CN104892396A - Preparation method of ammonia zinc citrate - Google Patents
Preparation method of ammonia zinc citrate Download PDFInfo
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- CN104892396A CN104892396A CN201510251951.0A CN201510251951A CN104892396A CN 104892396 A CN104892396 A CN 104892396A CN 201510251951 A CN201510251951 A CN 201510251951A CN 104892396 A CN104892396 A CN 104892396A
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- zinc citrate
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- ammonia
- citric acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a preparation method of ammonia zinc citrate. The ammonia zinc citrate is prepared from the raw materials: 100 parts of water, 17-18 parts of citric acid, 10-11 parts of a zinc oxide powder, and 35-40 parts of ammonia water. The preparation method comprises the steps: putting water and zinc oxide in a stirring device, dispersing evenly, adding citric acid, and continuing to stir until the solution becomes transparent; introducing 3/4 of the weight parts of ammonia water into the transparent solution, heating to be boiled, after concentration, naturally cooling, and then continuing to slowly add the rest ammonia water, to obtain a transparent solution; and then putting the transparent solution into a drying oven, drying moisture, cooling and crushing the obtained solid, and thus obtaining the finished ammonia zinc citrate product. The preparation method has the advantages that the secondary chelating technology is adopted for preparing the ammonia zinc citrate product with moderate chelating intensity, and when the product is used as a trace element regulator in plants, the product has the advantages of green environmental protection, no residue, good compatibility, good nutrient absorption, low raw material cost and the like, and complies with a new development direction of agriculture.
Description
Technical field
The present invention relates to a kind of preparation method that can be used as the zinc citrate ammonia that micro elements by plants conditioning agent uses.
Background technology
In present agriculture production, in order to pursue grain high yield, stable yields, long-term heavy dressing chemical fertilizer, light organic fertilizer; Diazonium phosphate fertilizer, light potash fertilizer; Great element is fertile, slightly fertile.Use the lower nitrogenous fertilizer of utilization ratio and phosphate fertilizer in a large number, like this, not only increased agricultural cost, waste resource, contaminate environment, also can cause soil compaction, topsoil eutrophication, cause the series of problems such as soil secondary salinization, Nitrate Accumulation and soil acidification.Soil acidification degree is higher, and the more, cause the shortage of topsoil calcium, magnesium, potassium and trace element, plant nutrient is seriously uneven, forms vicious cycle for the calcium in soil, magnesium, potassium, ammonium and trace element loss; Cause soil seriously to harden simultaneously.Problem at present about soil compaction has caused national attention.Lack supplementing of medium trace element due to excessive using of macroelement, cause a lot of soil " more and more barrenr, more and more bleak and desolate; more and more to harden ", increase using of medium trace element, alleviate soil compaction situation simultaneously, become the main development direction of modern agriculture.Have expert to point out, existing soil does not execute the macroelement such as nitrogen phosphorus in 10 years, and reasonable supplement regulates medium trace element, can not the element such as nitrogen stress phosphorus in soil yet, the crop not underproduction, can adjustment soil compaction problem progressively yet.
Supplementing still based on inorganic salt of the current medium trace element to soil, EDTA Chelating state instead of part inorganic salt market with stronger chelating ability, and sugar alcohol chelating, chelating amino acids product have also been got by some producers simultaneously, and Chelating state has formed a kind of trend.But, the fertilizer efficiency limited duration of inorganic salt, and the chelating intensity of EDTA chelating salt is comparatively large, is in use difficult to release.
Summary of the invention
The object of the present invention is to provide a kind of preparation method that can be used as the zinc citrate ammonia that micro elements by plants conditioning agent uses.
For achieving the above object, the present invention can take following technical proposals:
The preparation method of zinc citrate ammonia of the present invention, it is prepared from by following weight and method by raw water, citric acid, Zinc oxide powder and ammoniacal liquor:
Proportioning:
100 parts, water, citric acid 17 ~ 18 parts, Zinc oxide powder 10 ~ 11 parts, ammoniacal liquor 35 ~ 40 parts;
Preparation method:
The first step, is placed in whipping device by water and Zinc oxide powder and is uniformly dispersed;
Second step, adds citric acid, continues to be stirred to liquation and become transparent in the burnett's solution that the first step is obtained;
3rd step, is slowly passed in second step gained clear solution by the ammoniacal liquor of 3/4 weight part;
4th step, by the 3rd step gained solution ebuillition of heated, when being concentrated into 1/2 of original volume, naturally cooling, then continues slowly to add by remaining ammoniacal liquor, obtains clear solution;
5th step, is placed in baking oven by the 4th step clear solution and dries moisture, and namely gained solid cooled obtains zinc citrate ammonia finished product after pulverizing.
Described citric acid is Citric acid monohydrate Food grade.
The zinc citrate ammonia that the present invention obtains is as microelement regulator, and can supplement plant medium trace element, its using method is as follows:
1, use in soil: it can be used as base manure, seed manure or topdress and use.For saving fertilizer, improving fertilizer efficiency, usually adopting row replacement or method of spreading manuer in holes.Because soil application trace element fertilizer has certain aftereffect, can next year use.The amount of application of citric acid cuprammonium in soil is generally every mu of 5 ~ 10kg.
2, use on plant materials:
A, dress seed with a small amount of water will zinc citrate ammonia dissolve after be sprayed on seed, spray limit, limit stir, make seed-coat be stained with one deck solution, after drying in the shade sow.Seed dressing consumption is generally per kilogram seed consumption 1 ~ 6g, with water 40 ~ 60ml.
B, soaking seed zinc citrate ammonia to dissolve obtains the solution of concentration 0.01 ~ 0.1%, and immersed by seed, seed soaking time is 12 ~ 24h.
C, dip in root crop is transplanted to paddy rice and other, the zinc citrate ammonia solution of working concentration 0.1 ~ 1.0% can dip in root and use.
The tow sides of zinc citrate ammonia solution to plant leaf of d, root outer spraying concentration 0.02 ~ 0.1% spray, and are advisable so that blade surface is moistening.
The invention has the advantages that when it can be used as plant medium trace element conditioning agent to use, there is environmental protection, noresidue, compatibility is good, nutrition absorption is good, the advantages such as raw materials cost is low, can be widely used in Water soluble fertilizer, foliage fertilizer, plant-growth regulator, soil conditioner, comply with the agricultural development new direction of " green, organic, ecological ".
The complexing salt that the structure that zinc citrate ammonia is made up of zinc, ammonia and citric acid is not clear, its complexing provides lone-pair electron to carry out complexing with the metal ion with unoccupied orbital by the nitrogen-atoms in ammonia, in product preparation process, adopt secondary chelating technology: the 3rd step and the 4th step add ammoniacal liquor twice, secondary chelating is carried out under specific reaction conditions, the chelating salt of obtained medium tenacity, its complexation strength is less than EDTA chelating salt, when supplementing as plant medium trace element, the trace element in plant or soil can not only be supplemented, and can continue to act on.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
embodiment 1
First Zinc oxide powder 410g is accurately taken, Citric acid monohydrate Food grade 700g, ammoniacal liquor 1500ml, water 4000ml;
Preparation method is:
The first step, add water in reactor 4000 ml, adds 410g Zinc oxide powder, stirring and dissolving, be uniformly dispersed in water;
Second step, adds Citric acid monohydrate Food grade 700g, continues to be stirred to liquation and become transparent in the burnett's solution that the first step is obtained;
3rd step, opens stirring, slowly adds ammoniacal liquor 1125 ml in clear solution, continues to stir 0.5h after adding ammoniacal liquor again;
4th step, by the 3rd step gained solution ebuillition of heated, after being concentrated into 1/2 of original volume, stops heating, is continued slowly to add by remaining 375ml ammoniacal liquor, stir 0.5h after naturally cooling to room temperature;
5th step, the solution of the 4th step is placed in 120 ~ 130 DEG C, baking oven and dries moisture, namely gained solid cooled obtains zinc citrate ammonia finished product after pulverizing.
embodiment 2
First Zinc oxide powder 400g is accurately taken, Citric acid monohydrate Food grade 680g, ammoniacal liquor 1400ml, water 4000ml;
Preparation method is:
The first step, add water in reactor 4000 ml, adds 400g Zinc oxide powder, stirring and dissolving, be uniformly dispersed in water;
Second step, adds Citric acid monohydrate Food grade 680g, continues to be stirred to liquation and become transparent in the burnett's solution that the first step is obtained;
3rd step, opens stirring, slowly adds ammoniacal liquor 1050 ml in clear solution, continues to stir 0.5h after adding ammoniacal liquor again;
4th step, by the 3rd step gained solution ebuillition of heated, after being concentrated into 1/2 of original volume, stops heating, is continued slowly to add by remaining 350ml ammoniacal liquor, stir 0.5h after naturally cooling to room temperature;
5th step, the solution of the 4th step is placed in 120 ~ 130 DEG C, baking oven and dries moisture, namely gained solid cooled obtains zinc citrate ammonia finished product after pulverizing.
embodiment 3
First Zinc oxide powder 440g is accurately taken, Citric acid monohydrate Food grade 720g, ammoniacal liquor 1400ml, water 4000ml;
Preparation method is:
The first step, add water in reactor 4000 ml, adds 440g Zinc oxide powder, stirring and dissolving, be uniformly dispersed in water;
Second step, adds Citric acid monohydrate Food grade 720g, continues to be stirred to liquation and become transparent in the burnett's solution that the first step is obtained;
3rd step, opens stirring, slowly adds ammoniacal liquor 1200 ml in clear solution, continues to stir 0.5h after adding ammoniacal liquor again;
4th step, by the 3rd step gained solution ebuillition of heated, after being concentrated into 1/2 of original volume, stops heating, is continued slowly to add by remaining 400ml ammoniacal liquor, stir 0.5h after naturally cooling to room temperature;
5th step, the solution of the 4th step is placed in 120 ~ 130 DEG C, baking oven and dries moisture, namely gained solid cooled obtains zinc citrate ammonia finished product after pulverizing.
The zinc citrate ammonia end properties data sheet that table 1 is prepared for above-described embodiment 1-3:
Table 1
As can be seen from above-mentioned detected result: zinc citrate ammonia metal content and the nitrogen content index of preparation are stablized, necessary trace element zinc can be provided for plant when using as micro-fertilizer, macroelement can also be supplemented as nitrogenous fertilizer.
Get 200ml distilled water, add zinc citrate ammonia prepared by 2g embodiment 1, after stirring and dissolving, add 2g water soluble fertilizer, stirring and dissolving, observe phenomena is in table 2.
Table 2
Data as can be seen from table 2: when the zinc citrate ammonia prepared by the present invention is mixed with other water-soluble fertilizer, there is good compatibility.
Claims (3)
1. a preparation method for zinc citrate ammonia, is characterized in that: it is prepared from by following weight and method by raw water, citric acid, Zinc oxide powder and ammoniacal liquor:
Proportioning:
100 parts, water, citric acid 17 ~ 18 parts, Zinc oxide powder 10 ~ 11 parts, ammoniacal liquor 35 ~ 40 parts;
Preparation method:
The first step, is placed in whipping device by water and Zinc oxide powder and is uniformly dispersed;
Second step, adds citric acid, continues to be stirred to liquation and become transparent in the burnett's solution that the first step is obtained;
3rd step, is slowly passed in second step gained clear solution by the ammoniacal liquor of 3/4 weight part;
4th step, by the 3rd step gained solution ebuillition of heated, when being concentrated into 1/2 of original volume, naturally cooling, then continues slowly to add by remaining ammoniacal liquor, obtains clear solution;
5th step, is placed in baking oven by the 4th step clear solution and dries moisture, and namely gained solid cooled obtains zinc citrate ammonia finished product after pulverizing.
2. the preparation method of zinc citrate ammonia according to claim 1, is characterized in that: described citric acid is Citric acid monohydrate Food grade.
3. zinc citrate ammonia according to claim 1 is as the purposes of micro elements by plants conditioning agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510251951.0A CN104892396B (en) | 2014-10-16 | 2015-05-18 | Preparation method of ammonia zinc citrate |
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|---|---|---|---|
| CN2014105471928 | 2014-10-16 | ||
| CN201410547192.8A CN104387142A (en) | 2014-10-16 | 2014-10-16 | Zinc ammonium citrate preparation method |
| CN201510251951.0A CN104892396B (en) | 2014-10-16 | 2015-05-18 | Preparation method of ammonia zinc citrate |
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| CN104892396A true CN104892396A (en) | 2015-09-09 |
| CN104892396B CN104892396B (en) | 2017-05-17 |
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| CN201510251951.0A Active CN104892396B (en) | 2014-10-16 | 2015-05-18 | Preparation method of ammonia zinc citrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748732A (en) * | 2016-12-20 | 2017-05-31 | 湖北大学 | A kind of preparation method of zinc citrate ammonium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110894199A (en) * | 2019-12-11 | 2020-03-20 | 郑州瑞普生物工程有限公司 | Preparation method of ammonium magnesium citrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289754A (en) * | 1980-11-03 | 1981-09-15 | Richardson-Vicks Inc. | Zinc derivatives and their use in mouthwash compositions |
| US4325939A (en) * | 1980-09-22 | 1982-04-20 | Richardson-Vicks Inc. | Zinc derivatives and their use in dental compositions |
| CN101704738A (en) * | 2009-11-25 | 2010-05-12 | 郑州瑞普生物工程有限公司 | Production method of ammonium ferric citrate |
| CN103044134A (en) * | 2012-12-10 | 2013-04-17 | 山东金正大生态工程股份有限公司 | Device for carrying out anti-floating treatment on and adding microelements to coated controlled-release fertilizer, and working method of device |
-
2014
- 2014-10-16 CN CN201410547192.8A patent/CN104387142A/en active Pending
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2015
- 2015-05-18 CN CN201510251951.0A patent/CN104892396B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4325939A (en) * | 1980-09-22 | 1982-04-20 | Richardson-Vicks Inc. | Zinc derivatives and their use in dental compositions |
| US4289754A (en) * | 1980-11-03 | 1981-09-15 | Richardson-Vicks Inc. | Zinc derivatives and their use in mouthwash compositions |
| CN101704738A (en) * | 2009-11-25 | 2010-05-12 | 郑州瑞普生物工程有限公司 | Production method of ammonium ferric citrate |
| CN103044134A (en) * | 2012-12-10 | 2013-04-17 | 山东金正大生态工程股份有限公司 | Device for carrying out anti-floating treatment on and adding microelements to coated controlled-release fertilizer, and working method of device |
Non-Patent Citations (2)
| Title |
|---|
| 邓舜扬等: "《精细化工配方集锦》", 31 December 1998, 北京：化学工业出 * |
| 高天荣等: "《用气/质联用仪对可溶性柠檬酸锌组成的研究》", 《蒙自师专学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748732A (en) * | 2016-12-20 | 2017-05-31 | 湖北大学 | A kind of preparation method of zinc citrate ammonium |
| CN106748732B (en) * | 2016-12-20 | 2020-01-14 | 湖北大学 | Preparation method of ammonium zinc citrate |
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| CN104892396B (en) | 2017-05-17 |
| CN104387142A (en) | 2015-03-04 |
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Effective date of registration: 20180518 Address after: 467400 77 east section of Qianjin Road, Baofeng County, Pingdingshan, Henan. Patentee after: Henan rubijia Bio Technology Co., Ltd. Address before: 450001 west of Zhengzhou City, Henan Province, the intersection of Wu Tong Street and red pine road is 500 meters westward. Patentee before: Zhengzhou Ruipu Bioengineering Co., Ltd. |