的纵向截面呈八字形的旋流布膜器与结晶管的连接结构的纵向剖面结构示意图；
图20为冷热媒导流板与结晶管和冷热媒导流管的另一种安装方式的装配结构的纵向剖面结构示意图。
图示说明：1-筒体，2-进料口，3-出料口，410-第一管道，420-分液头，421-分液槽，430-第二管道，5-冷热媒导流板，51-导流孔，6-结晶管，61-凸台，62-防滑纹，7-换热管，8-旋流布膜头，810-漏斗本体，811-导流槽，820-管状部分，9-排气通道，10-通气管，101-通气孔，11-导流台，12-结晶管夹板，13-再布膜头，1301-物料再分布台，1302-导气管，13021-导气孔，1303-导流片，14-换热管夹板，15-过滤网，16-溢气口，17-冷热媒进出口，18-溢流口，19-连接片。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。
需要说明的是，本实施例中所提供的图示仅以示意方式说明本发明的基本构想，遂图式中仅显示与本发明中有关的组件而非按照实际实施时的组件数目、形状及尺寸绘制，其实际实施时各组件的型态、数量及比例可为一种随意的改变，且其组件布局型态也可能更为复杂。本说明书所附图式所绘示的结构、比例、大小等，均仅用以配合说明书所揭示的内容，以供熟悉此技术的人士了解与阅读，并非用以限定本发明可实施的限定条件，故不具技术上的实质意义，任何结构的修饰、比例关系的改变或大小的调整，在不影响本发明所能产生的功效及所能达成的目的下，均应仍落在本发明所揭示的技术内容得能涵盖的范围内。同时，本说明书中所引用的如“上”、“下”、“左”、“右”“中”等的用语，亦仅为 便于叙述的明了，而非用以限定本发明可实施的范围，其相对关系的改变或调整，在无实质变更技术内容下，当亦视为本发明可实施的范畴。
如图1所示的降膜熔融结晶器，该降膜熔融结晶器用于物料通过降膜结晶工艺进行分离提纯。
本发明实施例的降膜熔融结晶器包括筒体1。
筒体1的顶部设置有进料口2和溢气口16，进料口2为待提纯物料进入筒体1内部的入口。筒体1的底部设置有出料口3，出料口3为物料(如母液、发汗液、提纯后终产品)排出筒体1的通道。筒体1外壁的上部设置有溢流口18，溢流口18能够将过多的物料排出筒体。
筒体1内部从上至下依次设有物料分布器、上结晶区和下结晶区。
上结晶区、下结晶区均设置有结晶管6、换热管7、冷热媒进出口17和冷热媒导流板5。
具体的，如图1-5所示，物料分布器包括物料分布管网，进料口2通过进料管道与物料分布管网相连通，物料分布管网包括若干第一管道410和若干第二管道430，所有第一管道410以进料口2为中心呈径向分布，所有第二管道430为环形管道，且以进料口2为中心呈环向分布，并且所有的第一管道410和第二管道430相互交叉、相互连通。
第一管道410和第二管道430的交叉点处均设置有一个分液头420，分液头420与结晶管6一一对应。分液头420呈倒置的漏斗状，分液头420的内壁开设有若干分液槽421，分液槽421呈螺旋状(具体实施时可根据所处地理位置选择左旋或者右旋方式)。将分液头420设置于第一管道410和第二管道430交叉点处，有利于使分液头420内待提纯物料具备一定的周向初速度，降低待提纯物料的径向聚集趋势。分液头420内部侧壁设置的若干螺旋状分液槽421能够使待提纯物料呈旋流方式，使待提纯物料更均匀地进入结晶管6，其次，旋流使待提纯物料具备一定的周向初始速度，能够降低待提纯物料的径向聚集趋势，进一步改善结晶均匀性，旋流方式还能够提高待提纯物料的成膜速度，缩短结晶时间。
所有结晶管6的两端分别与进料口2和出料口3连通，结晶管6外侧套设有换热管7，换热管7的上端和下端分别与相邻的冷热媒进出口17连通，结晶管6通过结晶管夹板12固定于筒体1内壁上，结晶管夹板12板面上开设有通孔，通孔的孔径略大于结晶管6的外径。结晶管6可以采用圆筒状、方柱状、空心三棱柱状或空心多边形状。与传统的降膜熔融结晶器相比，采用本发明实施例的降膜熔融结晶器进行结晶时，能够将新的冷媒介质通过筒体1中部增设的冷热媒进出口17通入换热管7中，能够改善上层结晶区和下层结晶区结晶过程中的换热均匀性，进而改善上层结晶与下层结晶的结晶厚度均匀性。其次，物料自上而下流动过程中能够洗去下层结晶区的结晶管6内结晶层的杂质，提高结晶层的纯度。此外，在发汗阶段也能够起到冲洗作用，提高终产品的纯度。
如图1及图6-8所示，冷热媒导流板5设置于换热管7上端与其相邻上方的冷热媒进出口17之间。冷热媒导流板5设置有若干导流孔51，所有导流孔51分别与换热管7一一对应且相互连通，冷热媒导流板5的底面开设有供换热管7插入的凹槽。冷热媒导流板5能够使冷媒介质分流，进而使冷媒介质沿换热管7内壁呈膜状流动，使待提纯物料与冷媒介质换热更均匀，改善结晶均匀性。冷热媒导流板5还能够将换热管7和结晶管6固定于筒体1的内壁上。
如图1及图9-11所示，筒体1内还设有布膜器，布膜器包括若干旋流布膜器8，旋流布膜器8位于分液头420的正下方，并安装在结晶管6的顶端，旋流布膜器8与分液头420、结晶管6一一对应。旋流布膜器8呈漏斗状，包括漏斗本体810及与漏斗本体810下端相连的管状部分820，旋流布膜器8的漏斗本体810内壁上开设有螺旋状导流槽811(具体实施时可根据所处地理位置选择左旋或者右旋方式)。旋流布膜器8内设有通气管10，通气管10通过连接片19固定安装在旋流布膜器8的管状部分820内。通气管10的顶部设有导流台11，导流台11呈锥形或伞状。通气管10上部侧壁上设有通气孔101。
具体的，导流台11底端长度小于旋流布膜器8的管状部分820的内径，具体为旋流布膜器8的管状部分820内径的1/2-1/3。导流台11的高度小于旋流布膜器8的漏斗本体810的高度，具体为旋流布膜器8的漏斗本体810高度的1/3-1/2。
通气管10的顶部设置的锥形或伞状导流台11能够对物料起到“分流”作用，使物料均匀分布于管状部分820的内壁，并呈膜状沿管状部分820内壁均匀流动至上层的结晶管6，改善物料的结晶均匀性。
通气管10上部侧壁设置的通气孔101有利于将结晶管6内空气通过排气通道9排空，自上至下流动的液态待提纯物料与自下至上流动的空气逆流接触，气液两相逆流接触使待提纯物料形成旋流，保证良好的成膜效果，使待提纯物料更均匀地进入上层结晶区的结晶管6内。
为进一步固定结晶管6，每层结晶区还设置有结晶管夹板12，结晶管夹板12板面上开设有若干通孔，通孔的直径略大于结晶管6的外径，所有通孔分别与结晶管6一一对应连通。
为进一步固定换热管7，每层结晶区还设置有还设置有换热管夹板14，换热管夹板14板面上开设有若干通孔，通孔的直径略大于换热管7的外径，所有通孔分别与换热管7一一对应连通。
如图1及图12-14所示，下层结晶区的结晶管7内设置有再布膜头13，再布膜头13包括导气管1302和设置于导气管1302顶端的物料再分布台1301，导气管1302通过若干导流片1303固定于结晶管6的内壁，所有导流片以导气管1302为中心轴，呈圆周分布，导流片倾斜设置于导气管1302与结晶管6之间，导流片1303呈三棱柱状，物料再分布台1301呈锥形或伞状。
具体的，通气管10顶部设置的锥形或伞状导流台11能够对物料起到“分流”作用，使物料均匀分布于导流片1303上，并沿导流片1303流动至下层结晶区的结晶管6的内壁，并且与结晶管6内壁接触的导流片1303能够对待提纯物料起到“分流”作用，使待提纯物料换热、降温更均匀，改善待提纯物料的结晶均匀性。与结晶管6内壁接触的相邻导流片1303之间形成上宽下窄类似“V”型的卡口，该卡口能够有效支撑并卡住结晶，防止结晶脱落。
导气管1302上部设置的导气孔13021有利于将结晶管6内空气通过排气通道9排空，自上至下流动的液态待提纯物料与自下至上流动的空气逆流接触，气液两相逆流接触使待提纯物料形成旋流，保证良好的成膜效果，使待提纯物料均匀分布于下层结晶区的结晶管6的内壁。
筒体1内还设置有过滤网15，过滤网15设置于出料口3与结晶管6之间，且向下凹 陷。过滤网15能够防止结晶掉落堵塞出料口3与筒体1之间的出料管道，其次，过滤网15向下凹陷，能将物料收集到中部，进而融化后再次结晶，有利于提高收率，进而实现连续化生产。
本发明实施例的降膜熔融结晶器的工作过程如下：
将待提纯物料送入进料口2，待提纯物料经进料管道进入第一管道410和第二管道430实现分流，进而进入第一管道410和第二管道430交叉点处设置的分液头420内，进入分液头420内的待提纯物料具备一定的周向初速度，能够降低待提纯物料的径向聚集趋势。分流头420内部侧壁设置的螺旋状分液槽421使待提纯物料呈旋流方式进入旋流布膜器8。
旋流布膜器8的漏斗本体810内壁上设置的螺旋状导流槽811使待提纯物料呈旋流方式进入管状部分820，管状部分820内设置的通气管10上端的锥形或伞状导流台11对待提纯物料起到“分流”作用，使待提纯物料均匀分布于管状部分820的内壁，通气管10上部设置的通气孔101使结晶管6内空气通过排气通道9排空，并使待提纯物料形成旋流，保证了良好的成膜效果，使待提纯物料均匀分布于管状部分820的内壁，并呈膜状沿管状部分820的内壁流动至结晶管6内壁。
待提纯物料以旋流方式进入结晶管6，并沿结晶管6内壁呈膜状流动。冷媒介质自筒体6上部设置的冷热媒进出口17经冷热媒导流板5分流后进入换热管7中，并沿换热管7内壁呈膜状流动。流动过程中，待提纯物料与冷媒介质传热、降温进而结晶。在此过程中，冷媒介质温度逐渐升高，与物料之间的温差逐渐减小。
物料沿上层结晶区的结晶管6逐渐流动至上、下层结晶区相互连通的两结晶管6的连接处，上、下层结晶区相互连通的两结晶管6连接处设置的锥形或伞状物料再分布台1301对待提纯物料起到“分流”作用，使待提纯物料均匀分布于导流片1303上，并沿导流片1303流动至下层结晶区的结晶管6内壁。通过导气管1302上部开设的导气孔13021将下层结晶区的结晶管6内空气排空，并使待提纯物料形成旋流。
将新的冷媒介质通过筒体1中部设置的冷热媒进出口17通入换热管7中，待提纯物料与该冷媒介质换热、降温进而结晶。
如图15-16所示，在本发明的另一可选实施例中，结晶管6内壁均匀设置有若干凸台61，凸台61的轴向高度为0.5-3mm，优选为0.5-1mm，凸台61的，如三角形或弧形。具体而言，纵向截面上部呈上窄下宽的形状的凸台61对待提纯物料起到“分流”作用，使待提纯物料换热、降温更均匀，改善待提纯物料的结晶均匀性。左右相邻凸台61之间形成上宽下窄类似“V”型的卡口，该卡口能够有效支撑并卡住结晶，防止结晶脱落，由于结晶的厚度一般为1-2mm，若凸台61的高度过高，易使待提纯物料呈股状而非膜状流动，不利于改善结晶均匀性。若凸台61的高度过低，对物料的分流作用不明显。
如图17所示，在本发明的另一可选实施例中，结晶管6内壁还设置有防滑纹62，防滑纹62沿结晶管6内壁向外突或向内凹陷0.1-1mm，优选为0.1-0.5mm。防滑纹62能够提高结晶与结晶管6内壁壁面之间的抓臂力，防止结晶自结晶管6管壁脱落，防滑纹62可以采用星形、波浪形、十字形等，只要能够使结晶产生凹凸状结构即可。
如图18所示，在本发明的另一可选实施例中，分液头420的下端伸入旋流布膜头8的漏斗本体810内，且分液头420的底端半径小于旋流布膜头8的漏斗本体810的底端内径。具体而言，当物料自分液头420进入旋流布膜头8时，因分液头420的下端深入旋流 布膜头8的漏斗本体810内，且分液头420的底端半径小于旋流布膜头8的漏斗本体810的底端半径，能够防止待提纯物料飞溅出漏斗本体810，提高收率。
如图19所示，在本发明的另一可选实施例中，旋流布膜器8的管状部分820底部的内径由上至下逐渐增大，即管状部分820底部内壁的纵向截面呈八字形。将管状部分820底部内壁的纵向截面设置成八字形，待提纯物料形成旋流后，能够稳定地沿管状部分820的内壁过渡至结晶管6的内壁上，减小物料自管状部分820进入结晶管6时撞击在结晶管6内壁上的撞击力，从而更好地在结晶管6内壁上保持旋流效果。
如图20所示，在本发明的另一可选实施例中，冷热媒导流板5设置于换热管7上端与其相邻上方的冷热媒进出口17之间。冷热媒导流板5设置有若干导流孔51，所有导流孔51分别与换热管7一一对应且相互连通，导流孔51的孔径略大于换热管7的外径。
本发明中，可根据实际生产需要，对结晶区的层数进行调整，如可根据实际生产情况，将结晶区的层数调整为3层，相应的，3层结晶区上部均设置有冷热媒进出口17，3层相互连通的结晶管的总长度等于结晶区为2层时相互连通的结晶管的总长度。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

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  1. 一种降膜熔融结晶器，包括筒体，所述筒体的顶部和底部分别设置有进料口和出料口，其特征在于，所述筒体内部从上至下依次设有若干层结晶区，每层结晶区均设有若干竖向设置的结晶管，所述结晶管外均套设有换热管，相邻结晶区的结晶管、换热管一一对应并相互连通，位于最上层的结晶管与所述进料口连通，位于最下层的结晶管与所述出料口连通，所述筒体上设有与每层结晶区的换热管顶端相连通的冷热媒进出口，所述筒体的下部设有与位于最下层的换热管底端相连通的冷热媒进出口。
  2. 根据权利要求1所述的降膜熔融结晶器，其特征在于，所述筒体内还设置有若干旋流布膜器，所述旋流布膜器位于所述进料口与最上层结晶区的结晶管之间，并与最上层结晶区的结晶管一一对应且相互连通，所述旋流布膜器呈漏斗状，包括漏斗本体和管状部分，所述漏斗本体内壁开设有螺旋状导流槽。
  3. 根据权利要求2所述的降膜熔融结晶器，其特征在于，所述旋流布膜器内设置有通气管，所述通气管上部设置有通气孔，所述通气管顶端设置有导流台，所述通气管外径小于所述导流台的底端长度，所述通气管内径小于所述管状部分内径。
  4. 根据权利要求3所述的降膜熔融结晶器，其特征在于，所述导流台呈锥形或伞状。
  5. 根据权利要求1所述的降膜熔融结晶器，其特征在于，所述筒体内还设置有若干再布膜头，所述再布膜头安装于相邻结晶区相互连通的两结晶管的连接处，所述再布膜头包括物料再分布台和导气管，所述物料再分布台位于所述导气管的顶端，其呈锥形或伞状，所述导气管的外径小于所述导流台底端长度，且所述导气管内径小于所述结晶管内径。
  6. 根据权利要求5所述的降膜熔融结晶器，其特征在于，所述再布膜头还包括导流片，所述导气管通过所述导流片固定于结晶管的内壁，所述导流片呈三棱柱状。
  7. 根据权利要求1所述的降膜熔融结晶器，其特征在于，所述筒体内还设置有物料分布器，所述物料分布器与所述进料口连通，所述物料分布器用于将待提纯物料进行分流。
  8. 根据权利要求7所述的降膜熔融结晶器，其特征在于，所述物料分布器包括若干分液头，所述分液头呈倒置漏斗状，其内壁开设有螺旋状分液槽，所述分液头与最上层结晶区的结晶管一一对应。
  9. 根据权利要求1所述的降膜熔融结晶器，其特征在于，所述每层结晶区均设置有冷热媒导流板，所述冷热媒导流板位于所述冷热媒进出口的下方，所述冷热媒导流板上设置有若干导流孔，所述导流孔与所述换热管一一对应并相互连通。
  10. 根据权利要求1所述的降膜熔融结晶器，其特征在于，所述筒体内还设置有过滤网，所述过滤网设置于所述出料口与最下层结晶区的结晶管之间。
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