CN115739809A - Crystal separation washer - Google Patents

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 inside of the tank body is a hollow cavity, which is divided into an upper clarification section and a middle mixing-separation-washing section. section, as well as the lower settling section, a mixed washing unit and a separation unit are set in the middle mixing-separating-washing section of the tank, and the mixing washing unit includes an agitator arranged on the stirring shaft and an inclined plate mixer arranged on the tank, The inclined plate mixer is composed of an inclined plate group and an inclined plate fixed 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-separating-washing section. The stirring shaft is a hollow shaft. The top is connected with the washing liquid inlet, the upper part of the tank body is provided with a crystal liquid inlet, the upper part of the tank body is provided with a light phase liquid outlet, and the bottom of the tank body is provided with a heavy phase liquid outlet. The device has a simple structure and can realize continuous industrial production.

Description

A crystal separation scrubber

technical field

The invention belongs to the technical field of chemical equipment, in particular to a crystal separation scrubber.

Background technique

As an emerging industry, the extract industry is a new industry. Many equipments are borrowed from the existing equipment in the chemical industry or oil industry. In the process of crystal separation and washing, the current technology generally uses crystal separation tanks. Stage tank group separation or plate and frame filtration, centrifuge separation, the products obtained by these methods are not pure enough or have impurities, which cannot meet the requirements, and often need to be washed many times to meet the purity requirements, resulting in complicated processes and low yields ; When handling solvent-containing crystals, there are often multiple exposure operations in the transfer 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 closed crystal separation and washing device to solve the problem.

In the patent with the publication number CN215727198U, the light and heavy items are separated and then respectively entered into the secondary refining separation tank to realize the purpose of continuous separation and purification in multi-stage countercurrent. However, the multi-stage purification process is complicated, and multiple sets of mixing and separation tanks need to be configured, as well as the corresponding light and heavy item distribution mechanism, buffer device, and pouring pump. The operation process is complicated, the manual adjustment workload is large, and the effect is not ideal unstable. In the patent with the 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 the corrugated plate tube, and the crystals on the surface of the plate tube are removed in time by the scraper to ensure that the plate tube The heat transfer effect of the tube can improve the effect of crystallization and separation. The crystallization and separation of the device can only complete one separation, without purification function, and the output purity is low. In the patent with publication number CN214319182U, the raw material liquid enters from the upper part of the device and evaporates at the upper part of the device. The concentrated liquid enters the lower part for crystallization, the heavy phase crystallization is discharged from the lower part, and the light phase is withdrawn from the middle section and refluxed to continue crystallization. The crystallization and separation of the device can only complete one separation, without purification function, and the output purity is low.

In short, crystal separation and purification mostly adopt the method of multi-stage tank group separation or plate-and-frame filtration and centrifuge separation. There are many integrated equipment for crystallization and separation, which can produce purified products. Since there is no washing process, the purity is generally low and the amount of impurities is low. Large; The multi-stage tank group fractional purification system can produce high-purity products, but the process is complicated, 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 separate and wash crystals multiple times, simplify the process, and produce safely.

Contents of the invention

In order to overcome the shortcomings of the prior art, the present invention provides a crystal separation washer. The device has a simple structure and can separate and wash the crystals many times to meet the purity requirements, and the high-purity crystals produced by the device still have fluidity. Easy transport and subsequent drying.

For realizing above-mentioned object, the technical scheme that the present invention takes is:

A crystal separation scrubber, comprising a tank body and a stirring shaft arranged in the tank body, the tank body is divided into an upper clarification section, a middle mixing-separation-washing section, and a lower settling section, and the mixing-separation section in the middle part of the tank body - The washing section is equipped with a mixing washing unit and a separation unit. The mixing washing unit includes an agitator arranged on the stirring shaft and an inclined plate mixer arranged on the tank. The inclined plate mixer is composed of an inclined plate group and an inclined plate fixing connecting rod , the bottom end of the stirring shaft is provided with a liquid distributor, the liquid distributor is arranged at the bottom of the mixing-separating-washing section in the middle, the stirring shaft is a hollow shaft, the top of the stirring shaft is connected with the washing liquid inlet, and the upper part of the tank body is set There is a crystal liquid inlet, a light phase liquid outlet is arranged on the upper part of the tank body, and a heavy phase liquid outlet is arranged at the bottom of the tank body.

The further improvement of the technical solution of the present invention lies in 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.

The further improvement of the technical solution of the present invention lies in that the liquid inlet of the crystal enters liquid along the direction of rotation of the tank, and the inner pipe forms an angle of 5-10° with the tangent.

The further improvement of the technical solution of the present invention lies in: the separation unit is located below the mixing washing unit, and n groups of mixing washing units and separation units can be arranged, n≥3, and each mixing washing unit includes a group of agitators and inclined plate mixers.

The further improvement of the technical solution of the present invention lies in that the fixed connecting rods of the inclined plates are several straight rods arranged transversely on the tank body, the fixed connecting rods of the inclined plates are interspersed in several inclined plates, and the fixed connecting rods of the inclined plates and the group of inclined plates are arranged in warp and weft.

The further improvement of the technical solution of the present invention lies in that: the inclined angle of the inclined plates forming the inclined plate group is 60-85°, and the inclined angles of the inclined plate groups of adjacent mixed washing units are arranged in opposite directions.

The further improvement of the technical solution of the present invention lies in that: the stirrer is provided with 2-4 stirring paddles.

The further improvement of the technical solution of the present invention lies in that the liquid distributor is composed of several connected liquid distribution pipes, the liquid distribution pipe is a triangular pipe with a vertex angle of 45-60°, and there is a liquid outlet hole under the liquid distribution pipe.

The further improvement of the technical solution of the present invention lies in that the washing liquid is transported from the washing liquid inlet through the stirring shaft to the liquid distributor and then to the tank.

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

Owing to adopting above-mentioned technical scheme, the beneficial effect that the present invention obtains is:

The crystal separation and washing integration is realized, the equipment is simple, and the investment is low; for the crystal washing and separation, the process is simple, the process is short, the loss is small, and the cost is low; the recovery rate of the total crystal content is high; it is easy to realize continuous industrial production.

Description of drawings

Fig. 1 is a schematic diagram of a crystal separation scrubber of the present invention;

Fig. 2 is a schematic diagram of an agitator of the present invention;

Fig. 3 is a schematic diagram of a crystal feed port;

Fig. 4 is a schematic diagram of a mixed washing unit;

Fig. 5 is a schematic diagram of a liquid distributor;

Among them: 1. Tank body, 2. Upper clarification section, 3. Middle mixing-separation-washing section, 4. Lower settling section, 5. Crystal feeding port, 6. Washing liquid feeding port, 7. Heavy phase outlet Port, 8. Light phase outlet, 9. Stirrer, 10. Stirring 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 ways

The technical solutions of the present invention will be described in detail below in conjunction with specific embodiments.

As shown in Figures 1-5, a crystal separation scrubber includes a tank body 1 and a stirring shaft 10 arranged in the tank body 1. The inside of the tank body 1 is a whole hollow cavity. Different steps, it is divided into 3 parts, the upper clarification section 2, the middle mixing-separation-washing section 3, and the lower settling section 4, and the mixing-separating-washing section 3 in the middle of the tank is equipped with a mixing washing unit 11 and a separation unit 15. The mixing and washing unit 11 includes the agitator 9 arranged on the stirring shaft 10 and the 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. Stirring A liquid distributor 16 is provided at the bottom of the shaft 10, and the liquid distributor 16 is arranged at the bottom of the mixing-separation-washing section in the middle, the stirring shaft 10 is a hollow shaft, and the stirring power mechanism 19 is set on the top of the tank body 1, and the stirring power mechanism 19 controls the stirring Axis 10 runs.

The top of the stirring shaft 10 is connected to the washing liquid inlet 6, and the upper part of the tank body is provided with a crystal liquid inlet 5, and the crystal liquid inlet 5 rotates along the tank body 1 to enter the liquid, and the inner pipe is 5-10° away from the tangent Angle, the upper part of the upper part of the tank body is provided with a light phase liquid outlet 8, and the bottom of the tank body is provided with a heavy phase liquid outlet 7.

Below the mixing and washing unit 11 is a separation unit 15, and n groups of mixing and washing units 11 and separation units 15 can be set, n≥3, and each mixing and washing unit 11 includes a group of agitators 9 and inclined plate mixers 12. The stirrer 9 is provided with 2-4 stirring paddles.

Swash plate fixed link 14 is some straight rods that are horizontally arranged on the tank body 1, swash plate fixed link 14 intersperses in some slant plates, swash plate fixed link 14 and swash plate group 13 warp and weft settings. The inclined angles of the inclined plates 13 forming the inclined plate group 13 are 60-85°, and the inclined angles of the inclined plate groups 13 of the adjacent mixed washing units 11 are arranged in opposite directions.

The liquid distributor 16 is composed of several connected liquid distribution pipes 17. The liquid distribution pipe 17 is a triangular pipe with a vertex angle of 45-60°. There is a liquid outlet 18 under the liquid distribution pipe 17. Several liquid distribution pipes 17 communicate with each other, and lay flat on the bottom of the mixing-separation-washing section in the middle of the tank body 1, and the liquid distribution pipes 17 and the stirring shaft 10 are in communication. The washing liquid is transported from the washing liquid inlet 6 to the liquid distributor 16 through the stirring shaft 10 and then transported into the tank body 1 .

Preferred embodiment: the liquid distributor 16 is 100mm-200mm away from the lower settling section, and the distance between the agitator 9 and the inclined plate mixer 12 is 50mm-100mm.

The method for washing and separating using the crystal separation washer is as follows:

S1. Enter the washing solvent from the washing liquid feed port 6, transfer it to the liquid distributor 16 through the stirring shaft 10, and then enter the interior 1 of the tank body to fill up the tank body;

S2. Turn on the power mechanism 19, the agitator 9 starts to rotate, and the crystal to be extracted is put into the scrubber through the crystal feed port 5, according to the weight of the crystal to be extracted in kg: the volume of the washing liquid L=1: (3-6) The ratio continues to feed;

S3, the crystals to be extracted continue to fall to the settling section 4 after passing through multiple groups of mixing washing units and separation units, and after fully settling, the heavy phase comes out from the heavy phase liquid outlet 7, and the washing liquid flows out from the light phase liquid outlet;

S4. The heavy phase is precipitated to obtain the final product.

An example of actual crystal separation using the crystal separation scrubber of this application is as follows:

Example 1

(1) There are 5 sets of mixed washing unit 11 and separation unit 15 of the crystal separation washer, 400L of 80% ethanol enters from the washing liquid feed port 6, and is transferred to the liquid distributor 16 through the stirring shaft 10 and enters 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 agitator 9 to start rotating. 100kg of piperine crystals, with a content of 90%, enter the equipment through the crystal feed port 5, and continue to feed 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 stages of mixing and separation, they finally fall to the settling section 4 , after fully settling in the settling 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.

(2) After the washed piperine was subjected to the subsequent desolventization process, 80.35 kg of piperine crystals were obtained, the detected content was 98.11%, and the calculated content yield was 87.54%.

Example 2

(1) 300L of methanol enters from the washing liquid feed port 6, passes through the inside of the stirring shaft 10 to the liquid distributor 16 and enters the inside of the tank body 1, and after filling the equipment cavity 1, the power mechanism 19 is turned on to drive the stirring shaft 10, The stirrer 9 starts to rotate. 100kg of stevioside crystals, with a content of 86.16%, enter the equipment through the crystal feed port 5, and continue to enter the liquid according to the 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 stages of mixing and separation, they finally fall to the settling section 4. After sufficient settling in the settling 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.

(2) After the washed stevioside was subjected to the subsequent desolventization process, 79.25kg of stevioside crystals were obtained, the detected content was 97.37%, and the calculated content yield was 89.56%.

Example 3

(1) 500L of 90% ethanol enters from the washing liquid feed port 6, passes through the inside of the stirring shaft 10 to the liquid distributor 16 and enters the inside of the tank body 1. After filling the equipment cavity 1, turn on the power mechanism 19 to drive the stirring shaft 10 , Stirrer 9 starts to rotate. 100kg of curcumin crystals, with a content of 85.45%, enter the equipment through the crystal feed port 5, and continue to feed according to the 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, and continue to fall after passing through the separation unit 15. After a total of 5 stages of mixing and separation, they finally fall to the settling section 4 , after fully settling in the settling 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.

(2) The curcumin after washing was subjected to the subsequent desolventization process to obtain 81.62kg of curcumin crystals, the detected content was 98.23%, and the calculated content yield was 93.83%.

The structure of the device is simple, and multiple mixing, washing and separating units can be set according to the crystal purity requirements, and the crystals can be separated and washed multiple times to meet the purity requirements, and the high-purity crystals produced by the device still have fluidity, which is convenient for transportation and subsequent drying . After repeated experiments, the device has excellent separation and washing effects, and 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 (10)

1. A crystal separation scrubber, comprising: the tank comprises a tank body (1) and a stirring shaft (10) arranged in the tank body (1), wherein a hollow cavity is arranged in the tank body (1) and is divided into an upper clarifying section, a middle mixing-separating-washing section and a lower settling section, a mixing washing unit and a separating unit (15) are arranged in the middle mixing-separating-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) consists of 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-separating-washing section, the stirring shaft (10) is a hollow shaft, the top of the stirring shaft (10) is communicated with a liquid inlet washing liquid (6), a crystal liquid inlet (5) is arranged at the upper part of the mixing-separating-washing section at the middle of the tank body, a light phase liquid outlet (8) is arranged at the upper clarifying section of the tank body, and a heavy phase liquid outlet (7) is arranged at the bottom of the tank body.

2. A crystal separation scrubber as recited in claim 1, wherein: a stirring power mechanism (19) is arranged at the top of the tank body (1), and the stirring power mechanism (19) controls the stirring shaft (10) to run.

3. A crystal separation scrubber as recited in claim 1, wherein: the crystal liquid inlet (5) is spirally fed along the tank body (1), and an angle of 5-10 degrees is formed between the inner side pipeline and a tangent line.

4. A crystal separation scrubber as recited in claim 1, wherein: a separation unit (15) is arranged below the mixing washing unit (11), n groups of mixing washing units (11) and separation units (15) can be arranged, n is more than or equal to 3, and each mixing washing unit (11) comprises a group of stirrers (9) and inclined plate mixers (12).

5. The crystal separation scrubber of claim 4, wherein: the inclined plate fixing connecting rods (14) are a plurality of straight rods transversely arranged on the tank body (1), the inclined plate fixing connecting rods (14) are inserted into the inclined plates, and the inclined plate fixing connecting rods (14) and the inclined plate groups (13) are arranged in a longitude and latitude mode.

6. The plant extract crystal separation scrubber of claim 5, wherein: the inclined plates (13) forming the inclined plate group (13) have an inclined angle of 60-85 degrees, and the inclined plate groups (13) of the adjacent mixing and washing units (11) are arranged in opposite directions.

7. A crystal separation scrubber as recited in any one of claims 1-6, wherein: the stirrer (9) is provided with 2-4 stirring paddles.

8. A crystal separation scrubber as recited in claim 1, wherein: the liquid distributor (16) is composed of a plurality of communicated liquid distributing pipes (17), the liquid distributing pipes (17) are triangular pipes, the angle of the vertex angle is 45-60 degrees, liquid outlet holes (18) are formed below the liquid distributing pipes (17), and the liquid distributing pipes (17) are communicated with the stirring shaft (10).

9. The crystal separation scrubber of claim 8, wherein: the cleaning solution is conveyed to a liquid distributor (16) through a stirring shaft (10) from a cleaning solution inlet (6) and then conveyed into the tank body (1).

10. The crystal separation scrubber of claim 4, wherein: the distance between the liquid distributor (16) and the lower settling section is 100mm-200mm, and the distance between the stirrer (9) and the inclined plate mixer (12) is 50mm-100mm.

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