CN103554197A - Method for preparing tannin with gall flowers - Google Patents
Method for preparing tannin with gall flowers Download PDFInfo
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- CN103554197A CN103554197A CN201310533576.XA CN201310533576A CN103554197A CN 103554197 A CN103554197 A CN 103554197A CN 201310533576 A CN201310533576 A CN 201310533576A CN 103554197 A CN103554197 A CN 103554197A
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- weibull
- tannin
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Abstract
The invention discloses a method for preparing tannin with gall flowers. The method is characterized by firstly carrying out water extraction on the raw material gall flowers to obtain an extracting solution, adding complexing agents to the obtained extracting solution, stirring the mixture to carry out complexation to obtain a tannin complex precipitate, filtering the tannin complex precipitate, carrying out desorption reaction on the obtained tannin complex and desorption agents to reduce tannin, filtering, and evaporating the filtrate, thus obtaining tannin. The method has the beneficial effects that the process is simple, the industrial conditions are mild, the costs of the raw materials are low, and the prepared tannin has high yield and has purity in accordance with the national standard (LYT1300-2005).
Description
Technical field
The present invention relates to a kind of doubly flower raw material production of utilizing and doubly spend the preparation method of industrial tannic acid, belong to field of fine chemical.
Background technology
Weibull is that a class has biological activity polyphenols, has important use, and be the basic raw material of many organic syntheses at aspects such as chemical industry, food, anti-corrosion of metal, ink manufacture, mining and metallurgy, printing and dyeing, medicine, chemical analyses.Industrial tannic acid be generally with gall nut (angle doubly and tripe doubly) extract directly concentrated, be dried and make.Its Weibull content >=81%, but along with the deepening continuously of Nutgalls tannin chemical research and technological development, the purposes of Weibull is increasingly extensive, particularly the industrial tannic acid situation that supply falls short of demand especially.Gall nut raw material can not meet industrial demand, therefore, adopts and doubly spends alternative gall nut to become trend.Tannin chemical structure in Chinese gall Beihua tannin is consistent with the chemical structure of Gallotannin acid substantially, is also the compound combining with ester bond with β-D-Glucose with galloyl; Can doubly spend raw materials quality good by gall nut raw material, tannin content is high is 60% left and right, and impurity is few, and doubly spends the tannin content of raw material to only have 30% left and right, impurity is many, directly extracts the national standard requirement that its Weibull content of evaporation drying does not reach industrial tannic acid product between 62～70% at all.
The flower of take is doubly prepared industrial tannic acid as raw material production, adopt existing Weibull purification technique as: number of patent application is: 200810025371.X discloses a kind of preparation method of high-purity tarra edible tannic acid, main activated carbon and the macroporous resin adsorption impurity purifying industrial grade talas of tannic acid of adopting, but efficiency is lower, process is complicated; 94114973.0 disclose the method for separation purity Chinese gallotanninic acid from thick Chinese gallotanninic acid, mainly by porous aluminium glue sorbent material, first adsorb impurity, adopt again polymeric sorbent absorption Chinese gallotanninic acid, the Chinese gallotanninic acid purity obtaining improves, but output is lower, processing step is also complicated, and product cost is increased.
Summary of the invention
The object of the invention is to be to provide a kind of low cost, high yield to prepare the method for the Weibull of higher degree; The method technique is simple, and industrial condition is gentle, and raw materials cost is low, meets suitability for industrialized production.
The invention provides the method for preparing Weibull of doubly spending, the method is to obtain extracting solution by doubly spending raw material to carry out water extraction, in gained extracting solution, add the complexing agent of doubly spending raw materials quality 10～60%, stir complex reaction occurs, obtain Weibull complex compound sediment, filter, the Weibull complex compound of gained and desorbing agent are carried out to desorption reaction with solid-liquid mass ratio 1:2～5 and restore Weibull, filter, by filtrate evaporation, obtain;
Described complexing agent is one or more in plumbic acetate, monobasic lead acetate, copper sulfate, magnesium acetate, hydrated barta, calcium hydroxide, tin protochloride;
Described desorbing agent is that mass percent concentration is 5～20% acid solution, and described acid solution is one or more in sulphuric acid soln, phosphoric acid solution, oxalic acid solution; Wherein, the complexing agent of use and the desorbing agent of corresponding use can react and generate precipitation.
Described complex reaction is at 20～60 ℃, stirring reaction 1～4h.
The described desorption reaction time is 1.5～2.5h.
Described water extraction is at 50～80 ℃, extracts 16～48h.
Described water extraction solid-liquid mass ratio is controlled at 1:5～8.
The present invention be take doubly flower and is prepared the method for Weibull as raw material, comprises the following steps:
Step 1) water extraction:
Doubly flower raw material and water mix with solid-to-liquid ratio (mass ratio) 1:5～8, controlling temperature, are lixiviate 16～48h under the condition of 50～80 ℃, after standing 24～48h, filter, and obtain the extracting solution containing Weibull;
Step 2) prepare Weibull complex compound:
Step 1) gained containing slowly adding the complexing agent of doubly spending raw materials quality 10～60% in the extracting solution of Weibull; Stirring reaction 1～4 hour at 20～60 ℃, generates Weibull complex compound sediment again; Filter, obtain tannin complex compound; Wherein, the complexing agent of selecting is one or more in plumbic acetate, monobasic lead acetate, copper sulfate, magnesium acetate, hydrated barta, calcium hydroxide, tin protochloride;
Step 3) desorption reduction Weibull:
By step 2) gained Weibull complex compound take solid-to-liquid ratio (mass ratio) 1:2～5 and adds the acid solution that mass percent concentration is 5～20%, stir, rear standing 1.5～2.5h, desorption metal salt precipitate, filter, filtrate obtains powdery Chinese gall Beihua tannin through evaporation drying; Wherein: the acid solution of selecting is one or more in sulphuric acid soln, phosphoric acid solution, oxalic acid solution; The acid solution of selecting and the complexing agent of corresponding selection can generate insoluble or be slightly soluble in the precipitation of water.
Beneficial effect of the present invention: the present invention doubly spends direct high yield to prepare the Weibull that meets national standard (LYT1300-2005) with cheap raw material first, and processing condition are gentle, and flow process is simple, is applicable to suitability for industrialized production.The present invention is by using special complexing agent that the Weibull complexing salinization in aqueous extract is formed to precipitation, carry out solid-liquid separation, the desorbing agent of simultaneously selecting special energy and complexing agent to be used in conjunction with, desorbing agent can displace Weibull radical ion, generate stable metal salt precipitate with metal ion, can obtain expeditiously highly purified Weibull; Polymer adsorption Weibull relatively of the prior art, then the method for wash-out, the present invention is by chemical transformation, and solid-liquid separation, has improved separation efficiency and productive rate greatly; And there is the simple advantage of technique, greatly reduce the production cost of Weibull.Abundant experimental results shows: the present invention directly prepares the industrial tannic acid product of purity >=81% with the doubly flower raw material of cheapness, yield reaches 25% left and right, take and doubly spends the tannin content of raw material as 30% yield is not less than 82%, reaches as high as 85%.
Embodiment
Following examples are intended to further illustrate the present invention, rather than restriction the scope of protection of the invention.
Embodiment 1
Doubly spend the dry raw material 100g of gas, fragmentation adds water 800mL, 60 ℃ of lixiviates 24 hours, clarify 24 hours, filter to obtain extracting solution, the monobasic lead acetate complexing agent that slowly adds raw materials quality 45%, is uniformly mixed, reaction 4h, filter to obtain Weibull complex compound, it is 8% sulphuric acid soln 250mL that Weibull complex compound adds mass percent concentration, stirs 2h, filters to obtain Weibull liquid, be decompressed under the vacuum tightness of 0.08MPa concentrated, spray-dried, obtain powder-like product 26.14g, its Weibull content is 83.16%.
Embodiment 2
Doubly spend the dry raw material 200g of gas, fragmentation adds water 1400mL, 60 ℃ of lixiviates 30 hours, clarify 30 hours, filter to obtain extracting solution, 33% the magnesium acetate complexing agent that slowly adds raw materials quality amount, is uniformly mixed, reaction 4h, filter to obtain Weibull complex compound, it is 8% phosphoric acid solution 600mL that Weibull complex compound adds mass percent concentration, stirs 1.8h, filters to obtain Weibull liquid, be decompressed under the vacuum tightness of 0.08MPa concentrated, spray-dried, obtain powder-like product 48.02g, its Weibull content is 85.36%.
Embodiment 3
Doubly spend the dry raw material 200g of gas, fragmentation adds water 1400mL, 60 ℃ of lixiviates 36 hours, clarify 30 hours, filter to obtain extracting solution, the calcium hydroxide complexing agent that slowly adds raw materials quality 14%, is uniformly mixed, reaction 4h, filter to obtain Weibull complex compound, it is 10% oxalic acid solution 700mL that Weibull complex compound adds mass percent concentration, stirs 2.5h, filters to obtain Weibull liquid, be decompressed under the vacuum tightness of 0.08MPa concentrated, spray-dried, obtain powder-like product 50.21g, its Weibull content is 84.73%.
Embodiment 4
Doubly spend the dry raw material 200g of gas, fragmentation adds water 1000mL, 50 ℃ of lixiviates 40 hours, clarify 30 hours, filter to obtain extracting solution, the monobasic lead acetate complexing agent that slowly adds raw materials quality 50%, is uniformly mixed, reaction 4h, filter to obtain Weibull complex compound, it is 5% sulphuric acid soln 700mL that Weibull complex compound adds mass percent concentration, stirs, and filters to obtain Weibull liquid, be decompressed under the vacuum tightness of 0.08MPa concentrated, spray-dried, obtain powder-like product 53.82g, its Weibull content is 82.46%.
Claims (5)
1. times flower is prepared the method for Weibull, it is characterized in that, to doubly spend raw material to carry out water extraction and obtain extracting solution, in gained extracting solution, add the complexing agent of doubly spending raw materials quality 10～60%, and stir complex reaction occurs, obtain Weibull complex compound sediment, filter, the Weibull complex compound of gained and desorbing agent are carried out to desorption reaction with solid-liquid mass ratio 1:2～5 and restore Weibull, filter, by filtrate evaporation, obtain;
Described complexing agent is one or more in plumbic acetate, monobasic lead acetate, copper sulfate, magnesium acetate, hydrated barta, calcium hydroxide, tin protochloride;
Described desorbing agent is that mass percent concentration is 5～20% acid solution, and described acid solution is one or more in sulphuric acid soln, phosphoric acid solution, oxalic acid solution; Wherein, the complexing agent of use and the desorbing agent of corresponding use can react and generate precipitation.
2. the method for claim 1, is characterized in that, described complex reaction is at 20～60 ℃, stirring reaction 1～4h.
3. the method for claim 1, is characterized in that, the described desorption reaction time is 1.5～2.5h.
4. the method for claim 1, is characterized in that, described water extraction is at 50～80 ℃, extracts 16～48h.
5. method as claimed in claim 4, is characterized in that, described water extraction solid-liquid mass ratio is controlled at 1:5～8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310533576.XA CN103554197A (en) | 2013-10-30 | 2013-10-30 | Method for preparing tannin with gall flowers |
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| CN201310533576.XA CN103554197A (en) | 2013-10-30 | 2013-10-30 | Method for preparing tannin with gall flowers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762031A (en) * | 2019-02-01 | 2019-05-17 | 广州柿宝生物科技有限公司 | A method of extracting tannin from persimmon |
| CN114773410A (en) * | 2022-04-21 | 2022-07-22 | 昆明理工大学 | Method for recovering tannic acid from tannin germanium slag based on ultrasonic outfield |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830940A (en) * | 2010-05-21 | 2010-09-15 | 湖南土家人集团保靖生化科技有限公司 | Method for preparing Chinese gall Beihua tannin |
| CN102260299A (en) * | 2011-05-24 | 2011-11-30 | 保靖县林力科技开发有限公司 | Preparation method of gall flower tannic acid |
-
2013
- 2013-10-30 CN CN201310533576.XA patent/CN103554197A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830940A (en) * | 2010-05-21 | 2010-09-15 | 湖南土家人集团保靖生化科技有限公司 | Method for preparing Chinese gall Beihua tannin |
| CN102260299A (en) * | 2011-05-24 | 2011-11-30 | 保靖县林力科技开发有限公司 | Preparation method of gall flower tannic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762031A (en) * | 2019-02-01 | 2019-05-17 | 广州柿宝生物科技有限公司 | A method of extracting tannin from persimmon |
| CN114773410A (en) * | 2022-04-21 | 2022-07-22 | 昆明理工大学 | Method for recovering tannic acid from tannin germanium slag based on ultrasonic outfield |
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Application publication date: 20140205 |