CN103588793A - Complex type sustained/controlled release urea fertilizer - Google Patents
Complex type sustained/controlled release urea fertilizer Download PDFInfo
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- CN103588793A CN103588793A CN201310572675.9A CN201310572675A CN103588793A CN 103588793 A CN103588793 A CN 103588793A CN 201310572675 A CN201310572675 A CN 201310572675A CN 103588793 A CN103588793 A CN 103588793A
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Abstract
The invention relates to a complex type sustained/controlled release urea fertilizer which is prepared with the method as follows: (1) synthesis of a complex type urease inhibitor: 3,5-dibromo-2-hydroxy benzaldehyde and N-cyclohexyl propyl-1,3-diamine are dissolved in a 95% methanol solution, cupric acetate and an iso-ammonium thiocyanate methanol solution are dripped after stirring, the molar ratio of added 3,5-dibromo-2-hydroxy benzaldehyde, N-cyclohexyl propyl-1,3-diamine, cupric acetate and iso-ammonium thiocyanate is 200:200:200:1, stand aging is performed until blue crystals appear, the blue crystals are washed and dried, and during the synthesis process, the solution temperature ranges from 15 DEG C to 30 DEG C, the solution pH is 5.5 to 6.5, and the humidity is controlled to be 60% to 90%; (2) raw material mixing: the urease inhibitor obtained in the step (1) is uniformly mixed with urea in a weight ratio of 1: (20-50); and (3) starch coating. The complex type sustained/controlled release urea fertilizer has the advantages of simple complex synthesis, higher productivity and stable nitrogen dissolution rate of the fertilizer.
Description
Technical field
The invention belongs to agricultural fertilizer technical field, be specifically related to a kind of complex type sustained/controlled release urea fertilizer.
Background technology
Urea is the nitrogenous source of widespread use during current husbandry is produced, but the urase that occurring in nature extensively exists is catalytic hydrolysis urea rapidly, reduce the utilization of plant to nitrogen, increase agricultural cost, pollute agricultural-food, cause serious Rural Plane Source Pollution and body eutrophication.How to improve urea utilization ratio, solve the problems such as the caused economy of urase, environment, become a challenge subjects in husbandry Sustainable development.
Urease inhibitor is that soil urease liveness is had to an inhibiting class material.It can delay the hydrolysis of urea in a short time, reduces the loss of nitrogen.The compound that has now found that there is urease inhibiting effect has phosphorus ammonium class, phenol quinones, heterocyclic and other classes etc., but that existing urease inhibitor exists is expensive, high residue, toxic side effect are large, easily molten easy loss, effectively suppress the shortcomings such as the time is short, therefore development of new urease inhibitor has become the key point that overcomes existing urease inhibitor shortcoming.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of complex type sustained/controlled release urea fertilizer is provided, it has good restraining effect to urease activity, can improve the effective rate of utilization of urea.
The scheme that the present invention solve the technical problem is: a kind of complex type sustained/controlled release urea fertilizer, and it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1,3-diamines is dissolved in 95% methanol solution, stir over continuing to drip neutralized verdigris, isothiocyanic acid ammonium methanol solution after 30min, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, the mol ratio of 3-diamines, neutralized verdigris, isothiocyanic acid ammonium is 200:200:200:1, then still aging solution, until have blue colored crystal to occur, dry after blue colored crystal is rinsed with cold methanol; In building-up process, the temperature of solution is controlled to 15 ℃ ~ 30 ℃, the pH value of solution is controlled between 5.5 ~ 6.5, and humidity is controlled at 60% ~ 90%;
The synthetic route of complex type urease inhibitor is:
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:20 ~ 50;
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, and obtains product.
As further technical scheme, in described step (1), dry operation is to be placed with CaCl
2vacuum drier in carry out.
Beneficial effect of the present invention: the present invention has that title complex is synthetic simple, productive rate is higher, the nitrogen leaching rate of fertilizer advantage stably, has effectively improved nitrogen utilization efficiency.
Accompanying drawing explanation
Fig. 1: the sustained/controlled release urea product of the embodiment of the present invention 3 gained and the nitrogen of common urea accumulative total solubility rate comparison diagram.
Embodiment
A sustained/controlled release urea fertilizer is to make with the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1,3-diamines is dissolved in 95% methanol solution, stir over after 30min and continue to add neutralized verdigris, isothiocyanic acid ammonium methanol solution, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, the mol ratio of 3-diamines, neutralized verdigris, isothiocyanic acid ammonium is 200:200:200:1, standing solution afterwards, until there is blue colored crystal to occur, after being rinsed with cold methanol, blue colored crystal is being placed with CaCl
2vacuum drier in be dried; In building-up process, the temperature of solution is controlled to 15 ℃, the pH value of solution is controlled at 6.5, and humidity is controlled at 60%; The productive rate of complex type urease inhibitor is 76%.
By ultimate analysis, IR analyzes, and the character of definite title complexs such as single crystal X diffraction instrument, wherein carries out the analysis of C, H, N element with Perkin-Elmer 240C elemental analyser, with Nicolet AVATAR infrared spectra meter, take KBr as compressing tablet is at 4000-400 ㎝
-1place is detected, and crystalline structure data collection and analysis is with SMART APEX II single crystal diffractometer (SCD).Characterization result is: the molecular formula of title complex: C
36h
52br
4cuN
6o
4s
2.
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:50.
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in pasted starch and stirred simultaneously, cooling evenly, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, obtain product, product is 20～100 object pasted starch wrap urea particles.
A sustained/controlled release urea fertilizer, it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1,3-diamines is dissolved in 95% methanol solution, stir over after 30min and continue to add neutralized verdigris, isothiocyanic acid ammonium methanol solution, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, the mol ratio of 3-diamines, neutralized verdigris, isothiocyanic acid ammonium is 200:200:200:1, allow afterwards solution left standstill, until there is blue colored crystal to occur, after being rinsed with cold methanol, blue colored crystal is being placed with CaCl
2vacuum drier in be dried; In building-up process, the temperature of solution is controlled to 20 ℃, the pH value of solution is controlled at 6.0, and humidity is controlled at 70%; The productive rate of complex type urease inhibitor is 83%.
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:40.
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, obtain product, product is 20～100 object pasted starch wrap urea particles.
A sustained/controlled release urea fertilizer, it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines is dissolved in 95% methanol solution, stir over after 30min and continue to add neutralized verdigris, isothiocyanic acid ammonium methanol solution, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines, neutralized verdigris, the mol ratio of isothiocyanic acid ammonium is 200:200:200:1, allow afterwards solution left standstill, until there is blue colored crystal to occur, after being rinsed with cold methanol, blue colored crystal is dried in being placed with the vacuum drier of CaCl2, in building-up process, the temperature of solution is controlled to 30 ℃, the pH value of solution is controlled at 5.5, and humidity is controlled at 65%, the productive rate of complex type urease inhibitor is 81%.
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:35.
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, obtain product, product is 20～100 object pasted starch wrap urea particles.
The nitrogen accumulative total solubility rate of test products obtained therefrom and common urea, result as shown in Figure 1.
Products obtained therefrom is tested paddy rice.Experimental plot adopts Quarter Design, random alignment, and paddy rice row is apart from 0.25m, spacing in the rows 0.18m, and community surrounding is established 2m protection row.The field management of each processing is consistent, and in each group, the amount of discharging of urea is all by custom consumption 375kg/hm
2apply, pure nitrogen is 172.5 kg/hm
2.Sowing number all equates.Get representational plant 8 caves, after emerging, measure seedling rate, in ripening stage results paddy rice, replace table plant in sexual maturing period, measure the indexs such as number of grain per ear, thousand seed weight, analyze nitrogen content, result is as follows:
As shown in Table 1, the seedling rate of control group 1 is minimum, and 2 groups slightly high.Reason is that 2 groups of urea used are coated with by starch, and hydrolysis rate is slow compared with 1 group, and nitrogen utilization efficiency and seedling rate are slightly high compared with 1 group, and the seedling rate of 3,4 liang of groups is higher, and wherein 4 groups of seedling rates are up to 91.3%.Reason is that new inhibitor can suppress urease activity preferably, has reduced the hydrolysis rate of urea, and reduces the NH that hydrolysis of urea produces
3cause to the toxic action of rice plant.
each test group seeding ratio of table 1
Note: treatment group 1: common urea; Treatment group 2: starch wrap urea; Treatment group 3: quinhydrones sustained/controlled release urea; Treatment group 4: the present embodiment gained urea; Folding is executed pure nitrogen level and is 172.5kg/hm
2; Lower same.
As shown in table 2,3,4 liang of group paddy rice amount of nitrogen sucking harvesting time have improved 25.23% and 26.70% compared with control group 1 respectively.This shows that such is not to the transfer ability of fringe portion, and nitrogen utilization efficiency is the performance of crop to the middle nitrogen absorption and utilization degree that is manured into soil.In each test group, nitrogen harvest index, agronomy efficiency, utilization ratio all be take 3,4 groups as high, show this Cu
2+title complex can suppress the decomposition of urase to urea, effectively promotes that nitrogen shifts to grain from root, promotes the absorption of nitrogen, improves rice yield.
each test group Nitrogen Absorption data of table 2
As shown in Table 3,3,4 of processing groups of each measuring parameters all more untreated 1 group improve a lot.Wherein, 3,4 groups of rice yields are apparently higher than 1,2 group, especially 4 groups of output with than 1 group high by 19.60%, show that this additive can effectively suppress urease activity, improve rice yield.3,4 liang of group Plant Height of Rices are slightly high than 1,2 liang of group, and wherein 4 groups of plant heights increase 5.44% compared with control group, increase lessly, may be the self-controls of plant, by unnecessary nutritive substance confession, sent paddy growth.
each test group paddy growth data of table 3
Embodiment 4
A sustained/controlled release urea fertilizer, it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines is dissolved in 95% methanol solution, stir over after 30min and continue to add neutralized verdigris, isothiocyanic acid ammonium methanol solution, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines, neutralized verdigris, the mol ratio of isothiocyanic acid ammonium is 200:200:200:1, allow afterwards solution left standstill, until there is blue colored crystal to occur, after being rinsed with cold methanol, blue colored crystal is dried in being placed with the vacuum drier of CaCl2, in building-up process, the temperature of solution is controlled to 25 ℃, the pH value of solution is controlled at 6.5, and humidity is controlled at 90%, the productive rate of complex type urease inhibitor is 88%,
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:30;
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, obtain product, product is 20～100 object pasted starch wrap urea particles.
A sustained/controlled release urea fertilizer, it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines is dissolved in 95% methanol solution, stir over after 30min and continue to add neutralized verdigris, isothiocyanic acid ammonium methanol solution, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, 3-diamines, neutralized verdigris, the mol ratio of isothiocyanic acid ammonium is 200:200:200:1, allow afterwards solution left standstill, until there is blue colored crystal to occur, after being rinsed with cold methanol, blue colored crystal is dried in being placed with the vacuum drier of CaCl2, in building-up process, the temperature of solution is controlled to 25 ℃, the pH value of solution is controlled at 06.00, and humidity is controlled at 80%, the productive rate of complex type urease inhibitor is 90%,
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:20;
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, obtain product, product is 20～100 object pasted starch wrap urea particles.
As for the New Types of Urease Inhibitors mechanism of action, be still not clear, mainly contain 3 kinds of hypothesis: first may be by 2 Ni atoms contention at metal ion and urease activity center and the sulfydryl coordination at urase center; Second may be by the Ni Atomic coordinate in the donor atoms such as the N on organic molecule, O and urase; The 3rd may be that inhibitor works with noncompetitive suppressor mode, mainly contains polyphenol, mercaptoethanol, hydroxamic acid class etc.C
36h
52br
4cuN
6o
4s
2belong to complex type urease inhibitor, contain N, O atom, and metal ion, by its structure, to be inferred, its mechanism of action may be 2 Ni atom contention ligands by metal ion and urease activity center, reduces urease activity; Also may be by the Ni Atomic coordinate in the atoms such as the N on organic molecule, O and urase.
Claims (2)
1. a complex type sustained/controlled release urea fertilizer, is characterized in that: it makes by the following method:
(1) complex type urease inhibitor is synthetic: by 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1,3-diamines is dissolved in 95% methanol solution, stir over continuing to drip neutralized verdigris, isothiocyanic acid ammonium methanol solution after 30min, more than continuing again to stir 60min, add 3, the bromo-Benzaldehyde,2-hydroxy of 5-bis-, N-cyclohexyl propyl group-1, the mol ratio of 3-diamines, neutralized verdigris, isothiocyanic acid ammonium is 200:200:200:1, then still aging solution, until have blue colored crystal to occur, dry after blue colored crystal is rinsed with cold methanol; In building-up process, the temperature of solution is controlled to 15 ℃～30 ℃, the pH value of solution is controlled between 5.5～6.5, and humidity is controlled at 60%～90%;
(2) raw material mixes: the urease inhibitor obtaining from step (1) is mixed with the weight ratio of urea with 1:20～50;
(3) starch is coated: Zulkovsky starch is placed in to water, heats while stirring, the raw material mixing is joined in starch paste and stirred simultaneously, cooling after one-tenth pasty state, lucifuge is dried in the shade naturally, and after being shaped, fragmentation is sieved, and obtains product.
2. a kind of complex type sustained/controlled release urea fertilizer as claimed in claim 1, is characterized in that: in described step (1), dry operation is to carry out in being placed with the vacuum drier of CaCl2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107873454A (en) * | 2017-11-18 | 2018-04-06 | 五河县金满塘生态种养殖家庭农场 | A kind of fertilizing method of high yield high nutrition onion |
| CN109293686A (en) * | 2018-11-12 | 2019-02-01 | 辽宁大学 | One kind containing CuⅡSecondary complex and preparation method thereof and application as urease inhibitor |
| CN109810126A (en) * | 2018-12-20 | 2019-05-28 | 浙江万里学院 | Urease inhibitor, double-core slow-release carbamide fertilizer containing the inhibitor and preparation method thereof |
-
2013
- 2013-11-14 CN CN201310572675.9A patent/CN103588793A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| C.-Y.WANG: "synthesis, crystal structures and antibacterial activity of two copper(II) complexes derived from 2,4-dibromo-6-[(3-cyclohexylaminopropylimino)methyl] phenol", 《POLISH JOURNAL OF CHEMISTRY》 * |
| 查汝华: "过渡金属席夫碱配合物的合成及抑制脲酶活性的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107873454A (en) * | 2017-11-18 | 2018-04-06 | 五河县金满塘生态种养殖家庭农场 | A kind of fertilizing method of high yield high nutrition onion |
| CN109293686A (en) * | 2018-11-12 | 2019-02-01 | 辽宁大学 | One kind containing CuⅡSecondary complex and preparation method thereof and application as urease inhibitor |
| CN109293686B (en) * | 2018-11-12 | 2020-08-25 | 辽宁大学 | Containing CuⅡSecondary coordination compound, preparation method thereof and application thereof as urease inhibitor |
| CN109810126A (en) * | 2018-12-20 | 2019-05-28 | 浙江万里学院 | Urease inhibitor, double-core slow-release carbamide fertilizer containing the inhibitor and preparation method thereof |
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Application publication date: 20140219 |