CN209917311U

CN209917311U - Continuous multi-stage constant temperature difference cooling crystallizer

Info

Publication number: CN209917311U
Application number: CN201920547100.4U
Authority: CN
Inventors: 王建; 徐翔; 范泓焘
Original assignee: Jiangsu Hecheng Pharmaceutical Equipment Manufacturing Co Ltd
Current assignee: Jiangsu Hecheng Pharmaceutical Equipment Manufacturing Co Ltd
Priority date: 2019-04-22
Filing date: 2019-04-22
Publication date: 2020-01-10
Anticipated expiration: 2029-04-22

Abstract

The utility model belongs to the technical field of chemical equipment, in particular to a continuous multistage constant temperature difference cooling crystallizer, which comprises a crystallizer body, wherein the top and the bottom of the crystallizer body are respectively provided with a feed inlet and a discharge outlet, the crystallizer body is internally divided into a plurality of cavities through cavity dividing clapboards, and openable fluid channels are arranged on the cavity dividing clapboards; and a heat exchange device and a stirrer are independently arranged in each cavity, independent temperature control is carried out, a bottom stirrer is arranged at the lower part of the bottom cavity, and the stirrer and the bottom stirrer in each cavity are connected with a driving device through a stirring shaft. The utility model discloses can carry out serialization production, reduce artifical intensity of labour, reduce the energy consumption that the material was transported and pollute, increase the efficiency of equipment application to can guarantee the reproducibility of crystallization product quality reliable and stable and technology, reduce the difference between same material different batches.

Description

Continuous multi-stage constant temperature difference cooling crystallizer

Technical Field

The utility model relates to a multistage constant temperature difference cooling crystallizer of continuous type belongs to chemical industry equipment technical field.

Background

Crystallization is a basic chemical process, and the crystallization technology is a conventional technology for separating solid products from liquid, and is often applied to the production of products in various chemical fields, such as chemical reagents, medicines, foods and the like, which all involve crystallization. In industrial production, the crystallization commonly used is generally divided into evaporative crystallization and cooling crystallization. The cooling crystallization can be used not only to prepare crystalline material but also as an integral part of many processes, and on the other hand the cooling crystallization can be used to purify and purify material to obtain high purity products or intermediates. The crystallizer is a chemical equipment unit for cooling crystallization operation, and the optimization of the equipment structure and the adaptability to materials are particularly important.

In the cooling crystallization process, the material concentration, the material temperature, the heat transfer temperature difference, the heat transfer rate, the stirring form and the stirring speed have great influence on the quality of the crystallized material. The existing crystallization process equipment is an operation mode of multi-batch, intermittent, slow heat exchange rate and material feeding outside a kettle, and the defects of too fine crystal granularity, poor crystal form and the like of crystals and the possibility of causing the crystal purity to be incapable of meeting the requirements so as to seriously affect the product quality commonly exist in the defects that materials in a tank have no certain temperature gradient, the heat transfer temperature difference is difficult to control, the stirring is not uniform and the like; and the intermittent crystallization mode has high energy consumption, long operation period and high manual operation intensity, so that operation errors exist among different batches and the product quality is seriously influenced.

SUMMERY OF THE UTILITY MODEL

According to the not enough among the above prior art, the utility model discloses the technical problem who solves is: the continuous multi-stage constant temperature difference cooling crystallizer is strictly cooled step by step according to the process route, has obvious temperature gradient, can accurately control heat transfer temperature difference, is uniformly stirred, meets the high-quality requirement of crystallized materials, and has stable performance and compact structure.

The utility model discloses a multistage constant temperature difference cooling crystallizer of continuous type, including the crystallizer body, crystallizer body top and bottom are equipped with feed inlet and discharge gate respectively, divide into a plurality of cavitys through dividing the chamber baffle in the crystallizer body, divide the chamber baffle to be equipped with open closed fluid passage; and a heat exchange device and a stirrer are independently arranged in each cavity, independent temperature control is carried out, a bottom stirrer is arranged at the lower part of the bottom cavity, and the stirrer and the bottom stirrer in each cavity are connected with a driving device through a stirring shaft.

The material in the crystallizer is from last to walking away the material in the cauldron body all the time down, avoids receiving external environment temperature's influence, and the cooling step by step is carried out according to the process route regulation strictly, and the crystal particle distribution range of production is stable, satisfies the high-quality requirement of crystallization material. The crystal was stirred and mixed by a stirrer and a bottom stirrer. The utility model adopts the multi-stage independent crystallization cavities connected up and down, so that each crystallization cavity is controlled at the lower crystallization supersaturation degree of the process requirement, the metastable zone of the solution can be controlled well, and the reliable operation of the crystallization materials in the upper and lower units can be ensured; so that the crystallized particles can continuously grow and ensure the quality, thereby meeting the requirements of the process on the product quality. And the quality is not influenced by fine crystal explosion caused by excessive temperature difference between the crystallization cavities.

The cavity-dividing partition plate is of an inclined conical structure with a large upper part and a small lower part, and preferably, the taper angle alpha is 160 degrees. The fluid channel at the bottom of the cavity partition plate is eccentrically arranged, so that materials can smoothly flow into the lower cavity from the upper cavity, and the flowing of the materials is controlled by temperature without series flow.

A sealing device is arranged between the cavity separating plate and the stirring shaft, so that the material can be prevented from leaking from the gap between the shafts to influence the crystallization effect.

The heat exchange device is in a cylindrical ring structure, the upper part and the lower part of the middle heat exchange tube are respectively connected with a square upper tube box and a square lower tube box, the upper tube box is provided with a refrigerant outlet, and the lower tube box is provided with a refrigerant inlet; the heat exchange tubes are arranged in an inclined radial shape, preferably, the inclination angle lambda is 45 degrees, and the arrangement rotating direction is the same as the stirring direction. When making the agitator stir the material through such setting, arranging of heat exchange tube is unanimous with the material flow direction, and the heat exchange tube region of flowing through that the material can be better reaches better, more abundant heat transfer effect, improves heat utilization rate.

The stirrer is an inclined blade type stirrer and is provided with three stirring blades, the spiral curve angle gamma of the outer edge of each stirring blade is 83 degrees, the spiral curve angle beta of the inner edge of each stirring blade is 58 degrees, and the rotating direction of the stirrer is the same as the arrangement rotating direction of the middle heat exchange tube of the heat exchange device. When the stirrer stirs materials, the precipitated crystals can not be sheared, and the uniformity of crystal particles is ensured.

The bottom stirrer is provided with two bottom stirring paddles, the stirring paddles are of a porous plate structure, and preferably, the installation inclination angle theta of the bottom stirrer is 45 degrees. Make the stirring rake can not produce excessive striking and destroy the crystal granule to the crystal like this to can the homogeneous mixing lower part magma, make the supersaturation of discharge system's magma material get rid of, guarantee to arrange the material and stabilize in succession, and the magma solution solid content of discharge is high, reduces the discharge amount of mother liquor, easily solid-liquid separation's operation.

And a temperature measuring device is arranged in each cavity, so that the temperature in the crystallization process is monitored.

The fluid channel is controlled to be opened and closed by a clapboard communicating vessel which is arranged in the cavity in a sliding way; the clapboard communicating vessel comprises an opening and closing valve plate and an opening and closing shaft connected with the opening and closing valve plate.

The crystallizer body can be divided into any number of cavities through cavity dividing clapboards. The number of the cavities can be set according to the requirements of different materials and different processes so as to achieve more precise control and carry out continuous industrial production.

Compared with the prior art, the utility model beneficial effect who has is:

adopt the utility model discloses carry out serialization production, reduced artifical intensity of labour, reduce the energy consumption that the material was transported and pollute, increase the efficiency of equipment application to can guarantee the reproducibility of crystallization product quality reliable and stable and technology, reduce the difference between same material different batches. In operation, the input and output of material is in equal amounts throughout the system. The precise temperature and the stirring speed of the device can be controlled by combining with a PLC (programmable logic controller), and the device can continuously operate, thereby improving the operation efficiency and the quality stability.

Drawings

Fig. 1 is a schematic view of the overall structure of the present invention;

FIG. 2 is a schematic view of the construction of the agitator;

FIG. 3 is a schematic view of the spiral curve angle γ of the outer edge and the spiral curve angle β of the inner edge of the stirring vane;

FIG. 4 is a schematic view of the agitator rotating in the direction of rotation;

FIG. 5 is a schematic structural view of a chambered partition and a partition communicator;

FIG. 6 is a top partial cross-sectional view of a heat exchange device;

FIG. 7 is a partial enlarged view of portion A of FIG. 6;

FIG. 8 is a front cross-sectional view of a heat exchange device;

FIG. 9 is a perspective sectional view of the heat exchanger;

FIG. 10 is a front view of the bottom agitator;

FIG. 11 is a left side view of the bottom agitator;

FIG. 12 is a top view of the bottom agitator.

In the figure: 1. a discharge port; 2. a lower end enclosure; 3. a lower cylinder body; 4. a lower refrigerant outlet; 5. a lower flange; 6. a first flange; 7. a middle cylinder body; 8. an intercooling medium outlet; 9. a middle second flange; 10. a flange is arranged; 11. an upper cylinder body; 12. an upper two flanges; 13. a seal head flange; 14. an upper end enclosure; 15. an upper refrigerant outlet; 16. a drive device; 17. a feed inlet; 18. a stirring shaft; 19. a stirrer; 20. a heat exchange device; 21. a temperature measuring device; 22. an upper refrigerant inlet; 23. a cavity separation plate; 24. a partition communicating vessel; 25. an intercooling medium inlet; 26. a lower refrigerant inlet; 27. a bottom agitator;

191. a coupling shaft sleeve; 192. a stirring blade;

201. an upper header; 202. a heat exchange pipe; 203. a lower header;

231. a sealing device; 232. a fluid channel;

241. an opening and closing shaft; 242. opening and closing the valve plate;

271. the bottom is connected with a shaft sleeve; 272. a bottom paddle;

a. an outer edge spiral curve; b. an inner edge spiral curve; c. a suction side; d. and (5) extruding the noodles.

Detailed Description

The invention will be further described with reference to the following examples:

as shown in fig. 1-12, multistage constant temperature difference cooling crystallizer of continuous type, including the crystallizer body, the crystallizer body comprises low head 2, lower barrel 3, well barrel 7, upper barrel 11, upper cover 14, and low head 2 passes through welded fastening with lower barrel 3 and is connected, and lower barrel 3 passes through lower flange 5 with well barrel 7, a flange 6 is connected, and well barrel 7 is connected through two flanges 9 in with upper barrel 11, a last flange 10, and upper barrel 11 passes through two flanges 12, head flange 13 with upper cover 14 and is connected.

The top of the upper end enclosure 14 and the bottom of the lower end enclosure 2 are respectively provided with a feed inlet 17 and a discharge outlet 1, the crystallizer body is divided into three cavities by a cavity dividing clapboard 23, and the cavity dividing clapboard 23 is provided with an openable fluid channel 232; the heat exchange device 20 and the stirrer 19 are independently arranged in each cavity, the temperature is controlled independently, the bottom stirrer 27 is arranged at the lower part of the bottom cavity, and the stirrer 19 and the bottom stirrer 27 in each cavity are connected with the driving device 16 through the stirring shaft 18.

The cavity separation plate 23 is of an inclined conical structure with a large upper part and a small lower part, and the cone angle alpha is 160 degrees; a sealing device 231 is arranged between the cavity partition plate 23 and the stirring shaft 18.

The heat exchange device 20 is a cylindrical ring structure, the upper part and the lower part of the middle heat exchange tube 202 are respectively connected with a square upper tube box 201 and a square lower tube box 203, the upper tube box 201 is provided with a refrigerant outlet, and the lower tube box 203 is provided with a refrigerant inlet (the heat exchange device 20 of the upper cavity is provided with an upper refrigerant outlet 15 and an upper refrigerant inlet 22; the heat exchange device 20 of the middle cavity is provided with a middle refrigerant outlet 8 and a middle refrigerant inlet 25; and the heat exchange device 20 of the lower cavity is provided with a lower refrigerant outlet 4 and a lower refrigerant inlet 26); the heat exchange tubes 202 are arranged in an oblique radial shape, the inclination angle λ is 45 degrees, and the arrangement rotation direction is the same as the stirring direction.

The agitator 19 is a helical blade type agitator provided with three agitating blades 192, the agitating blades 192 are provided on the coupling boss 191, the outer edge spiral curve angle γ of the agitating blades 192 is 83 degrees, and the inner edge spiral curve angle β is 58 degrees. (in FIG. 3, a is an outer edge spiral curve, b is an inner edge spiral curve; in FIG. 4, c is a suction surface of the stirring vanes, and d is a discharge surface of the stirring vanes)

The bottom stirrer 27 is provided with two bottom stirring paddles 272, the bottom stirring paddles 272 are arranged on the bottom connecting shaft sleeve 271, and the stirring paddles 272 are of a porous plate structure, and the installation inclination angle theta of the stirring paddles 272 is 45 degrees.

A temperature measuring device 21 is arranged in each cavity for monitoring the temperature in the crystallization process.

The fluid channel 232 is controlled to be opened and closed by the clapboard communicating vessel 24, and the clapboard communicating vessel 24 is arranged in the cavity in a sliding way; the partition connector 24 includes an opening/closing blade 242 and an opening/closing shaft 241 connected to the opening/closing blade 242.

The utility model discloses a working process or theory of operation:

the material solution enters the upper cavity of the crystallizer through the feed inlet 17, and the upper cavity of the crystallizer is filled with the material under the action of the gravity of the material. Firstly, the driving device 16 is started, and the stirring shaft 18 drives the stirrer 19 to stir; the upper refrigerant inlet 22 is opened, the stirrer 19 pushes the materials to be cooled through the heat exchange device 20, heat exchange is sufficient and uniform, the utilization rate of the refrigerant is high, and the refrigerant is continuously subjected to heat exchange with the materials and then is discharged from the upper refrigerant outlet 15 for circulation; the temperature measuring device 21 is connected with the controller and the actuator, the temperature measuring device 21 detects the temperature of the material and continuously cools the material, when the temperature measuring device 21 detects that the material meets the process temperature requirement, the partition communicating vessel 24 opens and opens the fluid channel 232, and the material enters the next cavity through the fluid channel 232; further opening an inter-cooling medium inlet 25, and discharging and circulating the refrigerant from an inter-cooling medium outlet 8 after the refrigerant continuously exchanges heat with the material; the material is continuously cooled and begins to crystallize, the temperature is detected and controlled by the temperature measuring device 21, and the material is continuously cooled and enters the bottom cavity through the fluid channel 232 of the cavity dividing partition plate 23; a lower refrigerant inlet 26 is further opened, the refrigerant continuously exchanges heat with the material, when the temperature measuring device 21 detects that the material meets the process temperature requirement, the material is discharged from an upper refrigerant outlet 15 for circulation, is continuously cooled and largely crystallized, and is detected by the corresponding temperature measuring device 21 for temperature control; the inclined plane orifice plate stirring paddle at the lower part uniformly stirs the crystallized materials, the uniformly crystallized mixture is discharged from the discharge port 1 at the bottom of the lower end enclosure 2, and the crystallized and purified products are collected to enter the next procedure. The continuous crystallization operation is carried out by repeatedly feeding and continuously discharging crystallized materials, the operation efficiency is high, and the product quality is stable.

Taking a vitamin C solution with a daily treatment capacity of 140 tons as an example:

adopt the utility model discloses, through the concentrated material in second grade: the temperature is 50 ℃, and the crystal content is about 30 percent; the liquid enters a continuous multi-stage constant temperature difference cooling crystallizer from an external pipeline through a feed inlet 17;

the coolant of the solution in the upper cavity is circulating cooling water at 25 ℃, and the primary cooling temperature is 30 ℃; the coolant of the solution in the middle cavity is brine ice at the temperature of-5 ℃, and the secondary cooling temperature is 10 ℃; the refrigerant of the solution in the lower cavity is deep cold water with the temperature of-15 ℃, and the temperature of the third-stage cooling is-3 ℃; the cooling temperature is reduced step by step, and the influence on the product quality caused by temperature fluctuation caused by the interference of the external feed by the ambient temperature is avoided.

After the materials are stirred by a bevel orifice plate stirring paddle, the temperature of the materials discharged from the lower part is minus 3 ℃, and the crystal content is about 70 percent.

In the embodiment, the operation power of the crystallizer is 22Kw, the crystallization time of the vitamin C solution meeting the process control requirement is 2.5 hours, the operation material is 15 tons, and the continuous operation daily throughput is 144 tons; daily consumed power 528 Kw; the operation can adopt automatic control, 1 person operates the operation, low in labor intensity. The granularity (30-40 meshes) of the treated material product is not less than 65 percent, the uniformity is not less than 60 percent, and the heavy metal content is not more than 3 mg/L.

Compared with the prior art, the method has the following steps of continuously operating the materials with the same yield: 12 intermittent crystallizers are needed, the operation power of each crystallizer is 5Kw, and the operation crystallization time of each batch of materials is 5 hours; daily consumed power 1440 Kw; the process operation adopts manual control, and the operation is operated by a plurality of people, so that the labor intensity is high. The granularity (30-40 meshes) of the treated product is detected to be more than or equal to 50 percent, the uniformity is more than or equal to 50 percent, and the heavy metal content is less than or equal to 10 mg/L.

The material in the crystallizer is from last to walking away the material in the cauldron body all the time down, avoids receiving external environment temperature's influence, strictly carries out the cooling step by step according to the process route regulation, guarantees the reproducibility of technology to cooperate heat transfer device 20, agitator 19, end agitator 27 of special construction, make the crystal particle distribution range of production stable, satisfy the high-quality requirement of crystallization material.

Claims

1. The utility model provides a multistage constant temperature difference cooling crystallizer of continuous type, includes the crystallizer body, and crystallizer body top and bottom are equipped with feed inlet (17) and discharge gate (1) respectively, its characterized in that: the crystallizer body is divided into a plurality of cavities by cavity dividing clapboards (23), and openable fluid channels (232) are arranged on the cavity dividing clapboards (23); a heat exchange device (20) and a stirrer (19) are independently arranged in each cavity, independent temperature control is carried out, a bottom stirrer (27) is arranged at the lower part of the bottom cavity, and the stirrer (19) and the bottom stirrer (27) of each cavity are connected with a driving device (16) through a stirring shaft (18).

2. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the cavity-dividing partition plate (23) is of an inclined conical structure with a large upper part and a small lower part, and the cone angle alpha of the cavity-dividing partition plate is 160 degrees.

3. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: a sealing device (231) is arranged between the cavity partition plate (23) and the stirring shaft (18).

4. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the heat exchange device (20) is of a cylindrical ring structure, the upper part and the lower part of the middle heat exchange tube (202) are respectively connected with a square upper tube box (201) and a square lower tube box (203), the upper tube box (201) is provided with a refrigerant outlet, and the lower tube box (203) is provided with a refrigerant inlet; the heat exchange tubes (202) are arranged in an inclined radial shape, the inclination angle lambda is 45 degrees, and the arrangement rotating direction is the same as the stirring direction.

5. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the stirrer (19) is an inclined blade type stirrer and is provided with three stirring blades (192), the spiral curve angle gamma of the outer edge of each stirring blade (192) is 83 degrees, and the spiral curve angle beta of the inner edge of each stirring blade is 58 degrees.

6. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the bottom stirrer (27) is provided with two bottom stirring paddles (272), the stirring paddles (272) are of a porous plate structure, and the installation inclination angle theta of the stirring paddles is 45 degrees.

7. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: and a temperature measuring device (21) is arranged in each cavity.

8. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the fluid channel (232) is controlled to be opened and closed by a partition communicating vessel (24), and the partition communicating vessel (24) is arranged in the cavity in a sliding manner; the partition plate communicating vessel (24) includes an opening/closing valve plate (242) and an opening/closing shaft (241) connected to the opening/closing valve plate (242).

9. The continuous multi-stage constant temperature difference cooling crystallizer of claim 1, wherein: the crystallizer body can be divided into any number of cavities through cavity dividing clapboards (23).