CN107628961A - A kind of environmentally friendly iminodisuccinic acid chelated mineral salt - Google Patents
A kind of environmentally friendly iminodisuccinic acid chelated mineral salt Download PDFInfo
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- CN107628961A CN107628961A CN201710937874.3A CN201710937874A CN107628961A CN 107628961 A CN107628961 A CN 107628961A CN 201710937874 A CN201710937874 A CN 201710937874A CN 107628961 A CN107628961 A CN 107628961A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
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Abstract
The invention discloses a kind of environmentally friendly iminodisuccinic acid chelated mineral salt, especially a kind of metal-chelating salt, belong to the field of green fertilizer, product including raw material A, raw material B and raw material C reactions, raw material A is that alkaline hydrolysis can obtain any of compound of butene dioic acid root or several mixing, raw material B is that alkaline hydrolysis can obtain any of compound of aspartate or several mixing, and raw material C is that any of simple substance or compound of metal cation or several mixing can be generated with acid reaction.Simple production process of the present invention, one-step synthesis, without secondary compounding, active constituent content is high, without invalid components such as nitrate, sulfate, chloride, carbonate, belongs to environmentally friendly preparation technology, soil hardening can be effectively avoided, and reduces packaging, transport and use cost.
Description
Technical field
The present invention relates to chemical fertilizer, especially a kind of metal-chelating salt, belong to the field of green fertilizer, for crop or soil
Earth supplements metal trace element.
Background technology
Needed for growth and development of plants must element altogether there are about 16 kinds, wherein a great number of elements has carbon, hydrogen, oxygen, nitrogen, phosphorus, potassium,
Moderate-element has calcium, magnesium, sulphur, and also 7 kinds of trace elements are iron, zinc, manganese, copper, boron, molybdenum, chlorine.With the development of modern science,
The application of chemical fertilizer is made that tremendous contribution to agricultural volume increase, increases considerably the agricultural output of unit area, but applies fertilizer
Unbalanced some crises for also resulting in modern agriculture, serious harm is generated to environmental resource and human health.First,
The extensive application of nitrogen, phosphorus, potash fertilizer is to the very big facilitation that serves of plant growth, and while plant raised growth, also inhales
Receive metal trace element contained in soil, but metal trace element content is limited in soil, and often supplement not
In place, therefore metal trace element is difficult to fully meet plant growth needs, causes crop metabolism to be obstructed, agricultural product nutritional ingredient
It is unbalance, quality decline, taste variation etc..Secondly, nitrogen containing a great number of elements, phosphorus, the fertilizer of potassium can make the micro member of metal in soil
Element generation precipitation, so as to be inactivated by fixed, it is difficult to be absorbed and used by plants, but also soil hardening, crumb structure can be caused to break
The environmental pollutions such as bad, microorganism reduction.Therefore, metal trace element fertilizer application improves metal trace element in soil in other words
Activity has become industry common recognition.
Because plant is difficult to absorb with minor metallic element existing for inorganic salt form, and directly apply metal without
Machine salt can cause soil pollution, therefore generally require and metal trace element is protected with organic complexing agent, be formed relatively steady
Fixed water-soluble state, the compatibility between fertilizer is just can guarantee that, improve absorption rate of the plant to metal trace element.Traditional network
Mixture is edetate (English abbreviation EDTA).Although edetate has good complexation of metal ions
Ability, but itself can not be absorbed by crops utilization, can not be degraded by microorganisms, therefore the problem of pollution environment be present.
Iminobisuccinate (English abbreviation IDS), its anion can form coordination geometry knot with metal cation
Structure, the ability of complexation of metal ions is suitable with EDTA, and can be absorbed by crops completely, the utilization ratio of metal trace element
It is higher, there is the characteristic of without phosphorus, Nonpoisonous, non-environmental-pollution and easily biological-degradable, be a kind of environmental type complexing agent.Patent document
Chelating plant micronutrient formula is disclosed in CN200310102834.5：With iminodisuccinic acid sodium salt, sylvite or it
Mixture, compound with organic or inorganic zinc, manganese, iron, copper etc. trace element compound obtain product.Due to being to use imido
The sodium salt or sylvite of base disuccinic acid and metal salt occur metathesis reaction and are made, its compound production process can produce invalid salt into
Divide (inorganic or organic anion sodium salt or potassium salt form), such as sodium nitrate, potassium nitrate, these salt contents reach 30%-
50%, this production method not only increases production procedure, causes production cost to increase, and these extra salt branches cause
Product effective content reduces.Can be to unnecessary salinity be increased in soil, as sulfate radical is easily made using this metal-chelating salt
Into soil hardening, plant growth is influenceed；Chlorion has corrosiveness to equipment, and is not suitable for fear-chlorion crop；Nitrate anion has by force
Oxidation, increase the danger of accumulating；In addition, these invalid salt branches cause the content of product active ingredient to reduce, make bag
Dress, transport, the cost raising about 15% using process.
The content of the invention
The technical problem to be solved in the invention is to provide a kind of environmentally friendly iminodisuccinic acid chelated mineral salt,
Simple production process, one-step synthesis, without secondary compounding, active constituent content is high, without nitrate, sulfate, chloride, carbon
The invalid components such as hydrochlorate, belong to environmentally friendly preparation technology, effectively prevent soil hardening, and reduce packaging, transport and
Use cost.
In order to solve the above technical problems, the technical solution adopted in the present invention is：
A kind of environmentally friendly iminodisuccinic acid chelated mineral salt, including raw material A, raw material B and raw material C reactions
Product, raw material A are that alkaline hydrolysis can obtain any of compound of butene dioic acid root or several mixing, and raw material B is that alkaline hydrolysis can
Any of compound of aspartate or several mixing are obtained, raw material C is that can generate metal cation with acid reaction
Simple substance or any of compound or several mixing.
Technical solution of the present invention further improvement is that：Raw material A is maleic acid, maleic anhydride, maleic
Diacid salt, maleic acid derivative, fumaric acid, fumarate, fumaric acid derivative, fumaric acid acid anhydride
Any of or several mixing.
Technical solution of the present invention further improvement is that：Raw material B is L-Aspartic acid, L-Aspartic acid salt, L- asparagus ferns
Threonine derivative, D-Asp, D-Asp salt, D-Asp derivative, D, L- mix-configurations aspartic acid, D, L-
Any of mix-configuration aspartate, D, L- mix-configuration aspartames or several mixing.
Technical solution of the present invention further improvement is that：Raw material C is simple substance, oxide, hydroxide, the carbonic acid of metal
Salt, subcarbonate it is any, in raw material C contained metallic element be copper, iron, aluminium, zinc, calcium, magnesium, manganese, cobalt, chromium, nickel, tin,
Any of vanadium or molybdenum.
Technical solution of the present invention further improvement is that：A kind of environmentally friendly iminodisuccinic acid chelated mineral salt
Preparation method it is as follows：Raw material A, raw material B are added in solvent, raw material C is slow added into and stirs, heat until completely dissolved
To 80~110 DEG C, heating reflux reaction 25~40 hours under normal pressure, reaction is down to room temperature after terminating, and imino-diacetic amber is made
Sour chelated mineral salt.
Technical solution of the present invention further improvement is that：The solvent is water.
Technical solution of the present invention further improvement is that：The solvent is the mixing of water and auxiliary agent.
Technical solution of the present invention further improvement is that：The dosage of raw material A is 0.8~1.2 molar part, raw material B use
Measure as 0.8~1.2 molar part, raw material C dosage is 1~2 molar part, and the dosage of water is 20~25 molar parts.
Technical solution of the present invention further improvement is that：The auxiliary agent is ammoniacal liquor, poly yamanashi esters, Polyoxyethylene fatty
Any of esters of gallic acid, salicylic acid, cresols, aliphatic acid or several mixing.
Technical solution of the present invention further improvement is that：The mass fraction of the addition of the auxiliary agent in a solvent is
0.5~1.5%.
By adopting the above-described technical solution, the technological progress that the present invention obtains is：
A kind of environmentally friendly iminodisuccinic acid chelated mineral salt provided by the invention, simple production process, a step
Synthesis, without secondary compounding, active constituent content is high, without the invalid components such as nitrate, sulfate, chloride, carbonate, category
In environmentally friendly preparation technology, soil hardening is effectively prevent, and reduces packaging, transport and use cost.
The present invention uses one-step synthesis, has been complexed metal ion while iminobisuccinate is synthesized, has been not required to
Secondary compounding processing is wanted, reduces production procedure, production cost is reduced, production process non-pollutant discharge, is a kind of green
The production technology of environmental protection.
The preparation method of the present invention, which uses, adds acid anhydrides, amino acid in solvent, is slow added into simple substance or the change of metal
Compound, and stir, 80~110 DEG C are heated to until completely dissolved, heating reflux reaction 25~40 hours under normal pressure, reaction knot
Room temperature single step reaction is down to after beam and directly synthesizes iminodisuccinic acid chelated mineral salt, raw material availability is greatly improved, overcome
Metathesis reaction is carried out with metal salt prepare iminodisuccinic acid chelated mineral with iminodisuccinic acid sylvite or sodium salt
The problem of salt is present, invalid salt component is free of in product, impurity content is low, and iminodisuccinic acid root and metal cation have
It is high to imitate content, iminodisuccinic acid content reaches 70~80%, and metal cation content reaches 15%~20%.
The present invention uses iminobisuccinate complexation of metal ions, and overcoming traditional complexing agent EDTA can not be by crop
Absorb, can not be degraded by microorganisms caused by pollute environment the problems such as.Iminodisuccinic acid chelating salt is the same as EDTA chelas
Close salt to compare, micronutrient levels is suitable, but the metal ion utilization rate that iminobisuccinate chelating carries is high, in soil
In can be completely released absorption, anion iminodisuccinic acid root is degraded to butanedioic acid in plant can be metabolized suction
Receive, participate in the circulation of plant intracellular metabolite, promote plant growth, environmental pollution will not be caused.
The present invention is free of other additional invalid anion, such as has the nitrate anion of strong oxidizing property and carcinogenicity, improves
The security of product, the risk exploded is avoided, reduce the condition requirement to storage transport, reduce the danger to health
Evil.
The present invention not containing sulfate radicals and carbanion, overcome sulfate radical and carbonate in soil easily with calcium, iron,
Copper plasma etc. combines the problem of causing soil hardening, it also avoid combining to form precipitation with manganese ion and caused by hinder metal
The problem of absorption of trace elements, and solve during sprinkling irrigation sulfate radical and carbonate easily with the calcium ions and magnesium ions shape in water
The problems such as obstruction or fouling easily occurs caused by into precipitation at nozzle.
Any corrosive elements are free of in the product of the present invention, such as chlorion, phosphate anion, therefore can effectively be avoided
Chlorion damages to corrosivity caused by the container of stainless steel and other metal materials, to container during processing, transport and use
The range of choice of material is wider, more convenient during use., can and the administration scope of metal-chelating salt is also expanded
Enough it is applied to fear-chlorion crop, such as tobacco, sweet potato, potato.
The present invention adds the auxiliary agents such as ammoniacal liquor in preparation process, raw material can be made preferably to dissolve during the course of the reaction, promotees
Enter the progress of reaction, substantially increase the conversion ratio of raw material, feed stock conversion can reach more than 75%.
Embodiment
Here is certain specific embodiments of the invention, to be described in further detail.
A kind of environmentally friendly iminodisuccinic acid chelated mineral salt of the present invention, including raw material A, raw material B and raw material
The product of C reactions, raw material A is that alkaline hydrolysis can obtain any of compound of butene dioic acid root or several mix products, excellent
Select maleic acid, maleic anhydride, maleate, maleic acid derivative, fumaric acid, fumaric acid
Any of salt, fumaric acid derivative, fumaric acid acid anhydride or several mixing.The raw material B can obtain for alkaline hydrolysis
Any of compound of aspartate or several mixing, preferably L-Aspartic acid, L-Aspartic acid salt, L- asparagus fern ammonia
Acid derivative, D- aspartic acids, D-Asp salt, D-Asp derivative, D, L- mix-configurations aspartic acid, D, L-
Any of mix-configuration aspartate, D, L- mix-configuration aspartames or several mixing.Raw material C is gold
The simple substance of category, oxide, hydroxide, carbonate, subcarbonate it is any, in raw material C contained metallic element be copper,
Any of iron, aluminium, zinc, calcium, magnesium, manganese, cobalt, chromium, nickel, tin, vanadium or molybdenum.
The preparation method of metal-chelating salt comprises the following steps：
The raw material B of the raw material A of 0.8~1.2 molar part, 0.8~1.2 molar part is added in 20~25 molar part solvents,
It is slow added into the raw material C of 1~2 molar part and stirs, is heated to 80~110 DEG C until completely dissolved, is heated to reflux under normal pressure
Reaction 25~40 hours, reaction are down to room temperature after terminating, and iminodisuccinic acid chelated mineral salt is made.
The dissolution solvent is water, and auxiliary agent can be added when raw material is added into solvent, and the auxiliary agent species is ammoniacal liquor, gathered
Any of sorb esters, polyoxyethylene fatty acid ester class, salicylic acid, cresols, aliphatic acid or several mixing, promote raw material
Dissolving in a solvent, the mass fraction of the addition of the auxiliary agent in a solvent are 0.5~1.5%.
Embodiment 1
A kind of environmentally friendly iminodisuccinic acid chelated mineral salt, including raw material A, raw material B and raw material C reactions
Product, raw material A are maleic acid, and raw material B is L-Aspartic acid, and raw material C is Kocide SD.
The preparation method of metal-chelating salt comprises the following steps：
The raw material B of the raw material A of 0.8 molar part, 0.8 molar part is added in the water of 20 molar parts, adds ammonia spirit,
The addition of ammoniacal liquor is the 0.5% of the mass fraction of water, is slow added into Kocide SD and the stirring of 1 molar part, treats that raw material is complete
80 DEG C are heated to after fully dissolved, heating reflux reaction 25 hours under normal pressure, reaction is down to room temperature after terminating, and imino-diacetic amber is made
Amber acid chelated mineral salt.
Iminodisuccinic acid content is 70% in iminodisuccinic acid chelated mineral salt, content of copper ion 15%.
Embodiment 2~6 has a constituent with the identical category of above-described embodiment 1, selected in some generic compositions
Different compounds, and each composition different proportion of composing as shown in Table 1 below, embodiment 2~6 and above-described embodiment 1
Used preparation method step is identical, and different technological parameters is as shown in preparation method part in table 1 below.
Wherein, in feedstock portions, " raw material A " represents the constituent and ratio of raw material A, " NA" represent mole of raw material A
Part.
Table 1
In order to preferably verify superiority of the present invention on fertilization effect, inventor uses the embodiment of the present invention 1,2,3
In prepared metal-chelating salt carried out Product checking, and use the existing several metal-chelating product salts conducts pair of in the market
Same Product checking is carried out according to group, wherein control group 1 is Cu-IDHA, and control group 2 is Fe-IDHA, and control group 3 is Mn-
IDHA, produced by ADOB companies, above control set product applies equally to field experiment.Every group takes identical weight
The sample of (1kg) carries out composition detection and analysis, and specific testing result is as shown in Table 2 below.Wherein " metal " represents metal chelating
The weight/mass percentage composition sum (not including potassium, sodium) of minor metallic element contained in salt is closed, " invalid salt " represents metal-chelating
The weight/mass percentage composition sum (such as sulfate radical, nitrate anion, chlorion, phosphate radical) of contained invalid anion in salt, " potassium,
Sodium " represents the weight/mass percentage composition sum of potassium ion, sodium ion.
Table 2
| Metal (%) | Invalid salt (%) | Potassium, sodium (%) | |
| Example 1 | 15(Cu) | 0 | 0 |
| Example 2 | 12(Mn:Fe=1:2) | 0 | 0 |
| Example 3 | 13(Al:Zn:Ca:Co=1:2:1:2) | 0 | 0 |
| Average value 1 | 13.3 | 0 | 0 |
| Control 1 | 10 | 12 | 8 |
| Control 2 | 9 | 13 | 8.5 |
| Control 3 | 9 | 13 | 8 |
| Average value 2 | 9.3 | 12.6 | 8.2 |
Trace meter in iminodisuccinic acid chelated mineral salt can be seen that in embodiment 1~3 according to result in table 2
Constituent content is up to 12~15%, without invalid salt and potassium, sodium, and Trace Metals Contents in the chelated mineral salt in control group
Only 9~10%, invalid salt content is up to 12~13%, and potassium, sodium content are 12~13%.
Field experiment
Inventor further uses metal-chelating salt prepared in the embodiment of the present invention 1~6 to carry out field experiment, and
Same test process and sampling detection and analysis are carried out using the control set product in above-mentioned table 2, yield is Shijiazhuang City
The yield of Luquan area Tong Ye towns Nan Guyi villages winter wheat, the soil weight are the important indicators for characterizing soil compaction rate, are derived from earth's surface
Following 20cm clay soil.Testing result is as shown in Table 3 below.
Table 3
| The soil weight (g/cm3) | Yield (kg/ mus) | |
| Example 1 | 1.15 | 490 |
| Example 2 | 1.21 | 476 |
| Example 3 | 1.13 | 488 |
| Example 4 | 1.16 | 492 |
| Example 5 | 1.12 | 479 |
| Example 6 | 1.18 | 483 |
| Average value 1 | 1.16 | 484.7 |
| Control 1 | 1.21 | 449 |
| Control 2 | 1.24 | 452 |
| Control 3 | 1.28 | 438 |
| Average value 2 | 1.24 | 446.3 |
Soil weight average out to 1.16g/cm in embodiment 1~6 can be seen that according to result in table 33, and control group is put down
Average reaches 1.24g/cm3, yield average out to 484.7kg/ mus in embodiment 1~6, higher than the average 446.3kg/ mus of control group.
The above results show that the iminodisuccinic acid chelated mineral salt tenor that the present invention is prepared is higher, has
Beneficial to crop or soil supplement metal trace element, without invalid salt component, soil hardening is efficiently avoid, uses the imido
Base disuccinic acid chelated mineral salt can reduce the soil weight, improve crop yield.
Claims (10)
- A kind of 1. environmentally friendly iminodisuccinic acid chelated mineral salt, it is characterised in that：Including raw material A, raw material B and raw material The product of C reactions, raw material A are that alkaline hydrolysis can obtain any of compound of butene dioic acid root or several mixing, and raw material B is Alkaline hydrolysis can obtain any of compound of aspartate or several mixing, and raw material C is that can generate metal with acid reaction Any of the simple substance of cation or compound or several mixing.
- A kind of 2. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 1, it is characterised in that：It is former Material A is maleic acid, maleic anhydride, maleate, maleic acid derivative, fumaric acid, anti-butylene Any of diacid salt, fumaric acid derivative, fumaric acid acid anhydride or several mixing.
- A kind of 3. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 1, it is characterised in that：It is former Material B is L-Aspartic acid, L-Aspartic acid salt, L-Aspartic acid derivative, D-Asp, D-Asp salt, D- asparagus ferns Threonine derivative, D, L- mix-configurations aspartic acid, D, L- mix-configurations aspartate, D, L- mix-configuration aspartic acids spread out Any of biology or several mixing.
- A kind of 4. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 1, it is characterised in that：It is former Expect simple substance, oxide, hydroxide, carbonate, any, the contained metallic element in raw material C of subcarbonate that C is metal For any of copper, iron, aluminium, zinc, calcium, magnesium, manganese, cobalt, chromium, nickel, tin, vanadium or molybdenum.
- 5. a kind of environmentally friendly iminodisuccinic acid chelated mineral salt according to any one of Claims 1 to 4, it is special Sign is that preparation method is as follows：Raw material A, raw material B are added in solvent, raw material C is slow added into and stirs, until completely dissolved 80~110 DEG C are heated to, heating reflux reaction 25~40 hours under normal pressure, reaction is down to room temperature after terminating, and imino-diacetic is made Butanedioic acid chelated mineral salt.
- A kind of 6. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 5, it is characterised in that：Institute It is water to state solvent.
- A kind of 7. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 5, it is characterised in that：Institute State mixing of the solvent for water and auxiliary agent.
- 8. a kind of environmentally friendly iminodisuccinic acid chelated mineral salt according to any one of claim 5~7, it is special Sign is：The dosage of raw material A is 0.8~1.2 molar part, and raw material B dosage is 0.8~1.2 molar part, and raw material C dosage is 1 ~2 molar parts, the dosage of water is 20~25 molar parts.
- A kind of 9. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 7, it is characterised in that：Institute Auxiliary agent is stated as any of ammoniacal liquor, poly yamanashi esters, polyoxyethylene fatty acid ester class, salicylic acid, cresols, aliphatic acid or several Mixing.
- A kind of 10. environmentally friendly iminodisuccinic acid chelated mineral salt according to claim 7, it is characterised in that： The mass fraction of the addition of the auxiliary agent in a solvent is 0.5~1.5%.
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| CN115583893A (en) * | 2022-09-23 | 2023-01-10 | 济宁无内新材料技术研发中心(有限合伙) | Preparation method of IDS divalent metal chelate salt |
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| CN115583893A (en) * | 2022-09-23 | 2023-01-10 | 济宁无内新材料技术研发中心(有限合伙) | Preparation method of IDS divalent metal chelate salt |
| CN115583893B (en) * | 2022-09-23 | 2023-12-22 | 济宁无内新材料技术研发中心(有限合伙) | Preparation method of IDS divalent metal chelate salt |
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Application publication date: 20180126 |