A crystal separation scrubber

Abstract

The invention discloses a crystal separation washer, which belongs to the technical field of chemical equipment, and comprises a tank body and a stirring shaft arranged in the tank body. The interior of the tank body is a hollow cavity, which is divided into an upper clarification section, a middle mixing-separation-washing section, and a lower sedimentation section. A mixing-washing unit and a separation unit are arranged in the middle mixing-separation-washing section of the tank body. The mixing-washing unit comprises an agitator arranged on the stirring shaft and an inclined plate mixer arranged on the tank body. The inclined plate mixer is composed of an inclined plate group and an inclined plate fixing connecting rod. A liquid distributor is arranged at the bottom of the stirring shaft, and the liquid distributor is arranged at the bottom of the middle mixing-separation-washing section. The stirring shaft is a hollow shaft, and the top of the stirring shaft is connected to a washing liquid inlet. A crystal inlet is arranged at the upper middle section of the tank body, a light phase liquid outlet is arranged at the upper upper section of the tank body, and a heavy phase liquid outlet is arranged at the bottom of the tank body. The device has a simple structure and can realize continuous industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical equipment, and in particular relates to a crystal separation scrubber. Background Art

[0002] As an emerging industry, many equipment in the extract industry are based on existing equipment in the chemical or oil industry. In the process of crystal separation and washing, the current technology generally uses a crystal separation tank. After the crystals are naturally settled and separated in the tank, they are separated by a subsequent multi-stage tank group or plate and frame filtration, centrifuge separation. The products obtained by these methods are not pure enough or have impurities and cannot meet the requirements. They often need to be washed multiple times to meet the purity requirements, resulting in complex processes and low yields. When processing solvent-containing crystals, there are often multiple open operations in the transportation of materials, and a large amount of organic solvents leak or overflow, causing safety hazards to production and occupational health hazards to operators. It is necessary to develop a fully enclosed crystal separation and washing device to solve the problem.

[0003] In the patent with publication number CN215727198U, the light and heavy items are separated and then enter the secondary refining separation tank respectively, so as to achieve the purpose of multi-stage countercurrent continuous separation and purification. However, the multi-stage purification process is complicated, and multiple sets of mixing and separation tanks need to be configured, and corresponding light and heavy item distribution mechanisms, buffer devices, and liquid pouring pumps need to be configured. The operation process is complicated, the workload of manual adjustment is large, and the effect is not ideal, and the product quality is unstable. In the patent with publication number CN215137051U, the raw material liquid enters from the upper part of the device, and the heat exchange efficiency between the plate tube and the raw material liquid is improved by setting a corrugated plate tube, and the crystals on the surface of the plate tube are removed in time by a scraper to ensure the heat transfer effect of the plate tube, thereby improving the effect of crystallization separation. The crystallization and separation of the device can only complete one separation, without purification function, and the purity of the discharge is low. In the patent with publication number CN214319182U, the raw material liquid enters from the upper part of the device and evaporates on the upper part of the equipment. The concentrated liquid enters the lower part for crystallization, the heavy phase crystals are discharged from the lower part, and the light phase is collected from the middle section and refluxed for further crystallization. The crystallization and separation of the device can only complete one separation, without purification function, and the purity of the discharged material is low.

[0004] In short, crystal separation and purification mostly adopts multi-stage tank group separation or plate and frame filtration, centrifuge separation, and there are many integrated crystallization and separation equipment, which can produce purified products. However, due to the lack of washing process, the purity is generally low and the impurities are high. The multi-stage tank group graded purification system can produce high-purity products, but the process is complex, there are many process control points, the workload of personnel adjustment is large, and the product purity is unstable. Therefore, there is an urgent need for a device that can perform multiple separation and washing of crystals to simplify the process and ensure safe production. Summary of the invention

[0005] In order to overcome the shortcomings of the prior art, the present invention provides a crystal separation and washing device. The device has a simple structure and can separate and wash crystals multiple times to meet purity requirements. The high-purity crystals produced by the device are still fluid, which is convenient for transportation and subsequent drying.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A crystal separation washer comprises a tank body and a stirring shaft arranged in the tank body, wherein the tank body is divided into an upper clarification section, a middle mixing-separation-washing section, and a lower sedimentation section, wherein a mixing-washing unit and a separation unit are arranged in the middle mixing-separation-washing section of the tank body, wherein the mixing-washing unit comprises an agitator arranged on the stirring shaft and an inclined plate mixer arranged on the tank body, wherein the inclined plate mixer is composed of an inclined plate group and an inclined plate fixing connecting rod, wherein a liquid distributor is arranged at the bottom end of the stirring shaft, wherein the liquid distributor is arranged at the bottom of the middle mixing-separation-washing section, wherein the stirring shaft is a hollow shaft, wherein the top of the stirring shaft is connected to a washing liquid inlet, wherein a crystal inlet is arranged at the upper part of the middle section of the tank body, a light phase liquid outlet is arranged at the upper part of the upper section of the tank body, and a heavy phase liquid outlet is arranged at the bottom of the tank body.

[0008] A further improvement of the technical solution of the present invention is that a stirring power mechanism is arranged on the top of the tank body, and the stirring power mechanism controls the operation of the stirring shaft.

[0009] A further improvement of the technical solution of the present invention is that the crystal liquid inlet is rotated along the tank body to feed the liquid, and the inner pipe forms an angle of 5-10° with the tangent.

[0010] A further improvement of the technical solution of the present invention is that a separation unit is provided below the mixing and washing unit, and n groups of mixing and washing units and separation units can be provided, where n≥3, and each mixing and washing unit includes a group of agitators and an inclined plate mixer.

[0011] A further improvement of the technical solution of the present invention is that the inclined plate fixing connecting rod is a plurality of straight rods arranged transversely on the tank body, the inclined plate fixing connecting rod is inserted into a plurality of inclined plates, and the inclined plate fixing connecting rod and the inclined plate group are arranged in longitude and latitude.

[0012] A further improvement of the technical solution of the present invention is that the inclined plates constituting the inclined plate group have an inclination angle of 60-85°, and the inclinations of the inclined plate groups of adjacent mixed washing units are arranged in opposite directions.

[0013] A further improvement of the technical solution of the present invention is that the stirrer is provided with 2-4 stirring paddles.

[0014] A further improvement of the technical solution of the present invention is that the liquid distributor is composed of a plurality of interconnected liquid distribution pipes, the liquid distribution pipes are triangular pipes with a top angle of 45-60°, and a liquid outlet hole is opened below the liquid distribution pipes.

[0015] A further improvement of the technical solution of the present invention is that the washing liquid is transported from the washing liquid inlet to the liquid distributor via the stirring shaft and then transported into the tank body.

[0016] The further improvement of the technical solution of the present invention is that the distance between the liquid distributor and the lower sedimentation section is 100mm-200mm, and the distance between the agitator and the inclined plate mixer is 50mm-100mm.

[0017] Due to the adoption of the above technical solution, the beneficial effects achieved by the present invention are:

[0018] The crystal separation and washing are integrated, the equipment is simple and the investment is low; for the washing and separation of the crystals, the process is simple, the process is short, the loss is small and the cost is low; the total crystal content recovery rate is high; and it is easy to realize continuous industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 is a schematic diagram of a crystal separation scrubber of the present invention;

[0020] Figure 2 is a schematic diagram of an agitator of the present invention;

[0021] Figure 3 is a schematic diagram of the crystal feed port;

[0022] Figure 4 is a schematic diagram of a hybrid washing unit;

[0023] Figure 5 It is a schematic diagram of the liquid distributor;

[0024] Wherein: 1. tank body, 2. upper clarification section, 3. middle mixing-separation-washing section, 4. lower sedimentation section, 5. crystal feed inlet, 6. washing liquid feed inlet, 7. heavy phase liquid outlet, 8. light phase liquid outlet, 9. agitator, 10. agitator shaft, 11. mixing and washing unit, 12. inclined plate mixer, 13. inclined plate group, 14. inclined plate fixing connecting rod, 15. separation unit, 16. liquid distributor, 17. liquid distribution pipe, 8. liquid outlet, 19. stirring power mechanism. DETAILED DESCRIPTION

[0025] The technical solution of the present invention will be described in detail below in conjunction with specific implementation methods.

[0026] like Figure 1-5As shown, a crystal separation washer comprises a tank body 1 and a stirring shaft 10 arranged in the tank body 1. The interior of the tank body 1 is a whole hollow cavity. According to the different steps of the crystal in the tank, it is divided into three parts, an upper clarification section 2, a middle mixing-separation-washing section 3, and a lower sedimentation section 4. A mixing washing unit 11 and a separation unit 15 are arranged in the middle mixing-separation-washing section 3 of the tank body. The mixing washing unit 11 comprises an agitator 9 arranged on the stirring shaft 10 and an inclined plate mixer 12 arranged on the tank body. The inclined plate mixer 12 is composed of an inclined plate group 13 and an inclined plate fixing connecting rod 14. A liquid distributor 16 is arranged at the bottom of the stirring shaft 10. The liquid distributor 16 is arranged at the bottom of the middle mixing-separation-washing section. The stirring shaft 10 is a hollow shaft. A stirring power mechanism 19 is arranged on the top of the tank body 1. The stirring power mechanism 19 controls the operation of the stirring shaft 10.

[0027] The top of the stirring shaft 10 is connected to the washing liquid inlet 6, and a crystal inlet 5 is provided at the upper part of the middle section of the tank body. The crystal inlet 5 rotates along the tank body 1 to inlet liquid, and the inner pipe forms an angle of 5-10° with the tangent. A light phase outlet 8 is provided at the upper part of the upper section of the tank body, and a heavy phase outlet 7 is provided at the bottom of the tank body.

[0028] Below the mixing and washing unit 11 is a separation unit 15. The mixing and washing unit 11 and the separation unit 15 can be arranged in n groups, n≥3, and each mixing and washing unit 11 includes a group of agitators 9 and an inclined plate mixer 12. The agitator 9 is provided with 2-4 stirring paddles.

[0029] The inclined plate fixing connecting rods 14 are a plurality of straight rods arranged transversely on the tank body 1, and the inclined plate fixing connecting rods 14 are inserted in a plurality of inclined plates, and the inclined plate fixing connecting rods 14 and the inclined plate group 13 are arranged in the longitude and latitude. The inclined plates 13 constituting the inclined plate group 13 have an inclination angle of 60-85°, and the inclinations of the inclined plate groups 13 of adjacent mixing washing units 11 are arranged in opposite directions.

[0030] The liquid distributor 16 is composed of a plurality of interconnected liquid distribution pipes 17, which are triangular pipes with a vertex angle of 45-60°. A liquid outlet 18 is provided below the liquid distribution pipe 17. The plurality of liquid distribution pipes 17 are interconnected and laid flat on the bottom of the mixing-separating-washing section in the middle of the tank body 1. The liquid distribution pipes 17 are connected to the stirring shaft 10. The washing liquid is transported from the washing liquid inlet 6 to the liquid distributor 16 through the stirring shaft 10 and then transported to the tank body 1.

[0031] Preferred embodiment: the distance between the liquid distributor 16 and the lower sedimentation section is 100mm-200mm, and the distance between the agitator 9 and the inclined plate mixer 12 is 50mm-100mm.

[0032] The method of using the crystal separation scrubber for washing and separation is as follows:

[0033] S1, the washing solvent enters from the washing liquid feed port 6, is transmitted to the liquid distributor 16 through the stirring shaft 10, and then enters the interior 1 of the tank body to fill the tank body;

[0034] S2, start the power mechanism 19, the stirrer 9 starts to rotate, and the crystals to be extracted are added into the scrubber through the crystal feed port 5, and the liquid is continuously added according to the ratio of the weight of the crystals to be extracted kg: the volume of the washing liquid L=1:(3-6);

[0035] S3, the crystals to be extracted continue to fall to the sedimentation section 4 after passing through multiple groups of mixing washing units and separation units. After sufficient sedimentation, the heavy phase comes out from the heavy phase outlet 7, and the washing liquid flows out from the light phase outlet;

[0036] S4, desolventizing the heavy phase to obtain the final product.

[0037] The actual crystal separation example using the crystal separation scrubber of the present application is as follows:

[0038] Example 1

[0039] (1) The crystal separation scrubber has five groups of mixing washing units 11 and separation units 15. 400L of 80% ethanol enters from the washing liquid feed port 6, is transmitted to the liquid distributor 16 through the inside of the stirring shaft 10, and enters the inside of the tank body 1. After the tank body 1 is filled, the power mechanism 19 is turned on to drive the stirring shaft 10 and the stirrer 9 to start rotating. 100kg of piperine crystals with a content of 90% are introduced into the device through the crystal feed port 5, and the liquid is continuously introduced according to the ratio of piperine weight: washing liquid volume = 1:4. The piperine crystals move from top to bottom, contact with the 80% ethanol washing liquid moving from bottom to top in the mixing washing unit 11, and continue to fall after passing through the separation unit 15. After a total of 5 levels of mixing and separation, they finally fall to the sedimentation section 4. After sufficient sedimentation in the sedimentation section 4, the washing is completed through the heavy phase liquid outlet 7, and the washing liquid flows out from the light phase liquid outlet 8.

[0040] (2) After washing, the piperine was subjected to a subsequent desolventizing step to obtain 80.35 kg of piperine crystals with a detected content of 98.11% and a calculated content yield of 87.54%.

[0041] Example 2

[0042] (1) 300L methanol enters from the washing liquid feed port 6, is transmitted to the liquid distributor 16 through the stirring shaft 10, and enters the tank 1. After filling the equipment cavity 1, the power mechanism 19 is turned on to drive the stirring shaft 10 and the stirrer 9 to start rotating. 100kg of stevioside crystals with a content of 86.16% are fed into the equipment through the crystal feed port 5, and the liquid is continuously fed in a ratio of stevioside weight: washing liquid volume = 1:3. The stevioside crystals move from top to bottom, contact with the methanol washing liquid moving from bottom to top in the mixing washing unit 11, and continue to fall after passing through the separation unit 15. After a total of 5 levels of mixing and separation, they finally fall to the sedimentation section 4. After sufficient sedimentation in the sedimentation section 4, the washing is completed through the heavy phase liquid outlet 7, and the washing liquid flows out from the light phase liquid outlet.

[0043] (2) After washing, the stevioside was subjected to a subsequent desolventizing step to obtain 79.25 kg of stevioside crystals with a detected content of 97.37% and a calculated content yield of 89.56%.

[0044] Example 3

[0045] (1) 500L 90% ethanol enters from the washing liquid feed port 6, is transmitted to the liquid distributor 16 through the stirring shaft 10 and enters the tank 1. After filling the equipment cavity 1, the power mechanism 19 is turned on to drive the stirring shaft 10 and the stirrer 9 to start rotating. 100kg of curcumin crystals with a content of 85.45% are fed into the equipment through the crystal feed port 5, and the liquid is continuously fed in a ratio of curcumin weight (kg): washing liquid volume (L) = 1:5. The curcumin crystals move from top to bottom, contact with the 90% ethanol washing liquid moving from bottom to top in the mixing washing unit 11, continue to fall after passing through the separation unit 15, and undergo a total of 5 levels of mixing and separation, and finally fall to the sedimentation section 4. After sufficient sedimentation in the sedimentation section 4, the washing is completed through the heavy phase liquid outlet 7, and the washing liquid flows out from the light phase liquid outlet.

[0046] (2) After washing, the curcumin was subjected to a subsequent desolventizing step to obtain 81.62 kg of curcumin crystals, with a detected content of 98.23% and a calculated content yield of 93.83%.

[0047] The device has a simple structure and can be equipped with multiple mixing, washing and separation units according to the crystal purity requirements to separate and wash the crystals multiple times to meet the purity requirements. The high-purity crystals produced by the device still have fluidity, which is convenient for transportation and subsequent drying. After multiple experimental verifications, the separation and washing effect of the device is excellent, the content and yield of the obtained products are higher than those of conventional technologies, and it is easy to realize continuous industrial production.

Claims

1. A crystal separation scrubber, characterized in that: The invention comprises a tank body (1) and a stirring shaft (10) arranged in the tank body (1). The interior of the tank body (1) is a hollow cavity, which is divided into an upper clarification section, a middle mixing-separation-washing section, and a lower sedimentation section. A mixing-washing unit and a separation unit (15) are arranged in the middle mixing-separation-washing section of the tank body. The mixing-washing unit comprises a stirrer (9) arranged on the stirring shaft (10) and an inclined plate mixer (12) arranged on the tank body. The inclined plate mixer (12) comprises an inclined plate group (13) and an inclined plate fixing connecting rod (14). A liquid distributor (16) is arranged at the bottom end of the stirring shaft (10). The liquid distributor (16) is arranged at the bottom of the middle mixing-separation-washing section. The stirring shaft (10) is a hollow shaft. The top of the mixing shaft (10) is connected to the washing liquid inlet (6), the liquid distributor (16) is composed of a plurality of interconnected liquid distribution pipes (17), a liquid outlet hole (18) is opened below the liquid distribution pipe (17), and the liquid distribution pipe (17) and the mixing shaft (10) are connected. A crystal liquid inlet (5) is arranged at the top of the mixing-separation-washing section in the middle of the tank body, a light phase liquid outlet (8) is arranged at the top of the clarification section in the upper part of the tank body, and a heavy phase liquid outlet (7) is arranged at the bottom of the tank body. A separation unit (15) is arranged below the mixing and washing unit (11). The mixing and washing unit (11) and the separation unit (15) can be arranged in n groups, where n≥3. Each mixing and washing unit (11) includes a group of agitators (9) and an inclined plate mixer (12).

2. A crystal separation scrubber according to claim 1, characterized in that: A stirring power mechanism (19) is arranged on the top of the tank body (1), and the stirring power mechanism (19) controls the operation of the stirring shaft (10).

3. A crystal separation scrubber according to claim 1, characterized in that: The crystal liquid inlet (5) is rotated along the tank body (1) to feed the liquid, and the inner pipe forms an angle of 5-10° with the tangent.

4. A crystal separation scrubber according to claim 1, characterized in that: The inclined plate fixing connecting rod (14) is a plurality of straight rods arranged transversely on the tank body (1); the inclined plate fixing connecting rod (14) is inserted into a plurality of inclined plates; and the inclined plate fixing connecting rod (14) and the inclined plate group (13) are arranged in longitude and latitude.

5. A crystal separation scrubber according to claim 4, characterized in that: The inclined plates constituting the inclined plate group (13) have an inclination angle of 60-85°, and the inclined plate groups (13) of adjacent mixing and washing units (11) are arranged in opposite directions.

6. A crystal separation scrubber according to any one of claims 1 to 5, characterized in that: The stirrer (9) is provided with 2-4 stirring paddles.

7. A crystal separation scrubber according to claim 1, characterized in that: The liquid distribution pipe (17) is a triangular pipe with a top angle of 45-60°.

8. A crystal separation scrubber according to claim 7, characterized in that: The washing liquid is transported from the washing liquid inlet (6) through the stirring shaft (10) to the liquid distributor (16) and then transported into the tank body (1).

9. A crystal separation scrubber according to claim 3, characterized in that: The distance between the liquid distributor (16) and the lower sedimentation section is 100 mm to 200 mm, and the distance between the stirrer (9) and the inclined plate mixer (12) is 50 mm to 100 mm.

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