CN110938103A - Method for extracting food-grade tannin from persimmons - Google Patents

Method for extracting food-grade tannin from persimmons Download PDF

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CN110938103A
CN110938103A CN201911389302.1A CN201911389302A CN110938103A CN 110938103 A CN110938103 A CN 110938103A CN 201911389302 A CN201911389302 A CN 201911389302A CN 110938103 A CN110938103 A CN 110938103A
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concentrate
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李森
张静传
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    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H13/00Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
    • C07H13/02Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
    • C07H13/08Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals directly attached to carbocyclic rings
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    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
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Abstract

A method for extracting food-grade tannin from persimmons comprises the following steps: (1) raw material treatment: soaking and cleaning non-yellow green persimmon in 35-45 deg.C warm water, sorting to remove impurities; (2) pulping: making the processed green persimmon into green persimmon pulp under vacuum; (3) centrifugal separation: centrifuging fructus kaki pulp, separating into filtrate and residue, concentrating the filtrate to obtain concentrate, and oven drying the residue for use; (4) drying: drying the concentrate; (5) milling: crushing the dried concentrate to obtain powder particles; (6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting propane, and stirring for reaction, wherein the weight-volume ratio of the powder particles to the propane is 1: 2; (7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin. The invention has the advantages of high production efficiency, high product purity, low cost, low energy consumption, no environmental pollution, energy conservation, environmental protection and great economic and social benefits.

Description

Method for extracting food-grade tannin from persimmons
Technical Field
The invention relates to a chemical industry, in particular to a method for extracting food-grade tannin from persimmons, which takes the persimmons as raw materials to prepare tannin (tannic acid).
Background
Tannin (tannic acid) is a widely used raw material in chemical industry, has wide application, and various methods for preparing tannin at present are disclosed, and a known process for extracting tannin from persimmon fruits by using distilled water is discussed (the national chemical industry institute of university of sovereign of soverns chemce/guangxi light industry-2010 (4) · -23-24), and the method comprises the steps of taking a certain amount of frozen persimmon fruits, stirring the frozen persimmon fruits by using a stirrer, adding a certain proportion of an extracting agent, homogenizing, heating and refluxing the frozen persimmon fruits in a constant-temperature water bath kettle, filtering filtrate, and determining the content after constant volume. Extracting a sample at 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃, heating and refluxing for extraction, repeating for 3 times, filtering to fix the volume, and determining the content of the tannic acid in the extracting solution, but in practice, the content of the tannic acid is obviously increased along with the increase of the temperature within the range of 40 ℃ to 60 ℃, the content of the tannic acid is reduced while continuously increasing the temperature, and the result is zero when the temperature reaches 80 ℃, 90 ℃ and 100 ℃, which indicates that the increase of the extraction temperature in a certain time is beneficial to the dissolution of the tannic acid, but the tannic acid is denatured when the temperature is too high, the extraction temperature is suitable at 40 ℃ to 70 ℃, and the extraction effect at 60 ℃ is the best.
An optimized extraction process discussion of persimmon tannin (Guaifeng Li Chunmei Hui Zhen Shibaoqin/Huazhong agriculture university food science and technology college// food science and technology-2007 (2) -133-. Ethanol, methanol and acetone are selected as extracting agents, and the ethanol is found to dissolve out more impurities in the extraction as the extracting agents, so that the filtration is difficult, the subsequent treatment of experiments is not facilitated, and the filtration effect of the methanol and the acetone is better.
The two methods for extracting persimmon tannin have the disadvantage that the temperature is selected when tannin is extracted by using an organic solvent or distilled water. If the temperature is too low, the solid content is reduced due to too low extraction speed; the temperature is too high, on one hand, the organic solvent is volatilized quickly and lost, and on the other hand, the proposed tannin is oxidized quickly by oxygen in the air, so that the purity and the color of the tannin are influenced.
Preparation of persimmon tannin and its antioxidant activity research (Kyoho Li Chunmei Xuyujuan Zhang Jie Julian Lianglian Hongliang/Huazhong agriculture university food science and technology college// agriculture engineering newspaper-2007 (5) — 241-245) discloses a preparation method of persimmon tannin, which comprises taking a certain amount of persimmon pulp, peeling, mashing, extracting with 12 times of anhydrous methanol containing 1% hydrochloric acid at 90 ℃ for 3 times, each for 40min, and combining the extracting solutions. Standing the extract overnight, filtering, concentrating at 45 deg.C under reduced pressure, and loading the treated AB-8 macroporous resin into 2.0cm × 40cm glass chromatographic column with column bed volume of 60 mL. Diluting the concentrated solution with water to 12mg/mL, loading the concentrated solution onto a column at a rate of 2mL/min, fully adsorbing, then eluting with distilled water until the eluate cannot be detected to obtain sugar by a phenol-sulfuric acid method, eluting with 3 times of anhydrous methanol at a rate of 2mL/min, concentrating the eluate under reduced pressure, and vacuum drying at 50 ℃ to obtain a persimmon tannin crude product with poor quality which cannot meet the food-grade requirement;
chinese patent CN102229628B discloses a method for preparing persimmon tannin from persimmons, comprising the steps of cleaning and screening persimmons, juicing, adding yeast for concentrated fermentation, carrying out ultrasonic extraction, concentrating and drying to obtain tannin products, wherein sugar in materials is decomposed by adding yeast for fermentation without high temperature, absorption, leaching, elution and other series of processes in the production process, and the effective components with easy hydrolysis or oxidation characteristics are not damaged, but the content and yield of the obtained products are lower.
The method has the defects that the extract is subjected to a series of processes of sufficient adsorption, leaching, elution and the like after being subjected to reduced pressure concentration, particularly, distilled water is required to be repeatedly leached until sugar can not be detected in the eluate by a phenol-sulfuric acid method, the operation process is complicated, otherwise, in the later drying process, because the sugar content of the persimmon tannin concentrate is too high, the drier is seriously adhered to the wall, and the dried powdery solid state of the material can not be achieved; the sugar in the material is decomposed by adding yeast for fermentation, so that the active ingredients with the characteristic of easy hydrolysis or oxidation are not damaged, but the content and the yield of the obtained product are lower, and therefore, the improvement and innovation of the method for extracting the tannin from the persimmons are bound to meet the requirement of food-grade tannin.
Disclosure of Invention
In view of the above situation, in order to overcome the defects of the prior art, the present invention aims to provide a method for extracting food-grade tannin from persimmons, which can effectively solve the problem that the quality and yield of the final product are affected by the oxidation of tannin caused by long-time high-temperature heating in the persimmon tannin extraction process.
The technical scheme for solving the problem is that the method for extracting the food-grade tannin from the persimmons comprises the following steps:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon in 35-45 deg.C warm water, sorting to remove impurities;
(2) pulping: crushing the treated green persimmons for 8-12min at the speed of 380-420 r/min under vacuum to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging the green persimmon pulp for 13-17min at 550-650 r/min, separating into filtrate and filter residue, concentrating the filtrate to obtain concentrate with relative density of 1.2-1.5, and oven drying the filter residue for use;
(4) drying: drying the concentrate at 140-160 deg.C for 25-35 min;
(5) milling: crushing the dried concentrate for 4-6min under the conditions of 700 and 900 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, keeping the vacuum degree between-0.05 KPa and-0.08 KPa, injecting propane, wherein the weight-volume ratio of the powder particles to the propane is 1:2, and the weight-volume ratio refers to that the solid is counted by g and the liquid is counted by ml, and stirring and reacting for 28-32 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin.
The invention has the advantages of high production efficiency, high product purity, low cost, low energy consumption, no environmental pollution, energy conservation, environmental protection and great economic and social benefits.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings and examples.
In specific practice, the invention is illustrated by the following examples.
Example 1
A method for extracting food-grade tannin from persimmons comprises the following steps:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon 100Kg in warm water of 40 deg.C, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmons for 10 min at a speed of 400 r/min in vacuum by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging green persimmon pulp with centrifugal filter at 600 r/min for 15min, separating into filtrate and residue, pumping the filtrate into concentrator, concentrating at 60 r/min for 60min to obtain concentrate with relative density of 1.3, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 150 deg.C for 30 min;
(5) milling: crushing the dried concentrate for 5min by a crusher under the condition of 800 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 30 min;
(7) liquid pumping: and (3) pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain 35.6Kg of food-grade tannin.
Example 2
A method for extracting food-grade tannin from persimmons comprises the following steps:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon 100Kg in warm water of 35 deg.C, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmons for 12min at 380 r/min by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging the pulp of fructus kaki with centrifugal filter at 550 r/min for 17min, separating into filtrate and residue, concentrating the filtrate in a concentrator at 60 r/min for 60min to obtain concentrate with relative density of 1.2, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 140 deg.C for 35 min;
(5) milling: crushing the dried concentrate for 6min by a crusher under the condition of 700 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 28 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain 36.4Kg of food-grade tannin.
Example 3
A method for extracting food-grade tannin from persimmons comprises the following steps:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon 100Kg in 45 deg.C warm water, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmon for 8min at a speed of 420 r/min in vacuum by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging fructus kaki pulp with centrifugal filter at 650 r/min for 13min, separating into filtrate and residue, concentrating the filtrate in a concentrator at 60 r/min for 60min to obtain concentrate with relative density of 1.5, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 160 deg.C for 25 min;
(5) milling: crushing the dried concentrate for 4min by a crusher under the condition of 900 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 32 min;
(7) liquid pumping: and (3) pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain 37.2Kg of food-grade tannin.
The method is simple, easy to operate, rich in raw materials, easy to produce and prepare and low in cost, and compared with the prior art, the method has the following outstanding advantages:
1. the production efficiency is high and is improved by 30 to 50 percent compared with the production efficiency of the existing method;
2. the product has good quality, the purity is as high as 94-96%, and the yield is as high as 89-93%;
3. the tannin extraction rate is up to more than 36 percent, namely more than 36Kg of tannin can be extracted from every 100Kg of green persimmons;
4. the energy consumption is low, and is reduced by more than 40 percent compared with the energy consumption of the existing method through tests;
5. in the experimental process, no waste gas, waste water and solid are discharged through tests, namely, zero discharge is realized, no pollution is caused to the environment, and energy conservation and environmental protection are really realized;
6. the method is suitable for large-scale industrial production, the obtained process and data are based on the large-scale industrial production, the risk of tannin oxidation is reduced by using a vacuum crusher, the raw material storage cost is reduced, the tannin content in the material is improved, the use of a large amount of organic solvents is reduced in the rear-end purification process, and the environmental protection capability is improved; meanwhile, the use cost of production auxiliary materials is also reduced; the process design is simple, the stable and high-yield operation of the production line is guaranteed, the relatively advanced process and advanced production equipment are used based on the invention, the absolute safety guarantee is provided for the production, and the economic and social benefits are huge.

Claims (4)

1. A method for extracting food-grade tannin from persimmons is characterized by comprising the following steps:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon in 35-45 deg.C warm water, sorting to remove impurities;
(2) pulping: crushing the treated green persimmons for 8-12min at the speed of 380-420 r/min under vacuum to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging the green persimmon pulp for 13-17min at 550-650 r/min, separating into filtrate and filter residue, concentrating the filtrate to obtain concentrate with relative density of 1.2-1.5, and oven drying the filter residue for use;
(4) drying: drying the concentrate at 140-160 deg.C for 25-35 min;
(5) milling: crushing the dried concentrate for 4-6min under the conditions of 700 and 900 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, keeping the vacuum degree between-0.05 KPa and-0.08 KPa, injecting propane, wherein the weight-volume ratio of the powder particles to the propane is 1:2, and the weight-volume ratio refers to that the solid is counted by g and the liquid is counted by ml, and stirring and reacting for 28-32 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin.
2. The method of claim 1, comprising the steps of:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon with warm water of 40 deg.C, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmons for 10 min at a speed of 400 r/min in vacuum by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging green persimmon pulp with centrifugal filter at 600 r/min for 15min, separating into filtrate and residue, pumping the filtrate into concentrator, concentrating at 60 r/min for 60min to obtain concentrate with relative density of 1.3, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 150 deg.C for 30 min;
(5) milling: crushing the dried concentrate for 5min by a crusher under the condition of 800 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 30 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin.
3. The method of claim 1, comprising the steps of:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon with 35 deg.C warm water, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmons for 12min at 380 r/min by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging the pulp of fructus kaki with centrifugal filter at 550 r/min for 17min, separating into filtrate and residue, concentrating the filtrate in a concentrator at 60 r/min for 60min to obtain concentrate with relative density of 1.2, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 140 deg.C for 35 min;
(5) milling: crushing the dried concentrate for 6min by a crusher under the condition of 700 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 28 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin.
4. The method of claim 1, comprising the steps of:
(1) raw material treatment: soaking and cleaning non-yellow green persimmon in 45 deg.C warm water, and manually or mechanically removing impurities;
(2) pulping: crushing the processed green persimmon for 8min at a speed of 420 r/min in vacuum by using a vacuum crusher to obtain green persimmon pulp;
(3) centrifugal separation: centrifuging fructus kaki pulp with centrifugal filter at 650 r/min for 13min, separating into filtrate and residue, concentrating the filtrate in a concentrator at 60 r/min for 60min to obtain concentrate with relative density of 1.5, and oven drying the residue for use;
(4) drying: drying the concentrate with a disc dryer at 160 deg.C for 25 min;
(5) milling: crushing the dried concentrate for 4min by a crusher under the condition of 900 r/min to obtain powder particles which are sieved by a 300-400-mesh sieve;
(6) vacuum reaction: putting the powder particles into a vacuum reaction kettle, injecting 200Kg of propane into the vacuum reaction kettle with the vacuum degree of-0.05 KPa to-0.08 KPa, and stirring for reaction for 32 min;
(7) liquid pumping: and pumping out propane liquid in the reaction kettle, and relieving the pressure to obtain the food-grade tannin.
CN201911389302.1A 2019-12-30 2019-12-30 Method for extracting food-grade tannin from persimmons Pending CN110938103A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114052248A (en) * 2021-10-16 2022-02-18 湖南粟园酒庄有限责任公司 Comprehensive processing system and equipment for rough processing of grape seed tannin raw materials

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114052248A (en) * 2021-10-16 2022-02-18 湖南粟园酒庄有限责任公司 Comprehensive processing system and equipment for rough processing of grape seed tannin raw materials

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