CN104892150A - Instant slow-release nitrogen fertilizer and preparation method thereof - Google Patents
Instant slow-release nitrogen fertilizer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an instant slow-release nitrogen fertilizer and a preparation method thereof. The preparation method comprises the following steps: generating urea and formaldehyde prepolymer by utilizing urea and formaldehyde under heating and continuous stirring conditions, and adding organic acid A into prepolymer to regulate the pH value of the prepolymer to 2-3; then, adding a catalyst B and a surfactant C, and quickly stirring to generate solid slow-release nitrogen fertilizer with low molecular weight; adding a modifying synergist D into the solid low-release nitrogen fertilizer with low molecular weight to mix and grind until 95% of the particles are smaller than 1-3 microns, thereby preparing the water-soluble slow-release nitrogen fertilizer. The instant slow-release nitrogen fertilizer prepared by the preparation method is an excellent slow-release nitrogen fertilizer which is relatively small in molecular weight, easier to dissolve, lower in price, better in anti-caking performance, simpler in processing process, and lower in energy consumption as compared with a conventional common ureaformaldehyde slow-release nitrogen fertilizer.
Description
(1) technical field
The present invention relates to a kind of instant slow-release nitrogen fertilizer and preparation method thereof, being specifically related to one can either be quick
Dissolve the slow-release nitrogen fertilizer possessing again nutrient slowly-released performance, belong to new-type fertilizer production field.
(2) background technology
Water soluble fertilizer, it is a kind of polyelement composite fertilizer that can be completely water-soluble, it can promptly be dissolved in the water, more easily absorbed by crops, and its absorption rate is relatively high, more crucially it can be applied to the industrialized agricultures such as spray drop filling, realizes water-fertilizer integral, reaches the usefulness that water-saving economizes fertile saving of labor.At present, along with improving constantly of the degree such as facility, mechanize and automatization, the instant mainstream technology having become modern agriculture high added value farm crop water and fertilizer management with fertigation technology of fertilizer.Can for crop demand and soil nutrient supply characteristic, the principle of practicable " overall control " and " point period regulation ", by drip irrigation and micro irrigation technology, realizes the water and fertilizer synchronization method of supplying of " on a small quantity repeatedly ", greatly improves the utilising efficiency of liquid manure.China's water soluble fertilizer industry develops rapidly, end in July, 2015, put on record in the Ministry of Agriculture and produce the producer of water soluble fertilizer and have nearly 400 in the whole nation, all kinds of water soluble fertilizer products of registration reach more than 5000, and national water soluble fertilizer output reaches 2,000,000-300 ten thousand tons.Now, domesticly many outstanding water soluble fertilizer production companies are emerged.And, every year with more than 10% speed increase.
Along with the further scarcity of water resources, intensive, the large-scale development of agricultural, the expansion of water saving irrigation facility agricultural area, the importance of water soluble fertilizer will be day by day obvious.2012, the Ministry of Agriculture has issued " suggestion about advancing Developing Water-saving Agriculture " notice, by 2015 by input 38,000,000,000 yuan, the water saving completing 3,800 ten thousand mu increases grain area, and newly-increased the Northeast resisting drought saving water subsidy area 8,500 ten thousand mu, large-scale promotion efficient water-saving irrigation technology, the new stage that " 12 " period will be water soluble fertilizer and water-fertilizer integral fast development and leading market.Water soluble fertilizer faces brand-new opportunity, will be the new direction of 21 century Fertilizer Industry in China development.
China's water soluble fertilizer development is started late, developed country is lagged far behind in production technology and process aspect, as: most of factory adopts physics mixture method to produce water soluble fertilizer, mainly by material fertilizers such as urea, ammonium sulfate, monoammonium phosphate, potassium primary phosphate, saltpetre and Repone K, by the mechanical means such as pulverizer, stirrer, the direct mixture of physical admixture is adopted to become Water soluble fertilizer.Also have minority factory to adopt chemical reactive synthesis method to produce, the main polyphosphoric acid chemical combination that adopts compensate for the low shortcoming of physics mixture phosphorus element content, and nutrition is balanced and reasonable more, avoids the waste that other constituent content height causes, improves fertilizer absorption rate.Although can water soluble fertilizer be produced by above simple reason mixture method and chemical reactive synthesis method, but its shortcoming is also fairly obvious, as: 1. product easily lumps, the application effect extreme difference after caking, therefore need to add a large amount of anti-hard caking agents just can deal with problems, thus add production cost.2. selected nitrogenous fertilizer is common chemical nitrogen fertilizer, although can be water-soluble fast, possess slow release method, therefore need often to carry out fertigation, be generally weekly, the cost therefore causing fertigation is high, constrains the Rapid Popularization of the Integration of Water into Fertilizer.
Not only therefore developing one can rapid solution but also possess nutrient slowly-released performance, also possesses the slow-release nitrogen fertilizer of anti-caking function simultaneously, is applied to the production of water soluble fertilizer, will have great social and economic benefits and wide application prospect.
(3) summary of the invention
In order to solve the problem, the invention provides a kind of instant slow-release nitrogen fertilizer and preparation method thereof; The instant slow-release nitrogen fertilizer utilizing the present invention to prepare can either possess again nutrient slowly-released performance by rapid solution, also possesses the function of anti-caking simultaneously; The present invention utilizes urea and formaldehyde reaction, it is little, soluble and possess the instant slow-release nitrogen of nitrogen fertilizer slow-releasing performance that synthesis is controlled to molecular weight, be that a kind of urea formaldehyde slow-release nitrogen fertilizer molecular weight common is than ever less, more soluble, cheap, agglomeration preventing performance is good, complete processing is simple, energy consumption is low, can be used for the new sustained release nitrogenous fertilizer that Quick-dissolving fertilizer is produced.
A kind of instant slow-release nitrogen fertilizer, is obtained by following preparation method:
First utilize urea and formaldehyde to generate urea and formaldehyde pre-polymer under heating and the continuous condition stirred, in prepolymer, add organic acid A, the potential of hydrogen being adjusted to prepolymer is 2-3; Add catalyst B and tensio-active agent C again, rapid stirring generates the lower molecular weight slow-release nitrogen fertilizer of solid state; In the lower molecular weight slow-release nitrogen fertilizer of solid state, add modified synergist D mixed grinding again, the particle being ground to 95% is all less than 1-3 micron, obtained water-soluble slow-releasing nitrogen.
The preparation method of described prepolymer is: urea (nitrogenous is 46%) and formaldehyde (content is the formaldehyde solution of 36.5%) are according to the ratio hybrid reaction of mol ratio 2.5-3.2:1, constantly stir under air-proof condition, until urea dissolves, adjust the potential of hydrogen of above-mentioned reaction solution to 9.5-10 with the sodium hydroxide solution that concentration is 20% subsequently; React at 35 DEG C-45 DEG C and obtain prepolymer in 1-2 hour.
Described organic acid A is oxalic acid, Witco 1298 Soft Acid and thiacetic mixture, and described oxalic acid, Witco 1298 Soft Acid and thiacetic weight ratio are 1:1-3:0.5-1, and preferred ratio is 1:2:0.8.
Described catalyst B is the mixture of ammonium chloride and ammonium persulphate, and the weight ratio of described ammonium chloride and ammonium persulphate is 1:0.1-0.5, and preferred ratio is 1:0.25; The interpolation weight of catalyst B accounts for 0.3% of described urea and formaldehyde gross weight.
Described tensio-active agent C is the mixture of Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt, and the weight ratio of described Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt is 1:1-2, and preferred ratio is 1:1.5; The interpolation weight of described tensio-active agent C accounts for 0.1% of described urea and formaldehyde gross weight.
Described modified synergist D is the mixture of poly aspartic acid and N-acetylhydroxylamine, and the weight ratio of described poly aspartic acid and N-acetylhydroxylamine is 1:1-2, and preferred ratio is 1:1.5; The interpolation weight of described modified synergist D accounts for 0.2% of described urea and formaldehyde gross weight.
Unusual effect of the present invention is:
1, the instant had good sustained release effect of product: adopt the obtained instant slow-release nitrogen of this inventive method not only to possess the diffluent feature of lower molecular weight, but also possess the dual-sustained-release performance (sustained release performance of lower molecular weight urea formaldehyde and modified synergist are to the suppression of urase and nutrient slowly-released performance etc.) of nutrient.
2, anti-caking effect: grafting some tensio-active agents C in the instant slow-release nitrogen fertilizer of this invention synthesis, and then the equal particle through grinding to form 95% is less than the powdery of 1-3 micron, after mixing with other compositions in Quick-dissolving fertilizer, good agglomeration preventing performance can be played, therefore can reduce or alternative Quick-dissolving fertilizer produce in the consumption of tensio-active agent.
3, complete processing is simple, and the cost of sintetics is low: compared with synthesizing with traditional urea formaldehyde, the low generated time of the Heating temperature needed for this technique is short, and therefore energy consumption is low, efficiency is high, possesses the feature that production cost is low.
4, reduce irrigation frequency, saving of work and time: the Quick-dissolving fertilizer using the present invention to be configured to, the irrigation frequency of half can be reduced, possess the feature of saving of work and time, very wide popularizing application prospect will be had.
(4) accompanying drawing explanation
Fig. 1: preparation method's process flow sheet of the present invention
In figure, first urea and formaldehyde solution add in reactor by 1 in proportion; 2 heating and stirring, until urea dissolves and reaches 35 DEG C-45 DEG C; 3 pairs of urea and formaldehyde solution carry out regulation and control potential of hydrogen, control the reaction times, generate prepolymer; The potential of hydrogen of 4 regulation and control prepolymers; 5 add catalyst B; 6 add tensio-active agent C; 7 add modified synergist D; 8 grindings; 9 preparation water soluble fertilizers; 10 packagings, warehouse-in.
(4) embodiment
Embodiment 1:
By 100kg urea and content be 36.5% formaldehyde solution 54.85kg (mol ratio of urea and formaldehyde is 2.5:1) add reactor, under the condition constantly stirred, be rapidly heated to 35-45 DEG C, adjusting potential of hydrogen with the sodium hydroxide solution that concentration is 20% is 9.5-10, continue to react about 1-2 hour, obtain the prepolymer of urea formaldehyde.Then organic acid (oxalic acid is added, Witco 1298 Soft Acid and thiacetic weight ratio are 1:2:0.8), until the potential of hydrogen of urea formaldehyde prepolymer is 2-3, then catalyzer 0.47kg (weight ratio of ammonium chloride and ammonium persulphate is 1:0.25) and tensio-active agent 0.16kg (weight ratio of Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt is 1:1.5) is added, rapid stirring, the lower molecular weight slow-release nitrogen fertilizer of solid state can be generated in about 5-10 minute, finally add modified synergist 0.31kg (weight ratio of the mixture of poly aspartic acid and N-acetylhydroxylamine is 1:1.5), particle through ball mill grinding to 95% is all less than 1-3 micron, obtain water-soluble slow-releasing nitrogenous fertilizer, finally can add in proportion as required in other water soluble fertilizer components, the water soluble fertilizer containing instant slow nitrogen can be obtained after fully mixing.Add the water soluble fertilizer of this instant slow-release nitrogen, place at normal temperatures and can not lump for 6 months, and use in drip irrigation system, effectively can improve the utilization ratio of nitrogenous fertilizer, save the fertilizer of half and reduce the fertigation number of times of half.
Embodiment 2:
By 100kg urea and content be 36.5% formaldehyde solution 48.97kg (element and the mol ratio of formaldehyde are 2.8:1) add reactor, under the condition constantly stirred, be rapidly heated to 35-45 DEG C, adjusting potential of hydrogen with the sodium hydroxide solution that concentration is 20% is 9.5-10, continue to react about 1-2 hour, obtain prepolymer.Then organic acid (oxalic acid is added, Witco 1298 Soft Acid and thiacetic weight ratio are 1:2:0.8), until the potential of hydrogen of prepolymer is 2-3, then catalyzer 0.45kg (weight ratio of ammonium chloride and ammonium persulphate is 1:0.25) and tensio-active agent 0.15kg (weight ratio of Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt is 1:1.5) is added, rapid stirring, the lower molecular weight slow-release nitrogen fertilizer of solid state can be generated in about 5-10 minute, finally add modified synergist 0.30kg (weight ratio of the mixture of poly aspartic acid and N-acetylhydroxylamine is 1:1.5), after ball mill grinding (particle of 95% is less than 1-3 micron), obtain water-soluble slow-releasing nitrogenous fertilizer, finally can add in proportion as required in other water soluble fertilizer components, the water soluble fertilizer containing instant slow nitrogen can be obtained after fully mixing.Add the water soluble fertilizer of this instant slow-release nitrogen, place at normal temperatures and can not lump for 6 months, and use in drip irrigation system, effectively can improve the utilization ratio of nitrogenous fertilizer, save the fertilizer of half and reduce the fertigation number of times of half.
Embodiment 3:
By 100kg urea and content be 36.5% formaldehyde solution 45.71kg (element and the mol ratio of formaldehyde are 3:1) add reactor, under the condition constantly stirred, be rapidly heated to 35-45 DEG C, it is 9.5-10 that sodium hydroxide solution with 20% adjusts potential of hydrogen, continue to react about 1-2 hour, obtain prepolymer.Then organic acid (oxalic acid is added, Witco 1298 Soft Acid and thiacetic weight ratio are 1:2:0.8), until the potential of hydrogen of prepolymer is 2-3, then catalyzer 0.44kg (weight ratio of ammonium chloride and ammonium persulphate is 1:0.25) and tensio-active agent 0.146kg (weight ratio of Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt is 1:1.5) is added, rapid stirring, the lower molecular weight slow-release nitrogen fertilizer of solid state can be generated in about 5-10 minute, finally add modified synergist 0.29kg (weight ratio of the mixture of poly aspartic acid and N-acetylhydroxylamine is 1:1.5), after ball mill grinding (particle of 95% is less than 1-3 micron), obtain water-soluble slow-releasing nitrogenous fertilizer, finally can add in proportion as required in other water soluble fertilizer components, the water soluble fertilizer containing instant slow nitrogen can be obtained after fully mixing.Add the water soluble fertilizer of this instant slow-release nitrogen, place at normal temperatures and can not lump for 6 months, and use in drip irrigation system, effectively can improve the utilization ratio of nitrogenous fertilizer, save the fertilizer of half and reduce the fertigation number of times of half.
Embodiment 4:
By 100kg urea and content be 36.5% formaldehyde solution 42.85kg (element and the mol ratio of formaldehyde are 3.2:1) add reactor, under the condition constantly stirred, be rapidly heated to 35-45 DEG C, adjusting potential of hydrogen with the sodium hydroxide solution that concentration is 20% is 9.5-10, continue to react about 1-2 hour, obtain prepolymer.Then organic acid (oxalic acid is added, Witco 1298 Soft Acid and thiacetic weight ratio are 1:2:0.8), until the potential of hydrogen of prepolymer is 2-3, then catalyzer 0.43kg (weight ratio of ammonium chloride and ammonium persulphate is 1:0.25) and tensio-active agent 0.14kg (weight ratio of Sodium dodecylbenzene sulfonate and alkyl ethoxylated carboxylate salt is 1:1.5) is added, rapid stirring, the lower molecular weight slow-release nitrogen fertilizer of solid state can be generated in about 5-10 minute, finally add modified synergist 0.28kg (weight ratio of the mixture of poly aspartic acid and N-acetylhydroxylamine is 1:1.5), after ball mill grinding (particle of 95% is less than 1-3 micron), obtain water-soluble slow-releasing nitrogenous fertilizer, finally can add in proportion as required in other water soluble fertilizer components, the water soluble fertilizer containing instant slow nitrogen can be obtained after fully mixing.Add the water soluble fertilizer of this instant slow-release nitrogen, place at normal temperatures and can not lump for 6 months, and use in drip irrigation system, effectively can improve the utilization ratio of nitrogenous fertilizer, save the fertilizer of half and reduce the fertigation number of times of half.
Claims (5)
1. an instant slow-release nitrogen fertilizer, is characterized in that being obtained by following preparation method:
First utilize urea and formaldehyde to generate prepolymer, in prepolymer, add organic acid A, the potential of hydrogen being adjusted to prepolymer is 2-3; Add catalyst B and tensio-active agent C again, rapid stirring generates the lower molecular weight slow-release nitrogen fertilizer of solid state; In the lower molecular weight slow-release nitrogen fertilizer of solid state, add modified synergist D mixed grinding again, the particle being ground to 95% is all less than 1-3 micron, obtained water-soluble slow-releasing nitrogen;
The preparation method of described prepolymer is: urea and formaldehyde, according to the ratio hybrid reaction of mol ratio 2.5-3.2:1, constantly stir under air-proof condition, until urea dissolves; The potential of hydrogen of above-mentioned reaction solution is adjusted to 9.5-10 subsequently with the sodium hydroxide solution that concentration is 20%; React at 35 DEG C-45 DEG C and obtain prepolymer in 1-2 hour;
Described organic acid A is oxalic acid, Witco 1298 Soft Acid and the thioacetic acid mixture according to weight ratio 1:1-3:0.5-1;
Described catalyst B is ammonium chloride and the ammonium persulphate mixture according to weight ratio 1:0.1-0.5; The interpolation weight of catalyst B accounts for 0.3% of described urea and formaldehyde gross weight;
Described tensio-active agent C is Sodium dodecylbenzene sulfonate and the alkyl ethoxylated carboxylate salt mixture according to weight ratio 1:1-2; The interpolation weight of tensio-active agent C accounts for 0.1% of described urea and formaldehyde gross weight;
Described modified synergist D is poly aspartic acid and the N-acetylhydroxylamine mixture according to weight ratio 1:1-2; The interpolation weight of modified synergist D accounts for 0.2% of described urea and formaldehyde gross weight.
2. instant slow-release nitrogen fertilizer as claimed in claim 1, is characterized in that described organic acid A is oxalic acid, Witco 1298 Soft Acid and the thioacetic acid mixture according to weight ratio 1:2:0.8.
3. instant slow-release nitrogen fertilizer as claimed in claim 1, is characterized in that described catalyst B is ammonium chloride and the ammonium persulphate mixture according to weight ratio 1:0.25.
4. instant slow-release nitrogen fertilizer as claimed in claim 1, is characterized in that described tensio-active agent C is Sodium dodecylbenzene sulfonate and the alkyl ethoxylated carboxylate salt mixture according to weight ratio 1:1.5.
5. instant slow-release nitrogen fertilizer as claimed in claim 1, is characterized in that described modified synergist D is poly aspartic acid and the N-acetylhydroxylamine mixture according to weight ratio 1:1.5.
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Cited By (7)
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| CN105175155A (en) * | 2015-10-13 | 2015-12-23 | 黑龙江中农欣欣农业科技发展有限公司 | Device and method for improving urea formaldehyde compound fertilizer on amino acid compound fertilizer production line |
| CN107721537A (en) * | 2017-12-12 | 2018-02-23 | 鹿晓丹 | A kind of chemical fertilizer fast method for preparing |
| CN107857606A (en) * | 2017-11-08 | 2018-03-30 | 贵州省五谷惠生态农业科技有限公司 | A kind of ureaformaldehyde modifying agent and its preparation method and application |
| CN107857605A (en) * | 2017-11-08 | 2018-03-30 | 贵州省化工研究院 | One kind polymerization ureaformaldehyde method of modifying and modified poly ureaformaldehyde and its application |
| CN107879766A (en) * | 2017-11-08 | 2018-04-06 | 贵州省化工研究院 | A kind of ureaformaldehyde method of modifying and modified urea formaldehyde and its application |
| CN112390687A (en) * | 2020-11-26 | 2021-02-23 | 晟丰(烟台)农业科技有限公司 | Slow-release fertilizer and preparation method thereof |
| CN115849959A (en) * | 2023-02-22 | 2023-03-28 | 中北大学 | Organic acid modified urea formaldehyde slow-release nitrogen fertilizer and reactive extrusion low-cost preparation process thereof |
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| CN115849959A (en) * | 2023-02-22 | 2023-03-28 | 中北大学 | Organic acid modified urea formaldehyde slow-release nitrogen fertilizer and reactive extrusion low-cost preparation process thereof |
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Application publication date: 20150909 |