Purification equipment and process for preventing pipeline blockage

By designing a purification equipment including a concentration main machine and a concentration secondary machine, using vacuum scraper to concentrate, heat stirring and dissolving, condensing and recovery of solvents, problems such as pipeline blockage in the preparation of plant functional ingredients are solved, and a more efficient and continuous preparation process is achieved.

CN120114874APending Publication Date: 2025-06-10INSTITUTE OF APPLIED CHEMISTRY JIANGXI ACADEMY OF SCIENCES +1
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Patent Information

Application Number
CN202510296572.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-13
Publication Date
2025-06-10

AI Technical Summary

Technical Problem

During the preparation of plant functional ingredients, there are problems such as blockage of connection pipes, discontinuous production, long preparation cycle time, low yield and low purity.

Method used

A purification equipment including a concentration main machine and a concentration secondary machine was designed. The steps of concentrating by vacuum scraper, heating and stirring dissolving, condensing and recovery of solvents were avoided, and the pipeline was further separated and solvent recovery was carried out through a plate-frame filter press and a plate-type condensing device.

Benefits of technology

It effectively avoids pipeline blockage, shortens the preparation cycle, improves yield and purity, and optimizes the process flow through solvent recovery.

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Abstract

The invention discloses purification equipment and technology for preventing pipeline blockage, the equipment comprises a concentration main machine and a plurality of concentration auxiliary machines, the concentration main machine and the concentration auxiliary machines are in one-to-one butt joint, the concentration main machine is provided with an extracting solution inlet used for guiding in an extracting solution; the solvent inlet is used for introducing different solvents; the supernate outlet is used for leading out a primary extracting solution after the extracting solution and the solvent react; the solvent recovery device is used for recovering the residual solvent; the concentration auxiliary machine is provided with a primary extracting solution inlet which is in butt joint with the supernate outlet, and the concentration auxiliary machine is used for further concentrating the primary extracting solution. According to the method, the defects that traditional separation and purification preparation is long in cycle time, and connecting pipelines are blocked are overcome.
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Description

Technical Field

[0001] The invention belongs to the technical field of plant effective active ingredient extraction, and in particular relates to purification equipment and a process for preventing pipeline blockage. Background Art

[0002] The preparation of plant active ingredients includes extraction, concentration, purification (refining), crystallization and other steps, among which the concentration step is the most used process. However, after concentration, whether it is a flowing paste, a fluid of a certain density or a solid, there is a problem of connecting pipe blockage, which needs to be solved manually, which will cause discontinuous production.

[0003] Currently, the extract is concentrated and then pumped into the next process, and then concentrated again after the next process is completed, and this process is repeated. However, due to the characteristics of the concentrated material itself, such as high viscosity and high density, the connecting pipelines may be blocked when pumping, resulting in discontinuous production, long preparation cycle time, low yield, and low purity. Summary of the invention

[0004] In view of the disadvantages of the existing preparation process of plant efficacy components, such as blockage of connecting pipelines, discontinuous production, long preparation cycle time, low yield, low purity, etc., the present invention provides a purification device and process for preventing pipeline blockage.

[0005] In order to achieve the above-mentioned purpose, the technical solution adopted by the present invention is:

[0006] A purification device for preventing pipeline blockage, the device comprises a main concentrator and several auxiliary concentrators, the main concentrator and the auxiliary concentrators are connected one by one,

[0007] The concentrator host is equipped with:

[0008] An extracting liquid inlet, used for introducing the extracting liquid;

[0009] Solvent inlet, used to introduce different solvents;

[0010] A supernatant outlet is used to export the preliminary extract after the extract and the solvent react;

[0011] A solvent recovery device for recovering residual solvent;

[0012] The auxiliary concentrator is provided with:

[0013] The inlet of the preliminary extraction liquid is connected to the outlet of the supernatant liquid, and the auxiliary concentrator further concentrates the preliminary extraction liquid.

[0014] Furthermore, the concentrating host is also provided with:

[0015] The discharge port is used to discharge the concentrated high-concentration extract or solid material;

[0016] Temperature control ports, including steam inlet and outlet for heating and cold water inlet and outlet for cooling;

[0017] The reflux inlet and outlet are connected to the circulation channel inside the concentrator host through a reflux pipeline; a control valve is arranged on the reflux pipeline.

[0018] Furthermore, the concentrating host is also provided with:

[0019] A condensation component, the condensation component comprising:

[0020] The vertical condenser is installed at the steam outlet of the concentrating main unit, and its cooling medium inlet is connected to the external cooling water source through a pipeline, and the cooling medium outlet is connected to the external drainage system or circulating cooling system through a pipeline. It is used to preliminarily condense the solvent vapor discharged from the main unit, and condense the solvent vapor into liquid through heat exchange between the cooling medium and the solvent vapor;

[0021] and / or;

[0022] The horizontal condenser is connected to other parts of the concentrator. When the concentrator heats, stirs and dissolves the solvent and the material, when it is necessary to close other valves, open the horizontal condenser valve, and open the steam inlet and outlet for heating, the horizontal condenser plays the role of condensing and recovering the solvent. Its cooling medium inlet and outlet are connected to the external cooling system through pipelines.

[0023] The concentrated condensation outlet is connected to the condensation component of the concentrator host and is used to export the condensate.

[0024] Further, the solvent recovery device is:

[0025] The plate condensation device is used to recover the residual solvent of the previous process.

[0026] Furthermore, the supernatant outlet of the main concentrator and the auxiliary concentrator are also provided with:

[0027] Plate and frame filter press is used to further separate the solid and liquid of the preliminary extract.

[0028] Furthermore, the concentrating host is also provided with:

[0029] A stirring paddle is used to stir the materials and the solvent that reacts together.

[0030] A purification process for preventing pipeline blockage, used for the above-mentioned purification equipment for preventing pipeline blockage, characterized by comprising:

[0031] Step S1: Introduce the material into the concentration host through the extraction liquid inlet,

[0032] Step S2: The concentrating host performs vacuum scraper concentrating on the material to obtain a preliminary concentrated liquid;

[0033] Step S3: introducing the Nth solvent through the solvent inlet, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid;

[0034] Step S4: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool the dissolved mixed solution, i.e., the preliminary extract;

[0035] Step S5: The supernatant of the concentration main machine is pumped into a plate and frame filter press for further separation, and the separated liquid is further sent to a concentration auxiliary machine.

[0036] Step S6: using a plate condensation device to recover the Nth solvent remaining in the concentrator host;

[0037] Step S7: introducing the N+1th solvent through the solvent inlet, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid;

[0038] Step S8: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool down the dissolved mixed solution, i.e., the preliminary extract;

[0039] Step S9: The supernatant of the concentration main machine is pumped into a plate and frame filter press for further separation, and the separated liquid is further sent to a concentration auxiliary machine.

[0040] Step S10: using a plate condensation device to recover the N+1th solvent remaining in the concentration host;

[0041] Here, N represents a positive integer.

[0042] Furthermore, the material is turmeric extract, and the solvent includes petroleum ether as a first solvent, ethyl acetate as a second solvent, and acetone as a third solvent;

[0043] or,

[0044] The material is a kudzu root extract, and the solvent includes n-hexane as a first solvent, acetone as a second solvent, and ethyl acetate as a third solvent;

[0045] or,

[0046] The material is an extract of Eucommia ulmoides, an extract of Panax notoginseng, an extract of Lonicera japonica, an extract of Senecio truncatum or an extract of Lonicera japonica, and the solvent includes petroleum ether as a first solvent and ethyl acetate as a second solvent;

[0047] or,

[0048] The material is a Polygonum multiflorum extract, and the solvent includes ethyl acetate as a first solvent and methanol as a second solvent;

[0049] or,

[0050] The material is a camphor tree extract, and the solvent includes dichloromethane as a first solvent and ethyl acetate as a second solvent;

[0051] or,

[0052] The material is a mahonia extract, and the solvent includes petroleum ether as a first solvent and n-butanol as a second solvent.

[0053] The beneficial effects of the present invention are:

[0054] The present invention firstly avoids the disadvantages of the traditional separation and purification preparation cycle time being long, the connection pipeline being blocked, etc. In addition, the concentration main machine of the present invention includes all the processes used in plant extraction, that is, all the processes can be used in the concentration main machine. Another advantage of the present invention is that the mixing of the solvents used is avoided. After the previous solvent is used, the residue of the previous solvent is removed by a plate condensation device. The present invention can also increase the number of concentration auxiliary machines according to the amount of solvent used, and there is no situation of "large at the front and small at the back" during use, which affects the production cycle. BRIEF DESCRIPTION OF THE DRAWINGS

[0055] Figure 1 The present invention discloses a structural schematic diagram of a purification device for preventing pipeline blockage. DETAILED DESCRIPTION

[0056] The present invention can be further described in detail with reference to the following examples; however, the following examples are merely illustrative, and the present invention is not limited to these examples.

[0057] Reference Figure 1 A purification device for preventing pipeline blockage, the device comprises a main concentrator and several auxiliary concentrators, the main concentrator and the auxiliary concentrators are connected one by one,

[0058] The concentrator host is equipped with:

[0059] Extraction liquid inlet a, used for introducing the extraction liquid;

[0060] Solvent inlet h, used to introduce different solvents;

[0061] The supernatant outlet e is used to export the preliminary extract after the extract and the solvent react;

[0062] A solvent recovery device for recovering residual solvent;

[0063] The auxiliary concentrator is provided with:

[0064] The inlet of the preliminary extraction liquid is connected to the supernatant outlet e, and the concentrating auxiliary machine further concentrates the preliminary extraction liquid.

[0065] Furthermore, the concentrating host is also provided with:

[0066] The discharge port b is used to discharge the concentrated high-concentration extract or solid material;

[0067] Temperature control port c, including steam inlet and outlet for heating and cold water inlet and outlet for cooling;

[0068] The reflux inlet and outlet g are connected to the circulation channel inside the concentrator host through a reflux pipeline; a control valve is provided on the reflux pipeline.

[0069] Furthermore, the concentrating host is also provided with:

[0070] A condensation component, the condensation component comprising:

[0071] Vertical condenser j is installed at the steam outlet of the concentrating main unit, and its cooling medium inlet is connected to the external cooling water source through a pipeline, and the cooling medium outlet is connected to the external drainage system or circulating cooling system through a pipeline, and is used to preliminarily condense the solvent vapor discharged from the main unit, and condense the solvent vapor into liquid through heat exchange between the cooling medium and the solvent vapor;

[0072] and / or;

[0073] The horizontal condenser k is connected to other parts of the concentrator. When the concentrator heats, stirs and dissolves the solvent and the material, when it is necessary to close other valves, open the horizontal condenser valve, and open the steam inlet and outlet for heating, the horizontal condenser plays the role of condensing and recovering the solvent. Its cooling medium inlet and outlet are connected to the external cooling system through pipelines.

[0074] The concentrated condensation outlet i is connected to the condensation component of the concentrating host and is used to export the condensate.

[0075] Further, the solvent recovery device is:

[0076] The plate condensation device l is used to recover the residual solvent of the previous step.

[0077] Furthermore, the supernatant outlet of the main concentrator and the auxiliary concentrator are also provided with:

[0078] Plate and frame filter press f is used to further separate the solid and liquid from the preliminary extract.

[0079] Furthermore, the concentrating host is also provided with:

[0080] Stirring paddle d is used to stir the materials and the solvent to be reacted together.

[0081] A purification process for preventing pipeline blockage, used for the above-mentioned purification equipment for preventing pipeline blockage, characterized by comprising:

[0082] a extract inlet; b discharge port; c temperature control port; d stirring paddle; e supernatant extraction port; f plate and frame filter press; g reflux inlet and outlet; h solvent inlet; i concentration condensation outlet; j vertical condenser; k horizontal condenser; l plate condensation device

[0083] Step S1: Introduce the material into the concentration host through the extraction liquid inlet a,

[0084] Step S2: The concentrating host performs vacuum scraper concentrating on the material to obtain a preliminary concentrated liquid;

[0085] Step S3: introducing the Nth solvent through the solvent inlet h, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid;

[0086] Step S4: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool the dissolved mixed solution, i.e., the preliminary extract;

[0087] Step S5: The supernatant of the concentration main machine is pumped into the plate and frame filter press f for further separation, and the separated liquid is further sent to the concentration auxiliary machine.

[0088] Step S6: using a plate condensation device 1 to recover the Nth solvent remaining in the concentrator host;

[0089] Step S7: introducing the N+1th solvent through the solvent inlet h, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid;

[0090] Step S8: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool down the dissolved mixed solution, i.e., the preliminary extract;

[0091] Step S9: The supernatant of the concentration main machine is pumped into the plate and frame filter press f for further separation, and the separated liquid is further sent to the concentration auxiliary machine.

[0092] Step S10: using a plate condensation device 1 to recover the N+1th solvent remaining in the concentration host;

[0093] Here, N represents a positive integer.

[0094] Further, the material is turmeric extract, and the solvent includes petroleum ether as a first solvent, ethyl acetate as a second solvent, and acetone as a third solvent;

[0095] or,

[0096] The material is a kudzu root extract, and the solvent includes n-hexane as a first solvent, acetone as a second solvent, and ethyl acetate as a third solvent;

[0097] or,

[0098] The material is an extract of Eucommia ulmoides, an extract of Panax notoginseng, an extract of Lonicera japonica, an extract of Senecio truncatum or an extract of Lonicera japonica, and the solvent includes petroleum ether as a first solvent and ethyl acetate as a second solvent;

[0099] or,

[0100] The material is a Polygonum multiflorum extract, and the solvent includes ethyl acetate as a first solvent and methanol as a second solvent;

[0101] or,

[0102] The material is a camphor tree extract, and the solvent includes dichloromethane as a first solvent and ethyl acetate as a second solvent;

[0103] or,

[0104] The material is a mahonia extract, and the solvent includes petroleum ether as a first solvent and n-butanol as a second solvent.

[0105] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A purification device for preventing pipeline blockage, characterized in that: The device comprises a main concentrator and several auxiliary concentrators, wherein the main concentrator is connected to the auxiliary concentrators one by one. The concentrator host is equipped with: An extracting liquid inlet, used for introducing the extracting liquid; Solvent inlet, used to introduce different solvents; A supernatant outlet is used to export the preliminary extract after the extract and the solvent react; A solvent recovery device for recovering residual solvent; The auxiliary concentrator is provided with: The inlet of the preliminary extraction liquid is connected to the outlet of the supernatant liquid, and the auxiliary concentrator further concentrates the preliminary extraction liquid.

2. A purification device for preventing pipeline blockage according to claim 1, characterized in that: The concentrator host also has: The discharge port is used to discharge the concentrated high-concentration extract or solid material; Temperature control ports, including steam inlet and outlet for heating and cold water inlet and outlet for cooling; The reflux inlet and outlet are connected to the circulation channel inside the concentrator host through a reflux pipeline; a control valve is arranged on the reflux pipeline.

3. A purification device for preventing pipeline blockage according to claim 1, characterized in that: The concentrator host also has: A condensation component, the condensation component comprising: The vertical condenser is installed at the steam outlet of the concentrating main unit, and its cooling medium inlet is connected to the external cooling water source through a pipeline, and the cooling medium outlet is connected to the external drainage system or circulating cooling system through a pipeline. It is used to preliminarily condense the solvent vapor discharged from the main unit, and condense the solvent vapor into liquid through heat exchange between the cooling medium and the solvent vapor; and / or; The horizontal condenser is connected to other parts of the concentrator. When the concentrator heats, stirs and dissolves the solvent and the material, when it is necessary to close other valves, open the horizontal condenser valve, and open the steam inlet and outlet for heating, the horizontal condenser plays the role of condensing and recovering the solvent. Its cooling medium inlet and outlet are connected to the external cooling system through pipelines. The concentrated condensation outlet is connected to the condensation component of the concentrator host and is used to export the condensate.

4. A purification device for preventing pipeline blockage according to claim 1, characterized in that: The solvent recovery device is: The plate condensation device is used to recover the residual solvent of the previous process.

5. A purification device for preventing pipeline blockage according to claim 1, characterized in that: The supernatant outlet of the main concentrator and the auxiliary concentrator are also provided with: Plate and frame filter press is used to further separate the solid and liquid of the preliminary extract.

6. A purification device for preventing pipeline blockage according to claim 1, characterized in that: The concentrator host also has: A stirring paddle is used to stir the materials and the solvent that reacts together.

7. A purification process for preventing pipeline blockage, used in a purification device for preventing pipeline blockage as claimed in any one of claims 1 to 6, characterized in that: include: Step S1: Introduce the material into the concentration host through the extraction liquid inlet, Step S2: The concentrating host performs vacuum scraper concentrating on the material to obtain a preliminary concentrated liquid; Step S3: introducing the Nth solvent through the solvent inlet, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid; Step S4: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool the dissolved mixed solution, i.e., the preliminary extract; Step S5: The supernatant of the concentration main machine is pumped into a plate and frame filter press for further separation, and the separated liquid is further sent to a concentration auxiliary machine. Step S6: using a plate condensation device to recover the Nth solvent remaining in the concentrator host; Step S7: introducing the N+1th solvent through the solvent inlet, and the concentrating host heats, stirs and dissolves the first solvent and the preliminary concentrated liquid to obtain a mixed liquid; during this process, closing other valves, opening the horizontal condenser valve, and opening the steam inlet and outlet to heat and dissolve the mixed liquid; Step S8: After the mixed solution is dissolved, the cold water inlet and outlet are opened to cool down the dissolved mixed solution, i.e., the preliminary extract; Step S9: The supernatant of the concentration main machine is pumped into a plate and frame filter press for further separation, and the separated liquid is further sent to a concentration auxiliary machine. Step S10: using a plate condensation device to recover the N+1th solvent remaining in the concentration host; Here, N represents a positive integer.

8. A purification process for preventing pipeline blockage according to claim 7, characterized in that: The material is turmeric extract, and the solvent includes petroleum ether as a first solvent, ethyl acetate as a second solvent, and acetone as a third solvent; or, The material is a kudzu root extract, and the solvent includes n-hexane as a first solvent, acetone as a second solvent, and ethyl acetate as a third solvent; or, The material is an extract of Eucommia ulmoides, an extract of Panax notoginseng, an extract of Lonicera japonica, an extract of Senecio truncatum or an extract of Lonicera japonica, and the solvent includes petroleum ether as a first solvent and ethyl acetate as a second solvent; or, The material is a Polygonum multiflorum extract, and the solvent includes ethyl acetate as a first solvent and methanol as a second solvent; or, The material is a camphor tree extract, and the solvent includes dichloromethane as a first solvent and ethyl acetate as a second solvent; or, The material is a mahonia extract, and the solvent includes petroleum ether as a first solvent and n-butanol as a second solvent.