CN102001880A - Process for producing microelement complex fertilizer - Google Patents
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Abstract
The invention discloses a process for producing a microelement complex fertilizer. The method comprises the following steps of: reacting a chelant (ethylene diamine tetraacetic acid (EDTA) or diethylene triamine pentaacetic acid (DTPA) or a mixture of the EDTA and the DTPA), a metallic element compound and alkali (sodium hydroxide, potassium hydroxide or ammonia water) in a molar ratio of the chelant to the metallic element compound to the alkali of 1.01:1:2 (when the metallic element is a Fe element, the molar ratio is 1.01:1:1) at the temperature of between 50 and 125 DEG C for 20 to 60 minutes to obtain EDTA or DTPA chelating element complex fertilizer solution with required proportion content; and adjusting the pH of a product, filtering and drying to obtain a product. In the process, the product is prepared by a one-step process, the obtained product can be adjusted in a certain range (but cannot go beyond the reach of chelating), and a series of products are obtained to meet the specific requirements of various plants in various areas. The process is used for agriculture, forestry, flowers, gardening, soilless culture and the like and can correct adverse reaction due to plant deficiency.
Description
Technical field
The present invention relates to a kind of production technique of microelement complex fertilizer.
Background technology
At present, the microelement complex fertilizer on the fertilizer market, no matter be soil application, or foliage-spray, effect is not very desirable.Microelement complex fertilizer generally has the little fertilizer of humic acids, amino acid or citric acid, and their utilization ratios in use are all lower.
In the prior art, the patent No. is to disclose a kind of organic chelated Medium Trace Element Fertilizer technology in 200410029779.6 the Chinese patent, this technology comprises that extracting corruption from brown coal plants matter, through precipitation, obtain required liquid, add organic sequestering agent citric acid or its esters and trace element, resulting liquid potential of hydrogen furnishing neutrality, system promptly gets product of the present invention after doing.Though the present invention is at present unique by organic chelated and soda acid allotment, reach and in extract, keep all the technological process that matter is planted in effectively corruption, but the product chelating ability that obtains by this method is very little, insolubless such as the oxyhydroxide of metal or oxide compound in alkaline soil, saltings, will occur, obviously reduce fertilizer efficiency.
Application number is the production method that discloses a kind of EDTA complex metal salt in 02113215.1 the Chinese patent, this method comprises ethylenediamine tetraacetic acid (EDTA), alkali, add in the entry, stirring reaction, obtain edetate, add metal-salt again, above-mentioned alkali is sodium hydroxide, potassium hydroxide, a kind of in the ammonia, above-mentioned metal-salt is an ironic hydroxide, manganous hydroxide, copper hydroxide, zinc hydroxide, a kind of in the magnesium hydroxide, above-mentioned ethylenediamine tetraacetic acid (EDTA): alkali: the mole proportioning of metal-salt is 1: 0.8～2.2: 0.8～1.1, under 20～150 ℃ of conditions, reacted 0.5～5 hour, and removed insolubles after filtration and obtain liquid product.The inventive method is applicable to the high purity organic complex attitude trace element fertilizer of making various single-elements.Because this patent mainly is applicable to single metallo-chelate, and in actual applications, need several materials to be used according to certain ratio, so use extremely inconvenient in the reality, and this patent only uses the oxyhydroxide of metal, so not only be not easy to adjust prescription, and increased cost.
The patent No. is the production method that discloses a kind of EDTA complex metal salt in 01133707.9 the Chinese patent, this method comprises that ethylenediamine tetraacetic acid (EDTA), sodium hydroxide add in the entry, stirring reaction, obtain disodium edta, add metal-salt again, ethylenediamine tetraacetic acid (EDTA): sodium hydroxide: metal-salt: the mole proportioning of water is 1: 1.5～5.0: 0.1～1.1: 10～200, under 70～150 ℃, reacted 0.5～5 hour, and obtained product.Above-mentioned metal-salt is a kind of in iron trichloride, ferric sulfate, manganous carbonate, ventilation breather, zinc oxide, zinc subcarbonate, magnesium oxide, the magnesium basic carbonate.The inventive method is applicable to the high purity organic complex attitude trace element fertilizer of making various single-elements.Because this patent mainly is applicable to the organic complex attitude trace element fertilizer of single-element, but purity is not high, contains a large amount of chlorions or sulfate ion, with preceding patent basically identical, the former is the latter's improvement, so also be inconvenience very in the practical application.
Summary of the invention
In view of above-mentioned reason, the purpose of this invention is to provide new, easy, the microelement complex fertilizer of method production fast, difficulty that runs in the technology before overcoming and restriction.
Purpose of the present invention is intended to improve storage degree, the stability in the product, and fertility provides a kind of production technique of trace gold prime element plant nutrition fertilizer.
In the method for the invention: with ethylenediamine tetraacetic acid (EDTA) (hereinafter to be referred as EDTA) or diethylene triamine pentacetic acid (DTPA) (hereinafter to be referred as DTPA) or EDTA and DTPA mixing and metallic element compound, and alkali.According to certain molar ratio, reaction is 20-60 minute under 50-110 ℃ temperature, and preferred temperature is 70-125 ℃, needing to obtain the EDTA or the DTPA chelating element mixed fertilizer solution of ratio content, and the PH to product adjusts simultaneously.Add boric acid/or other solubility borates or contain the soluble compound of molybdenum or the soluble compound of cobalt in mixed fertilizer solution, obtain containing the more formulation product solution of multielement, through filtering, spraying drying obtains solid phase prod again.
The metallic element compound comprises metallic element oxide compound, metallic element carbonate, metallic element subcarbonate or metallic element oxyhydroxide, and described alkali comprises sodium hydroxide, potassium hydroxide or ammoniacal liquor.。
Described metallic element comprises iron, copper, manganese, zinc, magnesium or calcium.
Used ferro element raw material can be ironic hydroxide, iron oxide red (ferric oxide) or iron oxide black (Z 250) etc., through reaction, will obtain chelated iron, and water, does not have other by products.When in the needs product a certain amount of chlorion being arranged, also can use iron(ic) chloride.When needing a certain amount of sulphur in the product, also can use ferric sulfate or ferrous sulfate.
Used copper raw material can be cupric oxide or ventilation breather, through reaction, will obtain chelated copper, and water, and carbon dioxide does not have other by products.When in the needs product a certain amount of chlorion being arranged, also can use cupric chloride.When needing a certain amount of sulphur in the product, also can use copper sulfate.
Used zinc element raw material can be zinc oxide or zinc hydroxide, through reaction, will obtain chelating zinc, and water, does not have other by products.When in the needs product a certain amount of chlorion being arranged, also can use zinc chloride.When needing a certain amount of sulphur in the product, also can use zinc sulfate.
Used manganese element raw material, preferred manganous carbonate through reaction, will obtain Chelated Manganese, and water, and carbon dioxide does not have other by products.When in the needs product a certain amount of chlorion being arranged, also can use Manganous chloride tetrahydrate.When needing a certain amount of sulphur in the product, also can use manganous sulfate.
Used magnesium elements raw material, preferred magnesium oxide or magnesium hydroxide through reaction, will obtain chelated magnesium, and water, not have other by products.When in the needs product a certain amount of chlorion being arranged, also can use magnesium chloride.When needing a certain amount of sulphur in the product, also can use sal epsom.
Used calcium constituent raw material, preferred lime carbonate through reaction, will obtain chelating calcium, and water, and carbon dioxide does not have other by products.
The mol ratio of described EDTA and metallic element compound is 1-1.05: 1, with the mol ratio of sodium hydroxide or potassium hydroxide or ammoniacal liquor be 1-1.05: 1.0-2.1, like this can be with the whole chelatings of golden prime element.
The mol ratio of described DTPA and metallic element is 1-1.05: 1, with the mol ratio of sodium hydroxide or potassium hydroxide or ammoniacal liquor be 1-1.05: 2.0-3.1, like this can be with the whole chelatings of golden prime element.
The mol ratio of described EDTA and DTPA mixture and metallic element compound is 1-1.05: 1.The mol ratio of described EDTA and DTPA mixture and alkali is 1-1.05: 1.0-2.1.
The equation of above-mentioned reaction can be expressed as follows:
5EDTA+Fe(OH)
3+ZnO+MnCO
3+1/2Cu(OH)
2.CuCO
3+Mg(OH)
2+9NaOH＝EDTA.FeNa+EDTA.ZnNa
2+EDTA.MnNa
2+EDTA.CuNa
2EDTA.MgNa
2+CO
2+H
2O ……………………………(1)
5DTPA+Fe(OH)
3+ZnO+MnCO
3+1/2Cu(OH)
2.CuCO
3+Mg(OH)
2+9NaOH＝DTPA.FeNa
2+DTPA.ZnNa
3+DTPA.MnNa
3+DTPA.CuNa
3DTPA.MgNa
3+CO
2+H
2O ……………………………(2)
5EDTA+Fe(OH)
3+ZnO+MnCO
3+1/2Cu(OH)
2.CuCO
3+Mg(OH)
2+9KOH＝EDTA.FeK+EDTA.ZnK
2+EDTA.MnK
2+EDTA.CuK
2EDTA.MgK
2+CO
2+H
2O ……………………………(3)
5DTPA+Fe(OH)
3+ZnO+MnCO
3+1/2Cu(OH)
2.CuCO
3+Mg(OH)
2+9KOH＝DTPA.FeK
2+DTPA.ZnK
3+DTPA.MnK3+DTPA.CuK
3DTPA.MgK
3+CO
2+H
2O ……………………………(4)
In the equation, (1), (3) are the chelating mixture of EDTA, sodium hydroxide and golden prime element, and (2), (4) are the chelating mixture of DTPA, sodium hydroxide and golden prime element, owing to the wherein not trim of amount of carbonic acid gas and water of simple reason.In fact also can use the mixture of EDTA and DTPA as sequestrant.Reactant is except the product of needs, and other gas is directly discharged, and water is removed through super-dry, does not contain other byproducts in the product.
Its pH value of the said product of the present invention is neutral, generally remains between the 5.0-9.0, preferably at 6.0-8.0, further between 6.0-7.0.
In order to obtain such PH result, need to add sodium hydroxide or the potassium hydroxide or the ammoniacal liquor etc. of certain mol proportion, with sodium hydroxide is example, count according to EDTA, inner complex for iron, moles such as amount that need add and EDTA, other microelement chelates, the amount that needs adding is two times of EDTA molar weight.According to the DTPA meter, for the inner complex of iron, the amount that needs adding is two times of DTPA molar weight, other microelement chelates, and the amount that needs adding is three times of DTPA molar weight.If use potassium hydroxide or ammoniacal liquor instead, according to the mole adding of sodium hydroxide.DTPA is bigger to the chelating degree of metal, and the product that obtains is more stable, but price is higher relatively.
In fact, the pH value of product need be adjusted according to the test result of reality before reaction finishes, specifically on, if PH is higher, can be fine-tuning to normally with EDTA, on the contrary, can be fine-tuning to normally with diluted alkaline.
Other optional elements of the present invention can be selected inorganics, mainly are the boron and the molybdenum of trace, can the dissolved respective substance as long as select, and for example boric acid, Sodium Tetraborate (borax), potassium borate, ammonium borate etc., Sodium orthomolybdate, ammonium molybdate etc.
Because potassium, the nitrogen element is a macroelement, and sulphur is moderate-element, does not belong to trace element, under the condition of needs, also can be used as the effective element of product, reaches the purpose of complete first fertilizer, can economize on resources, reduce the content of sodium ion in the soil.Some place needs chlorion, can add in prescription.
In reaction, filter and obtain the solution of insolubles less than 0.1% (in dried weight).Reaction solution after the filtration obtains the particulate solid product by the spraying drying mode.
Positive progressive effect of the present invention is: the sequestrant that the present invention uses is EDTA or DTPA, for other acid such as humic acids, amino acid, the former has better chelating ability to the plain ion of gold, the stability constant of inner complex is bigger, the product of making has good preservation, stability in use, the fertility that effect is high.The present invention uses single stage method to make product, and the product that obtains can adjust (but can not exceed outside the sequestering power) in certain scope, obtains a series of product, to adapt to different areas, the specific demand of different plants.Be used for agricultural, forestry, flowers, gardening, soilless cultures etc. can be proofreaied and correct the untoward reaction that the plant nutritional deficiency causes.
Embodiment
The production technique of single stage method chelated microelement mixed fertilizer of the present invention further specifies in the specific embodiments below.
Embodiment 1
Have in the four-hole boiling flask of stirring, thermometer at 2000ml, add 1000ml water, add 2.22molEDTA (99% raw material 653.7g), under agitation add NaOH 3.05mol (32% raw material 381.2g), be warmed up to 70 ℃, add the iron 1.343mol (Fe of iron level 51% (OH) respectively
3Raw material 147.0g), copper 0.0472mol (the basic carbonate copper raw material 5.7g of copper content 53%), manganese 0.728mol (the manganous carbonate raw material 94.1g of manganese content 42.5%), zinc 0.0765mol (the crude zinc oxide materials 6.25g of zinc content 80%).Total mol amount of metallic element is 2.1947mol, and the mol ratio of EDTA and metallic element is 1.01: 1.00.Progressively be warmed up to 90-98 ℃, be incubated 30-60 minute, the reaction solution substantially transparent.Adjust PH at 5.0-7.0 with EDTA or alkali, be incubated ten minutes again.In this prescription, optionally add boric acid (99% time together) 28.57g, Sodium orthomolybdate (99% time together) 10.25g.Filter after drying, can obtain the yellow-green colour solid phase prod, the micro-ratio of product is: Fe 7.5%, and Cu 0.3%, and Mn 4.0%, and Zn 0.5%, and B 0.5%, and Mo 0.5%.Product before the said products stability is better than, the productive rate that obtains product counts 99.5% with golden prime element.
Can utilize suitable reactor, strainer, spray drying device to finish in the production.
Embodiment 2
Have in the four-hole boiling flask of stirring, thermometer at 2000ml, add 1000ml water, add 1.176molEDTA (99% raw material 346.8g, DTPA 0.723mol (98% raw material 253.8g) under agitation adds NaOH 3.798mol (32% raw material 474.7.0g), be warmed up to 70 ℃, add the iron 0.716mol (Fe of iron level 51% (OH) respectively
3Raw material 78.4g), copper 0.236mol (the basic carbonate copper raw material 28.3g of copper content 53%), manganese 0.546mol (the manganous carbonate raw material 70.6g of manganese content 42.5%), zinc 0.382mol (the crude zinc oxide materials 31.2g of zinc content 80%).Total mole amount of metallic element is 1.880mol, and total mol amount of EDTA and DTPA is 1.899mol, and the mol ratio of sequestrant and micro-metals and alkali is 1.01: 1.00: 2.015.Progressively be warmed up to 95-98 ℃, be incubated 30-60 minute, the reaction solution substantially transparent.Adjust PH at 5.0-7.0 with EDTA or alkali, be incubated ten minutes again.In this prescription, optionally add boric acid 57.1g, Sodium orthomolybdate 7.2g.Filter after drying, can obtain the grass green solid phase prod, the micro-ratio of product is: Fe 4.0%, and Cu 1.5%, and Mn 3.0%, and Zn 2.5%, and B 1.0%, and Mo 0.3%, and the productive rate that obtains product counts 99.6% with golden prime element.
。
Can utilize suitable reactor, strainer, spray drying device to finish in the production, product is graminaceous particle.
Embodiment 3
Have in the four-hole boiling flask of stirring, thermometer at 2000ml, add 1000ml water, add 1.93molEDTA (99% raw material 569.6g), under agitation add KOH 2.72mol (90% raw material 169.5g), MgO raw material 0.493mol (95% raw material 20.7g) is warmed up to 70 ℃, adds the iron 0.61mol (Fe of iron level 51% (OH) respectively
3Raw material 66.8g), copper 0.079mol (the basic carbonate copper raw material 9.5g of copper content 53%), manganese 0.582mol (the manganous carbonate raw material 85.18g of manganese content 42.5%), zinc 0.642mol (the crude zinc oxide materials 50.8g of zinc content 80%).Total mol amount of the metallic element except that K, Mg is 1.913mol, and the mol ratio of EDTA and metallic element is 1.01: 1.00.Progressively be warmed up to 95-98 ℃, be incubated 30-60 minute, the reaction solution substantially transparent.Adjust PH at 5.5-6.5 with EDTA or KOH dilute solution, be incubated ten minutes again.In this prescription, optionally add boric acid 57.2g, Sodium orthomolybdate 2.5g.Filter after drying, can obtain the yellow-green colour solid phase prod, the micro-ratio of product is: Fe 3.3%, Cu0.5%, and Mn 3.2%, and Zn 4.2%, and B 1.0%, and Mo 0.1%, also contains the Mg1.2% of inorganic states simultaneously, K10.5%.Because EDTA is very little to the chelating degree of magnesium, therefore can adopt inorganic magnesium, replace NaOH with KOH, can in product, increase potassium element fertilizer; Do not contain sodium in the product, be used for liquid level or fertigation, can not produce soil compaction, also be not prone to and burn the leaf phenomenon, the productive rate that obtains product counts 99.2% with golden prime element.
Can utilize suitable reactor, strainer, spray drying device to finish in the production.
Embodiment 4
Have in the four-hole boiling flask of stirring, thermometer at 2000ml, add 1000ml water, add 2.22molEDTA (99% raw material 655.3g), under agitation add NaOH 3.05mol (32% raw material 381.2g), be warmed up to 70 ℃, add iron 1.343mol (Fe of iron level 51% (OH) 3 raw material 147.0g) respectively, copper 0.0472mol (the cupric oxide raw material 3.74g of copper content 80%), manganese 0.728mol (the manganous carbonate raw material 94.1g of manganese content 42.5%), zinc 0.0765mol (the crude zinc oxide materials 6.25g of zinc content 80%).Total mol amount of metallic element is 2.1947mol, and the mol ratio of EDTA and metallic element is 1.01: 1.00.Progressively be warmed up to 115-125 ℃ (air-tight state), be incubated 20-40 minute, the reaction solution substantially transparent.Adjust PH 8.0 with EDTA or alkali, be incubated ten minutes again.In this prescription, optionally add boric acid 28.57g, Sodium orthomolybdate 10.25g.Filter after drying, can obtain the yellow-green colour solid phase prod, the micro-ratio of product is: Fe 7.5%, and Cu 0.3%, and Mn 4.0%, and Zn 0.5%, and B 0.5%, and Mo 0.4%, and the productive rate that obtains product counts 99.6% with EDTA.
Can utilize suitable reactor, strainer, spray drying device to finish in the production.
Embodiment 5
Have in the four-hole boiling flask of stirring, thermometer at 2000ml, add 1000ml water, add 2.22molDTPA (99% raw material 881.7g), under agitation add NaOH 4.05mol (32% raw material 506.2g), be warmed up to 70 ℃, add iron 1.343mol (Fe of iron level 51% (OH) 3 raw material 147.0g) respectively, copper 0.0472mol (the cupric oxide raw material 3.74g of copper content 80%), manganese 0.728mol (the manganous carbonate raw material 94.1g of manganese content 42.5%), zinc 0.0765mol (the crude zinc oxide materials 6.25g of zinc content 80%).Total mol amount of metallic element is 2.1947mol, and the mol ratio of EDTA and metallic element is 1.01: 1.00.Progressively be warmed up to 115-125 ℃ (air-tight state), be incubated 30-60 minute, the reaction solution substantially transparent.Adjust PH 6 with EDTA or alkali, be incubated ten minutes again.In this prescription, optionally add boric acid 28.57g, Sodium orthomolybdate 10.25g.Filter after drying, can obtain the yellow-green colour solid phase prod, the micro-ratio of product is: Fe 6.0%, and Cu 0.23%, and Mn 3.17%, and Zn 0.38%, and B 0.4%, and Mo 0.3%, and the productive rate that obtains product counts 99.7% with golden prime element.
Can utilize suitable reactor, strainer, spray drying device to finish in the production.
Above-mentioned concrete case study on implementation just to further elaboration of the present invention, is not limited to this three cases, can obtain a series of product in conjunction with the Technology reasonable change of actual demand and invention.
Claims (9)
1. the production technique of a microelement complex fertilizer, it is characterized in that in this technology: with sequestrant and metallic element compound, reaction is 20-60 minute under 50-125 ℃ temperature, needing to obtain the EDTA or the DTPA chelating element mixed fertilizer solution of ratio content, PH to product adjusts simultaneously, filter, drying obtains product.
2. production technique according to claim 1, it is characterized in that: described metallic element compound comprises metallic element oxide compound, metallic element carbonate, metallic element subcarbonate or metallic element oxyhydroxide, and described alkali comprises sodium hydroxide, potassium hydroxide or ammoniacal liquor.
3. production technique according to claim 2 is characterized in that: described metallic element comprises iron, copper, manganese, zinc, magnesium or calcium.
4. production technique according to claim 2 is characterized in that: the mol ratio of described EDTA and metallic element compound is 1-1.05: 1, and the mol ratio of described EDTA and alkali is 1-1.05: 1.0-2.1.
5. production technique according to claim 2 is characterized in that: the mol ratio of described DTPA and metallic element is 1-1.05: 1, and the mol ratio of DTPA and alkali is 1-1.05: 2.0-3.1.
6. production technique according to claim 2 is characterized in that: the mol ratio of described EDTA and DTPA mixture and metallic element compound is 1-1.05: 1, and the mol ratio of described EDTA and DTPA mixture and alkali is 1-1.05: 1.0-3.1.
7. according to the arbitrary described production technique of claim 1 to 7, it is characterized in that: in described mixed fertilizer solution, add boric acid/or other solubility borates or contain the soluble compound of molybdenum or the soluble compound of cobalt, obtain containing the more formulation product solution of multielement, through filtering, spraying drying obtains solid phase prod again.
8. production technique according to claim 8, it is characterized in that: described solubility borate comprises Sodium Tetraborate or potassium borate, the described soluble compound that contains molybdenum comprises ammonium molybdate or sodium aluminate, and the soluble compound of described cobalt comprises rose vitriol, Xiao Suangu or cobalt chloride.
9. production technique according to claim 8 is characterized in that: the PH of described reaction solution is controlled in the 6.0-8.0 scope.
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Cited By (8)
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| CN102219607A (en) * | 2011-05-09 | 2011-10-19 | 孙继民 | Fruit and vegetable nutrient regulator and use method thereof |
| CN102701850A (en) * | 2012-05-31 | 2012-10-03 | 上海永通化工有限公司 | Special fertilizer for preventing and controlling hami melon fruit cracking and preparation method of special fertilizer |
| CN103467159A (en) * | 2013-09-18 | 2013-12-25 | 张伟良 | Chelated compound trace element fertilizer and preparation method thereof |
| CN104086453A (en) * | 2014-06-11 | 2014-10-08 | 南通昊友食品添加剂有限公司 | Production method of nutrition enhancer ferric sodium ethylenediamine tetraacetate |
| CN105330419A (en) * | 2015-11-12 | 2016-02-17 | 成都九十度工业产品设计有限公司 | Intelligent preparation method of slow-release trace-element chelating agent |
| CN105330346A (en) * | 2015-11-12 | 2016-02-17 | 成都九十度工业产品设计有限公司 | Intelligent preparation system and method of slow-release trace element chelating agent |
| CN109651180A (en) * | 2019-01-22 | 2019-04-19 | 北京海德恒生科技发展有限公司 | A kind of production method of sodium iron ethylene diamine tetra acetate |
| CN115417721A (en) * | 2022-09-16 | 2022-12-02 | 南昌常茂新材料有限公司 | Preparation method of high-purity chelated rare earth fertilizer |
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| CN109651180A (en) * | 2019-01-22 | 2019-04-19 | 北京海德恒生科技发展有限公司 | A kind of production method of sodium iron ethylene diamine tetra acetate |
| CN115417721A (en) * | 2022-09-16 | 2022-12-02 | 南昌常茂新材料有限公司 | Preparation method of high-purity chelated rare earth fertilizer |
| CN115417721B (en) * | 2022-09-16 | 2024-04-19 | 南昌常茂新材料有限公司 | Preparation method of high-purity chelated rare earth fertilizer |
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Application publication date: 20110406 |