CN106922654A - One-step synthesis prepare hydroxyapatite pesticide, fertilizer slow release complex - Google Patents
One-step synthesis prepare hydroxyapatite pesticide, fertilizer slow release complex Download PDFInfo
- Publication number
- CN106922654A CN106922654A CN201611268306.0A CN201611268306A CN106922654A CN 106922654 A CN106922654 A CN 106922654A CN 201611268306 A CN201611268306 A CN 201611268306A CN 106922654 A CN106922654 A CN 106922654A
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- China
- Prior art keywords
- fertilizer
- solution
- step synthesis
- phosphate
- calcium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- 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
-
- 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
Abstract
The present invention discloses the one-step synthesis for preparing hydroxyapatite pesticide, fertilizer slow release complex, comprises the following steps：Chemical fertilizer or agricultural chemicals are dissolved in phosphate solution, then calcium salt soln is slowly dropped into and is stirred continuously, gained mixed solution is centrifuged again, being deposited under uniform temperature after centrifugation dries and obtain compound.Agricultural chemicals, chemical fertilizer are embedded in the inner mesh of HAP using one-step synthesis, the progressively release of nutrient in agricultural chemicals, fertilizer can be realized, avoid its it is prominent release effect, make drug effect for a long time, plant death or active ingredient losing issue will not be caused because of a large amount of aggregations of nutrient.Because HAP has biodegradable characteristics, products therefrom is phosphate anion and calcium ion after degraded, and these materials not only environmental sound is alternatively arranged as nutrient and gives crop, and long-term use can also improve soil environment.
Description
Technical field
The present invention relates to agricultural chemicals, the preparation method of slow-release fertilizer compound, one-step synthesis preparation is especially disclosed
Hydroxyapatite pesticide, slow-release fertilizer compound, belong to agriculture chemical production technical field.
Background technology
Agricultural chemicals, the sustained release agent of chemical fertilizer can greatly prolong the lasting period of same dose agricultural chemicals, reduce the use time of agricultural chemicals, chemical fertilizer
Number and total consumption, significantly reduce residual and the possibility of pollution, also reduce agricultural chemicals, the toxicity of chemical fertilizer and poisoning.
Existing agricultural chemicals, Chemical industry preparation method based on coating, coating, support methods.Coated fertilizer used is such as
Pitch, paraffin, sulphur etc., this method production process are complicated, relatively costly, itself do not dissolve in water, and insoluble drug release is difficult, and long
Phase, using that can cause soil acidification, destroys soil texture；And it was conventional such as sepiolite, clay, bentonite, diatom in the past in support methods
Used as carrier is bonded, by agricultural chemicals, chemical fertilizer absorption in its surface duct, and product load capacity prepared by this method has soil etc.
Limit, and have phenomenon of burst release；So be embedded in inside hydroxyapatite for agricultural chemicals, chemical fertilizer using one-step synthesis by the present invention, not only
Considerably increase load capacity, moreover it is possible to reach the purpose of sustained release release.
The content of the invention
The present invention discloses one-step synthesis and prepares hydroxyapatite pesticide, fertilizer slow release complex, solve it is existing such
Easily there is phenomenon of burst release in the slow release complex of type.
One-step synthesis of the invention prepare hydroxyapatite pesticide, fertilizer slow release complex, comprise the following steps：
Chemical fertilizer or agricultural chemicals are dissolved in phosphate solution, then calcium salt soln is slowly dropped into and is stirred continuously, gained mixing is molten
Liquid is centrifuged again, and being deposited under uniform temperature after centrifugation dries and obtain compound.
Above-mentioned method, comprises the following steps that：
Solution A is prepared：0.2-6.0mol/L calcium salt soln 4-23ml are weighed, is shaken up standby；
Solution B is prepared：25~the 100ml of phosphate solution of 0.2-6.0mol/L is weighed, pH value is adjusted in 7.5- with concentrated ammonia liquor
Between 10.5, shake up standby；
Solution A is 1.68 with the Ca/P ratios of solution B；
25~500mg of starting material is weighed, solution B dissolving is slowly stirred；Solution A is gradually added drop-wise in solution B again, is kept
Between 38 DEG C~60 DEG C, pH value is slowly stirred 1~3 hour temperature of reaction system between 6.5~11.0；Reaction solution room temperature
Lower 10000rpm/min is centrifuged 5-21 minutes；Centrifuged deposit is dried 24~72 hours at room temperature, and products therefrom is in 4 DEG C of preservations.
Calcium salt is selected from the methods described above：In calcium acetate, calcium sulfate, calcium phosphate, calcium chloride, calcium hydroxide, calcium oxide
Appoint.
Phosphate is selected from the methods described above：Ammonium hydrogen carbonate, diammonium hydrogen phosphate, Polyquaternium-10, NaOH, phosphorus
Appointing or various in sour potassium, dipotassium hydrogen phosphate, phosphoric acid, sodium dihydrogen phosphate.
The starting material that the above method is related to is appointing in nitrogenous fertilizer, phosphate fertilizer, potash fertilizer and its compound fertilizer or mixed fertilizer.
Starting material can also be：Appointing in mineral source pesticide, biogenic pesticide and chemical pesticide.
Bonding carrier (hydroxyapatite) used by the present invention due to being nano level carrier, so with very big ratio table
Area, thus have stronger absorption and bearing capacity；Adsorbed duct agricultural chemicals, chemical fertilizer elder generation outside HAP before this during release
Discharge, the degraded then as HAP makes inner material gradually discharge, so as to reach slow releasing function.
Specific embodiment
For the ease of understanding the present invention, especially exemplified by following examples.Its effect is understood to be to explaination of the invention
It is non-to any type of limitation of the invention.
Embodiment 1
Solution A is prepared：Accurately anhydrous calcium acetate 0.706g is weighed, plus redistilled water is settled to 10ml, shaken up standby；
Solution B is prepared：Ammonium hydrogen carbonate 1.374g, Polyquaternium-10 4.089g, plus redistilled water 45ml accurately are weighed, concentrated ammonia liquor is used
Regulation pH value adds redistilled water and is settled to 50ml 7.6 or so, shakes up standby；Polyquaternium-10, can be after Term Fertilization
Directional proliferation beneficial bacterium in culture medium or soil, excludes miscellaneous bacteria, builds up fertility.
Urea 300mg accurately is weighed, is dissolved in solution B (50ml), be slowly stirred to being completely dissolved；Again by solution A
(10ml) is gradually added drop-wise in solution B, is slowly stirred 2 hours；10000rpm/min is centrifuged 15 minutes reaction solution at room temperature；From
Precipitation is dried at room temperature for 48 hours after the heart, 4 DEG C of preservations.
Embodiment 2
Solution A is prepared：Accurately calcium sulfate 1.336g is weighed, plus redistilled water is settled to 10ml, shaken up standby；
Solution B is prepared：Ammonium phosphate 0.358g, plus redistilled water 45ml accurately are weighed, pH value is adjusted 8.6 or so with concentrated ammonia liquor, mended
Plus redistilled water is settled to 50ml, shake up standby；
Potassium sulfate 200mg accurately is weighed, is dissolved in solution B (50ml), be slowly stirred to being completely dissolved；Again by solution A (10ml)
Gradually it is added drop-wise in solution B, is slowly stirred 2 hours；12000rpm/min is centrifuged 12 minutes reaction solution at room temperature；Sunk after centrifugation
Shallow lake is dried at room temperature for 72 hours, 4 DEG C of preservations.
Embodiment 3
Solution A is prepared：Accurately calcium sulfate 0.759g is weighed, plus redistilled water is settled to 50ml, shaken up standby；
Solution B is prepared：Diammonium hydrogen phosphate 0.195g, plus redistilled water 245ml accurately are weighed, it is left 9.0 to adjust pH value with concentrated ammonia liquor
The right side, adds redistilled water and is settled to 500ml, shakes up standby；
Calcium phosphate 400mg accurately is weighed, is dissolved in solution B (500ml), be slowly stirred to being completely dissolved；Again by solution A (50ml)
Gradually it is added drop-wise in solution B, is slowly stirred 2 hours；13000rpm/min is centrifuged 10 minutes reaction solution at room temperature；Sunk after centrifugation
Shallow lake is dried at room temperature for 48 hours, 4 DEG C of preservations.
Embodiment 4
Solution A is prepared：Accurately calcium phosphate 0.654g is weighed, plus redistilled water is settled to 10ml, shaken up standby；
Solution B is prepared：Diammonium hydrogen phosphate 0.518g, plus redistilled water 45ml accurately are weighed, it is left 9.0 to adjust pH value with concentrated ammonia liquor
The right side, adds redistilled water and is settled to 50ml, shakes up standby；
Copper sulphate 50mg accurately is weighed, is dissolved in solution B (50ml), be slowly stirred；Solution A (10ml) is gradually added drop-wise to again molten
In liquid B, it is slowly stirred 2 hours；13000rpm/min is centrifuged 12 minutes reaction solution at room temperature；Centrifuged deposit is done at room temperature
Dry 48 hours, obtain final product.
Test example
Weigh the hydroxyapatite/thiourea slow release fertilizer 5.5g of embodiment 1, then with distilled water clean, dry after cross 20 mesh sieves
The 500g quartz sands in hole are well mixed, and are fitted into chromatographic column, make its elastic appropriateness of filling, then instill distilled water, and drop speed is
0.5ml/min, liquid is collected with receiver, and 10 receivers are set altogether, and each receiver collects 20min (about 10.0ml altogether),
Liquid 1.00ml is taken from each receiver again, adds the 3ml concentrated sulfuric acids to be digested, then distilled with semimicro azotometer,
Absorbed with 2% boric acid, titrated with 0.040NHCl, as a result see the table below.
Experimental data shows, compared with conventional use of urea, using this fertilizer, and more than one times of its leaching speed reduction,
Sustained release purpose is reached.The use of this fertilizer is to preserving the ecological environment with positive role and realistic meaning, while implementing
Cheng Sheng fertilizer savings of labor.
The nitrogen content change table of comparisons in urea and slow release fertilizer under Simulated rainwater Scouring Condition
The comparing of different embodiment gained slow release fertilizer slow release effects in soil
Claims (6)
1. the one-step synthesis of hydroxyapatite pesticide, fertilizer slow release complex are prepared, is comprised the following steps that：
1）Solution A is prepared：0.2-6.0mol/L calcium salt soln 4-23ml are weighed, is shaken up standby；
2）Solution B is prepared：25~the 100ml of phosphate solution of 0.2-6.0mol/L is weighed, pH value is adjusted in 7.5- with concentrated ammonia liquor
Between 10.5, shake up standby；
3）Solution A is 1.67 with the Ca/P ratios of solution B；25~500mg of fertilizer or agricultural chemicals is weighed, solution B dissolving is slowly stirred；
Solution A is gradually added drop-wise in solution B again, keep temperature of reaction system between 38 DEG C~60 DEG C, pH value 6.5~11.0 it
Between, it is slowly stirred 1~3 hour；10000rpm/min is centrifuged 10~20 minutes reaction solution at room temperature；Centrifuged deposit is done at room temperature
Dry 24~72 hours, products therefrom was in 4 DEG C of preservations.
2. one-step synthesis according to claim 1, it is characterised in that：Calcium salt be selected from calcium acetate, calcium sulfate, calcium phosphate,
Appointing in calcium chloride, calcium hydroxide, calcium oxide.
3. one-step synthesis according to claims 1, it is characterised in that：Phosphate is selected from ammonium hydrogen carbonate, phosphoric acid hydrogen two
Appointing or various in ammonium, Polyquaternium-10, NaOH, potassium phosphate, dipotassium hydrogen phosphate, phosphoric acid, sodium dihydrogen phosphate.
4. one-step synthesis according to claims 1, it is characterised in that starting material be nitrogenous fertilizer, phosphate fertilizer, potash fertilizer and its
Appointing in compound fertilizer or mixed fertilizer.
5. one-step synthesis according to claims 1, it is characterised in that starting material can also be：Mineral source pesticide,
Appointing in biogenic pesticide and chemical pesticide.
6. one-step synthesis according to claims 1, it is characterised in that bonding carrier (hydroxyapatite) used by
Then nano level carrier, so with very big specific surface area, thus have stronger absorption and bearing capacity；In release process
In adsorbed duct agricultural chemicals, chemical fertilizer outside HAP before this and first discharged, the degraded then as HAP makes inner material gradually release
Put, so as to reach slow releasing function.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611268306.0A CN106922654A (en) | 2016-12-31 | 2016-12-31 | One-step synthesis prepare hydroxyapatite pesticide, fertilizer slow release complex |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611268306.0A CN106922654A (en) | 2016-12-31 | 2016-12-31 | One-step synthesis prepare hydroxyapatite pesticide, fertilizer slow release complex |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106922654A true CN106922654A (en) | 2017-07-07 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611268306.0A Withdrawn CN106922654A (en) | 2016-12-31 | 2016-12-31 | One-step synthesis prepare hydroxyapatite pesticide, fertilizer slow release complex |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110881462A (en) * | 2019-11-25 | 2020-03-17 | 南京启佑生物科技有限公司 | Nano pesticide composite preparation based on phosphate and metal ions and preparation method thereof |
| CN112142526A (en) * | 2020-10-31 | 2020-12-29 | 青岛一亩地农业科技有限责任公司 | Environment-friendly multi-element slow-release fertilizer and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589709A (en) * | 2009-07-03 | 2009-12-02 | 吉林大学 | Adsorption method for preparing hydroxyapatite pesticide, slow-release fertilizer compound |
| CN101653114A (en) * | 2009-07-03 | 2010-02-24 | 吉林大学 | Hydroxyl apatite pesticide and fertilizer slow release complex prepared by one step synthesis |
| CN105327364A (en) * | 2015-12-15 | 2016-02-17 | 浙江理工大学 | Nanometer-hydroxyapatite-siRNA compound and preparing method thereof |
| CN106044734A (en) * | 2016-06-23 | 2016-10-26 | 宝钢发展有限公司 | Method for preparing nano-hydroxyapatite |
-
2016
- 2016-12-31 CN CN201611268306.0A patent/CN106922654A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589709A (en) * | 2009-07-03 | 2009-12-02 | 吉林大学 | Adsorption method for preparing hydroxyapatite pesticide, slow-release fertilizer compound |
| CN101653114A (en) * | 2009-07-03 | 2010-02-24 | 吉林大学 | Hydroxyl apatite pesticide and fertilizer slow release complex prepared by one step synthesis |
| CN105327364A (en) * | 2015-12-15 | 2016-02-17 | 浙江理工大学 | Nanometer-hydroxyapatite-siRNA compound and preparing method thereof |
| CN106044734A (en) * | 2016-06-23 | 2016-10-26 | 宝钢发展有限公司 | Method for preparing nano-hydroxyapatite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110881462A (en) * | 2019-11-25 | 2020-03-17 | 南京启佑生物科技有限公司 | Nano pesticide composite preparation based on phosphate and metal ions and preparation method thereof |
| CN112142526A (en) * | 2020-10-31 | 2020-12-29 | 青岛一亩地农业科技有限责任公司 | Environment-friendly multi-element slow-release fertilizer and preparation method thereof |
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Application publication date: 20170707 |
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| WW01 | Invention patent application withdrawn after publication |