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CN104892396A - Preparation method of ammonia zinc citrate - Google Patents

Preparation method of ammonia zinc citrate Download PDF

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CN104892396A
CN104892396A CN 201510251951 CN201510251951A CN104892396A CN 104892396 A CN104892396 A CN 104892396A CN 201510251951 CN201510251951 CN 201510251951 CN 201510251951 A CN201510251951 A CN 201510251951A CN 104892396 A CN104892396 A CN 104892396A
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ammonia
zinc
citrate
parts
water
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CN 201510251951
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CN104892396B (en )
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梅志恒
李良玉
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郑州瑞普生物工程有限公司
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05FORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00Other organic fertilisers
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part

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

柠檬酸锌氨的制备方法 Preparation zinc citrate ammonia

技术领域 FIELD

[0001] 本发明涉及一种可作为植物微量元素调节剂使用的柠檬酸锌氨的制备方法。 [0001] The present invention relates to a method for preparing zinc citrate as an ammonia plant trace elements moderators.

背景技术 Background technique

[0002] 现在农业生产中,为了追求粮食高产、稳产,常年重施化肥,轻施有机肥;重氮磷肥,轻钾肥;重大元素肥,轻微肥。 [0002] Now agricultural production in order to pursue high-yield grain yield, perennial heavy fertilizer, light organic fertilizer; diazonium phosphate fertilizer, potash fertilizer light; major elements of fat, slightly fat. 大量施用利用率较低的氮肥和磷肥,这样以来不仅增加农业成本,浪费资源,污染环境,还会造成土壤板结,耕层富营养化,引起土壤次生盐渍化、硝酸盐积累以及土壤酸化等一系列问题。 Administration of a large number of low utilization of nitrogen and phosphate fertilizer, since this not only increases the cost of agriculture, waste resources and pollute the environment, but also cause soil compaction, topsoil eutrophication, caused by soil salinization, nitrate accumulation and soil acidification and other issues. 土壤酸化程度越高,土壤中的钙、镁、钾、铵及微量元素损失愈多,造成耕层钙、镁、钾及微量元素的缺乏,植物营养元素严重不平衡,形成恶性循环;同时造成土壤严重板结。 The higher the degree of acidification, calcium, magnesium, potassium, ammonium, and trace elements in the more loss of soil, resulting in a lack of topsoil, calcium, magnesium, potassium and trace elements, plant nutrients serious imbalance, creating a vicious cycle; also causing severe soil compaction. 目前关于土壤板结的问题已引起国家的重视。 Currently the issue of soil compaction has attracted national attention. 由于过量大量元素的施用而缺乏中微量元素的补充,导致很多土壤"越来越贫瘠,越来越荒凉,越来越板结",增加中微量元素的施用,同时缓解土壤板结情况,已成为现代农业的主要发展方向。 Due to Excessive application of a large number of elements and the lack of trace elements supplement, resulting in many soil "more and more barren, more desolate, more compaction," adds the administration of trace elements, while alleviating soil compaction circumstances, it has become a modern the main direction of development of agriculture. 有专家指出,现有土壤十年不施氮磷等大量元素,合理补充调节中微量元素,土壤中也不会缺氮磷等元素,作物不减产,也会逐步的调节土壤板结问题。 Some experts pointed out that the existing soil decades is not applied nitrogen and phosphorus and other major elements, trace elements in a logical addition to regulation, soil nitrogen and phosphorus and other elements will not be missing, does not cut the crop, will gradually adjust soil compaction problems.

[0003] 目前对土壤的中微量元素的补充仍以无机盐为主,EDTA螯合态以较强的螯合性能取代了部分无机盐市场,同时一些厂家还打出了糖醇螯合、氨基酸螯合产品,螯合态已形成一种趋势。 [0003] It supplement trace elements in the soil is still mainly inorganic salts, EDTA chelated strong chelating ability to replace a part of the inorganic salt market, while some manufacturers also played a chelating sugar alcohol, amino acid chelated layered product, a trend has been chelated. 然而,无机盐的肥效持续时间有限,而EDTA螯合盐的螯合强度较大,在使用过程中难于释放。 However, inorganic fertilizer limited duration, intensity and chelating EDTA chelate salt is large, it is difficult to release during use.

发明内容 SUMMARY

[0004] 本发明的目的在于提供一种可作为植物微量元素调节剂使用的柠檬酸锌氨的制备方法。 [0004] The object of the present invention is to provide a method for preparing zinc citrate as an ammonia plant trace elements moderators.

[0005] 为实现上述目的,本发明可采取下述技术方案: 本发明所述的柠檬酸锌氨的制备方法,它是由原料水、柠檬酸、氧化锌粉末和氨水按下述重量份配比和方法制备而成: 配比: 水100份,柠檬酸17~18份,氧化锌粉末10~11份,氨水35~40份; 制备方法: 第一步,将水和氧化锌粉末置于搅拌设备中分散均匀; 第二步,在第一步制得的氧化锌溶液中加入柠檬酸,继续搅拌至熔液变为透明; 第三步,将3/4重量份的氨水缓慢通入到第二步所得透明溶液中; 第四步,将第三步所得溶液加热沸腾,浓缩至原体积的1/2时,自然冷却,然后将剩余的氨水继续缓慢加入,得到透明溶液; 第五步,将第四步透明溶液置于烘箱中烘干水分,所得固体冷却粉碎后即得柠檬酸锌氨成品。 [0005] To achieve the above object, the present invention may take the following technical scheme: Preparation of the zinc citrate ammonia present invention, which is a raw material water, citric acid, and zinc oxide powder with aqueous ammonia in the following parts by weight ratio and preparation method from: ratio: 100 parts of water, 17 to 18 parts of citric acid, zinc oxide powder 10 to 11 parts, from 35 to 40 parts of ammonia; preparation method: the first step, water and the zinc oxide powder was placed dispersed uniformly stirring device; a second step, citric acid is added in the first step to obtain a zinc oxide solution, stirring was continued until melt became transparent; a third step of 3/4 the parts by weight of aqueous ammonia was slowly passed into the second step the resulting clear solution; 1/2 a fourth step, the third step the resulting solution was boiled and concentrated to the original volume, allowed to cool, then the remaining aqueous ammonia was added slowly continued to give a clear solution; fifth step the fourth step a clear solution was placed in a drying oven the water, cooling the resulting solid was pulverized to obtain refined zinc ammonium citrate.

[0006] 所述柠檬酸为一水柠檬酸。 [0006] The citric acid is citric acid monohydrate.

[0007] 本发明制得的柠檬酸锌氨作为微量元素调节剂,可对植物中微量元素进行补充, 其使用方法如下: 1、在土壤中施用:将其作为基肥、种肥或追肥施用。 [0007] The present invention is made of ammonia as a trace element zinc citrate adjusting agent may be added trace elements in plants, which use is as follows: 1, administered in soil: it as a basic fertilizer, seed or fertilizer top dressing administration. 为节约肥料,提高肥效,通常采用条施或穴施方法。 To save fertilizers, improve efficiency, usually banding or fertilizing methods. 由于土壤施用微量元素肥料有一定的后效,可隔年使用。 Due to soil trace element fertilizers have some aftereffect, you can use next year. 柠檬酸铜氨在土壤中的施用量一般为每亩5~10kg。 Copper citrate is administered amount of ammonia in the soil generally acre 5 ~ 10kg.

[0008] 2、对植物体上施用: a、拌种用少量水将柠檬酸锌氨溶解后喷洒在种子上,边喷边搅拌,使种子表面沾上一层溶液,阴干后播种。 [0008] 2, administration of the plant: a, after seed dressing with a small amount of ammonia water was dissolved zinc citrate is sprayed onto the seed while stirring spray, seed coated with a layer surface of the solution, dried after sowing. 拌种用量一般为每公斤种子用量l~6g,用水40~60ml。 The amount of seed dressing per kilogram of seed generally the amount of l ~ 6g, water 40 ~ 60ml.

[0009] b、浸种将柠檬酸锌氨溶解得到浓度0. 〇l~〇. 1%的溶液,将种子浸入,浸种时间为12~24h。 [0009] b, zinc citrate Soaking the ammonia dissolving 0.5 billion 〇l ~ 1% solution concentration, immersing the seeds, soaking time is 12 ~ 24h.

[0010] C、蘸根对水稻及其他移植作物,可使用浓度0. 1~1. 0%的柠檬酸锌氨溶液蘸根使用。 [0010] C, dipping and other transplanted rice crops, using a concentration of 0.1 - 1.0% ammonia solution dipping of zinc citrate used.

[0011] d、根外喷施用浓度0. 02~0. 1%的柠檬酸锌氨溶液对植物叶片的正反两面进行喷洒,以叶片表面湿润为宜。 [0011] d, outer root spraying spraying both sides of the plant leaves with a concentration of 0.02 - 0.1% zinc citrate ammonia solution, preferably at a blade surface wet.

[0012] 本发明的优点在于将其作为植物中微量元素调节剂使用时,具有绿色环保、无残留,兼容性好、养分吸收好,原料成本低等优点,可广泛应用于水溶肥、叶面肥、植物生长调节剂、土壤调理剂中,顺应了"绿色、有机、生态"的农业发展新方向。 [0012] The advantage of the present invention is that it as a plant regulator of trace elements used are green, residue-free, good compatibility, nutrient absorption, and low cost of raw materials, it can be widely applied to water-soluble fertilizer foliar fertilizer, plant growth regulators, soil conditioners, conform to the "green, organic, eco," the new direction of agricultural development.

[0013] 柠檬酸锌氨是由锌、氨和柠檬酸组成的结构不明的络合盐,其络合是由氨中的氮原子提供孤对电子和具有空轨道的金属离子进行络合,在产物制备过程中,采用二次螯合技术:第三步和第四步两次添加氨水,在特定的反应条件下进行二次螯合,制得中等强度的螯合盐,其络合强度小于EDTA螯合盐,作为植物中微量元素补充时,不仅能够补充植物或土壤中的微量元素,而且能够持续进行作用。 [0013] Ammonia is a zinc from zinc citrate, ammonia and citric acid complex salt of unknown structure, which is complexed by ammonia nitrogen atom lone pair of electrons and a metal ion complexed with an empty orbit in preparation process of the product, using the second chelation technology: the third step and the fourth step adding ammonia water twice, secondary chelating under certain reaction conditions, the chelate salts prepared moderate intensity, complexation strength of less than EDTA chelation salt, as a supplement trace elements in plants, not only to supplement trace elements in plants or soil, and can continue to carry out the role.

具体实施方式 detailed description

[0014] 下面通过具体实施例对本发明做进一步的详述。 [0014] The following specific examples further by detailed description of the present invention.

[0015] 实施例1 首先准确称取氧化锌粉末410g,一水柠檬酸700g,氨水1500ml,水4000ml ; 制备方法为: 第一步,反应釜中加水4000 ml,水中加入410g氧化锌粉末,搅拌溶解,分散均匀; 第二步,在第一步制得的氧化锌溶液中加入一水柠檬酸700g,继续搅拌至熔液变为透明; 第三步,开搅拌,在透明溶液中缓慢加入氨水1125 ml,加完氨水后再继续搅拌0. 5h ; 第四步,将第三步所得溶液加热沸腾,浓缩至原体积的1/2后,停止加热,自然冷却至室温后将剩余的375ml氨水继续缓慢加入,搅拌0. 5h ; 第五步,将第四步的溶液置于烘箱中120~130°C烘干水分,所得固体冷却粉碎后即得柠檬酸锌氨成品。 [0015] Example 1 is first accurately weighed 410g zinc oxide powder, 700 g of a citric acid, ammonia water 1500ml, 4000ml water; preparation method: first, the kettle water was added 4000 ml, 410g zinc oxide powder added to the water, stirring dissolved, dispersed uniformly; a second step, in the first step was added to obtain a zinc oxide in a solution of citric acid, 700 g of water, stirring was continued until melt became transparent; the third step, open stirring, a clear solution was slowly added aqueous ammonia 1125 ml, stirring was continued for 0. 5h after completion of the addition of ammonia; a fourth step, the third step the resulting solution was boiled and concentrated to half the original volume, the heating was stopped, allowed to cool to room temperature the remaining aqueous ammonia 375ml continued slowly added, stirred for 0. 5h; a fifth step, the fourth step was placed in an oven dried 120 ~ 130 ° C water, cooling the resulting solid was pulverized to obtain zinc citrate ammonia finished.

[0016] 实施例2 首先准确称取氧化锌粉末400g,一水柠檬酸680g,氨水1400ml,水4000ml ; 制备方法为: 第一步,反应釜中加水4000 ml,水中加入400g氧化锌粉末,搅拌溶解,分散均匀; 第二步,在第一步制得的氧化锌溶液中加入一水柠檬酸680g,继续搅拌至熔液变为透明; 第三步,开搅拌,在透明溶液中缓慢加入氨水1050 ml,加完氨水后再继续搅拌0. 5h ; 第四步,将第三步所得溶液加热沸腾,浓缩至原体积的1/2后,停止加热,自然冷却至室温后将剩余的350ml氨水继续缓慢加入,搅拌0. 5h ; 第五步,将第四步的溶液置于烘箱中120~130°C烘干水分,所得固体冷却粉碎后即得柠檬酸锌氨成品。 [0016] Example 2 First zinc oxide powder was accurately weighed 400g, 680g citric acid monohydrate, 1400 ml of aqueous ammonia, water 4000ml; preparation method: first, the kettle water was added 4000 ml, 400g zinc oxide powder added to the water, stirring dissolved, dispersed uniformly; a second step, in the first step was added to obtain a zinc oxide in a solution of citric acid, 680g of water, stirring was continued until melt became transparent; the third step, open stirring, a clear solution was slowly added aqueous ammonia 1050 ml, stirring was continued for 0. 5h after completion of the addition of ammonia; fourth step, the third step the resulting solution was boiled and concentrated to half the original volume, heating was stopped, allowed to cool to room temperature the remaining aqueous ammonia 350ml continued slowly added, stirred for 0. 5h; a fifth step, the fourth step was placed in an oven dried 120 ~ 130 ° C water, cooling the resulting solid was pulverized to obtain zinc citrate ammonia finished.

[0017] 实施例3 首先准确称取氧化锌粉末440g,一水柠檬酸720g,氨水1400ml,水4000ml ; 制备方法为: 第一步,反应釜中加水4000 ml,水中加入440g氧化锌粉末,搅拌溶解,分散均匀; 第二步,在第一步制得的氧化锌溶液中加入一水柠檬酸720g,继续搅拌至熔液变为透明; 第三步,开搅拌,在透明溶液中缓慢加入氨水1200 ml,加完氨水后再继续搅拌0. 5h ; 第四步,将第三步所得溶液加热沸腾,浓缩至原体积的1/2后,停止加热,自然冷却至室温后将剩余的400ml氨水继续缓慢加入,搅拌0. 5h ; 第五步,将第四步的溶液置于烘箱中120~130°C烘干水分,所得固体冷却粉碎后即得柠檬酸锌氨成品。 [0017] Example 3 is first accurately weighed 440g zinc oxide powder, 720 g of citric acid monohydrate, 1400 ml of aqueous ammonia, water 4000ml; preparation method: first, the kettle water was added 4000 ml, 440g zinc oxide powder added to the water, stirring dissolved, dispersed uniformly; a second step, in the first step was added to obtain a zinc oxide in a solution of citric acid, 720 g of water, stirring was continued until melt became transparent; the third step, open stirring, a clear solution was slowly added aqueous ammonia 1200 ml, stirring was continued for 0. 5h after completion of the addition of ammonia; fourth step, the third step the resulting solution was boiled and concentrated to half the original volume, heating was stopped, allowed to cool to room temperature the remaining aqueous ammonia 400ml continued slowly added, stirred for 0. 5h; a fifth step, the fourth step was placed in an oven dried 120 ~ 130 ° C water, cooling the resulting solid was pulverized to obtain zinc citrate ammonia finished.

[0018] 表1为上述实施例1-3制备的柠檬酸锌氨成品的性能数据表: 表1 [0018] Table 1 above Preparation Example 1-3 of ammonia finished zinc citrate performance data: Table 1

Figure CN104892396AD00051

从上述检测结果可以看出:制备的柠檬酸锌氨金属含量和氮含量指标稳定,作为微肥使用时能够为植物提供必须的微量元素锌,还能作为氮肥补充大量元素。 From the above test results: zinc citrate and ammonia nitrogen content of the metal content of indicators of stability of the preparation, use as a fertilizer can provide the necessary trace elements zinc plant, but also a large number of elements as nitrogen supplement.

[0019] 取200ml蒸馏水,加入2g实施例1制备的柠檬酸锌氨,搅拌溶解后,加入2g水溶性肥料,搅拌溶解,观察现象见表2。 [0019] Take 200ml of distilled water, ammonia was added 2g zinc citrate prepared according to Example 1, after stirring and dissolving the water-soluble fertilizer was added 2g, stirred to dissolve, the phenomenon was observed Table 2.

[0020] 表2 [0020] TABLE 2

Figure CN104892396AD00061

从表2中数据可以看出:本发明所制备的柠檬酸锌氨与其他水溶性肥混用时具有很好的兼容性。 As can be seen from the data in Table 2: very good compatibility with zinc citrate prepared according to the invention ammonia and other water soluble fertilizer mix.

Claims (3)

  1. 1. 一种柠檬酸锌氨的制备方法,其特征在于:它是由原料水、柠檬酸、氧化锌粉末和氨水按下述重量份配比和方法制备而成: 配比: 水100份,柠檬酸17~18份,氧化锌粉末10~11份,氨水35~40份; 制备方法: 第一步,将水和氧化锌粉末置于搅拌设备中分散均匀; 第二步,在第一步制得的氧化锌溶液中加入柠檬酸,继续搅拌至熔液变为透明; 第三步,将3/4重量份的氨水缓慢通入到第二步所得透明溶液中; 第四步,将第三步所得溶液加热沸腾,浓缩至原体积的1/2时,自然冷却,然后将剩余的氨水继续缓慢加入,得到透明溶液; 第五步,将第四步透明溶液置于烘箱中烘干水分,所得固体冷却粉碎后即得柠檬酸锌氨成品。 1. A method for preparing zinc citrate ammonia, characterized in that: it is produced from raw water, citric acid, ammonia and zinc oxide powder according to the following method and parts by weight ratio of from: ratio: 100 parts of water, 17 to 18 parts of citric acid, zinc oxide powder 10 to 11 parts, from 35 to 40 parts of ammonia; preparation method: the first step, water and the zinc oxide powder was placed uniformly dispersed stirring device; a second step, in a first step the resulting zinc oxide citric acid was added and stirring was continued until melt became transparent; a third step of 3/4 the parts by weight of aqueous ammonia was slowly passed into the second stage the resulting clear solution; a fourth step, the first the resulting solution was 1/2 of the three-boiled and concentrated to the original volume, allowed to cool, then the remaining aqueous ammonia was added slowly continued to give a clear solution; a fifth step, the fourth step was placed in an oven dried clear water , cooling the resulting solid was pulverized to obtain zinc citrate ammonia finished.
  2. 2. 根据权利要求1所述的柠檬酸锌氨的制备方法,其特征在于:所述柠檬酸为一水柠檬酸。 2. A method for preparing zinc citrate ammonia according to claim 1, wherein: said citric acid is citric acid monohydrate.
  3. 3. 权利要求1所述的柠檬酸锌氨作为植物微量元素调节剂的用途。 Zinc citrate ammonia according to claim 1 for use as a plant regulator trace elements.
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