CN116875376A - Extraction process and extraction equipment of effective components of spina date seeds - Google Patents
Extraction process and extraction equipment of effective components of spina date seeds Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 136
- 238000000622 liquid--liquid extraction Methods 0.000 claims abstract description 95
- 238000000638 solvent extraction Methods 0.000 claims abstract description 95
- 238000000199 molecular distillation Methods 0.000 claims abstract description 49
- 238000000956 solid--liquid extraction Methods 0.000 claims abstract description 34
- 210000000582 semen Anatomy 0.000 claims abstract description 32
- 239000004480 active ingredient Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 18
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- 239000002904 solvent Substances 0.000 claims description 49
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- 238000003756 stirring Methods 0.000 claims description 32
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- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 8
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- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002028 Biomass Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
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- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 6
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- 240000008866 Ziziphus nummularia Species 0.000 description 17
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- 239000001397 quillaja saponaria molina bark Substances 0.000 description 5
- 229930182490 saponin Natural products 0.000 description 5
- 150000007949 saponins Chemical class 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- 239000005930 Spinosad Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 229940014213 spinosad Drugs 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 229930013930 alkaloid Natural products 0.000 description 2
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- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 2
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- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
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- BMWPBKOFJSHJAW-UHFFFAOYSA-N Saponin B Natural products CC1(C)CCC2(CCC3(C)C(=CCC4C5(C)CCC(OC6OC(CO)C(O)C(OC7OC(CO)C(O)C(O)C7O)C6=O)C(C)(C)C5CCC34C)C2C1)C(=O)O BMWPBKOFJSHJAW-UHFFFAOYSA-N 0.000 description 1
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- 229930003935 flavonoid Natural products 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses an extraction process and extraction equipment of active ingredients of spina date seeds, wherein the extraction process of the active ingredients of the spina date seeds adopts double solid-liquid extraction, three liquid-liquid extraction with different formulas and two molecular distillation processes according to the analysis of the ingredients in the spina date seeds, improves the precision of separating impurities, improves the yield of the active ingredients, is environment-friendly, and is suitable for large-scale industrialized production; the extraction equipment comprises a solid-liquid extraction system, an acid-base regulating device, a first molecular distillation device, a liquid-liquid extraction system and a second molecular distillation device, has the advantages of simple structure, low manufacturing cost, environmental friendliness, high automation degree, simple production operation and low labor cost, and is suitable for automatic continuous production operation of extracting and refining effective substances of various semen zizyphi spinosae cores.
Description
Technical Field
The invention relates to the field of extraction of plant functional components, in particular to an energy-saving and efficient extraction process and extraction equipment for extracting and refining spine date seed saponin and spinosin from spine date seed cores.
Background
In recent years, with the increase of working pressure, people are deeply puzzled by insomnia, and sleep improvement type health care products extracted by pure natural plants are increasingly popular. The wild jujube seed is a dry seed of wild jujube of the Rhamnaceae, is a Chinese medicine with homology of medicine and food, has the effects of hypnosis, sedation and the like, has good effects of treating and improving insomnia in clinic, is one of common raw materials in a pure natural plant health product for improving sleep, and is likely to come into huge market. At present, the health care products for improving sleep on the market mainly take the wild jujube seed powder as the raw material, but the wild jujube seed powder has lower content of active ingredients and poorer oral absorption effect, and greatly limits the application scene of the wild jujube seed, so that the wild jujube seed needs to be deeply processed.
Chinese patent application 201610294334.3 discloses a comprehensive extraction method of effective components of semen Ziziphi Spinosae, which adopts supercritical extraction method to extract lipid components of semen Ziziphi Spinosae from semen Ziziphi Spinosae to obtain semen Ziziphi Spinosae oil and semen Ziziphi Spinosae residue, and adopts molecular distillation technique to increase fatty acid content of semen Ziziphi Spinosae oil, and then adopts activated carbon, clay decolorization and monosodium glutamate removal treatment, and finally filtering to obtain edible semen Ziziphi Spinosae health oil. However, the supercritical extraction method adopted by the method needs to be carried out under the conditions of high temperature and high pressure, has high energy consumption and is easy to overheat and overburn the active ingredients in the materials, and the yield and quality of the active ingredients are affected, so that the active carbon and the clay are required to be used for decoloring and monosodium glutamate removing preparation in the later stage, the problems of large equipment investment and high production cost exist, and the method is difficult to meet the requirements of large-scale industrialized production.
Disclosure of Invention
The invention provides an extraction process and extraction equipment for effective components of spina date seeds, which are used for solving the technical problems of large investment, high production cost and the like in the prior extraction process and equipment.
In order to solve the technical problems, the invention adopts the following technical scheme:
an extraction process of effective components of semen Ziziphi Spinosae comprises the following steps:
s1, adding a solid extract A into the semen zizyphi spinosae particles for extraction, and filtering after the extraction is finished to obtain filter residue A and filtrate A; the solid extract A is Na 2 CO 3 And NaHCO 3 Na in the solid extract a 2 CO 3 And NaHCO 3 The mass of the semen zizyphi spinosae particles is 0.001 to 2 percent and 0.001 to 2 percent of the mass of the semen zizyphi spinosae particles respectively;
s2, adding a solid extract B into the filter residue A for extraction, and filtering solids after the extraction is finished to obtain filter residue B and filtrate B; the solid extract B is CH 3 COOH solution, CH in said solid extract B 3 The mass of COOH is 0.001% -2% of the mass of the filter residue A;
s3, mixing the filtrate A and the filtrate B, regulating the pH value to 6.5-7 to obtain a mixed solution, performing precise filtration on the mixed solution, and obtaining heavy components through molecular distillation to obtain a concentrated extract;
s4, extracting the concentrated extract for three times, separating to obtain a solvent phase and an effective component phase, and carrying out molecular distillation on the effective component phase to obtain a heavy component, thus obtaining the effective component of the spina date seed.
The design concept of the technical scheme is that the inventor obtains through component analysis contained in the semen zizyphi spinosae kernel, the semen zizyphi spinosae kernel mainly comprises triterpene, saponin a, B, flavonoid, spinosin, alkaloid, fatty acid, triglyceride, protein, starch and the like, wherein only the spinosin ab and the spinosin are main functional active substances of the semen zizyphi spinosae kernel, aiming at the component analysis, the technical scheme adopts a double solid-liquid extract formula of the solid extract A and the solid extract B, the double solid-liquid extract is used for separating the effective components from the protein and the starch, and simultaneously the solid extract A and the solid extract B can respectively react with the alkaloid, the fatty acid and the triglyceride to achieve the purpose of removing, so that the product quality and the production efficiency are greatly improved, and the production cost is reduced; meanwhile, after double solid-liquid extraction, a precise filtration process is adopted, so that impurities such as soaps generated by the reaction of the extraction liquid and the raw materials can be effectively removed, and the effect and the efficiency of subsequent molecular distillation are ensured; in addition, the technical scheme adopts a twice molecular distillation process, so that local overheating caused by overhigh temperature can be avoided.
As a further preferable mode of the technical scheme, in S1, the extraction operation temperature is 37-43 ℃, the extraction time is 5 hours, and the addition amount of the solid extractant A is 1.5 times of the mass of the semen zizyphi spinosae particles. Extraction operations within the above parameters can maximize the extraction effect and extraction efficiency of the active ingredients in the final product.
As a further preferable mode of the technical scheme, in S2, the extraction operation temperature is 37-43 ℃, the extraction time is 5 hours, and the addition amount of the solid extractant B is 150% of the mass of the filter residue A. Extraction operations within the above parameters can maximize the extraction effect and extraction efficiency of the active ingredients in the final product.
As a further preferable aspect of the above technical solution, the preparation method of the solid extract a and the solid extract B is: after the deionized water is heated to 30 ℃, na is slowly added 2 CO 3 And NaHCO 3 Or slowly add CH 3 COOH, stirring thoroughly until completely dissolved.
As a further preferable mode of the above technical scheme, in S4, the third extraction of the concentrated extract liquid includes a third liquid-liquid extraction operation, the concentrated extract liquid is subjected to a first liquid-liquid extraction by using an extraction solvent A1, and after the extraction is completed, the concentrated extract liquid is stood for delamination; taking a heavy phase obtained by the first liquid-liquid extraction, adopting an extraction solvent B2 for the second liquid-liquid extraction, and standing for layering after the extraction is completed; taking a heavy phase obtained by the second liquid-liquid extraction, adopting an extraction solvent C3 to perform the third liquid-liquid extraction, standing and layering after the extraction is completed, and obtaining a solvent phase positioned at the lower layer and an effective component phase positioned at the upper layer; wherein the extraction solvent A1 comprises C 5 H 12 、C 6 H 14 And C 7 H 16 (petroleum ether); the extraction solvent B2 comprises C 4 H 8 O 2 (B)Ethyl acid ester); the extraction solvent C3 comprises C 4 H 10 O (n-butanol). When the concentrated extract is subjected to refined extraction and solvent separation, the technical scheme adopts three different extraction solution extraction separation modes, wherein the extraction mode of raffinate phase is adopted for twice extraction, and the extraction mode of extract phase is adopted for once extraction, so that the impurity separation precision of the effective components is obviously improved, and the content of the effective components in the finished product is improved by more than 100 times by measuring the finished product by adopting a high performance liquid chromatograph.
As a further preferable mode of the technical scheme, the temperature of the three liquid-liquid extraction operations is 27-33 ℃, the extraction stirring time is 1h, and the addition amounts of the extraction solvent A1, the extraction solvent B2 and the extraction solvent C3 are 1.5 times of the mass of the semen zizyphi spinosae particles.
In a further preferred embodiment of the present invention, the active ingredient phase is subjected to molecular distillation at an evaporation temperature of 57 to 63℃and a vacuum degree of 2 to 3Pa.
As a further preferable aspect of the above technical solution, in S2, the filter residue B is pressed to be dried and dehydrated, and then used as a biofuel for a biomass boiler.
Based on the same technical conception, the invention also provides extraction equipment of the effective components of the spina date seeds, which comprises a solid-liquid extraction system, an acid-base regulating device, a first molecular distillation device, a liquid-liquid extraction system and a second molecular distillation device;
the solid-liquid extraction system comprises a first solid-liquid extraction device, a first filtering device, a first filtrate temporary storage device, a second solid-liquid extraction device, a second filtering device and a second filtrate temporary storage device; the material outlet of the first solid-liquid extraction component is communicated with the material inlet of the first filtering device, and the liquid outlet of the first filtering device is communicated with the inlet of the first filtrate temporary storage device; the material outlet of the second solid-liquid extraction component is communicated with the material inlet of the second filtering device, and the liquid outlet of the second filtering device is communicated with the inlet of the second filtrate temporary storage device; the outlet of the first filtrate temporary storage device and the outlet of the second filtrate temporary storage device are communicated with the inlet of the acid-base regulating device;
the inlet of the precise filtering device is communicated with the outlet of the acid-base regulating device, the liquid outlet of the precise filtering device is communicated with the inlet of the first molecular distillation device, the first molecular distillation device and the second molecular distillation device are respectively provided with a light component outlet and a heavy component outlet, the heavy component outlet of the first molecular distillation device is communicated with the inlet of the liquid-liquid extraction system, and the outlet of the liquid-liquid extraction system is communicated with the inlet of the second molecular distillation device.
As a further preferable mode of the above technical scheme, the liquid-liquid extraction system includes a first liquid-liquid extraction device, a first liquid-liquid extraction temporary storage device, a second liquid-liquid extraction temporary storage device, a third liquid-liquid extraction device and a third liquid-liquid extraction temporary storage device; the first liquid-liquid extraction device, the second liquid-liquid extraction device and the third liquid-liquid extraction device are provided with a liquid inlet and an extraction solvent inlet; the outlet of the first liquid-liquid extraction device is respectively communicated with the inlet of the first liquid-liquid extraction temporary storage device and the liquid inlet of the second liquid-liquid extraction device, the outlet of the second liquid-liquid extraction device is respectively communicated with the inlet of the second liquid-liquid extraction temporary storage device and the liquid inlet of the third liquid-liquid extraction device, and the outlet of the third liquid-liquid extraction device is respectively communicated with the inlet of the third liquid-liquid extraction temporary storage device and the inlet of the second molecular distillation device.
As a further preferable mode of the technical scheme, the systems and the devices in the extraction equipment are connected through closed pipelines.
Compared with the prior art, the invention has the advantages that:
(1) The extraction process has high production efficiency, good extraction effect and high impurity separation precision, so that the finally obtained finished product has good quality performance, the contents of the active ingredients of the spinosad a, the spinosad b and the spinosad in the product are high, the reaction condition in the extraction process is mild, the production cost is low, the generated waste residue can be recycled in a biomass boiler, and the method is environment-friendly, can be widely used for refining and automatic continuous production operation of various spinosa kernels, has no selection limitation on raw materials, and is suitable for large-scale industrial production;
(2) The extraction equipment provided by the invention has the advantages of simple structure and low manufacturing cost, all parts in the equipment are connected by adopting the totally-enclosed pipeline, the environment is friendly, the degree of automation is high, the complicated degree of production operation and the labor cost are reduced, and the extraction equipment is suitable for automatic continuous production operation of extracting and refining effective substances of various spina date seeds.
Drawings
Fig. 1 is a schematic diagram of the structure of an extraction apparatus for active ingredients of spina date seeds of example 2.
Legend description:
1. a No. 1 solid-liquid extraction kettle; 2. a No. 2 solid-liquid extraction kettle; 3. a primary kernel core filter; 4. a secondary kernel core filter; 5. a primary filtrate temporary storage tank; 6. a secondary filtrate temporary storage tank; 7. acid-base balance stirring kettle; 8. a precision filtration pump; 9. a precision filter; 10. a first-stage molecular distillation column; 11. an extraction solvent inlet; 12. a secondary liquid-liquid extraction kettle; 13. a secondary liquid-liquid extraction temporary storage tank; 14. a third liquid-liquid extraction kettle; 15. a material pump; 16. a light component outlet; 17. a temporary storage tank for three liquid-liquid extraction; 18. four times of back extraction kettles; 19. a four-time back extraction heavy phase temporary storage tank; 20. a light phase temporary storage tank for four times of back extraction; 21. a second-stage molecular distillation column; 22. heavy component outlet.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
the extraction process of the effective components of the spina date seeds comprises the following steps of:
s1, preparing a solid extract A and a solid extract B according to main components and weight of the main components of the spine date seed core to be planted and extracted:
through detection, the content of saponin a in the wild jujube seed raw material is 0.033%, the content of wild jujube seed saponin B is 0.028%, the content of spinosin is 0.053%, and the formula proportion of the agent A and the agent B is further verified according to the detection result; after determining the optimal dosage of the solid extract A and the solid extract B in a laboratory, determining the mixing proportion of the solid extract A and the solid extract B through a small sample test of the spina date seed raw material;
the preparation method of the solid extract A comprises the following steps: 1500kg of deionized water was warmed to 30℃and 5kg of Na was slowly added 2 CO 3 And 1kg of CH 3 COOH, stirring thoroughly until completely dissolved;
the preparation method of the solid extract B comprises the following steps: 1500kg of deionized water was warmed to 30℃and 6kg of NaHCO was slowly added 3 Stirring was sufficient until complete dissolution.
S2, crushing 1000kg of wild jujube seed raw materials to a particle size of about 10-20 meshes, adding solid extract A into crushed wild jujube seed core particles, fully stirring, slowly heating to 40+/-3 ℃ for extraction, preserving heat, stirring for 5 hours, extracting, and filtering to obtain filter residue A and filtrate A.
S3, adding a solid extract B into the filter residue A after the filter residue A is pressed to be dry, fully stirring, slowly heating to 40+/-3 ℃ for extraction, preserving heat and stirring for 5 hours, and filtering to obtain a filter residue B and a filtrate B; and the filter residue B is pressed to be dried and then used as a biofuel for a biomass boiler.
S4, mixing the filtrate A and the filtrate B to obtain a mixed solution, controlling the flow of the filtrate A and the flow of the filtrate B to adjust the pH value of the mixed solution to 6.5-7, and then performing precise filtration on the mixed solution to remove floccule impurities generated in the solid-liquid extraction process, thereby obtaining clear solid-liquid extraction liquid.
S5, carrying out molecular distillation on the solid-liquid extract, wherein in the distillation process, the evaporation temperature is 60+/-3 ℃, the vacuum degree is controlled to be 2 Pa-3 Pa, and when the flow ratio of the light component to the heavy component reaches 2: and 1, collecting heavy components to obtain concentrated extract, and reusing light components.
S6, performing primary liquid-liquid extraction on the concentrated extract by adopting an extraction solvent A1, controlling the temperature to be 30+/-3 ℃, fully stirring for 1 hour, and then performing extraction, standing and layering, wherein the extraction solvent A1 is C 5 H 12 、C 6 H 14 And C 7 H 16 The addition amount of the mixed solvent is 1.5 times of the weight of the spina date seeds; taking the heavy phase obtained by the first liquid-liquid extraction, adopting the extraction solvent B2 to carry out the second liquid-liquid extraction (the light phase can be repeatedly usedWith) the temperature is controlled at 30+/-3 ℃, the extraction is completed after fully stirring for 1 hour, the mixture is stood for layering, and the extraction solvent B2 is C 4 H 8 O 2 The addition amount is 1.5 times of the weight of the spina date seed; taking the heavy phase obtained by the second liquid-liquid extraction, adopting the extraction solvent C3 to perform the third liquid-liquid extraction (the light phase can be repeatedly used), controlling the temperature to be 30+/-3 ℃, fully stirring for 1 hour, completing the extraction, standing and layering to obtain a solvent phase positioned at the lower layer and an effective component phase positioned at the upper layer, wherein the extraction solvent C3 is C 4 H 10 The adding amount of O is 1.5 times of the weight of the spina date seeds; the content of the effective components of the wild jujube seeds in the detected solvent phase is lower than 0.001%, and the wild jujube seeds can be used as sewage for treatment.
S7, carrying out molecular distillation on the active ingredient phase, wherein in the distillation process, the evaporation temperature is 40+/-3 ℃, the vacuum degree is controlled at 2 Pa-3 Pa, when the flow ratio of the light component to the heavy component reaches 20:1, the heavy component is taken to obtain the active ingredient of the spina date seed, the weight of the active ingredient of the spina date seed is 8.32kg, the content of the spina date seed saponin a in the active ingredient of the spina date seed is 3.8%, the content of the spina date seed saponin b is 2.63%, the content of the spinosin is 6.2%, and the weight of the light component is 1390kg.
Example 2:
as shown in fig. 1, the extraction apparatus for the effective components of the semen Ziziphi Spinosae of this embodiment includes a solid-liquid extraction system (including a first solid-liquid extraction device, a first filtration device, a first filtrate temporary storage device, a second solid-liquid extraction device, a second filtration device, and a second filtrate temporary storage device), an acid-base adjustment device, a precise filtration device, a first molecular distillation device, a liquid-liquid extraction system (including a first liquid-liquid extraction device, a first liquid-liquid extraction temporary storage device, a second liquid-liquid extraction temporary storage device, a third liquid-liquid extraction device, and a third liquid-liquid extraction temporary storage device) and a second molecular distillation device.
In this embodiment, the first solid-liquid extraction device is a number 1 solid-liquid extraction kettle 1, the first filtration device is a primary kernel filter 3, the first filtrate temporary storage device is a primary filtrate temporary storage tank 5, the second solid-liquid extraction device is a number 2 solid-liquid extraction kettle 2, the second filtration device is a secondary kernel filter 4, the second filtrate temporary storage device is a secondary filtrate temporary storage tank 6, the acid-base adjusting device is an acid-base balance stirring kettle 7, the precise filtration device is a precise filter 9, the first molecular distillation device is a primary molecular distillation column 10, the first liquid-liquid extraction device is a secondary liquid-liquid extraction kettle 12, the first liquid-liquid extraction temporary storage device is a secondary liquid-liquid extraction temporary storage tank 13, the second liquid-liquid extraction device is a tertiary liquid-liquid extraction kettle 14, the second liquid-liquid extraction temporary storage device is a tertiary liquid-liquid extraction temporary storage tank 17, the third liquid-liquid extraction device is a quaternary stripping kettle 18, the third liquid-liquid extraction device comprises a quaternary stripping heavy phase temporary storage tank 19 and a quaternary stripping light phase temporary storage tank 20, the second molecular device is a secondary molecular distillation column 21, and pipelines are connected by adopting pipelines between the temporary storage columns.
The material outlet at the lower part of the No. 1 solid-liquid extraction kettle 1 is connected with the inlet of the primary kernel-core filter 3 through a pipeline, and the liquid outlet at the lower part of the primary kernel-core filter 3 is connected with the inlet of the primary filtrate temporary storage tank 5; the material outlet at the lower part of the No. 2 solid-liquid extraction kettle 2 is also connected with the inlet of the secondary kernel-core filter 4 through a pipeline, and the liquid outlet at the lower part of the secondary kernel-core filter 4 is connected with the inlet of the secondary filtrate temporary storage tank 6. The outlet of the lower part of the primary filtrate temporary storage tank 5 and the outlet of the lower part of the secondary filtrate temporary storage tank 6 are connected in parallel with the inlet of the acid-base balance stirring kettle 7 by pipelines; the outlet of the lower part of the acid-base balance stirring kettle 7 is connected with the inlet of a precise filter 9 through a precise filter pump 8 and a pipeline, the outlet of the precise filter 9 is connected with the upper inlet of a primary molecular distillation column 10, the primary molecular distillation column 10 is provided with a heavy component outlet 22 and a light component outlet 16, and the heavy component outlet 22 is connected with an extraction solvent inlet 11 on a secondary liquid-liquid extraction kettle 12. The outlet of the lower part of the secondary liquid-liquid extraction kettle 12 is respectively connected with the extraction solvent inlets 11 of the secondary liquid-liquid extraction temporary storage tank 13 and the tertiary liquid-liquid extraction kettle 14, and the outlet of the lower part of the tertiary liquid-liquid extraction kettle 14 is respectively connected with the extraction solvent inlets 11 of the tertiary liquid-liquid extraction temporary storage tank 17 and the quaternary stripping kettle 18 through a material pump 15 and a pipeline. The outlet of the lower part of the four-time stripping kettle 18 is connected with the inlets of a four-time stripping heavy phase temporary storage tank 19 and a four-time stripping light phase temporary storage tank 20 respectively; the outlet of the lower part of the four times back extraction light phase temporary storage tank 20 is connected with the inlet of the secondary molecular distillation column 21; the lower part of the secondary molecular distillation column 21 is provided with a heavy component outlet 22 and a light component outlet 16.
It should be noted that the above-mentioned devices are of course equipped with corresponding piping valves, flow meters, thermometers, etc. at each unit-to-unit connection, and are omitted in the embodiments for simplicity of description.
The extraction equipment for the effective components of the spina date seeds is adopted to extract the effective components of the spina date seeds, and comprises the following steps:
s1, preparing a solid extract A and a solid extract B according to main components and weight of the to-be-planted and extracted semen Ziziphi Spinosae kernel;
the preparation method of the solid extract A comprises the following steps: firstly, deionized water accounting for 150 percent of the weight of the core of the wild jujube is pumped into a No. 1 solid-liquid extraction kettle 1, a steam heating piece jacket is used for heating to 30 ℃, and then Na accounting for 0.5 percent of the weight of the core of the wild jujube is slowly added 2 CO 3 And 0.1% NaHCO 3 Stirring thoroughly until complete;
the preparation method of the solid extract B comprises the following steps: firstly, deionized water accounting for 150 percent of the weight of the core of the wild jujube is pumped into a No. 2 solid-liquid extraction kettle 2, a steam heating piece jacket is used for heating to 30 ℃, and then CH accounting for 0.5 percent of the weight of the core of the wild jujube is slowly added 3 COOH), stirring thoroughly until complete.
S2, putting granular semen Ziziphi Spinosae cores (particle size is about 10-20 meshes) into a No. 1 solid-liquid extraction kettle 1 filled with solid extract A, fully stirring and slowly heating to 40+ -3 ℃ for extraction, preserving heat and stirring for 5 hours, then extracting, filtering the materials in a primary kernel core filter 3 to obtain filter residues A and filtrate A, and putting the filtrate A into a primary filtrate temporary storage tank 5.
S3, pressing and drying filter residue A, putting the filter residue A into a No. 2 solid-liquid extraction kettle 2 filled with solid extract B, fully stirring and slowly heating to 40+/-3 ℃ for extraction, preserving heat and stirring for 5 hours, then extracting, filtering the material by a secondary kernel-kernel filter 4 to obtain filter residue B and filtrate B, putting the filtrate B into a secondary filtrate temporary storage tank 6 for standby, and pressing and drying the filter residue B to be used as biological fuel for a biomass boiler.
S4, slowly placing the filtrate in the primary filtrate temporary storage tank 5 and the secondary filtrate temporary storage tank 6 into the acid-base balance stirring kettle 7, starting stirring while discharging, detecting the pH value of the mixed solution when the liquid level in the acid-base balance stirring kettle 7 is half, and controlling the pH value of the mixed solution in the acid-base balance stirring kettle 7 by adjusting the liquid discharge flow of the primary filtrate temporary storage tank 5 and the secondary filtrate temporary storage tank 6 until the pH value of the mixed solution in the acid-base balance stirring kettle 7 is 6.5-7; the mixed solution in the acid-base balance stirring kettle 7 is pumped into a precise filter 9 through a precise filter pump 8 for precise filtration, floccule impurities generated in the solid-liquid extraction process are removed, clear solid-liquid extraction liquid is obtained, and a filter screen of the precise filter 9 needs to be cleaned and replaced regularly.
S5, introducing the solid-liquid extract into the primary molecular distillation column 10 for molecular distillation, wherein in the distillation process, the evaporation temperature is 60+/-3 ℃, the vacuum degree is controlled to be 2 Pa-3 Pa, the feeding quantity of the primary molecular distillation column 10 is slowly regulated, the flow meters of two outlets of the primary molecular distillation column 10 are observed, and when the flow ratio of the light component outlet to the heavy component outlet reaches 2: and 1, collecting heavy components to obtain concentrated extract, and reusing light components.
S6, placing the concentrated extract into a secondary liquid-liquid extraction kettle 12, simultaneously placing an extraction solvent A1 with the weight which is 1.5 times of the core weight of the spina date seeds into the secondary liquid-liquid extraction kettle 12 through an extraction solvent inlet 11, extracting by adopting the extraction solvent A1, controlling the temperature to be 30+/-3 ℃, fully stirring for 1 hour, and then completing extraction, standing and layering, wherein the extraction solvent A1 is C 5 H 12 、C 6 H 14 And C 7 H 16 Is a mixed solvent of (a) and (b); placing the heavy phase of the extraction liquid in the secondary liquid-liquid extraction kettle 12 in a static layering manner into a tertiary liquid-liquid extraction kettle 14, placing the light phase into a secondary liquid-liquid extraction temporary storage tank 13 (which can be recycled after recovery), simultaneously placing an extraction solvent B2 with the weight of 1.5 times of the core weight of the spina date seeds into the tertiary liquid-liquid extraction kettle 14 through an extraction solvent inlet 11, extracting by adopting the extraction solvent B2, controlling the temperature to be 30+/-3 ℃, fully stirring for 1 hour, and then completing the extraction, standing and layering, wherein the extraction solvent B2 is C 4 H 8 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The heavy phase of the extraction liquid which is still layered in the third liquid-liquid extraction kettle 14 is placed in a fourth back extraction kettle 18, and the light phase is placed in a third liquid-liquid extraction temporary storage tank 17 (which can be repeated after being recovered)Utilizing), simultaneously adding an extraction solvent C3 with the weight 1.5 times of the core weight of the wild jujube into a four-time back extraction kettle 18 through an extraction solvent inlet 11, extracting by adopting the extraction solvent C3, controlling the temperature to be 30+/-3 ℃, fully stirring for 1 hour, then completing the extraction, standing for layering, wherein the extraction solvent C3 is C 4 H 10 O; the light phase (effective component phase) of the extraction liquid which is still layered in the four times back extraction kettle 18 is put into a four-stage back extraction light phase temporary storage tank, the heavy phase is put into a four-stage back extraction heavy phase temporary storage tank, the effective substance content of the liquid in the four-stage back extraction heavy phase temporary storage tank is detected, when the effective component content is less than 0.001%, sewage treatment can be beaten, and when the effective component content is more than 0.001%, the second or third back extraction is needed until the effective component content is less than 0.001%.
S7, pumping the active ingredient phase in the four-stage stripping light phase temporary storage tank into a secondary molecular distillation column 21 for molecular distillation, wherein the evaporation temperature is 40+/-3 ℃ in the distillation process, the vacuum degree is controlled between 2Pa and 3Pa, the feeding quantity of the secondary molecular distillation column 21 is slowly regulated, the flow meters at two outlets of the secondary molecular distillation column 21 are observed, and when the flow ratio of the light ingredient outlet to the heavy ingredient outlet reaches 20:1, taking the heavy component to obtain the effective component of the spina date seed, and repeatedly using the light component.
The above description is merely a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above examples. Modifications and variations which would be obvious to those skilled in the art without departing from the spirit of the invention are also considered to be within the scope of the invention.
Claims (10)
1. An extraction process of effective components of spina date seeds is characterized by comprising the following steps:
s1, adding a solid extract A into the semen zizyphi spinosae particles for extraction, and filtering after the extraction is finished to obtain filter residue A and filtrate A; the solid extract A is Na 2 CO 3 And NaHCO 3 Na in the solid extract a 2 CO 3 And NaHCO 3 The mass of the semen zizyphi spinosae particles is 0.001 to 2 percent and 0.001 to 2 percent of the mass of the semen zizyphi spinosae particles respectively;
s2, adding a solid extract B into the filter residue A for extraction, and filtering after the extraction is finished to obtain filter residue B and filtrate B; the solid extract B is CH 3 COOH solution, CH in said solid extract B 3 The mass of COOH is 0.001% -2% of the mass of the filter residue A;
s3, mixing the filtrate A and the filtrate B, regulating the pH value to 6.5-7 to obtain a mixed solution, performing precise filtration on the mixed solution, and obtaining heavy components through molecular distillation to obtain a concentrated extract;
s4, extracting the concentrated extract for three times, separating to obtain a solvent phase and an effective component phase, and carrying out molecular distillation on the effective component phase to obtain a heavy component, thus obtaining the effective component of the spina date seed.
2. The process for extracting active ingredients from semen Ziziphi Spinosae of claim 1, wherein in S1, the extraction temperature is 37-43deg.C, the extraction time is 5h, and the addition amount of solid extractant A is 1.5 times of the mass of semen Ziziphi Spinosae granule.
3. The extraction process of the active ingredients of the spina date seeds according to claim 1, wherein in the step S2, the extraction operation temperature is 37-43 ℃, the extraction time is 5 hours, and the addition amount of the solid extractant B is 150% of the mass of the filter residue A.
4. The process for extracting active ingredients from semen zizyphi spinosae according to claim 1, wherein the preparation method of the solid extract a and the solid extract B is as follows: after the deionized water is heated to 30 ℃, na is slowly added 2 CO 3 And NaHCO 3 Or slowly add CH 3 COOH, stirring thoroughly until completely dissolved.
5. The process for extracting active ingredients from semen Ziziphi Spinosae as claimed in claim 1, wherein in S4, three times of extraction of concentrated extract comprises three times of liquid-liquid extraction, wherein the concentrated extract is subjected to first liquid-liquid extraction with extraction solvent A1Standing and layering after extraction is completed; taking a heavy phase obtained by the first liquid-liquid extraction, adopting an extraction solvent B2 for the second liquid-liquid extraction, and standing for layering after the extraction is completed; taking a heavy phase obtained by the second liquid-liquid extraction, adopting an extraction solvent C3 to perform the third liquid-liquid extraction, standing and layering after the extraction is completed, and obtaining a solvent phase positioned at the lower layer and an effective component phase positioned at the upper layer; wherein the extraction solvent A1 comprises C 5 H 12 、C 6 H 14 And C 7 H 16 The method comprises the steps of carrying out a first treatment on the surface of the The extraction solvent B2 comprises C 4 H 8 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The extraction solvent C3 comprises C 4 H 10 O; the temperature of the three liquid-liquid extraction operations is 27-33 ℃, the extraction stirring time is 1h, and the addition amounts of the extraction solvent A1, the extraction solvent B2 and the extraction solvent C3 are about 1.5 times of the mass of the semen zizyphi spinosae particles.
6. The process for extracting active ingredients from semen Ziziphi Spinosae according to claim 5, wherein in S4, the evaporation temperature is 57-63deg.C and vacuum degree is 2-3 Pa when molecular distillation is performed on the active ingredient phase.
7. The process for extracting active ingredients from semen Ziziphi Spinosae according to any one of claims 1-6, wherein in S2, the residue B is dried and dehydrated and used as a biofuel for biomass boiler.
8. The extraction equipment of the effective components of the spina date seeds is characterized by comprising a solid-liquid extraction system, an acid-base regulating device, a precise filtering device, a first molecular distillation device, a liquid-liquid extraction system and a second molecular distillation device;
the solid-liquid extraction system comprises a first solid-liquid extraction device, a first filtering device, a first filtrate temporary storage device, a second solid-liquid extraction device, a second filtering device and a second filtrate temporary storage device; the material outlet of the first solid-liquid extraction component is communicated with the material inlet of the first filtering device, and the liquid outlet of the first filtering device is communicated with the inlet of the first filtrate temporary storage device; the material outlet of the second solid-liquid extraction component is communicated with the material inlet of the second filtering device, and the liquid outlet of the second filtering device is communicated with the inlet of the second filtrate temporary storage device; the outlet of the first filtrate temporary storage device and the outlet of the second filtrate temporary storage device are communicated with the inlet of the acid-base regulating device; the inlet of the precise filtering device is communicated with the outlet of the acid-base regulating device, the liquid outlet of the precise filtering device is communicated with the inlet of the first molecular distillation device, the first molecular distillation device and the second molecular distillation device are respectively provided with a light component outlet and a heavy component outlet, the heavy component outlet of the first molecular distillation device is communicated with the inlet of the liquid-liquid extraction system, and the outlet of the liquid-liquid extraction system is communicated with the inlet of the second molecular distillation device.
9. The apparatus for extracting effective components from semen Ziziphi Spinosae of claim 9, wherein the liquid-liquid extraction system comprises a first liquid-liquid extraction device, a first liquid-liquid extraction temporary storage device, a second liquid-liquid extraction temporary storage device, a third liquid-liquid extraction device, and a third liquid-liquid extraction temporary storage device; the first liquid-liquid extraction device, the second liquid-liquid extraction device and the third liquid-liquid extraction device are provided with a liquid inlet and an extraction solvent inlet; the outlet of the first liquid-liquid extraction device is respectively communicated with the inlet of the first liquid-liquid extraction temporary storage device and the liquid inlet of the second liquid-liquid extraction device, the outlet of the second liquid-liquid extraction device is respectively communicated with the inlet of the second liquid-liquid extraction temporary storage device and the liquid inlet of the third liquid-liquid extraction device, and the outlet of the third liquid-liquid extraction device is respectively communicated with the inlet of the third liquid-liquid extraction temporary storage device and the inlet of the second molecular distillation device.
10. The apparatus for extracting effective components from semen Ziziphi Spinosae according to any one of claims 8-9, wherein the systems and devices are connected by closed pipeline.
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