Purification device for crocetin

Abstract

The utility model relates to a purification device for crocetin, which comprises a tank body, end covers are respectively arranged at two ends of the tank body, and a liquid inlet and a liquid outlet are arranged on the end covers; the two groups of filtering assemblies are respectively arranged in the end covers and are respectively communicated with the liquid inlet and the liquid outlet; the circulating assembly comprises a circulating pipeline and a diaphragm pump arranged on the circulating pipeline, and the two ends of the circulating pipeline are communicated with the liquid inlet and the liquid outlet respectively to form a circulating system. The device has the beneficial effects that the circulating assembly is adopted to form a filtering system, filtering operation is completed through the titanium rod with the micropores, materials are prevented from making contact with the external environment for many times, and the GMP certification standard is met; the concentration of the solvent is changed in a stepless manner for many times, so that the purity of substances to be purified is more easily increased, the purification efficiency is greatly improved, and the working time is shortened; by adopting intermittent application of the ultrasonic rod, the blockage of micropores in the surface of the titanium rod can be effectively prevented, the purification efficiency is improved, and the working time is shortened.

Description

TECHNICAL FIELD

[0001] The utility model relates to a purification device technical field, concretely relates to a kind of for crocetin purification device. BACKGROUND

[0002] Crocetin is also named safflower acid or crocetin, is colorless crystal, is one of main effective components of safflower, is derived from baulinaceae plant gardenia fruit, has polyunsaturated conjugated enoic acid structure, belongs to carotenoid material.Crocetin is difficult to dissolve in water, ethanol, methanol, acetone, normal propyl alcohol, isopropyl alcohol, normal butanol, isobutyl alcohol, tetrahydrofuran and acetonitrile etc., relatively easy to dissolve in alkaline solvent.

[0003] In the process of purifying preparation crocetin, gradient ethanol washing process is used (can refer to invention patent CN202410119051.X), microporous filter membrane is used for filtering, and filtering time is acceptable in laboratory and small-scale amplification, but to pilot production, even if filter membrane area is expanded to 50 square decimeters, each filtering time is as long as ten hours, and it needs to be completed multiple times, and filter equipment is cumbersome to disassemble and assemble, time is long, and material is contacted with external air multiple times, so as not to meet GMP certification standard.

[0004] In addition, the cost of polytetrafluoroethylene filter membrane is high, and one 80cm diameter filter membrane costs more than 100 yuan, to obtain crocetin with content of more than 90%, more than 50 filter membranes are needed in one purification process, and the cost of filter membranes is more than 6000 yuan, plus labor, water and electricity, and equipment depreciation, the cost is extremely high.Although filter rod can be used instead of filter membrane, but due to filter device, residual solution is left in filter after each filtering, which will affect the purity of beating and purifying.

[0005] Therefore, the utility model provides a kind of for crocetin purification device, which does not need to use filter membrane to realize the purification of gardenia extract. UTILITY MODEL CONTENT

[0006] In view of the deficiencies of the prior art, the utility model provides a kind of for crocetin purification device.

[0007] To achieve the above object, the utility model provides the following technical scheme:

[0008] A kind of for crocetin purification device, comprising:

[0009] Tank body, end cap is respectively arranged at both ends of the tank body, and inlet and outlet are arranged on the end cap;

[0010] Two groups of filter components are respectively arranged in the end cap and are respectively connected with the inlet and outlet;

[0011] The circulating assembly comprises a circulating pipeline and a diaphragm pump arranged on the circulating pipeline, two ends of the circulating pipeline are connected with the liquid inlet and the liquid outlet respectively, and a circulating system is formed;

[0012] The heat preservation assembly is arranged outside the tank body and provides heat energy for the tank body.

[0013] The bronchial pipeline is arranged at the liquid inlet and is connected with the nitrogen tank and provides nitrogen for the tank body.

[0014] The liquid supply pipeline is arranged at the liquid inlet and is connected with the supply tank and provides solvent for the tank body.

[0015] The filter pipeline is arranged at the liquid outlet and is connected with the filtrate recovery tank and recovers the filtrate.

[0016] As a preferred technical scheme, the filter assembly comprises a carrier plate, a plurality of titanium rods inserted into the tank body and at least one ultrasonic rod, the ultrasonic rod is arranged at the center of the carrier plate, the titanium rods are uniformly distributed on the carrier plate and are arranged outside the ultrasonic rod, and filter holes are uniformly distributed on the surface of the titanium rods.

[0017] As a preferred technical scheme, the diameter of the titanium rod is 10-35 cm.

[0018] As a preferred technical scheme, the diameter of the filter hole is 3-10 μm.

[0019] As a preferred technical scheme, the length of the titanium rod is not greater than half of the length of the tank body.

[0020] As a preferred technical scheme, the supply tank comprises a solvent supply tank and a pure water supply tank, a mixer is arranged between the solvent supply tank and the pure water supply tank, and the solvent mixed by the mixer is pumped into the tank body.

[0021] As a preferred technical scheme, the solvent is ethanol.

[0022] As a preferred technical scheme, the tank body is provided with a disturbance assembly, the disturbance assembly is a magnetic stirring device, and the magnetic stirring device is used to increase the stirring of materials in the tank body.

[0023] As a preferred technical scheme, the heat preservation assembly is provided with a constant temperature solvent, and the constant temperature solvent is water or water vapor or silicone oil.

[0024] Beneficial effects: (1) The circulating assembly forms a filter system, the filter operation is completed by the titanium rod with micropores, the contact of materials with the external environment is avoided, and the GMP certification standard is met.

[0025] (2) The use of multiple different concentrations of solvent change or no change in the concentration of the solvent, more easily make the need to be purified substances high purity, greatly improve the efficiency of purification, shorten the working time.

[0026] (3) The use of ultrasonic rod intermittent application, can effectively prevent the titanium rod surface microporous blockage, improve the efficiency of purification, shorten the working time. BRIEF DESCRIPTION OF DRAWINGS

[0027] In order to more clearly illustrate the technical means, the creation features, the purposes and the effects of the embodiments of the present application, the following will be further described with reference to the accompanying drawings.

[0028] Fig. 1 For the present application: a structure diagram of a device for the purification of crocetin;

[0029] Fig. 2 For the present application: a structure diagram of a filter assembly of a device for the purification of crocetin;

[0030] Fig. 3 For the present application: a side view structure diagram of a filter assembly of a device for the purification of crocetin.

[0031] Wherein: tank 100, filter assembly 200, circulating assembly 300, heat preservation assembly 400, branch air pipe 500, liquid supply pipe 600, filter pipe 700, disturbance assembly 800;

[0032] End cover 101, liquid inlet 102, liquid outlet 103, carrier plate 201, titanium rod 202, ultrasonic rod 203, filter hole 204, circulating pipe 301, diaphragm pump 302, nitrogen tank 501, supply tank 601, solvent supply tank 6011, pure water supply tank 6012, mixer 6013, filtrate recovery tank 701. DETAILED DESCRIPTION

[0033] In order to make the technical means, the creation features, the purposes and the effects of the present application easy to understand, the following will be further described with reference to the specific drawings.

[0034] Example 1

[0035] Referring to Figs. 1-3 As shown in the figure, a device for the purification of crocetin, comprising: tank 100, two filter assemblies 200, circulating assembly 300, heat preservation assembly 400, branch air pipe 500, liquid supply pipe 600, and filter pipe 700.

[0036] The tank body 100 is in a cylindrical shape and horizontally placed on a rack, and end covers 101 are arranged at two ends of the tank body 100, liquid inlet 102 and liquid outlet 103 are arranged on the end covers 101, and two groups of filter assemblies 200 are arranged in the end covers 101 and respectively connected with the liquid inlet 102 and the liquid outlet 103.

[0037] The circulating assembly 300 comprises a circulating pipeline 301 and a diaphragm pump 302 arranged on the circulating pipeline 301, two ends of the circulating pipeline 301 are respectively connected with the liquid inlet 102 and the liquid outlet 103, and a circulating system is formed, in the use process, the diaphragm pump 302 is started to realize the circulation of the material in the tank body 100, and when the material passes through the filter assembly 200, the purification of the material is completed.

[0038] The heat preservation assembly 400 is arranged outside the tank body 100 and used for providing heat energy to the tank body 100, generally, a constant temperature solvent is arranged in the heat preservation assembly 400, and the constant temperature solvent is water or water vapor or silicon oil.

[0039] The bronchial pipeline 500 is arranged at the liquid inlet 102 and used for connecting a nitrogen tank 501 and supplying gas to the tank body 100.

[0040] The filter pipeline 700 is arranged at the liquid outlet 103 and connected with a filtrate recovery tank 701 and used for recovering the filtrate.

[0041] The filter assembly 200 comprises a carrier plate 201, a plurality of titanium rods 202 extending into the tank body 100 and at least one ultrasonic rod 203, the ultrasonic rod 203 is arranged at the center of the carrier plate 201, the titanium rods 202 are uniformly arranged on the carrier plate 201 and arranged outside the ultrasonic rod 203, and filter holes 204 are uniformly arranged on the surfaces of the titanium rods 202.

[0042] It is worth mentioning that the diameter of the titanium rod 202 is 10-35 cm, and the diameter of the filter hole 204 is 3-10 μm. Since crocetin is difficult to dissolve in water, ethanol, methanol, acetone, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, tetrahydrofuran and acetonitrile and other commonly used solvents, and is relatively easy to dissolve in alkaline solvents. The above design can prevent crocetin crystals from passing through the filter hole 204 during use, thereby more effectively improving the purification efficiency and shortening the working time.

[0043] Generally, the length of the titanium rod 202 is not more than half the length of the tank body 100. The length of the titanium rod 202 should not be too long, and during installation, the titanium rods 202 at both ends should avoid touching each other.

[0044] The supply tank 601 of the utility model includes solvent supply tank 6011 and pure water supply tank 6012, and a mixer 6013 is arranged between the solvent supply tank 6011 and the pure water supply tank 6012. The solvent mixed by the mixer 6013 is pumped into the tank body 100. The solvent in the embodiment is ethanol. Taking ethanol as an example, when 30% concentration ethanol is needed, the flow rate switches of the solvent supply tank 6011 and the pure water supply tank 6012 can be controlled, and 30% concentration ethanol can be obtained after passing through the mixer 6013; when 60% concentration ethanol is needed, the flow rate switches of the solvent supply tank 6011 and the pure water supply tank 6012 can be controlled, and 60% concentration ethanol can be obtained after passing through the mixer 6013; when 90% concentration ethanol is needed, the flow rate switches of the solvent supply tank 6011 and the pure water supply tank 6012 can be controlled, and 90% concentration ethanol can be obtained after passing through the mixer 6013. In the above supply process, different supply containers do not need to be switched.

[0045] The tank body 100 is provided with a disturbance assembly 800, which is a magnetic stirring device, to increase the stirring of the material in the tank body 100 and ensure that the material in the tank body 100 can be uniformly mixed. This stirring method not only improves the mixing efficiency, but also avoids the pollution problem that may be caused by mechanical stirring. The use of the magnetic stirring device ensures that the material does not come into contact with any mechanical parts during stirring, thereby ensuring the cleanliness and safety of the purification process. In addition, the magnetic stirring device has low operating noise and small impact on the operating environment, and is suitable for use in laboratories or production environments that need to maintain silence. By accurately controlling the speed of the magnetic stirring device, the mixing effect of the material can be further optimized, and the stability and reliability of the purification process can be ensured.

[0046] Taking the purification process of crocetin as an example, the operation process of the utility model is described as follows:

[0047] Feeding: open the end cover 101 on one side of the tank 100, put 2 liters of crocetin concentrated slurry (obtained by centrifugation of a disc centrifuge) 2 into the tank 100, close the end cover 101, and introduce hot water at 60°C into the heat preservation assembly 400 so that the tank 100 is kept in a constant temperature state.

[0048] Primary purification: open the liquid supply pipeline 600, inject 9 liters of 60°C 30% ethanol solvent (the concentration is obtained by mixing the solvent supply tank 6011 and the pure water supply tank 6012) into the tank 100, close the liquid supply pipeline 600, open the diaphragm pump 302 to circulate the liquid, and at the same time, open the ultrasonic wave, after 30 minutes, close the diaphragm pump 302 and the ultrasonic wave, open the filter pipeline 700 and the branch pipeline 500, supply nitrogen at 0.2 MPa from the branch pipeline 500, and dry the ethanol solution in the tank 100 from the filter pipeline 700, and the primary purification is completed.

[0049] Secondary purification: open the liquid supply pipeline 600, inject 9 liters of 60°C 60% ethanol solvent (the concentration is obtained by mixing the solvent supply tank 6011 and the pure water supply tank 6012) into the tank 100, close the liquid supply pipeline 600, open the diaphragm pump 302 to circulate the liquid, and at the same time, open the ultrasonic wave, after 30 minutes, close the diaphragm pump 302 and the ultrasonic wave, open the filter pipeline 700 and the branch pipeline 500, supply nitrogen at 0.2 MPa from the branch pipeline 500, and dry the ethanol solution in the tank 100 from the filter pipeline 700, and the secondary purification is completed.

[0050] Tertiary purification: open the liquid supply pipeline 600, inject 9 liters of 60°C 90% ethanol solvent (the concentration is obtained by mixing the solvent supply tank 6011 and the pure water supply tank 6012) into the tank 100, close the liquid supply pipeline 600, open the diaphragm pump 302 to circulate the liquid, and at the same time, open the ultrasonic wave, after 30 minutes, close the diaphragm pump 302 and the ultrasonic wave, open the filter pipeline 700 and the branch pipeline 500, supply nitrogen at 0.2 MPa from the branch pipeline 500, and dry the ethanol solution in the tank 100 from the filter pipeline 700, and the tertiary purification is completed.

[0051] Drying: take out the material in the tank 100, dry, and obtain 70.3 grams. The crocetin content is 93.8% detected by HPLC.

[0052] After the above operation process, the utility model has the following advantages:

[0053] (1) The filter system is formed by the circulating assembly 300, the filtration operation is completed by the titanium rod 202 with micropores, the material is prevented from being in contact with the external environment for multiple times, and the GMP certification standard is met.

[0054] (2) The use of multiple concentration changes, more easily make the purified material purity is high, greatly improve the purification efficiency, shorten the working time.

[0055] (3) The use of ultrasonic rod 203 intermittent application, can effectively prevent the titanium rod 202 surface microporous blockage, improve the purification efficiency, shorten the working time.

[0056] The above only for the preferred specific embodiments of the present application, but the scope of the present application is not limited to this, any skilled in the art of the technical range disclosed by the present application, according to the technical scheme of the present application and the utility model concept of equivalent replacement or change, should be covered within the scope of the present application.

[0057] In the description of the present application, it is understood that the terms "coaxial", "bottom", "one end", "top", "middle", "the other end", "upper", "one side", "top", "inner", "front", "central", "both ends" and the like indicate the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application.

Claims

1. A device for the purification of crocetin, characterized in that, The application relates to a filter device for filtering liquid, which comprises the following parts: a tank body, which is provided with end covers at two ends, and is provided with liquid inlet and outlet ports on the end covers; two groups of filter assemblies, which are arranged in the end covers respectively, and are connected with the liquid inlet and outlet ports respectively; a circulating assembly, which comprises a circulating pipeline and a diaphragm pump arranged on the circulating pipeline, and the two ends of the circulating pipeline are connected with the liquid inlet and outlet ports respectively, and form a circulating system; a heat preservation assembly, which is arranged outside the tank body, and is used for providing heat energy to the tank body; a branch pipeline, which is arranged at the liquid inlet port, and is used for connecting a nitrogen tank, and supplying nitrogen to the tank body; a liquid supply pipeline, which is arranged at the liquid inlet port, and is used for connecting a supply tank, and supplying solvent to the tank body; a filter pipeline, which is arranged at the liquid outlet port, and is connected with a filtrate recovery tank, and is used for recovering filtrate.

2. A device for the purification of crocetin according to claim 1, characterized in that, The filter assembly comprises a carrier plate, a plurality of titanium rods inserted into the tank body, and at least one ultrasonic rod, the ultrasonic rod is arranged at the center of the carrier plate, the titanium rods are uniformly distributed on the carrier plate and are arranged outside the ultrasonic rod, and filter holes are uniformly distributed on the surface of the titanium rods.

3. A device for the purification of crocetin according to claim 2, characterized in that, The diameter of the titanium rod is 10-35 cm.

4. A device for the purification of crocetin according to claim 2, characterized in that, The diameter of the filter hole is 3-10 mu m.

5. A device for the purification of crocetin according to claim 2, characterized in that, The length of the titanium rod is not more than half of the length of the tank body.

6. A device for the purification of crocetin according to claim 1, characterized in that, The supply tank comprises a solvent supply tank and a pure water supply tank, a mixer is arranged between the solvent supply tank and the pure water supply tank, and the solvent mixed by the mixer is pumped into the tank body.

7. A device for the purification of crocetin according to claim 1, characterized in that, A disturbance assembly is arranged in the tank body, the disturbance assembly is a magnetic stirring device, and is used for increasing the stirring of materials in the tank body.

8. A device for the purification of crocetin according to claim 1, characterized in that, A constant temperature solvent is arranged in the heat preservation assembly, and the constant temperature solvent is water or water vapor or silicon oil.

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