CN101353282B - Production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation - Google Patents
Production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation Download PDFInfo
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- CN101353282B CN101353282B CN2008102220477A CN200810222047A CN101353282B CN 101353282 B CN101353282 B CN 101353282B CN 2008102220477 A CN2008102220477 A CN 2008102220477A CN 200810222047 A CN200810222047 A CN 200810222047A CN 101353282 B CN101353282 B CN 101353282B
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Abstract
The invention discloses a production method for a melamine formaldehyde-polyvinyl alcohol formaldehyde fertilizer slow-release agent, which comprises the following steps: the preparation of melamine formaldehyde polymer solution, the preparation of polyvinyl formal solution, and the preparation of a slow-release agent. The production method makes use of the characteristics of the good water resistance of the melamine formaldehyde and sol-water glass, and the good caking property and flexibility of the polyvinyl formal to produce an endoplasmic slow-release agent with good combination with urea or compound fertilizer paste. The production method has the advantages of simple process, short production period, and the like; compared with slow-release urea or slow-release compound fertilizer by the secondary processing and production, the method can save energy and reduce transportation.
Description
Technical field
The present invention relates to a kind of production method of producing the built-in property sustained release dosage of slow-release carbamide or slow-release compound fertilizer, be specifically related to a kind of production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation.
Background technology
In order to improve the fertilizer nitrogen utilization ratio, scientist all is devoted to the research of slow release fertilizer both at home and abroad.At present mainly is that fertiliser granulates is carried out coating reducing the rate of release of nutrient, its technology be material after granulation, oven dry, cooling, screening, will delay again, controlled-release material is wrapping to the granulated fertilizer surface.This product membrane wrapping thickness in process of production is difficult to control, and it is consistent with the fertilizer efficiency burst size of coated fertilizer to cause the needed fertilizer amount of the different process of growth of farm crop to be difficult to.Development such as China's Zhang Fudao adhesive type slow release fertilizer; but still belong to secondary processing type slow release fertilizer; the characteristics of this secondary processing type slow-release fertilizer production method are the further processing on finished product fertilizer basis; increase the complexity and the process period of the course of processing, on certain first time, be unfavorable for large-scale production.
Summary of the invention
The objective of the invention is to provide a kind of production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation at the deficiencies in the prior art, it is the water resistance that utilizes melamino-formaldehyde and colloidal sol water glass, the cohesiveness and the good characteristics of flexility of polyvinyl formal, produces the fertile slurry of a kind of and urea or compound and has better confluent endoplasm sustained release agent.
Polyvinyl formal belongs to linear polymeric, and molecular chain is longer, has cohesiveness and snappiness preferably, and the network structure that simultaneously also can its macromole forms is nutrient fixedly.The polymkeric substance that trimeric cyanamide and formaldehyde form has tridimensional network, and stronger hydrophobic nature is arranged.Water glass also has certain water resistance simultaneously.The present invention is that host prepares sustained release dosage with these three kinds of components, forms slow-release carbamide or the slow-release compound fertilizer with sustained release performance behind the fertile slurry of adding urea or compound.
The technical solution adopted in the present invention is: a kind of production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation, comprise the preparation section of melamino-formaldehyde polymers soln, the preparation section of polyvinyl formal solution, the preparation section of sustained release dosage, its concrete steps are as follows:
1, the preparation section of melamino-formaldehyde polymers soln
(1), presses mass ratio 445 parts of 37% formaldehyde solutions are regulated pH value to 8.0～9.5 scopes with 10% sodium hydroxide solution;
(2), add 200～300 parts of trimeric cyanamides and 10～30 parts of polyvinyl alcohol, 85～95 ℃ of controlled temperature reacted 0.8～1.2 hour;
(3), be cooled to 75～85 ℃, add 40～60 parts of 95% ethanol, regulate pH to 8.0～9.5 scopes then, react and add 40～60 parts of 95% ethanol, 90～110 parts of deionized waters after 1.2～1.7 hours, add 5～25 parts in urea after stirring, continue to stir 20 minutes, regulate pH to 6.5～7.5, obtain the melamino-formaldehyde polymers soln after being cooled to 40 ℃, standby.
The pH value of described 37% formaldehyde solution also can be regulated pH value to 1.0～4.5 scopes with 15% salpeter solution.
2, the preparation section of polyvinyl formal solution
(1), get 900～1100 parts of distilled water, 85～95 ℃ of controlled temperature add 40～80 parts of polyvinyl alcohol, stir so that polyvinyl alcohol dissolves fully, regulate pH value to 1.0～5.5 scopes then by mass ratio;
(2), controlled temperature is 55～95 ℃, add 20～50 parts of 37% formaldehyde solutions, reacted 30～40 minutes, add 250～350 parts of sol sodium silicates, stir, add 20～40 parts in urea then, stir and regulate pH to 6.5～7.5 after 10 minutes, obtain polyvinyl formal solution after being cooled to 40 ℃, standby.
The preparation method of described sol sodium silicate is: (1), press mass ratio and in 200 part of 10% sulphuric acid soln, add 15～25 parts of trolamines, and it is standby to stir; (2), to add modulus in 900 parts of distilled water be 80～120 parts of 3.2～3.6 liquid soluble glass, stir to make water glass dissolve fully; (3), add 160～200 parts of the triethanolamine solutions that step (1) obtains, after stirring, regulate pH value to 10.5～12.0, cooling is afterwards standby to the gained water glass solution.
3, the preparation section of sustained release dosage
The melamino-formaldehyde polymers soln that obtains and the polyvinyl formal solution mixed with 1:0.5～1:2.0 is stirred, 75～85 ℃ of controlled temperature, add distilled water regulator solution solid content 10～30%, prepare melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation.
Add in secondary mixing tank urea production line spray granulating before with volume pump melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation or in the secondary mixing tank before the compound fertilizer pelletizing, add-on is 1%～1.5% of urea quality or the fertile quality of compound, is slow-release carbamide or slow-release compound fertilizer behind the fertile granulating of urea or compound.
The present invention utilizes the water resistance of melamino-formaldehyde and colloidal sol water glass, the characteristics that the cohesiveness of polyvinyl formal and flexility are good, produce the fertile slurry of a kind of and urea or compound and have better confluent endoplasm sustained release agent, it is simple to have technology, advantages such as the time is short, the endoplasm sustained release agent of preparation can directly add in urea or the fertile secondary mixing of compound produces slow-release carbamide or slow-release compound fertilizer, content is big, the sustained release dosage consumption is low, produce simple and be easy to and control, compare with secondary processing production slow-release carbamide or slow-release compound fertilizer, can conserve energy and minimizing transportation.
Embodiment
The invention will be further described with indefiniteness embodiment below.
Embodiment,
One, the preparation of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation
1.1, sol sodium silicate preparation:
(1), at 200kg10%H
2SO
4Add trolamine 20kg in the solution, stir, standby.
(2), in the 900kg deionized water, add 100kg water glass, stirring, dissolving fully.
(3), in above-mentioned water glass solution, add the 10%H that 180kg contains trolamine
2SO
4Stir, regulate pH value to 12.0, become the colloidal sol caking after 1 hour, be colloidal sol water glass.
1.2, the preparation of polyvinyl formal solution
(1) in reactor, adds deionized water 940kg, start agitator and low-pressure steam heat temperature raising to 95 ℃.
(2) add polyvinyl alcohol 60kg,, need 1.5 hours to dissolving fully.
(3) be cooled to 82 ℃, with dilute hydrochloric acid adjust pH to 2.0.
(4) add formaldehyde solution 24kg, filling tube should be below liquid level, reaction 45min.
(5) add sol sodium silicate 300kg, stir, regulate pH value to 8.5.
(6) add urea 40kg, mix 0.5h.After reaction finished, regulating the pH value was 7.0.
(7) be cooled to 40 ℃ of blowings, go into the bucket standby.
1.3, the preparation of melamino-formaldehyde polymers soln
(1) squeezes into formaldehyde solution 445kg with volume pump to reactor, start agitator, add the 1%NaOH aqueous solution and regulate pH value to 9.0.
(2) add 245kg trimeric cyanamide, 20kg polyvinyl alcohol.
(3) open low-pressure steam, be warming up to 92 ℃, reaction 1h.
(4) be cooled to 82 ℃, add 95% ethanol 50kg, regulate pH value to 8.5 then, react 1.5h down at 82 ℃.
(5) add 95% ethanol 50kg, deionized water 100kg after mixing, regulates pH value to 8.0, continues to stir 0.5h.
(6) add urea 20kg, stir 0.5h.After reaction finished, regulating the pH value was 7.0.
(7) be cooled to 40 ℃ of blowings, go into the bucket standby.
1.4, the preparation of sustained release dosage
Under agitation condition, add 1000kg melamino-formaldehyde solution and 1000kg polyvinyl formal solution, mix, 80 ℃ of controlled temperature, regulating the pH value is 7.0.Adding distil water adjusting solid content is 20% then.
The preparation of two slow-release compound fertilizers
In the fertile system of the high tower compound of producing 150000 tons per year, carry out the productivity pilot scale, N-P
2O
5-K
2O=20-12-8, total nutrient amount 40%, in the secondary mixing tank, add the above-mentioned endoplasm sustained release agent that the fertile quality 1% of compound contains solid substance 20%, because of the sustained release dosage completely solidified needs about 21 days, so slow-release compound fertilizer need be placed 21 days to realize completely solidified with the pressurization flow pump.
Three water wash effects
Get the sample determination of in plastics bag, placing behind the slow-release compound fertilizer sample after 30 days.
47.6%, 5 cumulative leaching rate 97.7% of the fertile elementary solubility rate of nitrogen of common compound.
31.85%, 20 cumulative leaching rate 93.97% of the elementary solubility rate of endoplasm type slow-release compound fertilizer nitrogen.
Japan's fertilizer law (1996) is to the elementary solubility rate of field crop regulation nitrogen＜50%." national soil fertility and fertilizer benefit monitoring base complex " by 16 years monitoring results, field crop nitrogen requirement in early stage accounted for 1/3 of whole growing total nitrogen, and the intermediary and later stages account for 2/3.The elementary solubility rate of endoplasm type slow-release compound fertilizer meets the need nitrogen rule of field crop basically.
Four land for growing field crops fertilizer efficiency
4.1, test soil and fertilising situation
Changping, Beijing " national brown moisture soil soil fertility and fertilizer benefit monitoring base ", the moisture soil great soil group, brown moisture soil great soil group, the soil texture is a silt loam.Soil physical and chemical property: pH value 8.11, organic 16.42gkg
-1, full nitrogen (N) 1.03gkg
-1, full phosphorus (P
2O
5) 0.89gkg
-1, alkali-hydrolyzable nitrogen (N) 61.67mgkg
-1, rapid available phosphorus (P
2O
5) 9.79mgkg
-1, available potassium (K
2O) 40mgkg
-1Corn variety: middle list 8578.District area: 2.5m * 4m, 3 repetition rate of fertilizer application: N/180kg/1hm
2, phosphorus (P
2O
5) 96kg/hm
2, potassium (K
2O) 96kg/hm
2Blank NPK such as (CK) contrast if do not apply fertilizer.
4.2, the summer corn test-results
Table 2 different treatment summer corn yield result
Annotate: " * * " expression difference reaches utmost point conspicuous level in the table
Test-results, the summer corn grain yield, NPK such as endoplasm type slow-release compound fertilizer ratio handle volume increase 20.73%.Comprehensive above-mentioned water wash result, the slow release effect of endoplasm type slow-release compound fertilizer is better.
Claims (2)
1. the production method of a melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation, it is characterized in that: comprise the preparation section of melamino-formaldehyde polymers soln, the preparation section of polyvinyl formal solution, the preparation section of sustained release dosage, its step is as follows:
1), the preparation section of melamino-formaldehyde polymers soln
(1), presses mass ratio 445 parts of 37% formaldehyde solutions are regulated pH value to 8.0～9.5 scopes with 10% sodium hydroxide solution;
(2), add 200～300 parts of trimeric cyanamides and 10～30 parts of polyvinyl alcohol, 85～95 ℃ of controlled temperature reacted 0.8～1.2 hour;
(3), be cooled to 75～85 ℃, add 40～60 parts of 95% ethanol, regulate pH to 8.0～9.5 scopes then, react and add 40～60 parts of 95% ethanol, 90～110 parts of deionized waters after 1.2～1.7 hours, add 5～25 parts in urea after stirring, continue to stir 20 minutes, regulate pH to 6.5～7.5, obtain the melamino-formaldehyde polymers soln after being cooled to 40 ℃, standby;
2), the preparation section of polyvinyl formal solution
(1), get 900～1100 parts of distilled water, 85～95 ℃ of controlled temperature add 40～80 parts of polyvinyl alcohol, stir so that polyvinyl alcohol dissolves fully, regulate pH value to 1.0～5.5 scopes then by mass ratio;
(2), controlled temperature is 55～95 ℃, add 20～50 parts of 37% formaldehyde solutions, reacted 30～40 minutes, add 250～350 parts of sol sodium silicates, stir, add 20～40 parts in urea then, stir and regulate pH to 6.5～7.5 after 10 minutes, obtain polyvinyl formal solution after being cooled to 40 ℃, standby;
The preparation method of described sol sodium silicate is: (1), press mass ratio and in 200 part of 10% sulphuric acid soln, add 15～25 parts of trolamines, and it is standby to stir; (2), to add modulus in 900 parts of distilled water be 80～120 parts of 3.2～3.6 liquid soluble glass, stir to make water glass dissolve fully; (3), add 160～200 parts of the triethanolamine solutions that step (1) obtains, after stirring, regulate pH value to 10.5～12.0, cooling is afterwards standby to the gained water glass solution;
3), the preparation section of sustained release dosage
The melamino-formaldehyde polymers soln that obtains and the polyvinyl formal solution mixed with 1:0.5～1:2.0 is stirred, 75～85 ℃ of controlled temperature, add distilled water regulator solution solid content 10～30%, prepare melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation.
2. the production method of melamine formaldehyde-polyvinyl formal fertilizer slow-release formulation according to claim 1 is characterized in that: the pH value of 37% formaldehyde solution is regulated pH value to 1.0～4.5 scopes with 15% salpeter solution in the preparation section of described melamino-formaldehyde polymers soln.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101585953B (en) * | 2009-06-23 | 2010-12-29 | 中国林业科学研究院林产化学工业研究所 | Method for preparing melamine formaldehyde molding compound |
| CN103058797B (en) * | 2012-02-28 | 2014-01-29 | 五洲丰农业科技有限公司 | Production method of slow release fertilizer |
| CN103288564B (en) * | 2012-02-28 | 2014-05-07 | 五洲丰农业科技有限公司 | Production method of encapsulated sustained release agent specially for urea or compound fertilizer |
| CN102924176A (en) * | 2012-11-20 | 2013-02-13 | 中南林业科技大学 | Sustained oxygen release fertilizer and preparation method thereof |
| CN104926444A (en) * | 2015-06-05 | 2015-09-23 | 宁夏共享生物化工有限公司 | Method for preparing slow/controlled release fertilizer by use of modified urea resin coating material |
| CN106748303A (en) * | 2017-02-20 | 2017-05-31 | 山东鲁北企业集团总公司 | A kind of chemical fertilizer controlled release agent and preparation method thereof |
| CN107202818A (en) * | 2017-05-26 | 2017-09-26 | 四川诺特科技有限公司 | Soil electron ion detecting system on preventing thunderbolt |
| CN107219871A (en) * | 2017-05-26 | 2017-09-29 | 四川诺特科技有限公司 | Using in improvement underground electric layer constructional device |
| CN112961008B (en) * | 2021-02-25 | 2023-05-02 | 中国科学院合肥物质科学研究院 | Preparation method of low-water-solubility nitrogen-containing coating material and prepared nitrogen-containing coating material |
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Owner name: OFFSHORE OIL FUDAO CO., LTD. Free format text: FORMER OWNER: CHINA MARINE PETROLEUM GENERAL CO. Effective date: 20110803 Free format text: FORMER OWNER: CHINA BLUECHEMICAL LTD. |
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Effective date of registration: 20110803 Address after: 572600 No. 3 Jiangnan Avenue, Dongfang City, Hainan Province Patentee after: CNOOC Fudao Limited Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: China Blue Chemical Ltd. Patentee before: China National Offshore Oil Corporation |