CN111111256A - Method and device for purifying plant water extracting solution - Google Patents
Method and device for purifying plant water extracting solution Download PDFInfo
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- CN111111256A CN111111256A CN202010008794.1A CN202010008794A CN111111256A CN 111111256 A CN111111256 A CN 111111256A CN 202010008794 A CN202010008794 A CN 202010008794A CN 111111256 A CN111111256 A CN 111111256A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention provides a purification method of plant water extract, which comprises the steps of shredding plant raw materials to obtain filamentous plant fragments; extracting filamentous plant fragments with water containing macromolecular substance dissolution inhibitor, and filtering to remove residue to obtain water extractive solution; then, precipitating macromolecular impurity components with acidic groups in the obtained water extract by using an alkaline precipitator; then, using a composite polymer flocculating agent to enable macromolecular impurity components with basic groups in the water extracting solution to carry out flocculating reaction, and neutralizing the basic precipitating agent to form flocs; and finally, filtering the water extract after the flocculation reaction to obtain the purified plant water extract. The invention also provides a device for realizing the method. The plant water extract obtained by the method has improved light transmittance and useful substance yield.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a purification method, in particular to a method and a device for purifying a plant water extracting solution.
Background
The extraction of water-soluble useful components from plants and their purification and separation to produce a natural product is a method commonly used in the food and pharmaceutical fields, particularly the production of various natural sugar products.
The traditional water extract purification method which is widely used at present is that the plant raw materials are firstly crushed, then the raw material powder is soaked in water, and the water extract is obtained by preliminary slag-water separation; adding a large amount of lime, iron salt and other agents into the water extract, generating floccules from macromolecular impurities such as protein, cellulose and the like through salting out and precipitation adsorption, and finally filtering and separating the floccules to obtain the purified water extract.
The traditional water extract purification production method generates a large amount of solid waste substances and wastewater containing high-concentration soluble salt and high hardness, causes great environmental protection pressure, and also influences the reuse and reuse of water in the process; in addition, the method causes that the extract contains a large amount of divalent and trivalent ions, which affects the production steps of resin adsorption, membrane separation, crystallization and the like of the subsequent separation and purification products (water-soluble useful components), and causes the problems of reduced resin adsorption capacity and regeneration rate, membrane material blockage failure and service life reduction, difficult crystallization operation and the like. Therefore, the traditional plant water extract purification production link has high cost and serious pollution.
However, as the raw materials such as lime, ferrous sulfate, ferrous chloride and the like are cheap and the production steps are simple to control, the traditional water extraction liquid purification process technology is still largely used in production.
Disclosure of Invention
The invention aims to solve the technical problems that a purification method and a purification device for plant water extract are provided, and the purification method and the purification device for plant water extract aim to solve the technical problems that a large amount of solid waste substances and wastewater containing high-concentration soluble salt and high hardness are generated by the purification method in the prior art, so that great environmental protection pressure is caused, and the application and recycling of process water are influenced.
The invention provides a purification method of a plant water extracting solution, which comprises the following steps:
step 1: shredding plant material to obtain filamentous plant pieces;
step 2: extracting filamentous plant fragments obtained in step 1 with water containing dissolution inhibitor of macromolecular substances, and filtering to remove residue to obtain water extractive solution, wherein the temperature of water is 10-100 deg.C;
and step 3: firstly, precipitating macromolecular impurity components with acidic groups in the water extracting solution obtained in the step 2 by using an alkaline precipitator; then, using a composite polymer flocculating agent to enable macromolecular impurity components with basic groups in the water extracting solution to carry out flocculating reaction, and neutralizing the basic precipitating agent to form flocs;
and 4, step 4: and (3) filtering the water extracting solution after the flocculation reaction in the step (3) to obtain a purified plant water extracting solution.
Further, in the step 1, the cutting width of the plant is controlled to be 0.01-10% of the maximum length of the root, stem and leaf of the plant.
Further, in the step 1, the thickness of the cut plant is controlled to be 0.1 to 10 times of the width of the cut plant.
Further, in the step 2, the dissolution inhibitor for macromolecular substances is one or a mixture of two or more of acids, bases, alcohols, ketones, divalent or higher metal salts, and halogenated alkyl compounds.
Further, in the step 3, the alkaline precipitant is at least one of an alkaline compound containing a divalent or trivalent transition metal, an alkaline compound containing a boron group element, or an alkaline compound containing a carbon group element.
Further, in the step 3, the composite polymer flocculant is a compound aqueous solution of one or more than two organic polymer polymers containing acidic groups and an inorganic polymer, the organic polymer is polyacrylamide, polymaleic acid or ionized starch, and the inorganic polymer is polyaluminium chloride, polyaluminium sulfate, polyferric chloride or polyferric sulfate.
Furthermore, in the compound aqueous solution, the mass percentage concentration of the solute is 1-10%, and the mass ratio of the organic high molecular polymer to the inorganic high molecular polymer is 1: 1000-1: 100.
The invention also provides a plant water extracting solution purifying production device for realizing the method, which comprises a shredder, wherein the shredder is connected with a soaking extractor, the soaking extractor is connected with a residue filter, the residue filter is connected with a flocculation reactor, the flocculation reactor is respectively connected with an alkaline precipitator dosing machine and a composite polymer flocculation precipitator dosing machine, and the flocculation reactor is also connected with an extracting solution filtering device.
Specifically, the liquid medicine output by the composite polymer flocculating agent dosing machine and dilution water are quickly mixed in a pipeline according to a proportion and then enter a flocculating reactor.
Preferably, in the step 1, the length of the plant shreds is controlled to meet the requirements of a hydraulic conveying machine.
Specifically, the plant extract may be water extract containing glycogen such as stevioside.
The invention adopts the shredder to crush the plant raw materials, so as to reduce the damage or exposure of macromolecular impurity components in the plants, inhibit the dissolution of the substances, have sufficient wall breaking effect and cannot reduce the dissolution rate of useful components. The extraction liquid obtained by the method of the invention has improved light transmittance and useful substance yield.
The impurity elution inhibitor of the present invention can reduce the solubility of macromolecular impurities (proteins, cellulose, gums, starches, etc.) in water, but does not substantially affect the elution of useful components (e.g., small molecular substances such as various saccharides).
Compared with the prior art, the invention has remarkable technical progress. The invention can inhibit the dissolution of macromolecular impurities in the water extraction step of plants and remove the dissolved macromolecular impurities in the extracting solution so as to facilitate the subsequent production of separation and purification of useful components in the water extracting solution, wherein the macromolecular impurities naturally existing in the plants comprise: protein, cellulose, pectin, starch, pigment, etc. Compared with the similar plant water extract purifying device and system, the plant water extract purifying device and system have the advantages that the produced residue amount is less, the process water is used for multiple times, so that a large amount of water is saved, the sewage treatment difficulty is reduced, the treatment cost is reduced, the obtained water extract has low impurity content, the yield of useful substances is improved, the service life of materials such as resin, filter membranes and the like in the subsequent production device and system is long, and the production stability is good.
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FIG. 1 is a schematic process diagram of the method for purifying a plant water extract according to the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teachings of the present invention, and such equivalents also fall within the scope of the invention as defined by the appended claims.
Example 1
The invention provides a device for purifying plant water extracting solution, which comprises a shredder 1, wherein the shredder 1 is connected with a soaking extractor 2, the soaking extractor 2 is connected with a residue filter 3, the residue filter 3 is connected with a flocculation reactor 4, the flocculation reactor 4 is respectively connected with an alkaline precipitator dosing machine 6 and a composite polymer flocculation agent dosing machine 7, and the flocculation reactor 4 is also connected with an extracting solution filtering device 5.
The technological process of the present invention includes the steps of shredding plant, soaking and extracting plant, sieving residue, depositing extracted liquid, adding alkali precipitant, adding composite polymer flocculant, filtering extracted liquid and clarifying.
The plant shredding process is used for crushing the plant, the plant soaking extractor 2 is carried to the ejection of compact of plant shredder 1, the residue screen filter 3 is carried to the ejection of compact that the plant soaked extractor 2, extract flocculation and precipitation reactor 4 is carried to the filtrating of residue screen filter 3, alkaline precipitant dosing machine 6 and compound polymer flocculation and precipitation dosing machine 7 are successively with the agent ration pour into extract flocculation and precipitation reactor 4, extract filter equipment 5 is carried to the ejection of compact of extract flocculation and precipitation reactor 4, extract filter equipment 5's purification extract gets into follow-up production step.
Example 2
A method for purifying plant water extract adopts a plant water extract purification production device in figure 1, and comprises the following steps:
step 1: adding 100kg of stevia leaf raw material into plant shredder 1, removing hard substances such as stone and metal before adding, and cutting into filaments with width of about 1mm, thickness of about 1mm and length of about 10mm to obtain filamentous stevia leaf fragments;
step 2: conveying filiform stevia rebaudiana leaf fragments to a plant soaking extractor 2, adding an inhibitor (calcium hydroxide 1kg) for preventing macromolecular substances from dissolving out into 2000kg of hot water (the water temperature is about 60 ℃), placing the mixture in the plant soaking extractor 2, carrying out countercurrent extraction on the filiform stevia rebaudiana leaf fragments for 60min by using the inhibitor, conveying the discharge material of the plant soaking extractor 2 to a residue screen filter 3 to filter out residues, and obtaining a primary water extracting solution of about 1950 kg;
and step 3: conveying the primary water extracting solution to an extracting solution flocculation and precipitation reactor 4, adding an alkaline precipitator (1 kg of sodium silicate) into 2000kg of the primary water extracting solution by using an alkaline precipitator dosing machine 6 to enable the pH value to reach 10, stirring for 10min, and precipitating macromolecular impurity components with acidic groups in the primary water extracting solution by using the alkaline precipitator; adding a composite polymer flocculating agent (1 kg of polymeric basic aluminum chloride and 0.1kg of ionized polyacrylamide) into the water extracting solution by using a composite polymer flocculating agent dosing machine 7, stirring for 10min, carrying out flocculating reaction on macromolecular impurity components with basic groups in the water extracting solution by using the composite polymer flocculating agent, and neutralizing the basic precipitating agent to form flocs;
and 4, step 4: and (3) conveying the discharged material of the extracting solution flocculation and precipitation reactor 4 to an extracting solution filtering device 5, and filtering the water extracting solution subjected to flocculation and precipitation reaction by using a filter cloth filtering device 5 to obtain about 1900kg of purified plant water extracting solution, wherein the light transmittance of the plant water extracting solution is 65 percent, and the stevioside yield is 95 percent.
Example 3
A method for purifying plant water extract adopts a plant water extract purification production device in figure 1, and comprises the following steps:
step 1: adding 100kg of stevia leaf raw material into plant shredder 1, removing hard substances such as stone and metal before adding, and cutting into filaments with width of about 2mm, thickness of about 1mm and length of about 10mm to obtain filamentous stevia leaf fragments;
step 2: conveying filiform stevia rebaudiana leaf fragments to a plant soaking extractor 2, adding an inhibitor (calcium hydroxide 1kg) for preventing macromolecular substances from dissolving out into 2000kg of hot water (the water temperature is about 60 ℃), placing the mixture in the plant soaking extractor 2, carrying out countercurrent extraction on the filiform stevia rebaudiana leaf fragments for 60min by using the inhibitor, conveying the discharge material of the plant soaking extractor 2 to a residue screen filter 3 to filter out residues, and obtaining a primary water extracting solution of about 1950 kg;
and step 3: conveying the primary water extracting solution to an extracting solution flocculation and precipitation reactor 4, adding an alkaline precipitator (1 kg of sodium silicate) into 2000kg of the primary water extracting solution by using an alkaline precipitator dosing machine 6 to enable the pH value to reach 11, stirring for 10min, and precipitating macromolecular impurity components with acidic groups in the primary water extracting solution by using the alkaline precipitator; adding a composite polymer flocculating agent into a water extracting solution (1 kg of polymeric basic aluminum chloride and 0.1kg of ionized polyacrylamide) by using a composite polymer flocculating agent adding machine 7 to ensure that the pH value reaches 7, stirring for 10min, carrying out flocculating reaction on macromolecular impurity components with alkaline groups in the water extracting solution by using the composite polymer flocculating agent, and neutralizing the alkaline precipitating agent to form flocs;
and 4, step 4: and (3) conveying the discharged material of the extracting solution flocculation and precipitation reactor 4 to an extracting solution filtering device 5, and filtering the water extracting solution subjected to flocculation and precipitation reaction by using a filter cloth filtering device 5 to obtain about 1900kg of purified plant water extracting solution, wherein the light transmittance is 75 percent, and the stevioside yield is 90 percent.
Example 4
A method for purifying plant water extract adopts a plant water extract purification production device in figure 1, and comprises the following steps:
step 1: adding 100kg of stevia leaf raw material into plant shredder 1, removing hard substances such as stone and metal before adding, and cutting into filaments with width of about 1mm, thickness of about 1mm and length of about 10mm to obtain filamentous stevia leaf fragments;
step 2: conveying filiform stevia rebaudiana leaf fragments to a plant soaking extractor 2, adding an inhibitor (calcium hydroxide 1kg) for preventing macromolecular substances from dissolving out into 2000kg of hot water (the water temperature is about 60 ℃), placing the mixture in the plant soaking extractor 2, carrying out countercurrent extraction on the filiform stevia rebaudiana leaf fragments for 60min by using the inhibitor, conveying the discharge material of the plant soaking extractor 2 to a residue screen filter 3 to filter out residues, and obtaining a primary water extracting solution of about 1950 kg;
and step 3: conveying the primary water extracting solution to an extracting solution flocculation and precipitation reactor 4, adding an alkaline precipitator (1 kg of sodium silicate) into 2000kg of the primary water extracting solution by using an alkaline precipitator dosing machine 6 to enable the pH value to reach 9, stirring for 10min, and precipitating macromolecular impurity components with acidic groups in the primary water extracting solution by using the alkaline precipitator; adding a composite polymer flocculating agent (1 kg of polymeric basic aluminum chloride and 0.1kg of ionized polyacrylamide) into a water extracting solution by using a composite polymer flocculating agent dosing machine 7 to enable the pH to reach 7, stirring for 10min, carrying out flocculating reaction on macromolecular impurity components with alkaline groups in the water extracting solution by using the composite polymer flocculating agent, and neutralizing the alkaline precipitator to form flocs;
and 4, step 4: and (3) conveying the discharged material of the extracting solution flocculation and precipitation reactor 4 to an extracting solution filtering device 5, and filtering the water extracting solution subjected to flocculation and precipitation reaction by using a filter cloth filtering device 5 to obtain about 1900kg of purified plant water extracting solution, wherein the light transmittance is 55 percent, and the stevioside yield is 90 percent.
The light transmittance in the above examples is measured by a spectrophotometer, a light wave with a wavelength of 420nm is used, the yield is measured by a saccharimeter for the concentration of stevioside in the extract, the total amount of stevioside in the extract is obtained, and the yield of the stevioside extraction step is calculated and obtained compared with the total amount of stevioside contained in the plant.
The plant shredder 1 of each of the above embodiments can control the shredding width.
In step 2 of the above embodiments, the amount and formulation of the dissolution inhibitor need to match the composition and content of macromolecular impurities such as protein, cellulose, pectin, starch, pigment, etc. in the plant material, and are usually determined by compatibility tests.
In the above embodiments, the production combination device and process for extracting stevioside from stevia rebaudiana leaves are taken as examples, but the method can be widely used for purifying water extract of other plants, and the specific step control parameters can be adjusted by referring to the embodiment of the invention.
By adopting the combined device, the efficiency improvement of inhibiting the dissolution of macromolecular impurities and removing dissolved macromolecular impurities in the extracting solution is realized in the purification production of the plant water extracting solution, and compared with the traditional technology, the combined device has better technical effect.
Claims (8)
1. A method for purifying plant water extract is characterized by comprising the following steps:
step 1: shredding plant material to obtain filamentous plant pieces;
step 2: extracting filamentous plant fragments obtained in step 1 with water containing dissolution inhibitor of macromolecular substances, and filtering to remove residue to obtain water extractive solution, wherein the temperature of water is 10-100 deg.C;
and step 3: firstly, precipitating macromolecular impurity components with acidic groups in the water extracting solution obtained in the step 2 by using an alkaline precipitator; then, using a composite polymer flocculating agent to enable macromolecular impurity components with basic groups in the water extracting solution to carry out flocculating reaction, and neutralizing the basic precipitating agent to form flocs;
and 4, step 4: and (3) filtering the water extracting solution after the flocculation reaction in the step (3) to obtain a purified plant water extracting solution.
2. The method for purifying plant water extract as claimed in claim 1, wherein in the step 1, the width of the plant shreds is controlled to 0.01-10% of the maximum length of the plant roots, stems and leaves.
3. The method for purifying a plant water extract according to claim 1, wherein in the step 1, the thickness of the cut plant thread is controlled to be 0.1 to 10 times the width of the cut plant thread.
4. The method according to claim 1, wherein the dissolution inhibitor for macromolecular substances in step 2 is one or a mixture of two or more of acids, bases, alcohols, ketones, divalent or higher metal salts, and halogenated alkyl compounds.
5. The method according to claim 1, wherein in the step 3, the basic precipitant is at least one of a basic compound containing a divalent or trivalent transition metal, a basic compound containing a boron group element, and a basic compound containing a carbon group element.
6. The method according to claim 1, wherein in the step 3, the composite polymer flocculant is a mixed aqueous solution of one or more organic polymers containing acidic groups and an inorganic polymer, the organic polymer is polyacrylamide, polymaleic acid or ionized starch, and the inorganic polymer is polyaluminium chloride, polyaluminium sulfate, polyferric chloride or polyferric sulfate.
7. The method for purifying a plant water extract according to claim 6, wherein the solute concentration in the compounded aqueous solution is 1 to 10% by mass, and the mass ratio of the organic high molecular polymer to the inorganic high molecular polymer is 1:1000 to 1: 100.
8. A plant water extract purification production device for realizing the method of claim 1, comprising a shredder, wherein the shredder is connected with a soaking extractor, the soaking extractor is connected with a residue filter, the residue filter is connected with a flocculation reactor, the flocculation reactor is respectively connected with an alkaline precipitator dosing machine and a composite polymer flocculation agent dosing machine, and the flocculation reactor is further connected with an extract filtering device.
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Application publication date: 20200508 |