CN103275318A - Production method of selenium-enriched polyaspartic acid calcium salt - Google Patents
Production method of selenium-enriched polyaspartic acid calcium salt Download PDFInfo
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- CN103275318A CN103275318A CN201310197066XA CN201310197066A CN103275318A CN 103275318 A CN103275318 A CN 103275318A CN 201310197066X A CN201310197066X A CN 201310197066XA CN 201310197066 A CN201310197066 A CN 201310197066A CN 103275318 A CN103275318 A CN 103275318A
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- aspartic acid
- calcium salt
- poly aspartic
- selenium
- acid calcium
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Abstract
The invention relates to a production method of selenium-enriched polyaspartic acid calcium salt. The method comprises the following steps of stirring the polyaspartic acid and calcium hydroxide in an aqueous solution to have reaction; and adding seleninic acid into the solution, filtering the solution, and concentrating and drying the filtering liquid to obtain the selenium-enriched polyaspartic acid calcium salt. The production method is simple and has the advantages of high resource utilization rate, short production time and high efficiency.
Description
Technical field
The present invention relates to the production method of poly aspartic acid calcium salt, relate in particular to a kind of production method of rich selenium poly aspartic acid calcium salt.
Background technology
Selenium, symbol of element Se is a kind of micro elements needed by human, is the active centre of Selenoperoxidase, has cancer-resisting, anti-oxidant anti-aging and biological characteristicses such as raising body immunity, antagonism heavy metal.General people absorb selenium by agricultural-food, and NI recommends that every day, intake was the 50-200 microgram per capita, but the selenium intake of China only is the 26-32 microgram.In order to increase the intake of selenium, the market begins plantation and sells rich selenium product.
Poly aspartic acid (poly-peptide organized enzyme) is the efficient synergistic agent of a kind of fertilizer and novel plant dietetic alimentation promotor and conditioning agent, plant desired nutritional composition is possessed extremely strong chelating function, and effectively nitrogen, phosphorus, potassium and trace element supply the plant absorbing utilization in the enrichment soil.Calcium polyaspartate is active more excellent polyaspartic acid salts, can promote plant to the absorption of calcium, and nontoxic pollution-free, and calcium polyaspartate can promote other trace elements absorbed in addition, improves the dietetic alimentation of soil and fertilizer.
Disclose the preparation method of the poly-asparagus fern ammonia calcium of a kind of calcium-nutrition intensifying agent among the CN101100510, mainly obtained by poly aspartic acid and calcium hydroxide reaction, regulated neutralization with HCl again, added ethanol calcium polyaspartate is separated out.Consumed above the average age for marriage calcium hydroxide in the aforesaid method, introduced a large amount of chlorions again, excessive chlorion can have a negative impact to product.
CN102504253 discloses a kind of environment-friendly preparation method of agriculture calsium supplement calcium polyaspartate, and its calcium hydroxide and poly-succinimide react in water, add formic acid again, obtain calcium polyaspartate.This method has added a large amount of formic acid, makes pH value of solution reach 4-5, carries out spraying drying again, and formic acid volatilizees or decomposes in the spraying drying, therefore can't realize the good effect of said dried powder dissolution in the patent.
Summary of the invention
The object of the present invention is to provide a kind of production method of rich selenium poly aspartic acid calcium salt, its calcium polyaspartate simple, that obtain contains a large amount of selenium, and be easy to store and transport,
For achieving the above object, the present invention takes following technical scheme:
A kind of production method of rich selenium poly aspartic acid calcium salt, it may further comprise the steps:
1) stirring reaction in the aqueous solution with poly aspartic acid and calcium hydroxide;
2) add selenous acid in above-mentioned solution, filter, the filtrate concentrate drying both got.
As a further improvement on the present invention, described poly aspartic acid and sodium hydroxide mol ratio are 1:3-4.
As a further improvement on the present invention, in the described step 1), temperature of reaction is 30-50 ℃, and the reaction times is 1-2h.
As a further improvement on the present invention, step 2) pH value of filtrate is 3.5-4.5.
In order to obtain being fit to the rich selenium poly aspartic acid calcium salt that agricultural fertilizer is used, the inventor has carried out a large amount of groping and studying, wherein the consumption of poly aspartic acid and calcium hydroxide is 1:3 the best, when the consumption of poly aspartic acid more for a long time, cause hydrolysis insufficient, because poly aspartic acid solvability in neutral aqueous solution and acidic aqueous solution is bad, cause the material waste.
The amount that adds selenous acid also has significant effects to the finished product, the selenous acid adjust pH, and the pH value is low excessively, product acidity is excessive after causing product to redissolve, and is unfavorable for the absorption of farm crop, if the pH value is excessive, can cause poly aspartic acid calcium salt solubility bad, can't satisfy agricultural demand.
The present invention compared with prior art, obtained beneficial effect is:
The present invention adopts poly aspartic acid and calcium hydroxide hydrolysis, directly obtain calcium polyaspartate, adding selenous acid transfers pH to acid, on the one hand can be unnecessary calcium hydroxide neutralization, can provide sour environment on the other hand, guarantee the dissolving of calcium polyaspartate, in addition can also increase the selenium content of farm crop as the nutrient of farm crop.The present invention's filtration obtains the by product calcium selenite and can be used as fodder additives, increases selenium content in the fowl poultry kind body.The production method of rich selenium poly aspartic acid calcium salt provided by the present invention possesses that production method is simple, resource takes full advantage of, and the production time is short, the advantage that efficient is high.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1: the production method of rich selenium poly aspartic acid calcium salt
1) 30 ℃ of stirring reactions in the aqueous solution with 5000g poly aspartic acid and calcium hydroxide 292g;
2) add selenous acid in above-mentioned solution, adjust pH is 4 until pH value of solution, filters, and the filtrate concentrate drying obtains rich selenium poly aspartic acid calcium salt.
Embodiment 2:
1) 50 ℃ of stirring reactions in the aqueous solution with 5000g poly aspartic acid and calcium hydroxide 232g;
2) add selenous acid in above-mentioned solution, adjust pH is 3.5 until pH value of solution, filters, and the filtrate concentrate drying obtains rich selenium poly aspartic acid calcium salt.
Embodiment 3:
1) 40 ℃ of stirring reactions in the aqueous solution with 5000g poly aspartic acid and calcium hydroxide 260g;
2) add selenous acid in above-mentioned solution, adjust pH is 4.5 until pH value of solution, filters, and the filtrate concentrate drying obtains rich selenium poly aspartic acid calcium salt.
Comparative Examples 1: rich selenium poly aspartic acid calcium salt provided by the present invention compares test with the poly aspartic acid calcium salt for preparing according to the CN102504253 method
Take by weighing the rich selenium poly aspartic acid calcium salt 3Kg that the present invention prepares, cooperate 1 ton of urea to mix, it is fertile to be prepared into test; The poly aspartic acid calcium salt 3Kg of the method preparation that provides according to CN102504253 is provided, cooperates 1 ton of urea to mix, it is fertile to be prepared into contrast.
Control measures unanimities such as 15 mu of wheatland areas, sowing apply fertilizer to the subsoil.Wheat period of seedling establishment in 2012 is divided into two districts controlled trial of applying fertilizer:
Test site: test fertile 20Kg/ mu;
Check plot: contrast fertile 20Kg/ mu;
Clear area: common urea 20Kg/ mu;
Result's demonstration: use the wheat of testing fertilizer and the wheat of using contrast fertilizer and common urea and compare, leaf is thick and big, cold-resistant, drought-resistant ability is strong; Be difficult for lodging.Wheat fruit fringe grain is praised quality better greatly.Each index sees Table 1:
Table 1
| Project | Selenium content (μ g/Kg) | Stimulation ratio |
| The test site | 400 | 39.1% |
| The check plot | 60 | 14.4% |
| The clear area | 23 | — |
Conclusion: rich selenium poly aspartic acid calcium salt provided by the present invention can significantly provide the output of farm crop, improves the selenium content in the farm crop, satisfies people to the requirement of selenium content in the grain.
The above only is the preferred embodiments of the present invention; be not limited to the present invention; for a person skilled in the art; the present invention can have change and change; within the spirit and principles in the present invention all; any modification of doing, improvement etc. all should be included within protection scope of the present invention.
Claims (4)
1. the production method of a rich selenium poly aspartic acid calcium salt is characterized in that it may further comprise the steps:
1) stirring reaction in the aqueous solution with poly aspartic acid and calcium hydroxide;
2) add selenous acid in above-mentioned solution, filter, the filtrate concentrate drying both got.
2. a kind of rich selenium poly aspartic acid calcium salt according to claim 1 is characterized in that described poly aspartic acid and sodium hydroxide mol ratio are 1:3-4.
3. a kind of rich selenium poly aspartic acid calcium salt according to claim 1 is characterized in that in the described step 1), temperature of reaction is 30-50 ℃, and the reaction times is 1-2h.
4. according to each described a kind of rich selenium poly aspartic acid calcium salt of claim 1-3, it is characterized in that described step 2) pH value of filtrate is 3.5-4.5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310197066.XA CN103275318B (en) | 2013-05-24 | 2013-05-24 | A kind of production method of rich selenium polyaspartic acid calcium salt |
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| CN201310197066.XA CN103275318B (en) | 2013-05-24 | 2013-05-24 | A kind of production method of rich selenium polyaspartic acid calcium salt |
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| CN103275318A true CN103275318A (en) | 2013-09-04 |
| CN103275318B CN103275318B (en) | 2016-01-20 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100510A (en) * | 2006-07-04 | 2008-01-09 | 北京联合大学 | Calcium polyaspartate |
| CN101302171A (en) * | 2008-06-30 | 2008-11-12 | 瑞发医药股份有限公司 | Production process of pure amino acid chelate and use thereof |
| CN102504253A (en) * | 2011-10-25 | 2012-06-20 | 石家庄开发区德赛化工有限公司 | Environmental-protection preparation method for calcium polyaspartate as agricultural calcium supplement |
| CN102503672A (en) * | 2011-10-25 | 2012-06-20 | 惠州市海纳粮油食品有限公司 | Selenium and ferrum-enriched organic inorganic fertilizer and application method thereof |
| CN103030458A (en) * | 2012-09-18 | 2013-04-10 | 吴江 | Fertilizer synergist and preparation method thereof |
-
2013
- 2013-05-24 CN CN201310197066.XA patent/CN103275318B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100510A (en) * | 2006-07-04 | 2008-01-09 | 北京联合大学 | Calcium polyaspartate |
| CN101302171A (en) * | 2008-06-30 | 2008-11-12 | 瑞发医药股份有限公司 | Production process of pure amino acid chelate and use thereof |
| CN102504253A (en) * | 2011-10-25 | 2012-06-20 | 石家庄开发区德赛化工有限公司 | Environmental-protection preparation method for calcium polyaspartate as agricultural calcium supplement |
| CN102503672A (en) * | 2011-10-25 | 2012-06-20 | 惠州市海纳粮油食品有限公司 | Selenium and ferrum-enriched organic inorganic fertilizer and application method thereof |
| CN103030458A (en) * | 2012-09-18 | 2013-04-10 | 吴江 | Fertilizer synergist and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郎宁等: "《新编肥料施用技术》", 30 June 2002, 广西科学技术出版社 * |
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| CN103275318B (en) | 2016-01-20 |
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