CN106631630A - Organic slow-release nitrogen fertilizer and method for preparing same - Google Patents

Organic slow-release nitrogen fertilizer and method for preparing same Download PDF

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Publication number
CN106631630A
CN106631630A CN201610812386.5A CN201610812386A CN106631630A CN 106631630 A CN106631630 A CN 106631630A CN 201610812386 A CN201610812386 A CN 201610812386A CN 106631630 A CN106631630 A CN 106631630A
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urea
release
slow
organic matter
reaction
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CN201610812386.5A
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CN106631630B (en
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刘玉
刘宇
侯宝霞
邵英朝
杨桂花
陈嘉川
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Ningxia Wodidi Water And Fertilizer Technology Co ltd
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Qilu University of Technology
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/90Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C9/00Fertilisers containing urea or urea compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Soil Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Fertilizers (AREA)

Abstract

The invention provides a method for preparing organic slow-release urea. The method includes dissolving sodium lignin sulfonate and urea in a beaker to obtain mixtures, then regulating the pH (potential of hydrogen) of the mixtures; transferring the mixtures into a four-opening flask, adding peracetic acid and copper oxide into the mixtures, carrying out reaction, and carrying out freeze drying on concentrated reaction liquid after reaction is completely carried out so as to obtain dry powder; extracting the dry powder by the aid of absolute ethyl alcohol to remove unreacted urea, carrying out vacuum drying on products to obtain the organic slow-release urea and analyzing the nitrogen content of the organic slow-release urea. The method has the advantages that the utilization rate of the urea can be increased as compared the organic slow-release urea, which is an organic slow-release nitrogen fertilizer, to slow-release fertilizers enveloped by refractory materials in current markets, the organic slow-release nitrogen fertilizer can be completely degraded, and accordingly harm on ecological environments can be prevented; the method includes simple steps and is convenient to implement and high in practicality.

Description

A kind of organic matter slow-release nitrogen fertilizer and preparation method thereof
Technical field
The invention belongs to organic matter slow-release nitrogen fertilizer preparation field, more particularly to a kind of organic matter slow-release nitrogen fertilizer and its preparation side Method.
Background technology
Traditional nitrogenous fertilizer, such as urea, ammonium carbonate can cause the heavy losses of nitrogen due to approach such as leaching and denitrifications, Loss amount is up to 55%, and the utilization rate of such nitrogen is very low.Simultaneously excessive use inorganic fertilizer also results in lacking for carbon in soil Lose and leaching of nitrate loss causes body of groundwater to be contaminated.
In order to improve the utilization rate of fertilizer and reduce the impact to environment, slow release fertilizer obtains the green grass or young crops of enterprise and scientific research personnel Look at.Popular slow-release nitrogen fertilizer is mainly coated carbamide on domestic market, and the material of coating mainly includes phenolic aldehyde, urea The materials such as aldehyde, polyethylene, the advantage of this kind of slow release fertilizer is that still coated fertilizer is difficult to be degraded release time length in soil, Degradable resin is even adopted, the shortening of its degradation time is also limited, and can not possibly be completely degraded, therefore limited The popularization and application of this kind of fertilizer.Not only there is biological material such as lignin higher pore structure to strengthen the gas permeability of soil And water holding capacity, most important this kind of material can be completely degraded in soil.Simultaneously lignin has higher biology Stability, the stronger ability to Resistance to microbes, if lignin can not only be slowed down into fertilizer as the carrier of slow-release material The rate of release of nutrient, improves the utilization rate of fertilizer, moreover it is possible to bring good ecological environment benefit.
The content of the invention
In order to overcome above-mentioned deficiency, the invention provides a kind of organic matter slow-release carbamide of environmental protection and its preparation side Method.Compared to the slow release fertilizer prepared as coating using difficult degradation material in existing market, the organic matter slow-release nitrogen fertilizer of the present invention, The utilization rate of urea can not only be improved, can also be completely degraded will not bring harm to ecological environment.
To achieve these goals, the present invention is adopted the following technical scheme that:
A kind of preparation method of organic matter slow-release carbamide, including:
Under Peracetic acid and cupric oxide existence condition, reaction is modified as raw material with urea and sodium lignin sulfonate;
After reaction terminates, product is concentrated, is dried, unreacted urea is removed, being obtained final product organic matter sustained release urine Element.
Industrial lignin sodium sulfonate and urea are modified reaction for raw material, and the part nitrogen in urea can be converted into wood Then quality is slowly discharged nitrogen by the biodegradation process of lignin with the nitrogen of chemical bonds.The addition of Peracetic acid The benzene ring structure that can make sodium lignin sulfonate is destroyed, oxidized portion sulfonic acid group, effectively improves the knot of lignin and urea Close activity.Cupric oxide can be greatly reduced the activation energy of lignin and urea reaction, promote lignin oxidation to be degraded to small molecule, So as to expose more carboxyls, increase the binding site of lignin and nitrogen, improve the load capacity of nitrogen.
Preferably, the sodium lignin sulfonate and the mass ratio of urea are 8~10:4~7.
Preferably, the mass ratio of the Peracetic acid and cupric oxide is 100~120:1~3.Research finds:When peroxide second The mass ratio of acid and cupric oxide is less than 40:When 1, conversion rate of urea is low, and reaction rate is slow, low yield, and ammonium nitrogen content declines bright It is aobvious.When the mass ratio of Peracetic acid and cupric oxide is more than 100:When 1, the nitrogen content of slow-release nitrogen fertilizer is not high, and side reaction increases, reaction Product purity declines.
Preferably, the modified condition is:2~6h is reacted at 60~100 DEG C.
Preferably, the sodium lignin sulfonate is prepared using following raw material, and the raw material includes:Needlebush, leaf wood or Herbaceous plant.
Preferably, the pH value of the modified-reaction is 3.0-5.0.
Preferably, the Peracetic acid can be replaced hydrogen peroxide.
Present invention also offers a kind of preparation method of preferably organic matter slow-release carbamide, specifically includes following steps:
(1) sodium lignin sulfonate, urea and water are weighed, after being well mixed, pH is adjusted to 3.0-5.0, mixed liquor is obtained;
(2) in the mixed liquor of step (1) add mass fraction for mixed liquor gross mass 5%-20% Peracetic acid and Mass fraction is the cupric oxide of mixed liquor gross mass 0.05~0.08%, is heated to 60~100 DEG C, reacts 2~6h;
(3) after reaction terminates, by reactant liquor concentration, freeze-drying, dry powder is obtained;Dry powder is extracted 3-5 time with absolute ethyl alcohol To remove unreacted urea, obtain final product.
Organic matter slow-release carbamide prepared by the above-mentioned method of any one of present invention.
Organic matter slow-release carbamide prepared by the above-mentioned method of any one of present invention all can be used for biological plantation or fertilizer system Make, obtain preferably effect, reached the requirement of concerned countries and international standard.
Beneficial effects of the present invention
(1) organic matter slow-release carbamide of the invention.Compared to what is prepared as coating using difficult degradation material in existing market Slow release fertilizer, the organic matter slow-release nitrogen fertilizer of the present invention, can not only improve the utilization rate of urea, and can also be completely degraded will not be to Ecological environment brings harm.
(2) organic matter slow-release carbamide (or organic matter slow-release nitrogen fertilizer) of the invention uses sodium lignin sulfonate former as making Material.Pulping and paper-making industry produces every year the industrial lignin of flood tide, and the high-qualityization utilization rate of current lignin is also very low, Hen Duoqi Black liquor is directly carried out burning process by industry, and some little companies are even directly by black liquid discharging, the pollution ring that this not only can be serious Border also result in the significant wastage of resource simultaneously.The present invention not only realizes high-qualityization of lignin using lignin as primary raw material Utilize, also protect environment.
(3) price of industrial lignin is very low on market, therefore the organic matter slow-release fertilizer that the present invention is provided is prepared into This is relatively low and reasonable.
(4) organic matter slow-release carbamide, method process is simple safety, the letter of product subsequent treatment are prepared using the inventive method It is single, meanwhile, the oxidation system environmental protection is free from environmental pollution.
Specific embodiment
Feature of present invention and other correlated characteristics are described in further detail by the following examples, in order to the same industry The understanding of technical staff:
Embodiment 1
(1) the sodium lignin sulfonate 10g, the water of urea 7g and 70mL are weighed to stir in beaker to being completely dissolved, is used 20% sulfuric acid solution adjusts pH to 3.0.
(2) mixed liquor of step (1) is transferred into 4 mouthfuls of flasks (with thermometer, condenser pipe and constant pressure funnel), and is added Enter the Peracetic acid of mixed liquor quality 5% and 0.05% cupric oxide, be heated to 60 DEG C, react 2h.
(3) after reaction terminates, again freeze-drying obtains dry powder after reactant liquor is concentrated;Dry powder is extracted 3 times with absolute ethyl alcohol To remove unreacted urea, then analysis of nitrogen content is carried out to product.
The total nitrogen and ammonium nitrogen content of resulting organic matter slow-release carbamide is respectively 6.12% and 0.75%.
Embodiment 2
As described in Example 1, except that being the hydrogen peroxide for Jia 5% in step (2).Resulting organic matter sustained release urine The total nitrogen and ammonium nitrogen content of element is respectively 4.37% and 0.31%.
Embodiment 3
As described in Example 1, except that pH is 4.0 in step (1).The total nitrogen of resulting organic matter slow-release carbamide and Ammonium nitrogen content is respectively 7.55% and 0.62%.
Embodiment 4
As described in Example 1, except that Peracetic acid addition is 10% in step (2).Resulting organic matter delays The total nitrogen and ammonium nitrogen content for releasing urea is respectively 8.77% and 0.92%.
Embodiment 5
As described in Example 1, except that reaction temperature is 80 DEG C in step (2).Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content be respectively 6.06% and 0.35%.
Embodiment 6
As described in Example 1, except that in step (2) reaction time be 4h.Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content are respectively 8.16% and 0.88%.
Embodiment 7
As described in Example 3, except that peroxyacetic acid concentration is 10% in step (2).Resulting organic matter sustained release The total nitrogen and ammonium nitrogen content of urea is respectively 12.33% and 1.48%.
Embodiment 8
As described in Example 3, except that reaction temperature is 80 DEG C in step (2).Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content be respectively 10.53% and 1.25%.
Embodiment 9
As described in Example 3, except that in step (2) reaction time be 4h.Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content are respectively 10.77% and 1.35%.
Embodiment 10
As described in Example 8, except that Peracetic acid addition is 10% in step (2).Resulting organic matter delays The total nitrogen and ammonium nitrogen content for releasing urea is respectively 14.69% and 2.55%.
Embodiment 11
As described in Example 8, except that in step (2) reaction time be 4h.Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content are respectively 13.38% and 2.03%.
Embodiment 12
As described in Example 10, except that in step (2) reaction time be 4h.Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content are respectively 16.50% and 3.25%.
Embodiment 13
As described in Example 12, except that in step (2) reaction time be 6h.Resulting organic matter slow-release carbamide Total nitrogen and ammonium nitrogen content are respectively 14.11% and 2.88%.
Embodiment 14
As described in Example 12, except that reaction temperature is 100 DEG C in step (2).Resulting organic matter sustained release urine The total nitrogen and ammonium nitrogen content of element is respectively 13.75% and 2.67%.
Embodiment 15
As described in Example 12, except that Peracetic acid addition is 15% in step (2).Resulting organic matter delays The total nitrogen and ammonium nitrogen content for releasing urea is respectively 15.02% and 2.94%.
Embodiment 16
As described in Example 12, except that pH is 5.0 in step (1).The total nitrogen of resulting organic matter slow-release carbamide And ammonium nitrogen content is respectively 14.62% and 2.54%.
Finally it should be noted that the foregoing is only the preferred embodiments of the present invention, this is not limited to Bright, although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it is still Technical scheme described in previous embodiment can be modified, or equivalent is carried out to which part.It is all at this Within bright spirit and principle, any modification, equivalent substitution and improvements made etc. should be included in protection scope of the present invention Within.Although the above-mentioned specific embodiment to the present invention is described, not limiting the scope of the invention, institute Category art personnel should be understood that on the basis of technical scheme those skilled in the art need not pay wound The various modifications made by the property made work or deformation are still within protection scope of the present invention.

Claims (10)

1. a kind of preparation method of organic matter slow-release carbamide, it is characterised in that include:
Under Peracetic acid and cupric oxide existence condition, reaction is modified as raw material with urea and sodium lignin sulfonate;
After reaction terminates, product is concentrated, is dried, unreacted urea is removed, being obtained final product organic matter slow-release carbamide.
2. the method for claim 1, it is characterised in that the sodium lignin sulfonate is 8~10 with the mass ratio of urea: 4~7.
3. the method for claim 1, it is characterised in that the mass ratio of the Peracetic acid and cupric oxide is 100~ 120:1~3.
4. the method for claim 1, it is characterised in that the modified condition is:2~6h is reacted at 60~100 DEG C.
5. the method for claim 1, it is characterised in that the sodium lignin sulfonate is prepared using following raw material, described Raw material includes:Needlebush, leaf wood or herbaceous plant.
6. the method for claim 1, it is characterised in that the pH value of the modified-reaction is 3.0-5.0.
7. the method for claim 1, it is characterised in that the Peracetic acid can be replaced hydrogen peroxide.
8. the method for claim 1, it is characterised in that specifically include following steps:
(1) sodium lignin sulfonate, urea and water are weighed, after being well mixed, pH is adjusted to 3.0-5.0, mixed liquor is obtained;
(2) mass fraction is added in the mixed liquor of step (1) for the Peracetic acid and quality of mixed liquor gross mass 5%-20% Fraction is the cupric oxide of mixed liquor gross mass 0.05~0.08%, is heated to 60~100 DEG C, reacts 2~6h;
(3) after reaction terminates, by reactant liquor concentration, freeze-drying, dry powder is obtained;Dry powder absolute ethyl alcohol extracts 3-5 time to remove Unreacted urea is removed, is obtained final product.
9. the organic matter slow-release carbamide that prepared by the method described in any one of claim 1-8.
10. application of the organic matter slow-release carbamide described in claim 9 in biological plantation or Production of manure.
CN201610812386.5A 2016-09-09 2016-09-09 Organic matter slow-release nitrogen fertilizer and preparation method thereof Active CN106631630B (en)

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Publication number Priority date Publication date Assignee Title
CN102515980A (en) * 2011-12-06 2012-06-27 中国农业科学院农业资源与农业区划研究所 Organic matter coated urea and production method thereof
CN103396266A (en) * 2013-08-12 2013-11-20 东营万鑫肥料有限公司 Organic matter sustained-release urea and preparation method thereof
CN103804075A (en) * 2014-01-20 2014-05-21 中国农业科学院农业资源与农业区划研究所 Charcoal-base polyaspartic acid slow-release urea as well as preparation method and application thereof
CN103804069A (en) * 2014-03-14 2014-05-21 中盐安徽红四方股份有限公司 Controlled-release fertilizer and production method thereof
CN104447133A (en) * 2014-11-12 2015-03-25 成都新柯力化工科技有限公司 Natural macromolecular slow release nitrogen fertilizer and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515980A (en) * 2011-12-06 2012-06-27 中国农业科学院农业资源与农业区划研究所 Organic matter coated urea and production method thereof
CN103396266A (en) * 2013-08-12 2013-11-20 东营万鑫肥料有限公司 Organic matter sustained-release urea and preparation method thereof
CN103804075A (en) * 2014-01-20 2014-05-21 中国农业科学院农业资源与农业区划研究所 Charcoal-base polyaspartic acid slow-release urea as well as preparation method and application thereof
CN103804069A (en) * 2014-03-14 2014-05-21 中盐安徽红四方股份有限公司 Controlled-release fertilizer and production method thereof
CN104447133A (en) * 2014-11-12 2015-03-25 成都新柯力化工科技有限公司 Natural macromolecular slow release nitrogen fertilizer and preparation method thereof

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Effective date of registration: 20240511

Address after: 750299, 300 meters northeast of the intersection of Changtai Road and Hongyun East Road in Hongguang Town, Helan County Industrial Park, Yinchuan City, Ningxia Hui Autonomous Region

Patentee after: Ningxia Wodidi Water and Fertilizer Technology Co.,Ltd.

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Address before: 250353 University Road, Changqing District, Ji'nan, Shandong Province, No. 3501

Patentee before: Qilu University of Technology

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