CN103275318B - A kind of production method of rich selenium polyaspartic acid calcium salt - Google Patents
A kind of production method of rich selenium polyaspartic acid calcium salt Download PDFInfo
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- CN103275318B CN103275318B CN201310197066.XA CN201310197066A CN103275318B CN 103275318 B CN103275318 B CN 103275318B CN 201310197066 A CN201310197066 A CN 201310197066A CN 103275318 B CN103275318 B CN 103275318B
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Abstract
The present invention relates to a kind of production method of rich selenium polyaspartic acid calcium salt, it comprises the following steps: by poly aspartic acid and calcium hydroxide stirring reaction in aqueous; In above-mentioned solution, add selenous acid, filter, filtrate concentrate drying both obtained.The production method of rich selenium polyaspartic acid calcium salt provided by the present invention, possesses that production method is simple, resource makes full use of, and the production time is short, the advantage that efficiency is high.
Description
Technical field
The present invention relates to the production method of polyaspartic acid calcium salt, relate in particular to a kind of production method of rich selenium polyaspartic 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 characteristics such as raising body immunity, antagonism heavy metal etc.General people absorb selenium by agricultural-food, and NI recommends daily intake to be per capita 50-200 microgram, but the selenium intake of China is only 26-32 microgram.In order to increase the intake of selenium, market starts 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, extremely strong chelating function is possessed to plant desired nutritional composition, can effectively in Enriching soil nitrogen, phosphorus, potassium and trace element utilize for plant absorption.Calcium polyaspartate is activity preferably polyaspartic acid salts, can promote that plant is to the absorption of calcium, and nontoxic pollution-free, calcium polyaspartate can promote the absorption of other trace elements in addition, improves the dietetic alimentation of soil and fertilizer.
Disclose the preparation method that a kind of calcium-nutrition intensifying agent gathers asparagus fern ammonia calcium in CN101100510, obtain primarily of poly aspartic acid and calcium hydroxide reaction, then regulate neutralization with HCl, add ethanol and calcium polyaspartate is separated out.Consume above the average age for marriage calcium hydroxide in aforesaid method, in turn introduce a large amount of chlorions, 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, then add formic acid, obtain calcium polyaspartate.The method adds a large amount of formic acid, makes pH value of solution reach 4-5, then carries out spraying dry, and in spraying dry, formic acid has volatilized or decomposed, and therefore cannot realize the effect that in patent, said dried powder dissolution is good.
Summary of the invention
The object of the present invention is to provide a kind of production method of rich selenium polyaspartic acid calcium salt, its calcium polyaspartate that is simple, that obtain contains a large amount of selenium, and be easy to storage and transport,
For achieving the above object, the present invention takes following technical scheme:
A production method for rich selenium polyaspartic acid calcium salt, it comprises the following steps:
1) by poly aspartic acid and calcium hydroxide stirring reaction in aqueous;
2) in above-mentioned solution, add selenous acid, filter, filtrate concentrate drying both obtained.
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 described step 1), temperature of reaction is 30-50 DEG C, 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 the rich selenium polyaspartic acid calcium salt of applicable agricultural fertilizer, present inventor has performed a large amount of groping and studying, wherein the consumption of poly aspartic acid and calcium hydroxide is that 1:3 is best, when the consumption of poly aspartic acid is more, cause hydrolysis insufficient, because poly aspartic acid solvability in neutral aqueous solution and acidic aqueous solution is bad, cause material waste.
The amount adding selenous acid also has important impact to the finished product, selenous acid adjust pH, and pH value is too low, after causing product to redissolve, product acidity is excessive, is unfavorable for the absorption of farm crop, if pH value is excessive, polyaspartic acid calcium salt solubility can be caused bad, cannot agricultural demand be met.
Compared with prior art, acquired beneficial effect is in the present invention:
The present invention adopts poly aspartic acid and calcium hydroxide to be hydrolyzed, directly obtain calcium polyaspartate, adding selenous acid adjusts pH to acid, unnecessary calcium hydroxide can be neutralized on the one hand, sour environment can be provided on the other hand, ensure 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 by product calcium selenite as fodder additives, can increase selenium content in fowl poultry kind body.The production method of rich selenium polyaspartic acid calcium salt provided by the present invention, possesses that production method is simple, resource makes full use of, and the production time is short, the advantage that efficiency is high.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1: the production method of rich selenium polyaspartic acid calcium salt
1) by 5000g poly aspartic acid and calcium hydroxide 292g 30 DEG C of stirring reactions in aqueous;
2) in above-mentioned solution, add selenous acid, adjust pH, until pH value of solution is 4, filter, filtrate concentrate drying obtains rich selenium polyaspartic acid calcium salt.
Embodiment 2:
1) by 5000g poly aspartic acid and calcium hydroxide 232g 50 DEG C of stirring reactions in aqueous;
2) in above-mentioned solution, add selenous acid, adjust pH, until pH value of solution is 3.5, filter, filtrate concentrate drying obtains rich selenium polyaspartic acid calcium salt.
Embodiment 3:
1) by 5000g poly aspartic acid and calcium hydroxide 260g 40 DEG C of stirring reactions in aqueous;
2) in above-mentioned solution, add selenous acid, adjust pH, until pH value of solution is 4.5, filter, filtrate concentrate drying obtains rich selenium polyaspartic acid calcium salt.
Comparative example 1: rich selenium polyaspartic acid calcium salt provided by the present invention compares test with the polyaspartic acid calcium salt prepared according to CN102504253 method
Take the rich selenium polyaspartic acid calcium salt 3Kg that the present invention prepares, coordinate 1 ton of urea mixing, be prepared into test fertile; Polyaspartic acid calcium salt 3Kg prepared by the method that taking provides according to CN102504253, coordinates 1 ton of urea mixing, is prepared into contrast fertile.
Wheatland area 15 mu, the sowing control measures such as to apply fertilizer to the subsoil are consistent.Wheat period of seedling establishment in 2012 is divided into Liang Ge district and carries out fertilising controlled trial:
Test site: test fertile 20Kg/ mu;
Check plot: contrast fertile 20Kg/ mu;
Clear area: common urea 20Kg/ mu;
Result shows: use the fertile wheat of test and use the wheat contrasting fertilizer and common urea and compare, leaf thick and large, cold-resistant, drought-resistant ability is strong; Not easily lodge.Wheat fruit fringe grain is large and praise, quality better.Each index is in table 1:
Table 1
| Project | Selenium content (μ g/Kg) | Stimulation ratio |
| Test site | 400 | 39.1% |
| Check plot | 60 | 14.4% |
| Clear area | 23 | — |
Conclusion: rich selenium polyaspartic acid calcium salt provided by the present invention significantly can provide the output of farm crop, improves the selenium content in farm crop, meets the requirement of people to selenium content in grain.
The foregoing is only 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; the any amendment, improvement etc. done, all should be included within protection scope of the present invention.
Claims (1)
1., for a production method for the rich selenium polyaspartic acid calcium salt of agricultural fertilizer, it is characterized in that it comprises the steps:
By 5000g poly aspartic acid and sodium hydroxide 232g 50 DEG C of stirring reactions in aqueous;
In above-mentioned solution, add selenous acid, until solution ph is 3.5, filter, filtrate concentrate drying had both obtained rich selenium polyaspartic acid calcium salt;
Described rich selenium polyaspartic acid calcium salt adopts following methods for the preparation of during agricultural fertilizer: the rich selenium polyaspartic acid calcium salt 3000g taking above-mentioned preparation, coordinates 1 ton of urea mixing obtained.
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| Application Number | Priority Date | Filing Date | Title |
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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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| 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 CN103275318A (en) | 2013-09-04 |
| CN103275318B true 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 |
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| CN103275318A (en) | 2013-09-04 |
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