CN105085089A - Fertilizer synergist and preparation method thereof - Google Patents
Fertilizer synergist and preparation method thereof Download PDFInfo
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- CN105085089A CN105085089A CN201510610947.9A CN201510610947A CN105085089A CN 105085089 A CN105085089 A CN 105085089A CN 201510610947 A CN201510610947 A CN 201510610947A CN 105085089 A CN105085089 A CN 105085089A
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Abstract
The invention belongs to the technical field of chemical fertilizer, and particularly relates to a fertilizer synergist and a preparation method thereof. The fertilizer synergist aims at achieving the technical purposes of selecting a more reasonable hydrolysis technology which ensures the molecular weight of synergistic components and ensures the more durable potency of polyaspartic acid, and simplifying the production technology. According to the technical scheme, the preparation method of the fertilizer synergist comprises the steps that in the presence of water, potassium or sodium or ammonium carbonate or bicarbonate reacts with polysuccinimide to obtain a polyaspartic acid solution, then the polyaspartic acid solution reacts with zinc EDTA, and therefore the fertilizer synergist is obtained. The production technological conditions are mild, and preparation is easy. The obtained fertilizer synergist can be mixed with urea for granulation to obtain synergistic urea and can also be independently used as an aqueous solution to be directly mixed with various kinds of fertilizer for crops.
Description
Technical field
The invention belongs to technical field of fertilizer, be specifically related to a kind of fertilizer synergist and preparation method thereof.
Background technology
Chemical fertilizer occupies an important position in agriculture production, is also investment maximum in agriculture production, accounts for 50% of the whole property expenditure of agriculture production.China is a large agricultural country, and chemical fertilizer is the material guarantee of agricultural sustainable development, is the basis of increases in grain production.World agriculture development facts have proved, use chemical fertilizer be the soonest, the most effective, most important well stimulation.But traditional fertilizer utilization ratio is low, and the long-term poor efficiency of chemical fertilizer is used, and will cause elements in Soil enrichment, soil nutrient structural imbalance, soil physical property is deteriorated, and makes underground water, river, lake eutrophication, brings contaminate environment.
Poly-aspartic-acid effectively can improve utilization rate of fertilizer, slows down nutrient element loss.
Tianjin University of Technology delivers Ph D dissertation " the Synthesis and application research of poly aspartic acid " for 2005, carry out the applied research of poly aspartic acid in agricultural at home first, test with regard to using the impact of poly aspartic acid on corn, cucumber, strawberry, paddy rice respectively, conclusion shows on the basis of applying fertilizer, Ji Shi and impose poly aspartic acid and all have good promoter action to plant-growth.Capital Normal University within 2007, deliver Master's thesis " poly aspartic acid on blood urea nitrogen migrate in soil impact research ", literature research shows that poly-aspartic-acid has the effect of obvious slowly-releasing to urea, the nutrient ionic concn that the nitrogenous fertilizer that with the addition of poly-aspartic-acid discharges in unit time, unit distance is less than common nitrogenous fertilizer, but the amount of the nutrient that total amount discharges or transforms is greater than the corresponding amount of common nitrogenous fertilizer.Relevant field experiment also shows, just because of the feature of slowly-releasing, just embodies ageing and oligosaprobic feature when poly-aspartic-acid is applied to nitrogenous fertilizer.
This molecule be polymerized by amido linkage of poly-aspartic-acid has good biocompatibility, can is amino acid small molecules by microorganism, fungus degrading efficiently and stably, finally be degraded to water and the carbonic acid gas end product of environmental sound.The analytical results of the people such as Ross, Low of the U.S. and the Xiong Rongchun of China all shows, poly-aspartic-acid is the excellent green chemical of a kind of biodegradability.
From published Research Literature and patented technology, the poly-aspartic-acid preparation technology for fertilizer synergist industry has no further investigation, generally adopts sodium hydroxide, potassium hydroxide direct hydrolysis.
A cold glad use sodium hydroxide hydrolysis polysuccinimide of Nanjing University of Technology obtains polyaspartic acid solution, have studied the application of poly aspartic acid in agriculture production.
Patent 200810117094.5 makes polysuccinimide and excessive potassium hydroxide react in 75 DEG C ~ 90 DEG C temperature ranges, until polysuccinimide all dissolves, obtain the intermediate product containing excessive potassium ion, maintain temperature of reaction, organic polycarboxylic acid is added in this intermediate product, pH value to 7 ~ 8 of adjustment reaction system, filter and collect filtrate, making poly-aspartic-acid chelating potassium.
Patent 200910075297.7 discloses the preparation method of the special poly aspartic acid of a kind of agricultural, and its step for add catalyzer phosphoric acid in aspartic acid, and be polymerized to obtain polysuccinimide under normal pressure, alkaline hydrolysis obtains poly-aspartic-acid.In embodiment, alkaline hydrolysis reagent is potassium hydroxide.
Patent 201310094341.5 invention fertilizer additive, the aqueous solution being closed the salt such as zinc, ammonium borate, ethylenediamine tetraacetic acid (EDTA) manganese by the polyaspartic acid alkaline earth metal salt aqueous solution and ASPARTIC ACID huge legendary turtle carries out composite in proportion, concentrated, dry further, the product obtained.In embodiment, salt of poly aspartic acid preparation technology is as follows: add water and polysuccinimide in a kettle., add the solid sodium hydroxide hydrolysis that purity is greater than 99%, temperature is controlled between 70 ~ 90 DEG C in reaction process, until polysuccinimide all dissolves, adjustment solution pH value, about 7, can obtain the transparent red-brown sodium polyaspartate aqueous solution after filtration.
Oxyhydroxide is used to have following shortcoming as the hydrolysis material of poly-aspartic-acid: to find after deliberation, oxyhydroxide is as highly basic, poly-aspartic-acid can be caused under strongly alkaline conditions alkaline hydrolysis to occur, reduce the polymerization degree of poly-aspartic-acid potassium, make it be easier to be decomposed in soil, and then reduce the persistence of poly-aspartic-acid building capability; After using oxyhydroxide hydrolysis, polyaspartic acid solution becomes strong basicity, and PH must be regulated just to be applied to agriculture production to neutrality, complex operation; Oxyhydroxide itself as highly basic, also for production brings more risk.
In trace element, zinc is outstanding protein synthesis element.Zinc can promote protein metabolism, or the integral part of ribose and proteoplast, and is keep ribonucleoprotein structural integrity institute required.Zinc participates in the metabolism of growth hormone, and zinc can promote the synthesis of tryptophane, and tryptophane is the predecessor of growth hormone.When lacking zinc, farm crop tumor growth arrested development, blade diminishes.Situations such as blooming less, result is abnormal is often caused when farm crop lack zinc.Reasonable zinc is great on crop impact.
In the poly-aspartic-acid potassium zinc synergistic agent that can look into, generally adopt L-Aspartic acid zinc or L-Aspartic acid chelated zinc, this material practical structures is only carboxylate salt or the inner complex salt of zinc, has easy loss, easily and the negative ion such as carbonate, hydroxide radical, phosphate radical react the shortcoming generating insolubles.And the chelating ability of EDTA zinc is obviously more superior, its reason is the stability constant (lgK is generally between 4 ~ 10) of the complex compound that the stability constant (lgK is generally about 18.8) of the inner complex (EDTA-M) of EDTA and divalent-metal ion is formed much larger than the organism such as amino acid, little peptide and metal.
Summary of the invention
The technical problem to be solved in the present invention selects out more reasonably hydrolysis process, and this technique will ensure the molecular weight of synergistic component, ensures that poly-aspartic-acid effect is more lasting, and simplify production technique.
Technical scheme of the present invention is a kind of method preparing synergistic agent, comprises the steps:
A, add deionized water in a kettle., be heated to 40 ~ 90 DEG C, add the hydrolysis of polysuccinimide reaction 20 ~ 300min of molecular weight 2000 ~ 15000, obtain salt of poly aspartic acid solution, this solution is without the need to regulating pH, and its pH is namely between 7.5 ~ 8.5; Weak base salt and polysuccinimide mol ratio are 0.50 ~ 1.60 ︰ 0.80 ~ 1.20, and described weak base salt is carbonate or the supercarbonate of potassium or sodium or ammonium;
B, in salt of poly aspartic acid solution, add appropriate ethylenediamine tetraacetic acid (EDTA) zinc sodium (EDTA zinc), be stirred to dissolving, filter to obtain synergistic agent.
Concrete, in step a, the carbonate of potassium or sodium or ammonium and the mol ratio of polysuccinimide are 0.50 ~ 0.65 ︰ 0.80 ~ 1.20; Or the supercarbonate of potassium or sodium or ammonium and the mol ratio of polysuccinimide are 1.00 ~ 1.30 ︰ 0.80 ~ 1.20; Or when the carbonate of use potassium or sodium or ammonium mixes with supercarbonate and polysuccinimide reacts, the mol ratio of this weak base salt and polysuccinimide is 0.50 ~ 1.30 ︰ 0.80 ~ 1.20.
Concrete, the weak base salt used in step a is salt of wormwood.
Concrete, in step a, Heating temperature is 50 ~ 65 DEG C.
Preferably, in step a, the molecular weight of polysuccinimide is 3000 ~ 7000.
Preferably, in step a, hydrolysis time is 30 ~ 120min.
Concrete, in step b, to obtaining adding food grade colorant in synergistic agent.After making this handicraft product be applied to synergistic urea production, synergistic urea clearly can be distinguished with common urea.
Present invention also offers the synergistic agent prepared by described method.
Use synergistic agent prepared by above-mentioned technique, salt of poly aspartic acid accounts for total proportion 5% ~ 50%, EDTA zinc and accounts for total proportion 5 ~ 50%, and food grade colorant accounts for total proportion 0 ~ 10%.
Reaction equation of the present invention is as follows:
Beneficial effect of the present invention: manufacturing condition is gentle, uses weakly alkaline salt hydrolysis, and strict temperature control, protect peptide bond not by alkaline hydrolysis, and make production technique safer.Select rational zinc supplementation reagent, strengthen zinc supplementation ability.Production technique is simpler, by the choose reasonable of starting material and material proportion and adjustment, makes product discharge pH namely between 7.5 ~ 8.5, without the need to regulating pH.Use synergistic agent prepared by the inventive method, salt of poly aspartic acid accounts for total proportion 5% ~ 50%, EDTA zinc and accounts for total proportion 5 ~ 50%, and food grade colorant accounts for total proportion 0 ~ 10%.Synergistic agent of the present invention can obtain synergistic urea with urea mixing granulation; Also can use as aqua separately, directly used in combination in crop with all kinds of fertilizer.
Accompanying drawing explanation
Fig. 1, present invention process poly-aspartic-acid potassium GPC spectrogram; Adopt embodiment 9 technique to prepare poly-aspartic-acid potassium, and measure gained spectrogram in gel permeation chromatography (GPC) is upper.Obtained by embodiment 1 ~ 8, poly-aspartic-acid potassium is all close with this spectrogram, but by differences such as raw material, reaction times, temperature of reaction, molecular weight and molecular weight distribution may occur slight fluctuations.
Fig. 2, highly basic technique poly-aspartic-acid potassium GPC spectrogram; Adopt embodiment 10 technique to prepare poly-aspartic-acid potassium, and measure gained spectrogram in gel permeation chromatography (GPC) is upper.
Embodiment
Sylvite, sodium salt, zinc salt all use atomic absorption spectrophotometry analysis, and ammonium salt adopts indophenols colorimetrically analysing.Salt of poly aspartic acid weight-average molecular weight uses gel chromatography (GPC) analysis.
The preparation of embodiment 1 synergistic agent of the present invention
Water 243.57g is added in 500ml four-hole boiling flask, be heated to 45 DEG C, salt of wormwood 13.53g is added under agitation condition, salt of wormwood adds polysuccinimide 15.32g sustained reaction 300min after dissolving, and adds EDTA zinc 30.00g and stirs 30min, add food grade colorant 1.05g and be stirred to dissolving, filter to obtain 300g synergist solution, containing active sylvite 9.28%, active zinc salt 9.05%.
The preparation of embodiment 2 synergistic agent of the present invention
Water 123.83g is added in 500ml four-hole boiling flask, be heated to 90 DEG C, salt of wormwood 40.60g is added under agitation condition, salt of wormwood adds polysuccinimide 56.99g sustained reaction 25min after dissolving, and adds EDTA zinc 90.00g and stirs 30min, add food grade colorant 1.50g and be stirred to dissolving, filter to obtain 300g synergist solution, containing active sylvite 29.15%, active zinc salt 29.34%.
The preparation of embodiment 3 synergistic agent of the present invention
Water 204.12g is added in 500ml four-hole boiling flask, be heated to 65 DEG C, saleratus 34.31g is added under agitation condition, saleratus adds polysuccinimide 26.60g sustained reaction 75min after dissolving, and adds EDTA zinc 87.5g and stirs 45min, add food grade colorant 3.50g and be stirred to dissolving, filter to obtain 350g synergist solution, containing active sylvite 14.97%, active zinc salt 24.08%.
The preparation of embodiment 4 synergistic agent of the present invention
Water 168.32g is added in 500ml four-hole boiling flask, be heated to 75 DEG C, saleratus 45.75g is added under agitation condition, saleratus adds polysuccinimide 35.46g sustained reaction 45min after dissolving, and adds EDTA zinc 105.00g and stirs 20min, add food grade colorant 3.50g and be stirred to dissolving, filter to obtain 350g synergist solution, containing active sylvite 19.46%, active zinc salt 29.88%.
The preparation of embodiment 5 synergistic agent of the present invention
Water 342.21g is added in 1000ml four-hole boiling flask, be heated to 55 DEG C, sodium carbonate 139.19g is added under agitation condition, sodium carbonate adds polysuccinimide 254.76g sustained reaction 150min after dissolving, and adds EDTA zinc 120.00g and stirs 60min, add food grade colorant 1.6g and be stirred to dissolving, filter to obtain 800g synergist solution, containing active sodium salt 44.60%, active zinc salt 14.37%.
The preparation of embodiment 6 synergistic agent of the present invention
Water 341.49g is added in 1000ml four-hole boiling flask, be heated to 60 DEG C, sodium carbonate 46.40g is added under agitation condition, sodium carbonate adds polysuccinimide 65.32g sustained reaction 120min after dissolving, and adds EDTA zinc 360.00g and stirs 20min, add food grade colorant 10.40g and be stirred to dissolving, filter to obtain 800g synergist solution, containing active sodium salt 15.52%, active zinc salt 45.13%.
The preparation of embodiment 7 synergistic agent of the present invention
Water 202.97g is added in 500ml four-hole boiling flask, be heated to 75 DEG C, add volatile salt 23.27g under agitation condition, volatile salt adds polysuccinimide 32.27g after dissolving, sustained reaction 90min, add EDTA zinc 64.00g and stir 30min, add food grade colorant 4.80g and be stirred to dissolving, filter to obtain 300g synergist solution, containing active ammonium salt 19.20%, active zinc salt 20.07%.
The preparation of embodiment 8 synergistic agent of the present invention
Water 341.77g is added in 1000ml four-hole boiling flask, be heated to 80 DEG C, sodium bicarbonate 91.92g is added under agitation condition, sodium bicarbonate adds polysuccinimide 101.10g sustained reaction 100min after dissolving, and adds EDTA zinc 225.00g and stirs 75min, add food grade colorant 13.13g and be stirred to dissolving, filter to obtain 750g synergist solution, containing active sodium salt 20.25%, active zinc salt 30.46%.
The preparation of embodiment 9 main component poly-aspartic-acid of the present invention potassium
Add water 213.08g in 500ml four-hole boiling flask, be heated to 65 DEG C, salt of wormwood 47.37g (analytical pure is added under agitation condition, content 99%, is roughly equal to 0.34mol), after salt of wormwood dissolves, add polysuccinimide 51.15g, sustained reaction 75min, filters to obtain poly-aspartic-acid potassium solution, weight-average molecular weight 103730g/mol.Salt of poly aspartic acid weight-average molecular weight uses gel chromatography (GPC) analysis, the results are shown in Figure 1 and table 1.
Table 1 present invention process poly-aspartic-acid potassium molecular weight analyse data
The preparation simultaneous test of embodiment 10 main component poly-aspartic-acid of the present invention potassium
Add water 213.08g in 500ml four-hole boiling flask, be heated to 65 DEG C, potassium hydroxide 44.71g (analytical pure is added under agitation condition, content 85%, is roughly equal to 0.68mol), after potassium hydroxide dissolves, add polysuccinimide 51.15g, sustained reaction 75min, filters to obtain poly-aspartic-acid potassium solution, weight-average molecular weight 69948g/mol.Salt of poly aspartic acid weight-average molecular weight uses gel chromatography (GPC) analytical results to see Fig. 2 and table 2.
Table 2 highly basic technique poly-aspartic-acid potassium molecular weight analyse data
When each experiment condition is consistent, the weight-average molecular weight of the poly-aspartic-acid potassium of the present invention's synthesis is apparently higher than highly basic technique, poly-aspartic-acid potassium chelating ability in soil of high molecular is stronger, and is more not easily decomposed by the microorganisms, and then enhances the timeliness of synergistic agent.
The field test of embodiment 11 synergistic agent
One, asparagus lettuce field experiment
Trial crops asparagus lettuce, test site soil type drab soil, test period year February in November, 2013 to 2014.Have synergistic agent of the present invention, commercially available synergistic agent A for examination synergistic agent, all synergistic agent all with 4 ‰ ratios and urea mix mutually after synergistic urea, then to be manured into soil, and to establish CK group not use synergistic agent.Trial plot, tested district are 0.5 mu, and each group rate of fertilizer application is consistent (the results are shown in Table 3).
Table 3 asparagus lettuce field experiment result
| Sequence number | Synergistic agent | Crop | Per mu yield value, kg | Units increased in production | Stimulation ratio |
| 1 | CK (without synergistic agent) | Asparagus lettuce | 1428 | 0 | 0％ |
| 2 | Similar commercially available synergistic agent A | Asparagus lettuce | 1794 | 366 | 26％ |
| 3 | Synergistic agent of the present invention | Asparagus lettuce | 1889 | 461 | 32％ |
Two, rape field experiment
Trial crops rape, test site soil type drab soil, test period year May in November, 2013 to 2014.Synergistic agent of the present invention, similar commercially available synergistic agent A, commercially available synergistic agent B, commercially available synergistic agent C, commercially available synergistic agent D, commercially available synergistic agent E is had for examination synergistic agent, all synergistic agent are all with after 4 ‰ ratios and urea mutually mixed synergistic urea, be manured into soil again, and establish CK group not use synergistic agent.Trial plot, tested district are 0.2 mu, and each group rate of fertilizer application is consistent (see table 4).
Experimental result between table 4 Rapeseed Field
All can find out from the field test of asparagus lettuce and rape, the synergism of synergistic agent of the present invention is obvious, and synergism is better than commercially available multiple salt of poly aspartic acid synergistic agent.
Claims (8)
1. prepare a method for synergistic agent, it is characterized in that: comprise the steps:
A, add deionized water in a kettle., be heated to 40 ~ 90 DEG C, add the hydrolysis of polysuccinimide reaction 20 ~ 300min of molecular weight 2000 ~ 15000, obtain salt of poly aspartic acid solution, this solution is without the need to regulating pH, and its pH is namely between 7.5 ~ 8.5; Weak base salt and polysuccinimide mol ratio are 0.50 ~ 1.60 ︰ 0.80 ~ 1.20, and described weak base salt is carbonate or the supercarbonate of potassium or sodium or ammonium;
B, in salt of poly aspartic acid solution, add appropriate ethylenediamine tetraacetic acid (EDTA) zinc sodium, be stirred to dissolving, filter to obtain synergistic agent.
2. the method for claim 1, is characterized in that: in step a, and the carbonate of potassium or sodium or ammonium and the mol ratio of polysuccinimide are 0.50 ~ 0.65 ︰ 0.80 ~ 1.20; Or the supercarbonate of potassium or sodium or ammonium and the mol ratio of polysuccinimide are 1.00 ~ 1.30 ︰ 0.80 ~ 1.20; Or when the carbonate of use potassium or sodium or ammonium mixes with supercarbonate and polysuccinimide reacts, the mol ratio of this weak base salt and polysuccinimide is 0.50 ~ 1.30 ︰ 0.80 ~ 1.20.
3. method as claimed in claim 1 or 2, is characterized in that: the weak base salt used in step a is salt of wormwood.
4. the method as described in any one of claims 1 to 3, is characterized in that: in step a, Heating temperature is 50 ~ 65 DEG C.
5. the method as described in any one of Claims 1 to 4, is characterized in that: in step a, the molecular weight of polysuccinimide is 3000 ~ 7000.
6. the method as described in any one of Claims 1 to 5, is characterized in that: in step a, hydrolysis time is 30 ~ 120min.
7. the method as described in any one of claim 1 ~ 6, is characterized in that: in step b, to obtaining adding food grade colorant in synergistic agent.
8. the synergistic agent that described in any one of claim 1 ~ 7, method prepares.
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| CN108503469A (en) * | 2018-07-03 | 2018-09-07 | 重庆建峰工业集团有限公司 | A kind of organic chelated selenium fertilizer synergist and its preparation method and application |
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