CN102260112A - Method for preparing humic acid urea complex in urea meltwater medium - Google Patents
Method for preparing humic acid urea complex in urea meltwater medium Download PDFInfo
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- CN102260112A CN102260112A CN2011101266668A CN201110126666A CN102260112A CN 102260112 A CN102260112 A CN 102260112A CN 2011101266668 A CN2011101266668 A CN 2011101266668A CN 201110126666 A CN201110126666 A CN 201110126666A CN 102260112 A CN102260112 A CN 102260112A
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Abstract
The invention provides a method for preparing humic acid urea complex in urea meltwater medium. According to the method, 20 to 200 parts of urea is heated to a temperature of 80 to 140 DEG C in a reaction vessel while stirring; when urea is melted, 20 to 100 parts of humic acid feed coal is slowly added into the reaction vessel; the materials are subject to a reaction for 10 to 90 minutes while stirring, such that humic acid urea complex meltwater is obtained; the meltwater is dried, such that solid humic acid urea complex is obtained. The raw material sources for producing the complex are abundant, cheap and easy to obtain. The production procedure is short; the equipment is easy to operate; continuous production is easy to be carried out; the production procedure is environment protecting; and no pollutant is discharged. The product is nontoxic, and has good water-solubility. The production has a good compatibility with N, P, K, micronutrient elements, and pesticides. The material can be used in urea coating for producing sustained-release fertilizer, and can be directly blended into humic acid foliar fertilizer, humic acid liquid rinsing and irrigating fertilizer, saline land modifier, and humic acid composite fertilizer. The material can be used for preparing humic acid liquid state mulch film, and humic acid water-retaining agent. Also, the material can be used as animal feedstuffs.
Description
Technical field
The invention belongs to the slow release fertilizer technical field, particularly relate to a kind of method that in the urea melting liquid medium, prepares complex of humic acids and urea.
Background technology
In order to improve urea efficiency and nitrogen use efficiency, all pay close attention to very much research slow released urea release and release control fertilizer both at home and abroad.Relevant this respect has more bibliographical information, and summary reduces, and adds the urease activity inhibitor method, coating coated urea method, and polycondensation becomes urea aldehyde macromole indissoluble thing method, humic Acid Coated Urea or complex of humic acids and urea method etc.Because technical sophistication or production cost are than problems such as height, first three methods is not all seen large-scale industrial production and large scale application, and bulk article is put on market and also just is used for trying out on flowers, lawn, golf course or the cash crop.
Humic acid fertilizer is applied and is allowed people recognize for many years, and the humic acids structure of improving the soil is improved the soil microorganisms ecotope, stimulates crop absorption nutrition branch, improves crop drought resistance, anti-adversity, improves crop yield, improves crop quality.Humic acids can also suppress urease activity and nitrobacteria activity, and urea is slowly decomposed, and improves urea efficiency and nitrogen use efficiency.The humic acid urea fertilizer efficiency prolongs 30-35d than common urea, and nitrogen utilization efficiency on average improves 10.4% than common urea.Domestic and international agriculturalization, coalification, chemical science and technology worker actively are devoted to humic acids coated urea and complex of humic acids and urea research, have obtained some gratifying achievements in research.Japan special permission bulletin clear 348375 and 348376 provides application liquefied ammonia and organic solvent methyl alcohol, ethanol, acetone etc. as reaction medium respectively, prepares the method for complex of humic acids and urea under high-temperature and high-pressure conditions.Japan 15917 provides a kind of and in humic acid solution urea, formaldehyde and humic acids is carried out polycondensation, prepares the method for insoluble humic acid urea formaldehyde condensation products.Because technical qualification are harsh and production cost than higher, Japanese these three kinds of methods suitability for industrialized production that all is unrealized.Domesticly also disclose some about preparation complex of humic acids and urea patent, CN 96108848.6 reacts with weathered coal and ammoniacal liquor to make ammonium humate, makes complex of humic acids and urea with urea reaction again; CN 971088.48, and CN 99117649.9 and CN 01111071.6 are same types, and weathered coal with ammoniacal liquor and carbonated aqueous ammonia or sig water activation, is wrapped in urea surface then.CN 200610052445.X is in urea melting liquid mist projection granulating process, sprays into that humic acids or humate and tackiness agent carry out the shower nozzle granulation or humic acid urea is made in the solid granulation, and the other two kinds of technologies that provide are difficult to realize industrial production.CN 200810080040.6 is that humic acids is wrapped in the urea granules, can not effectively suppress the urase decomposing urea with fusing urea parcel humic acids or ammonium humate particle.The defective of above-mentioned domestic these patents is production operation troubles, and production cost is higher, and some is that technical difficulty is bigger, all be unrealized large-scale industrial production and large scale application." process exploitation of humic acids-urea complex compound " of Cheng Shaoxin report (Cheng Shaoxin etc., humic acids, 1994,4, pp29-32) similar with the content of CN 96108848.6." Study on Preparation of humic urea mixture " of Lanzhou University's stone brightness literary composition report (Shi Huiwen etc., humic acids, 2002,3, pp33-34), be earlier weathered coal to be made pure humic acids by alkali-soluble acid analysis, again with fusing urea prepared in reaction humic urea mixture.As raw materials for production, not only the technological process of production is long with pure humic acids for this kind method, and troublesome poeration also and increased production cost, is difficult for realizing large-scale industrial production.
Summary of the invention
In order to overcome the defective of above-mentioned domestic and international patent and document public technology, the present invention discloses a kind of bibliographical information of not seeing, prepares the method for complex of humic acids and urea in the urea melting liquid medium with the humic acid material coal.
Technical scheme of the present invention is as follows: with 20-200 part urea in reactor, be heated to 80-140 ℃ under stirring, after treating urea melting, slowly add 20-100 part humic acid material coal, continued stirring reaction 10-90 minute, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea then.
Humic acid material coal described in the technique scheme is any or multiple combination in weathered coal, brown coal, the peat, and water content is 0-40%, and humic acids content 〉=20% was pulverized the 30-200 mesh sieve.
Urea described in the scheme is industrial goods or agricultural supplie.
The complex of humic acids and urea of method preparation provided by the invention, its main component is: contain water-soluble humic acids 5.0-18.0%, nitrogen 34-40%, water-insoluble 9.5-17.5%, the pH=8.0-8.8 of complex of humic acids and urea 1.0% aqueous solution.
Method provided by the invention is compared with disclosed method, has following advantage:
1. raw material weathered coal, brown coal, the peat aboundresources of the present invention's use are cheap and easy to get; The technological process of production is brief, and production unit is easy to the continuous industry operation, and is easy and simple to handle; Product toxicological harmless, good water solubility, production cost is low, non-pollutant discharge, non-environmental-pollution.
2. the complex of humic acids and urea chemical stability and the Heat stability is good (130 ℃ are not decomposed) of method preparation provided by the invention, applied range, can be used for coated urea and make slow release long-acting fertilizer, good with N, P, K, micronutrient element, agricultural chemicals compatibility, can directly prepare the humic acids foliage fertilizer, humic acid solution (cream) body dashes and executes (drip irrigation) fertilizer, alkaline land modifying agent, multi-nutrient element humic acid compound manure; The liquid mulch film of preparation humic acids, moisture holding agent of humic acid can also be used for animal-feed etc.
3. the method for preparing complex of humic acids and urea in the urea melting liquid medium provided by the invention is applicable to weathered coal, brown coal and the peat of different sources, all obtains reasonable effect.
4. complex of humic acids and urea applied range in agricultural, forestry, plant husbandry of method preparation provided by the invention, can be used as long-acting slow-release fertilizer, soil improvement agent, plant growth stimulant, both can make base manure, can topdress again, seed manure, also be applicable to seed soaking, dress seed, dip in root, can stimulate crop to absorb nutrient, strengthen drought resisting, anti-adversity, improve crop yield, improve crop quality.
Embodiment
Embodiment 1: get 100 parts of urea in reactor, be heated to about 125 ℃ under stirring, behind the urea fine melt, slowly add 25 parts and contain humic acids 69% (butt), Wuchuan, Inner Mongol leonardite of moisture 28%, continue reaction 45 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 12.6%, and N 36.6%, water-insoluble 15.0%, complex of humic acids and urea 1% aqueous solution pH=8.2.
Embodiment 2: get 100 parts of urea in reactor, be heated to about 120 ℃ under stirring, behind the urea fine melt, slowly add 33 parts and contain humic acids 69% (butt), Wuchuan, Inner Mongol leonardite of moisture 28%, continue reaction 40 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 17.1%, and N 39.1%, water-insoluble 10.9%, complex of humic acids and urea 1% aqueous solution pH=8.5.
Embodiment 3: get 100 parts of urea in reactor, be heated to about 123 ℃ under stirring, behind the urea fine melt, slowly add 25 parts and contain humic acids 70% (butt), moisture 20% Inner Mongol Wuhai weathered coal, continue reaction 50 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 7.9%, and N 35.7%, water-insoluble 15.1%, complex of humic acids and urea 1% aqueous solution pH=8.5.
Embodiment 4: get 100 parts of urea in reactor, be heated to about 128 ℃ under stirring, behind the urea fine melt, slowly add 20 parts and contain humic acids 70% (butt), moisture 20% Inner Mongol Wuhai weathered coal, continue reaction 45 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 4.6%, and N 34.1%, water-insoluble 17.4%, complex of humic acids and urea 1% aqueous solution pH=8.5.
Embodiment 5: get 100 parts of urea in reactor, be heated to about 125 ℃ under stirring, behind the urea fine melt, slowly add 33 parts and contain humic acids 44% (butt), Wuchuan, Inner Mongol leonardite of moisture 26.5%, continue reaction 50 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 9.7%, and N 40.0%, water-insoluble 14.6%, complex of humic acids and urea 1% aqueous solution pH=8.8.
Embodiment 6: get 100 parts of urea in reactor, be heated to about 122 ℃ under stirring, behind the urea fine melt, slowly add 25 parts and contain humic acids 44% (butt), Wuchuan, Inner Mongol leonardite of moisture 26.5%, continue reaction 40 minutes, make the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea.The present embodiment products obtained therefrom contains water-soluble humic acids 8.5%, and N 39.5%, water-insoluble 9.6%, complex of humic acids and urea 1% aqueous solution pH=8.5.
Claims (4)
1. method that in the urea melting liquid medium, prepares complex of humic acids and urea, it is characterized in that: with 20-200 part urea in reactor, be heated to 80-140 ℃ under stirring, after treating urea melting, slowly add 20-100 part humic acid material coal, continued stirring reaction 10-90 minute, and made the complex of humic acids and urea fused solution, drying makes the solid complex of humic acids and urea then.
2. according to claim 1, it is characterized in that: described humic acid material coal is any or multiple combination in weathered coal, brown coal, the peat.
3. according to claim 1, it is characterized in that: described humic acid material coal water content is 0-40%, and humic acids content 〉=20% was pulverized the 30-200 mesh sieve.
4. according to claim 1, it is characterized in that: described urea is industrial goods or agricultural supplie.
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| CN2011101266668A CN102260112A (en) | 2011-05-17 | 2011-05-17 | Method for preparing humic acid urea complex in urea meltwater medium |
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| CN2011101266668A CN102260112A (en) | 2011-05-17 | 2011-05-17 | Method for preparing humic acid urea complex in urea meltwater medium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819266A (en) * | 2014-01-28 | 2014-05-28 | 广西喷施宝股份有限公司 | Three-dimensional fertilizer applying method for crops |
| CN105272467A (en) * | 2015-10-30 | 2016-01-27 | 贵州双赢生态肥有限公司 | Preparation process of ecological organic composite fertilizer |
| CN105272469A (en) * | 2015-10-30 | 2016-01-27 | 贵州双赢生态肥有限公司 | Ecological organic composite fertilizer |
| CN109970488A (en) * | 2017-12-28 | 2019-07-05 | 许传高 | The liquid fertilizer made using amino acid fermentation tail washings |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1169975A (en) * | 1996-07-08 | 1998-01-14 | 中国科学院山西煤炭化学研究所 | Preparation of complex of humic acids and urea |
| CN1304659A (en) * | 2000-12-06 | 2001-07-25 | 云南云大应用化学开发研究所 | Comprehensive utilization method of brown coal |
| CN101054314A (en) * | 2007-04-03 | 2007-10-17 | 王怀欣 | Composite organism slow release fertilizer product and producing method |
| CN101074179A (en) * | 2007-06-28 | 2007-11-21 | 东北师范大学 | Special Ginseng composite mixed fertilizer |
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2011
- 2011-05-17 CN CN2011101266668A patent/CN102260112A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1169975A (en) * | 1996-07-08 | 1998-01-14 | 中国科学院山西煤炭化学研究所 | Preparation of complex of humic acids and urea |
| CN1304659A (en) * | 2000-12-06 | 2001-07-25 | 云南云大应用化学开发研究所 | Comprehensive utilization method of brown coal |
| CN101054314A (en) * | 2007-04-03 | 2007-10-17 | 王怀欣 | Composite organism slow release fertilizer product and producing method |
| CN101074179A (en) * | 2007-06-28 | 2007-11-21 | 东北师范大学 | Special Ginseng composite mixed fertilizer |
Non-Patent Citations (1)
| Title |
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| 林海涛: "腐植酸尿素新型生产工艺及田间应用效果的研究", 《腐植酸》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819266A (en) * | 2014-01-28 | 2014-05-28 | 广西喷施宝股份有限公司 | Three-dimensional fertilizer applying method for crops |
| CN103819266B (en) * | 2014-01-28 | 2016-04-20 | 广西喷施宝股份有限公司 | A kind of method of three-D crop fertilising |
| CN105272467A (en) * | 2015-10-30 | 2016-01-27 | 贵州双赢生态肥有限公司 | Preparation process of ecological organic composite fertilizer |
| CN105272469A (en) * | 2015-10-30 | 2016-01-27 | 贵州双赢生态肥有限公司 | Ecological organic composite fertilizer |
| CN109970488A (en) * | 2017-12-28 | 2019-07-05 | 许传高 | The liquid fertilizer made using amino acid fermentation tail washings |
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Application publication date: 20111130 |