CN107324924A - A kind of nanometer selenium fertilizer with slow-release function and preparation method thereof - Google Patents
A kind of nanometer selenium fertilizer with slow-release function and preparation method thereof Download PDFInfo
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- CN107324924A CN107324924A CN201710741833.7A CN201710741833A CN107324924A CN 107324924 A CN107324924 A CN 107324924A CN 201710741833 A CN201710741833 A CN 201710741833A CN 107324924 A CN107324924 A CN 107324924A
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- selenium
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- release function
- ethanol
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
- C05G5/37—Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of nanometer selenium fertilizer with slow-release function and preparation method thereof.The described nanometer selenium fertilizer with slow-release function is to be reacted with elder generation with the ethanol solution of raw material elemental selenium grain and borohydride salts, then hydroxyl beta cyclodextrin and the reaction of polyvinyl alcohol liquid are added, N, P, K salt and starch are being added, spray-dried granulation, which obtains object, has the nanometer selenium fertilizer of slow-release function；The primary dissolution rate of the described nanometer selenium fertilizer with slow-release function is 10 ~ 15%, and differential solubility is 1 ~ 3%.It is to mix the ethanol solution of borohydride salts with elemental selenium at 0 ~ 90 DEG C of temperature, add the mixture formation mixed system of ethanol and dimethyl carbonate, in 10 ~ 60min of stirring reaction at 0 ~ 90 DEG C of temperature, then add hydroxyl beta cyclodextrin and polyvinyl alcohol liquid continues to react addition solubility 10 ~ 30min of N, P, K salt and starch reaction after 10 ~ 60min is red, transparent to solution, spray-dried granulation, which obtains object, has the nanometer selenium fertilizer of slow-release function.
Description
Technical field
The invention belongs to technical field of fertilizers, and in particular to a kind of with the nanometer selenium fertilizer of slow-release function and its preparation side
Method.
Background technology
One of micronutrient element necessary to selenium is animals and humans, with many important physiological functions.Selenium is in the earth
Upper distribution is very unbalanced, it is known to more than 40 countries and regions selenium deficiency.China's selenium deficiency area is related to 22 provinces (urban district), the whole nation
72% or so county is selenium deficiency Huo Dixi counties.The many region of China disease occurred frequently, such as Keshan disease, Kaschin-Beck disease, cancer, heart and brain blood
The diseases such as pipe disease, diabetes, immunity of organisms decline and aging course are relevant with selenium intake deficiency in meals.Although excessive
Take in selenium harmful, but the harm that selenium deficiency is caused then can not be ignored.Therefore, in the regional selenium-supply of low selenium and selenium deficiency, oneself turns into people
Disease preventing and treating, ensure one of focus of health.Selenium-enriched food is one of main path that people reach selenium-supply purpose.Many is ground
Study carefully proof, the plant such as wheat, tomato, potato and tea tree has the ability of stronger Enriching Selenium.Raising has stronger accumulation ability to selenium
The content of selenium in crops, it has also become one of study hotspot of current Crops in Applying Fertilizer.It is mainly at present using the method for selenium fertilizer
Foliage spray selenate or selenite solution and soil is directly applied selenium fertilizer, but so easily cause selenium be lost in, selenosis and into
This is higher, and increases the pollution to environment.In this context, it is considered to the suction according to crops different growth phases to selenium
Receive and require, artificially control supply and the rate of release of selenium, i.e., when crop needs, selenium can be discharged for its profit
With, and unwanted when, then can be retained in soil, so that applied once disclosure satisfy that the need of each growth phase of crop
Will, it is the developing direction for researching and developing selenium fertilizer.As far as we know, there is presently no the relevant report on controlled release selenium fertilizer for root.
Therefore, controlled release selenium fertilizer is prepared, leaching loss, degenerations, volatilization in soil of selenium etc. is reduced and loses, at the same it is saving of labor, time saving, laborsaving,
Once a large amount of use will not produce injury to crop root, and improve the utilization rate of selenium, reduce the pollution to environment, this has
Important meaning and practical value.
The content of the invention
The first object of the present invention is to provide a kind of nanometer selenium fertilizer with slow-release function；Second purpose is to provide
The preparation method of the described nanometer selenium fertilizer with slow-release function.
The first object of the present invention is achieved in that the described nanometer selenium fertilizer with slow-release function is with original with elder generation
Expect that the ethanol solution of elemental selenium grain and borohydride salts reacts, then add hydroxy-beta cyclodextrin and the reaction of polyvinyl alcohol liquid,
N, P, K salt and starch are being added, spray-dried granulation, which obtains object, has the nanometer selenium fertilizer of slow-release function；Described tool
The primary dissolution rate for having the nanometer selenium fertilizer of slow-release function is 10 ~ 15%, and differential solubility is 1 ~ 3%.
The second object of the present invention is achieved in that the ethanol solution and list of borohydride salts at 0 ~ 90 DEG C of temperature
Matter selenium is mixed, and adds the mixture formation mixed system of ethanol and dimethyl carbonate, in stirring reaction 10 at 0 ~ 90 DEG C of temperature ~
60min, then adds hydroxy-beta cyclodextrin and polyvinyl alcohol liquid continues to react 10 ~ 60min to solution for after red, transparent
Solubility 10 ~ 30min of N, P, K salt and starch reaction is added, spray-dried granulation, which obtains object, has receiving for slow-release function
Rice selenium fertilizer.
The present invention prepares selenium fertilizer using biological natural polymer raw material, and is wrapped on this basis using polymer
Wrap up in, system respectively goes out the selenium fertilizer of secondary embedding.Using hydride occur an atomic fluorescence spectrometry to selenium fertilizer primary dissolution rate and
Differential solubility is determined, and carries out effect assessment to selenium fertilizer.The index of the Controlled Release Fertilizer proposed in the world is imprisoned to be primary molten
Extracting rate is less than 15%, differential solubility 0.25% ~ 2.5%.The too high fertilizer of primary dissolution rate shows that controlled release properties are poor, differential
Dissolution rate too low release and release control fertilizer, because rate of release is too slow, when being administered alone, needs fertile peak period in crop, easily supports
The problem of dividing insufficient.Nanometer selenium fertilizer of the present invention with slow-release function is combined the index of Controlled Release Fertilizer.
Embodiment
With reference to embodiment, the present invention is further illustrated, but the present invention is not any limitation as in any way,
Based on present invention teach that any conversion or replacement made, belong to protection scope of the present invention.
Nanometer selenium fertilizer of the present invention with slow-release function is with raw material elemental selenium grain and borohydride salts with elder generation
Ethanol solution reacts, and then adds hydroxy-beta cyclodextrin and the reaction of polyvinyl alcohol liquid, is adding N, P, K salt and starch, warp
Spray drying granulation, which obtains object, has the nanometer selenium fertilizer of slow-release function；The described nanometer selenium fertilizer with slow-release function
Primary dissolution rate be 10 ~ 15%, differential solubility be 1 ~ 3%.
Nanometer selenium fertilizer of the present invention with slow-release function, is by the ethanol of borohydride salts at 0 ~ 90 DEG C of temperature
Solution is mixed with elemental selenium, adds the mixture formation mixed system of ethanol and dimethyl carbonate, is stirred at 0 ~ 90 DEG C of temperature
10 ~ 60min of reaction is mixed, it is red to solution then to add hydroxy-beta cyclodextrin and polyvinyl alcohol liquid continuation 10 ~ 60min of reaction
Solubility 10 ~ 30min of N, P, K salt and starch reaction is added after color is transparent, spray-dried granulation, which obtains object, has sustained release
The nanometer selenium fertilizer of function.
Described borohydride salts are the one or more in hydroboration metal salt.
Described borohydride salts are sodium borohydride or potassium borohydride.
The mass concentration of the ethanol solution of described borohydride salts is 1 ~ 99%.
The mol ratio of borohydride salts and elemental selenium is 1 ~ 15 in the ethanol solution of borohydride salts:1~10.
The volume ratio of ethanol and dimethyl carbonate in described ethanol and the mixture formation mixed system of dimethyl carbonate
For 1:0.1~50.
The volume ratio of ethanol and dimethyl carbonate in described ethanol and the mixture formation mixed system of dimethyl carbonate
For 1:1~5.
Hydroxy-beta cyclodextrin and polyvinyl alcohol liquid mol ratio are 1~20: 1~10.
Soluble N, P, K salt is ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium sulfate, urea, potassium chloride, potassium hydrogen phosphate or phosphoric acid
Potassium dihydrogen.
The temperature of mixed system reaction is 60 DEG C.
Dry temperature is 50 ~ 70 DEG C.
So that case is embodied, the present invention will be further described below：
Embodiment 1
15g elemental selenium grain is taken, 15g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml adds in 30 C water baths
The ethanol that heat is crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 40ml：40ml）, reaction temperature is warming up to 50 DEG C, at this
At a temperature of shake up reaction 20 minutes, after after selenium grain reaction completely, add hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 100
（Its mixed proportion is 50ml：50ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g sulfuric acid after solution is red, transparent
Potassium, 5g starch, the completely water-soluble blush nano selenium fertilizers of 158g are obtained after continuing reaction 20 minutes in 130 DEG C of spray drying granulations
Material.After tested, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 13.8%, differential
Dissolution rate is 1.98%, is combined the index of Controlled Release Fertilizer.
Embodiment 2
20g elemental selenium grain is taken, 15g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml adds in 50 C water baths
The ethanol that heat is crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 40ml：4ml）, reaction temperature is warming up to 80 DEG C, at this
At a temperature of shake up reaction 10 minutes, after after selenium grain reaction completely, add hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 150
（Its mixed proportion is 100ml：50ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g sulfuric acid after solution is red, transparent
Potassium, 10g starch, the completely water-soluble blush nano selenium fertilizers of 182g are obtained after continuing reaction 30 minutes in 130 DEG C of spray drying granulations
Material.After tested, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 12.2%, differential
Dissolution rate is 2.2%, is combined the index of Controlled Release Fertilizer.
Embodiment 3
15g elemental selenium grain is taken, 20g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml adds in 10 C water baths
The ethanol that heat is crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 1ml：50ml）, reaction temperature is warming up to 50 DEG C, at this
At a temperature of shake up reaction 20 minutes, after after selenium grain reaction completely, add hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 100
（Its mixed proportion is 50ml：50ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g sulfuric acid after solution is red, transparent
Potassium, 5g starch, the completely water-soluble blush nano selenium fertilizers of 158g are obtained after continuing reaction 20 minutes in 130 DEG C of spray drying granulations
Material.After tested, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 11.8%, differential
Dissolution rate is 2.98%, is combined the index of Controlled Release Fertilizer.
Embodiment 4
5g elemental selenium grain is taken, 15g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml is heated in 20 C water baths
The ethanol crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 40ml：40ml）, reaction temperature is warming up to 50 DEG C, in the temperature
Reaction 20 minutes is shaken up under degree, after after selenium grain reaction completely, hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 33 is added（Its
Mixed proportion is 30ml：3ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g potassium sulfates, 5g after solution is red, transparent
Starch, the completely water-soluble blush nanometer selenium fertilizer of 158g is obtained after continuing reaction 20 minutes in 130 DEG C of spray drying granulations.Through surveying
Examination, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 10.8%, and differential solubility is
1.88%, it is combined the index of Controlled Release Fertilizer.
Embodiment 5
10g elemental selenium grain is taken, 15g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml adds in 80 C water baths
The ethanol that heat is crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 40ml：40ml）, reaction temperature is warming up to 90 DEG C, at this
At a temperature of shake up reaction 10 minutes, after after selenium grain reaction completely, add hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 100
（Its mixed proportion is 60ml：40ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g sulfuric acid after solution is red, transparent
Potassium, 5g starch, the completely water-soluble blush nano selenium fertilizers of 158g are obtained after continuing reaction 10 minutes in 130 DEG C of spray drying granulations
Material.After tested, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 13.9%, differential
Dissolution rate is 1.98%, is combined the index of Controlled Release Fertilizer.
Embodiment 6
25g elemental selenium grain is taken, 10g sodium borohydrides are sequentially placed into three-neck flask, and injection 80ml adds in 20 C water baths
The ethanol that heat is crossed and dimethyl carbonate mixed liquor（Its mixed proportion is 40ml：80ml）, reaction temperature is warming up to 60 DEG C, at this
At a temperature of shake up reaction 20 minutes, after after selenium grain reaction completely, add hydroxy-beta cyclodextrin and the ml of polyvinyl alcohol liquid 100
（Its mixed proportion is 50ml：50ml）Continue to react, enter plus 50g ammonium dihydrogen phosphates, 40g sulfuric acid after solution is red, transparent
Potassium, 5g starch, the completely water-soluble blush nano selenium fertilizers of 158g are obtained after continuing reaction 20 minutes in 130 DEG C of spray drying granulations
Material.After tested, the primary dissolution rate for the nanometer selenium fertilizer with slow-release function that the present embodiment is prepared is 12.6%, differential
Dissolution rate is 1.78%, is combined the index of Controlled Release Fertilizer.
Claims (10)
1. a kind of nanometer selenium fertilizer with slow-release function, it is characterised in that the described nanometer selenium fertilizer with slow-release function is
Reacted with elder generation with the ethanol solution of raw material elemental selenium grain and borohydride salts, then add hydroxy-beta cyclodextrin and polyvinyl alcohol
Liquid reacts, and is adding N, P, K salt and starch, spray-dried granulation, which obtains object, has the nanometer selenium fertilizer of slow-release function；
The primary dissolution rate of the described nanometer selenium fertilizer with slow-release function is 10 ~ 15%, and differential solubility is 1 ~ 3%.
2. the nanometer selenium fertilizer with slow-release function described in a kind of claim 1, it is characterised in that be at 0 ~ 90 DEG C of temperature
The ethanol solution of borohydride salts is mixed with elemental selenium, the mixture formation mixed system of ethanol and dimethyl carbonate is added,
In 10 ~ 60min of stirring reaction at 0 ~ 90 DEG C of temperature, then add hydroxy-beta cyclodextrin and polyvinyl alcohol liquid continues to react 10
10 ~ 30min of addition solubility N, P, K salt and starch reaction, spray-dried to granulate after ~ 60min is red, transparent to solution
There is the nanometer selenium fertilizer of slow-release function to object.
3. preparation method according to claim 2, it is characterised in that described borohydride salts is in hydroboration metal salts
It is one or more of.
4. the preparation method of the high-purity nm selenium material according to Claims 2 or 3, it is characterised in that described borohydride salts
For sodium borohydride or potassium borohydride.
5. the preparation method of high-purity nm selenium material according to claim 1, it is characterised in that described borohydride salts
The mass concentration of ethanol solution is 1 ~ 99%.
6. the preparation method of high-purity nm selenium material according to claim 1, it is characterised in that the ethanol of borohydride salts is molten
The mol ratio of borohydride salts and elemental selenium is 1 ~ 15 in liquid:1~10.
7. the preparation method of high-purity nm selenium material according to claim 1, it is characterised in that described ethanol and carbonic acid
The volume ratio of ethanol and dimethyl carbonate is 1 in the mixture formation mixed system of dimethyl ester:0.1~50.
8. the preparation method of the high-purity nm selenium material according to claim 1 or 7, it is characterised in that described ethanol and carbon
The volume ratio of ethanol and dimethyl carbonate is 1 in the mixture formation mixed system of dimethyl phthalate:1~5.
9. the preparation method of high-purity nm selenium material according to claim 1, it is characterised in that hydroxy-beta cyclodextrin and poly-
Vinyl alcohol mixed liquor mol ratio is 1~20: 1~10.
10. the preparation method of high-purity nm selenium material according to claim 1, it is characterised in that soluble N, P, K salt is
Ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium sulfate, urea, potassium chloride, potassium hydrogen phosphate or potassium dihydrogen phosphate.
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| CN201710741833.7A CN107324924A (en) | 2017-08-25 | 2017-08-25 | A kind of nanometer selenium fertilizer with slow-release function and preparation method thereof |
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| CN201710741833.7A CN107324924A (en) | 2017-08-25 | 2017-08-25 | A kind of nanometer selenium fertilizer with slow-release function and preparation method thereof |
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2017
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| CN1594236A (en) * | 2004-07-06 | 2005-03-16 | 湖南大学 | Nano selenium nutrition conditioning agent for fruit and vegetable and its preparing process |
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Effective date of registration: 20191029 Address after: Room 305, building a, innovation and entrepreneurship center, 227 Zixi Avenue, Chuxiong hi tech Zone, Chuxiong Yi Autonomous Prefecture, Yunnan Province Applicant after: Chuxiong hi tech Zone nuclear degree selenium rich Biotechnology Development Co., Ltd. Address before: Panlong District Jinchen Street Village 650000 Yunnan city of Kunming Province, a 31 Building 5 Applicant before: Yunnan Nuclear Biological Industry Development Co., Ltd. |