CN102106481A - Method for preparing tannin chelate zinc feed additive - Google Patents
Method for preparing tannin chelate zinc feed additive Download PDFInfo
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Abstract
The invention aims to provide a method for preparing tannin chelate zinc feed additive. The method has simple production process and low cost, and the feed additive has remarkable effect of preventing and treating diarrhea of piglets. The preparation method mainly comprises the following steps of: preparing tannin solution, preparing zinc acetate solution, and mixing the tannin solution and the zinc acetate solution to prepare a tannin chelate zinc product. The yield of the tannin chelate zinc prepared by the method is high and is about 57.9 to 58.9 percent, wherein the chelate zinc reaches 24 percent. Besides the intestine astringing and diarrhea relieving effects of tannin, the prepared tannin chelate zinc can meet the requirement of animals on trace element zinc. Therefore, the feed additive can effectively prevent and treat diarrhea of the piglets and promote the growth of animals.
Description
Technical field
The present invention relates to a kind of preparation method of organic Polyphenols chelating zinc, especially relate to a kind of preparation method of feed addictive tannin chelating zinc.
Background technology
Tannin is the contained polyhydric phenols derivative of finished leather of rawhide being tanned in the plant, so claim vegetable tannin again, is the class material in the Secondary Metabolism of Plant product phenols polymer.The molecular weight of tannin: 1701.20, molecular formula: C
76H
52O
46, belong to the complex compound of multi-phenol.Tannin extensively is present in each organ structure of plant, content reaches 20-40% in many coniferous barks, particularly the tannin content in the Chinese gall is up to the 60-80% (distribution of tannin among three kinds of important tannin vegetable nutritoriums, " tropical and subtropical zone Botany Gazette ", 1997 02 phases), be distribute the natural reproducible resource wide, wide in variety, that quantity is big (the Chen Jia letter. China's nutgall tannin chemistry utilizes status and prospects [J]. chemistry of forest product and industry, 2000,20 (2): 71-72).Vegatable tannin mainly contains two kinds, and a kind of is Hydrolysable Tannins, and a kind of is condensed tannin, wherein Hydrolysable Tannins can be used as the chelate raw material (Sun Dawang. vegatable tannin chemistry [M]. Beijing: China Forest publishing house, 1992.411-426).A plurality of ortho positions phenolic hydroxyl structure of tannin can be used as a kind of polyhydroxy part and metal ion generation complex reaction, and forms stable five-membered ring chelate.
Tannin is the native compound of a class biologically active, and it has and reacts with protein, alkaloid, metal ion etc. and a series of chemical property such as anti-oxidant, has much obtained research in fields in chemistry, biology, medical science, agriculture and animal husbandry etc.Tannin can be alleviated the stimulation to intestinal mucosa, or directly protects intestinal mucosa, reduces to ooze out and bring into play anti-diarrhea effect; behind oral astringent tannalbin, in stomach, do not decompose, decomposite tannic acid and play astriction to small intestine; can make the protein coagulating on inflammatory cell surface; form layer protecting film, diffusate is reduced, and alleviate the spread effect of intestinal contents the intestines wall; reduce enterocinesia; and normal intestinal motility is not had very influence, owing to its astriction alleviates intestinal inflammatory, so can prevent diarrhoea.But because the tannin chemical property is active, tannin in the feed generates deposit by combining with protein, carbohydrate, enzyme, metal ion, have a strong impact on livestock and poultry to the digestion of nutriment with absorb, reduce the nutritive value of feed, the anti-oxidant action of Here it is tannin (Lv Yuan equality. the anti-trophism of vegatable tannin and biodegradation [J] thereof in the feed. Chinese herding magazine, 2003, (02)).The feed intake, digestibility and the animal that significantly reduce animal live and increase weight.
Zinc (Zn) is as a kind of indispensable element in the animal body, it is the constituent of more than 40 kind of metalloenzyme in the body, the activity factor of 200 plurality of enzymes participates in that nucleic acid and protein are synthetic, energetic supersession, cellular immunity and humoral immunity process etc., often is called as " biological element ".In daily ration, add 2000mg/kg～3000mg/kg zinc oxide, can significantly reduce diarrhea of weaned piglets the incidence of disease, reduce ablactation stress, improve daily gain, improve the price of deed (Hu Xiangdong, Hong Zuopeng, Wang Minqi. high dose zinc promotes pig Research Progress on Growth [J]. Chinese feed, 2004 (7): 8-9).Therefore, zinc is widely used in as a kind of effective feed addictive and raises pigs.But high zinc daily ration has a strong impact on the late growing stage of animal grows, influence growing of immunity of organism organ, suppressing the content of immunoglobulin (Ig) and the cascade of complement amplifies, reduce immunity of organisms (Chen Liang, high zinc daily ration long term exposure is to the immunopathology research [D] of weanling pig influence. Agricultural University Of Anhui's thesis for the doctorate, 2008).And, add the high dose inorganic zinc exist equally the wasting of resources and environmental pollution two big adverse consequences (guilt rubine, Tong Xiaoli, Zhong Zhengze. high zinc growth promotion mechanism and environmental pollution thereof are studied [J]. Chinese feed,, the 06th phase in 2004).So 2009 the 1224th middle regulations of bulletin " feed addictive safe handling standard " of The Ministry of Agriculture of the People's Republic of China, MOA: the zinc level in the daily ration can not be no more than 2250mg/kg above the addition of the zinc of zinc oxide form in preceding 2 all mixed feeds behind the weaned piglet.
For the anti-oxidant action that solves tannin and the side effect of high zinc, the present invention utilizes the chelatropic reaction of tannin and zinc, forms tannin chelating zinc.Can either utilize the physiological role of tannin, also can utilize zinc to alleviate grice diarrhoea, both can be complementary like this, reaches the control grice diarrhoea, avoids the anti-oxidant action of tannin and high zinc to the pollution of environment, has the effect of double gain.
Summary of the invention
The principle of the invention is that vegatable tannin (Hydrolysable Tannins), the zinc acetate with cheapness is reaction raw materials, and use NaOH cheap and easy to get to be reactant, i.e. preparation can be used for the tannin chelating zinc of feed addictive in the reaction environment of routine, need not special or expensive consersion unit.
Therefore, the object of the present invention is to provide a kind of cost low, production technology is simple, to the preparation method of the significant a kind of feed addictive vegatable tannin chelating zinc of grice diarrhoea prevention effect.To achieve these goals, to adopt vegatable tannin (Hydrolysable Tannins), zinc acetate, NaOH etc. be raw material in the present invention.
Its feature comprises the following steps:
(1) preparation of tanning solution: the vegatable tannin of getting certain mass, add and be equivalent to vegatable tannin mass volume ratio 4-10 water doubly, after mixing, regulating the pH value with sodium hydroxide solution is 4.5-6.5, bath temperature (60-80 ℃) heating 15-25 minute, obtain tanning solution;
(2) preparation of acetic acid zinc solution: get the zinc acetate of certain mass, add and be equivalent to zinc acetate mass volume ratio 2-5 water doubly, stirring and dissolving after mixing, bath temperature (60-80 ℃) heating 15-25 minute, obtains acetic acid zinc solution;
(3) prepared acetic acid zinc solution is joined in the tanning solution that step (1) makes, the while stirring and evenly mixing, regulate the pH value with sodium hydroxide solution, reaching 4.5-6.5 up to the pH value gets final product, behind bath temperature (60-80 ℃) reaction 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product, and wherein the mass ratio of vegatable tannin in step (1) and (2) and zinc acetate was near 1: 1.
In one embodiment, the preferred 4-6 of the water yield that adds in the step 1 times, the preferred 65-75 of bath temperature ℃, preferred 15-20 minute heat time heating time.
In another embodiment, the preferred 2.5-3.0 of the water yield that adds in the step 2 times, the preferred 65-75 of bath temperature ℃, preferred 15-20 minute heat time heating time.
According to above scheme, in other specific embodiments, described step comprises:
(1) preparation of tanning solution: get the vegatable tannin of 15-25g, add 100-150mL water, after mixing, regulating the pH value with the 3M sodium hydroxide solution is 4.5-6.5, bath temperature (60-80 ℃) heating 15-25 minute, obtains tanning solution;
(2) preparation of acetic acid zinc solution: get the 16-29g zinc acetate, add 50-80mL water, stirring and dissolving after mixing, bath temperature (60-80 ℃) heating 15-25 minute, obtains acetic acid zinc solution;
(3) prepared acetic acid zinc solution is joined in the tanning solution that step (1) makes, stirring and evenly mixing is regulated with sodium hydroxide solution simultaneously, until pH is 4.5-6.5, behind bath temperature (60-80 ℃) reaction 1h, obtains tannin chelating zinc precipitation, filter, drying obtains product.
Tannin chelating zinc yield=(quality of tannin chelating zinc/(tannin quality * 2.2788)) * 100%, wherein 2.2788 is the ratio of 2 times of tannin chelating zinc relative molecular weight and tannin relative molecular weights, i.e. 3874 ÷ 1700=2.2788.
The assay formula=(Na of zinc in the gained tannin chelating zinc
2EDTA (concentration) * Na2EDTA (volume) * 65 * 10
-3The quality of/tannin chelating zinc) * 100%, 65 be the atomic weight of zinc wherein.
The assay of zinc in the tannin chelating zinc, be ten thousand in accuracy/ balance on take by weighing chelating zinc 0.0035g, add water 50mL, be added on 5 of the hydrochloric acid of 6mol/L, make it to dissolve fully, add NH
3-NH
4Cl buffer solution (pH=10) 10mL, 4 of the black T indicator of network are with the Na of 0.10mol/L
2The titration of EDTA solution is to blue, and record consumes Na
2The amount of EDTA gets final product according to above-mentioned formula calculating.
Employed tannin powder (being similar to starch) derives from plant among the present invention, such as extracting from coniferous tree bark, Rhizophoraceae plant and Chinese gall etc., also can directly buy (content is greater than 99%) from the market.
Technique effect
The present invention has following outstanding advantage:
1. the prepared tannin chelating zinc yield productive rate height of the inventive method, yield is about 57.9-58.9%, and wherein chelating zinc reaches 24%;
2. prepare tannin chelating zinc from tannin, raw material is easy to get, and reaction scheme is short, but finishes at Routine Test Lab under the normal temperature and pressure, need not expensive production equipment, and production cost is low, therefore is convenient to suitability for industrialized production.
3. tannin chelating zinc of the present invention has stable chemical constitution, as trace mineral supplement, safety non-toxic, nonirritant, its infiltration rate is fast, absorptivity improves greatly, the biological value height can be protected environment, reduce pollute, and meets the development spirit of " environmentally friendly, resource-conserving " that country advocates;
4. tannin chelating zinc of the present invention removes the effect of the relieving diarrhea with astringents of performance tannin, also can satisfy the needs of animal to trace element zinc, so can promote growth of animal, can significantly improve the utilization rate of feed.
5. the tannin chelating zinc of this method preparation, cost is low, and technology is simple, and chelating zinc reaches 24%.In 21 age in days weanling pig daily rations, add tannin chelating zinc 700g/ ton, during to 28 ages in days, to compare with control group, diarrhea rate reduces by 21.23%.The result shows that test group diarrhea rate after 5 days obviously descends, and control group diarrhea rate in whole process is higher, and diarrhoea is longer perdurabgility, and weaning still had 20% diarrhea rate in 12-15 days.
Embodiment
According to above production procedure, below provide several specific embodiment.
Embodiment 1:
A. with vegatable tannin weight be 15g (from the market buy, Hydrolysable Tannins content 〉=99%), water 100mL to mix the back in the 500mL beaker be 4.5 with 3mol/L sodium hydroxide solution adjusting pH value, heated 15 minutes for 60 ℃ at bath temperature, obtain tanning solution.
B. with zinc acetate 16g, water 50mL in beaker, 60 ℃ of bath temperatures heating 15 minutes, obtain acetic acid zinc solution.
C. the acetic acid zinc solution of b is joined in the tanning solution that step a obtains, stir while adding, and to regulate the pH value with the 3mol/L sodium hydroxide solution be 4.5, behind 60 ℃ of reactions of bath temperature 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product 19.8g.
Tannin chelating zinc yield=(quality of tannin chelating zinc/(tannin quality * 2.2788)) * 100%=57.9%.
Embodiment 2:
A. be that 20g, water 120mL mix the back to regulate the pH value with the 3mol sodium hydroxide solution be 5 with vegatable tannin weight in the 500mL beaker, heated 15 minutes for 65 ℃, obtain tanning solution at bath temperature.
B. with zinc acetate 22g, water 60mL in beaker, 65 ℃ of bath temperatures heating 15 minutes, obtain acetic acid zinc solution.
C. the acetic acid zinc solution of b is joined in the tanning solution that step a obtains, stir while adding, and to regulate the pH value with the 3mol/L sodium hydroxide solution be 5.0, behind 65 ℃ of reactions of bath temperature 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product 26.6g.
Tannin chelating zinc yield is 58.3%.
Embodiment 3:
A. be that 22g, water 130mL mix the back to regulate the pH value with the 3mol sodium hydroxide solution be 5.5 with vegatable tannin weight in the 500mL beaker, heated 15 minutes for 70 ℃, obtain tanning solution at bath temperature.
B. with zinc acetate 24g, water 70mL in beaker, 70 ℃ of bath temperatures heating 15 minutes, obtain acetic acid zinc solution.
C. the acetic acid zinc solution of b is joined in the tanning solution that step a obtains, stir while adding, and to regulate the pH value with the 3mol/L sodium hydroxide solution be 5.5, behind 70 ℃ of reactions of bath temperature 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product 29.2g.
Tannin chelating zinc yield is 58.3%.
Embodiment 4:
A. be that 23g, water 140mL mix the back to regulate the pH value with the 3mol sodium hydroxide solution be 6 with vegatable tannin weight in the 500mL beaker, heated 15 minutes for 75 ℃, obtain tanning solution at bath temperature.
B. with zinc acetate 26g, water 75mL in beaker, 75 ℃ of bath temperatures heating 15 minutes, obtain acetic acid zinc solution.
C. the acetic acid zinc solution of b is joined in the tanning solution that step a obtains, stir while adding, and to regulate the pH value with the 3mol/L sodium hydroxide solution be 6.0, behind 75 ℃ of reactions of bath temperature 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product 30.8g.
Tannin chelating zinc yield is 58.9%.
Embodiment 5: the animal feeding effect test
The tannin chelating zinc of this method preparation, cost is low, and technology is simple, and the content of zinc reaches 24% in the tannin chelating zinc.In 21 age in days weanling pig daily rations, add tannin chelating zinc 500g/ ton, during to 28 ages in days, to compare with control group (adding zinc oxide 1500g/ ton), diarrhea rate reduces by 21.23%.The result shows that test group diarrhea rate after 5 days obviously descends, and control group diarrhea rate in whole process is higher, and diarrhoea is longer perdurabgility, and the wean back still had 10% diarrhea rate in 7-14 days.The results are shown in Table one, this table has reflected the influence of the feed of present embodiment to growth pig production performance.From growth performance, be reduced to 1/5th situation than zinc consumption in the feed market prescription under, growth performance effect of the present invention is better than control group, illustrates promptly that also tannin chelating zinc can effectively reduce the advantages such as diarrhea rate of weanling pig.
Table one: daily ration adds the influence of tannin chelating zinc to weanling pig growth performance and diarrhea rate
| Project | Contrast | Tannin chelating zinc |
| ZnO (g/ ton) | 2000 | 0 |
| Tannin chelating zinc adds level (g/ ton) | 0 | 500.00 |
| Diarrhea rate (%) | 12.71±0.16 | 2.13±0.13 |
Claims (4)
1. the preparation method of a feed addictive tannin chelating zinc, step comprises:
(1) preparation of tanning solution: the vegatable tannin of getting certain mass, add and be equivalent to vegatable tannin mass volume ratio 4-10 water doubly, after mixing, regulating the pH value with sodium hydroxide solution is 4.5-6.5, bath temperature (60-80 ℃) heating 15-25 minute, obtain tanning solution.
(2) preparation of acetic acid zinc solution: get the zinc acetate of certain mass, add and be equivalent to zinc acetate mass volume ratio 2-5 water doubly, stirring and dissolving after mixing, bath temperature (60-80 ℃) heating 15-25 minute, obtains acetic acid zinc solution.
(3) prepared acetic acid zinc solution is joined in the tanning solution that step (1) makes, the while stirring and evenly mixing, regulate the pH value with sodium hydroxide solution, reaching 4.5-6.5 up to the pH value gets final product, behind bath temperature (60-80 ℃) reaction 1h, obtain tannin chelating zinc precipitation, filter, drying obtains product, and wherein the mass ratio of vegatable tannin in step (1) and (2) and zinc acetate was near 1: 1.
2. the process of claim 1 wherein the preferred 4-6 of the water yield that adds in the step 1 doubly, the preferred 65-75 of bath temperature ℃, preferred 15-20 minute heat time heating time.
3. the process of claim 1 wherein the preferred 2.5-3.0 of the water yield that adds in the step 2 doubly, the preferred 65-75 of bath temperature ℃, preferred 15-20 minute heat time heating time.
4. the method for claim 1 to 3, wherein said step comprises:
(1) preparation of tanning solution: get the vegatable tannin of 15-25g, add 100-150mL water, after mixing, regulating the pH value with the 3M sodium hydroxide solution is 4.5-6.5, bath temperature (60-80 ℃) heating 15-25 minute, obtains tanning solution;
(2) preparation of acetic acid zinc solution: get the 16-29g zinc acetate, add 50-80mL water, stirring and dissolving after mixing, bath temperature (60-80 ℃) heating 15-25 minute, obtains acetic acid zinc solution;
(3) prepared acetic acid zinc solution is joined in the tanning solution that step (1) makes, stirring and evenly mixing is regulated with sodium hydroxide solution simultaneously, until pH is 4.5-6.5, behind bath temperature (60-80 ℃) reaction 1h, obtains tannin chelating zinc precipitation, filter, drying obtains product.
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| CN104592318B (en) * | 2014-12-25 | 2017-04-26 | 广州天科生物科技有限公司 | Semi-solid phase preparation method of tannin zinc |
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| CN107712353A (en) * | 2017-11-10 | 2018-02-23 | 王芳 | A kind of feed addictive for preventing diarrhea of pigs and preparation method and application |
| CN109287868A (en) * | 2018-11-28 | 2019-02-01 | 中国科学院东北地理与农业生态研究所 | A kind of preparation method of feed addictive tannin chelate iron |
| CN109820098A (en) * | 2019-04-23 | 2019-05-31 | 中国林业科学研究院林产化学工业研究所 | A kind of additive of organic zinc feed and preparation method thereof and bacteriostatic activity application |
| CN114642241A (en) * | 2022-04-01 | 2022-06-21 | 武汉轻工大学 | Composite plant polyphenol chelate and using method thereof |
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Cited By (8)
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| CN104592318B (en) * | 2014-12-25 | 2017-04-26 | 广州天科生物科技有限公司 | Semi-solid phase preparation method of tannin zinc |
| CN107027973A (en) * | 2017-05-25 | 2017-08-11 | 广州汇加生物科技有限公司 | A kind of tannin mixture for reducing or eliminating vegatable tannin astringent taste and preparation method and application |
| CN107027973B (en) * | 2017-05-25 | 2021-03-19 | 广州汇加生物科技有限公司 | Tannin mixture capable of reducing or eliminating astringent taste of plant tannin and preparation method and application thereof |
| CN107712353A (en) * | 2017-11-10 | 2018-02-23 | 王芳 | A kind of feed addictive for preventing diarrhea of pigs and preparation method and application |
| CN109287868A (en) * | 2018-11-28 | 2019-02-01 | 中国科学院东北地理与农业生态研究所 | A kind of preparation method of feed addictive tannin chelate iron |
| CN109820098A (en) * | 2019-04-23 | 2019-05-31 | 中国林业科学研究院林产化学工业研究所 | A kind of additive of organic zinc feed and preparation method thereof and bacteriostatic activity application |
| CN114642241A (en) * | 2022-04-01 | 2022-06-21 | 武汉轻工大学 | Composite plant polyphenol chelate and using method thereof |
| CN114642241B (en) * | 2022-04-01 | 2024-01-26 | 武汉轻工大学 | Composite plant polyphenol chelate and application method thereof |
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