Supercritical nano-molecule crystallization equipment and crystal substance

Abstract

The utility model discloses supercritical nanometer molecule crystallization equipment and a crystal substance, and belongs to the technical field of chemical engineering, and the supercritical nanometer molecule crystallization equipment comprises a pretreatment unit (100), a primary reverse osmosis membrane unit (200), a supercritical molecule rectification unit (300), a secondary reverse osmosis membrane unit (400) and a crystal growth collection unit (500) which are connected in sequence; the pretreatment unit (100) is used for pretreating the target mixture to obtain a pretreated mixture; the first-stage reverse osmosis membrane unit (200) is used for performing first reverse osmosis membrane treatment on the pretreated mixture to obtain a primarily purified component; the supercritical molecular rectification unit (300) is used for carrying out supercritical molecular rectification treatment on the primarily purified component to obtain a rectified component; the second-stage reverse osmosis membrane unit (400) is used for performing second reverse osmosis membrane treatment on the rectification component to obtain a second-stage purification component; and the crystal growth collection unit (500) is used for collecting crystals of the target object.

Description

Technical Field

[0001] The present application belongs to the field of chemical technology, and specifically relates to a supercritical nanomolecular crystallization device and a crystal. Background Art

[0002] Supercritical fluid extraction (SCFE) was introduced into the field of separation of effective components of traditional Chinese medicine in the late 1980s as a new and efficient separation and extraction technology. After decades of research and development, SCFE technology has become one of the new technologies for realizing the modernization of traditional Chinese medicine. It has been widely used in the extraction, concentration and refining of effective components of traditional Chinese medicine and the removal of organic solvents, and has achieved good results.

[0003] The working principle of this technology is mainly to use the special properties of supercritical fluids between gas and liquid above the critical temperature (Tc) and critical pressure (Pc) to achieve synchronous extraction and separation. The density of supercritical fluids is close to that of liquids, the viscosity is similar to that of gases, and the diffusion coefficient is 10 to 100 times that of liquids. Therefore, they have strong solubility and good flow, permeation and transfer properties. In addition, near the critical point, slight changes in temperature and pressure can lead to significant changes in the physical and chemical properties of supercritical fluids. Therefore, the extraction and separation of active ingredients of natural medicines can be well achieved. Summary of the invention

[0004] The purpose of this application is to provide a supercritical nanomolecular crystallization device and crystals to achieve industrial extraction and separation of effective ingredients of natural medicines.

[0005] According to a first aspect of an embodiment of the present application, a supercritical nanomolecular crystallization device is provided, characterized in that it comprises: a pretreatment unit, a primary reverse osmosis membrane unit, a supercritical molecular distillation unit, a secondary reverse osmosis membrane unit and a crystal growth collection unit connected in sequence;

[0006] The pretreatment unit is used to pretreat the target mixture to obtain a pretreated mixture;

[0007] The primary reverse osmosis membrane unit is used to perform a first reverse osmosis membrane treatment on the pre-treated mixture to obtain a preliminarily purified component;

[0008] The supercritical molecular distillation unit is used to perform supercritical molecular distillation on the preliminarily purified components to obtain distillation components;

[0009] A secondary reverse osmosis membrane unit is used to perform a second reverse osmosis membrane treatment on the distillation components to obtain secondary purified components;

[0010] The crystal growth collection unit is used to collect crystals of the target object.

[0011] In some optional embodiments of the present application, the pretreatment unit includes: a filtering subunit and a pH adjusting subunit connected in sequence;

[0012] The pH regulating subunit is in communication with the primary reverse osmosis membrane unit;

[0013] The filtering subunit is used to remove large particle impurities;

[0014] The pH adjusting subunit is used to adjust the pH value.

[0015] In some optional embodiments of the present application, the pre-processing unit further includes: an elevator, a crusher, a conveyor and a stirrer;

[0016] The elevator is used to lift the material to the crusher for crushing, and the crushed material is conveyed to the mixer via the conveyor for mixing;

[0017] The output end of the stirrer is communicated with the input end of the filtering subunit.

[0018] In some optional embodiments of the present application, the pore size of the first reverse osmosis membrane of the primary reverse osmosis membrane unit ranges from 1 nanometer to 100 nanometers.

[0019] In some optional embodiments of the present application, the pore size of the second reverse osmosis membrane of the secondary reverse osmosis membrane unit ranges from 10 nanometers to 50 nanometers.

[0020] In some optional embodiments of the present application, the pretreatment unit, the primary reverse osmosis membrane unit, the supercritical molecular distillation unit, the secondary reverse osmosis membrane unit and the crystal growth collection unit are connected by pipelines.

[0021] In some optional embodiments of the present application, the supercritical molecular distillation unit includes: a heater and a high-pressure container connected in sequence.

[0022] In some optional embodiments of the present application, the temperature range of the heater is between 150°C and 400°C.

[0023] In some optional embodiments of the present application, the pressure range of the high-pressure container is between 1000psi and 5000psi.

[0024] According to a second aspect of the embodiments of the present application, a crystal is provided, which is obtained by crystallization using the supercritical nanomolecular crystallization device described in any one of the embodiments of the first aspect.

[0025] The above technical solution of the present application has the following beneficial technical effects:

[0026] The device of the embodiment of the present application realizes the extraction and separation of effective components through the sequentially connected pretreatment unit, the first-level reverse osmosis membrane unit, the supercritical molecular distillation unit, the second-level reverse osmosis membrane unit and the crystal growth collection unit. The device has good selectivity for the target substance, high extraction efficiency, low energy consumption, and basically achieves synchronous separation of the product and the solvent. It is particularly suitable for the extraction and purification of volatile and heat-sensitive substances. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 is a schematic structural diagram of a supercritical nanomolecular crystallization device in an exemplary embodiment of the present application;

[0028] Figure 2 It is a schematic diagram of the structure of a supercritical nanomolecular crystallization device in a specific embodiment of the present application.

[0029] Description of Reference Numerals

[0030] 100: pretreatment unit; 200: primary reverse osmosis membrane unit; 300: supercritical molecular distillation unit; 400: secondary reverse osmosis membrane unit; 500: crystal growth collection unit; 110: elevator; 120: crusher; 130: conveyor; 140: agitator; 150: filtering subunit; 160: pH adjustment subunit. DETAILED DESCRIPTION

[0031] In order to make the purpose, technical solutions and advantages of the present application clearer, the present application is further described in detail below in conjunction with specific implementations and with reference to the accompanying drawings. It should be understood that these descriptions are only exemplary and are not intended to limit the scope of the present application. In addition, in the following description, the description of known structures and technologies is omitted to avoid unnecessary confusion of the concepts of the present application.

[0032] The accompanying drawings show schematic diagrams of layer structures according to embodiments of the present application. These figures are not drawn to scale, and some details are magnified and some details may be omitted for the purpose of clarity. The shapes of various regions and layers shown in the figures and the relative sizes and positional relationships therebetween are only exemplary, and may deviate in practice due to manufacturing tolerances or technical limitations, and those skilled in the art may additionally design regions / layers with different shapes, sizes, and relative positions according to actual needs.

[0033] Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0034] In the description of the present application, it should be noted that the terms "first", "second" and "third" are used for descriptive purposes only and should not be understood as indicating or implying relative importance.

[0035] In addition, the technical features involved in the different embodiments of the present application described below can be combined with each other as long as they do not conflict with each other.

[0036] The supercritical nanomolecular crystallization device and the crystals provided in the embodiments of the present application are described in detail below through specific embodiments and their application scenarios in conjunction with the accompanying drawings.

[0037] like Figure 1 As shown, in a first aspect of an embodiment of the present application, a supercritical nanomolecular crystallization device is provided, which may include: a pretreatment unit 100, a primary reverse osmosis membrane unit 200, a supercritical molecular distillation unit 300, a secondary reverse osmosis membrane unit 400 and a crystal growth collection unit 500 connected in sequence;

[0038] The pretreatment unit 100 is used to pretreat the target mixture to obtain a pretreated mixture;

[0039] The primary reverse osmosis membrane unit 200 is used to perform a first reverse osmosis membrane treatment on the pre-treated mixture to obtain a preliminarily purified component;

[0040] The supercritical molecular distillation unit 300 is used to perform supercritical molecular distillation on the preliminarily purified components to obtain distilled components;

[0041] A secondary reverse osmosis membrane unit 400 is used to perform a second reverse osmosis membrane treatment on the distillation components to obtain secondary purified components;

[0042] The crystal growth collection unit 500 is used to collect crystals of the target object.

[0043] In some embodiments, the pretreatment unit 100 includes: a filtering subunit 150 and a pH adjusting subunit 160 connected in sequence;

[0044] The pH regulating subunit 160 is in communication with the primary reverse osmosis membrane unit 200;

[0045] The filtering subunit 150 is used to remove large particles of impurities;

[0046] The pH adjustment subunit 160 is used to adjust the pH value.

[0047] Specifically, the filtering subunit 150 can use a screen with a suitable aperture to filter and intercept large particles of impurities in the mixture. This can be done by selecting screens with different apertures to control the size of the filtered particles. Centrifugal separation can also be used to place the mixture in a centrifuge for centrifugal separation. The gravity causes the large particles of impurities to settle to the bottom of the centrifuge tube, and the clear supernatant can be collected from the top of the centrifuge tube.

[0048] The pH adjustment subunit 160 can add an appropriate amount of acid or alkaline solution to the mixture according to the properties of the mixture and the target pH value to adjust its pH. For example, if the mixture is alkaline, an acidic solution can be added to neutralize it; and vice versa.

[0049] like Figure 2 As shown, in a specific embodiment, the pre-processing unit 100 further includes: an elevator 110, a crusher 120, a conveyor 130 and a stirrer 140;

[0050] The elevator 110 is used to lift the material to the crusher 120 for crushing, and the crushed material is conveyed to the mixer 140 for mixing via the conveyor 130;

[0051] The output end of the agitator 140 is communicated with the input end of the filtering subunit 150 .

[0052] In some embodiments, the pore size of the first reverse osmosis membrane of the primary reverse osmosis membrane unit 200 is in a range of 1 nanometer to 100 nanometers.

[0053] The pore size of the reverse osmosis membrane determines its selectivity for molecules. In the case of removing large molecular impurities, the pore size should be small enough to prevent large molecules from passing through, while allowing small molecules to pass through. Because the primary reverse osmosis treatment is a preliminary purification treatment, the requirements for the reverse osmosis membrane are not so stringent. Therefore, the pore size range of the primary reverse osmosis membrane is also relatively wide, ranging from 1 nanometer to 100 nanometers.

[0054] In some embodiments, the pore size of the second reverse osmosis membrane of the secondary reverse osmosis membrane unit 400 is in a range of 10 nanometers to 50 nanometers.

[0055] The solution after the primary reverse osmosis membrane treatment may still contain trace impurities and water, so it needs to be treated with a secondary reverse osmosis membrane for further purification; similar to the primary reverse osmosis membrane treatment, the secondary reverse osmosis membrane treatment also requires pressure to push the solvent and small molecules through the membrane; after the secondary reverse osmosis membrane treatment, the trace impurities and water remaining in the solution are further removed to obtain a purer target component; the final purified target component is collected through flow control for subsequent application or processing.

[0056] Because the secondary reverse osmosis membrane treatment is the final purification treatment, the pore size range of the secondary reverse osmosis membrane is more stringent, and needs to be between 10 nanometers and 50 nanometers.

[0057] In some embodiments, the pretreatment unit 100, the primary reverse osmosis membrane unit 200, the supercritical molecular distillation unit 300, the secondary reverse osmosis membrane unit 400 and the crystal growth collection unit 500 are connected by pipelines. The pipelines in this embodiment are stainless steel pipelines. They are cheap and corrosion-resistant, and suitable for industrial production.

[0058] In some embodiments, the supercritical molecular distillation unit 300 includes: a heater and a high-pressure container connected in sequence.

[0059] In some embodiments, the temperature of the heater ranges from 150°C to 400°C.

[0060] In some embodiments, the pressure range of the high pressure vessel is between 1000 psi and 5000 psi.

[0061] In a second aspect of the embodiments of the present application, a crystal is provided, which is obtained by crystallization using the supercritical nanomolecular crystallization device described in any one of the embodiments of the first aspect.

[0062] The crystals in this embodiment can be plant oils, aromatic compounds, pigments, vitamins, medicinal ingredients in herbs, bioactive substances in marine organisms, etc.

[0063] The embodiments of the present application are described above in conjunction with the accompanying drawings, but the present application is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Under the guidance of the present application, ordinary technicians in this field can also make many forms without departing from the purpose of the present application and the scope of protection of the claims, all of which are within the protection of the present application.

Claims

1. A supercritical nanomolecular crystallization device, characterized in that: include: A pretreatment unit (100), a first-stage reverse osmosis membrane unit (200), a supercritical molecular distillation unit (300), a second-stage reverse osmosis membrane unit (400) and a crystal growth collection unit (500) connected in sequence; The pretreatment unit (100) is used to pretreat the target mixture to obtain a pretreated mixture; The primary reverse osmosis membrane unit (200) is used to perform a first reverse osmosis membrane treatment on the pre-treated mixture to obtain a preliminarily purified component; The supercritical molecular distillation unit (300) is used to perform supercritical molecular distillation on the preliminarily purified components to obtain distilled components; A secondary reverse osmosis membrane unit (400) is used to perform a second reverse osmosis membrane treatment on the distillation component to obtain a secondary purified component; The crystal growth collection unit (500) is used for collecting crystals of the target object.

2. The supercritical nanomolecular crystallization device according to claim 1, characterized in that: The pretreatment unit (100) comprises: a filtering subunit (150) and a pH adjusting subunit (160) connected in sequence; The pH adjustment subunit (160) is in communication with the primary reverse osmosis membrane unit (200); The filtering subunit (150) is used to remove large particle impurities; The pH adjustment subunit (160) is used to adjust the pH value.

3. The supercritical nanomolecular crystallization device according to claim 2, characterized in that: The pre-processing unit (100) further includes: an elevator (110), a crusher (120), a conveyor (130) and a stirrer (140); The elevator (110) is used to lift the material to the crusher (120) for crushing, and the crushed material is conveyed to the stirrer (140) via the conveyor (130) for stirring; The output end of the agitator (140) is in communication with the input end of the filtering subunit (150).

4. The supercritical nanomolecular crystallization device according to claim 1, characterized in that: The pore size of the first reverse osmosis membrane of the primary reverse osmosis membrane unit (200) ranges from 1 nanometer to 100 nanometers.

5. The supercritical nanomolecular crystallization device according to claim 1, characterized in that: The pore size of the second reverse osmosis membrane of the secondary reverse osmosis membrane unit (400) ranges from 10 nanometers to 50 nanometers.

6. The supercritical nanomolecular crystallization device according to claim 1, characterized in that: The pretreatment unit (100), the primary reverse osmosis membrane unit (200), the supercritical molecular distillation unit (300), the secondary reverse osmosis membrane unit (400) and the crystal growth collection unit (500) are connected via pipelines.

7. The supercritical nanomolecular crystallization device according to claim 1, characterized in that: The supercritical molecular distillation unit (300) comprises: a heater and a high-pressure container which are connected in sequence.

8. The supercritical nanomolecular crystallization device according to claim 7, characterized in that: The temperature of the heater ranges from 150°C to 400°C.

9. The supercritical nanomolecular crystallization device according to claim 7, characterized in that: The pressure range of the high pressure vessel is between 1000 psi and 5000 psi.

10. A crystal, characterized in that: The product is obtained by crystallization using the supercritical nanomolecular crystallization device described in any one of claims 1 to 9.

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