CN115594545A - Method for producing Gly-containing water-soluble fertilizer - Google Patents

Method for producing Gly-containing water-soluble fertilizer Download PDF

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CN115594545A
CN115594545A CN202211424128.1A CN202211424128A CN115594545A CN 115594545 A CN115594545 A CN 115594545A CN 202211424128 A CN202211424128 A CN 202211424128A CN 115594545 A CN115594545 A CN 115594545A
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glycine
amino acid
mother liquor
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gly
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张战战
赵晓兰
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Shijiazhuang Shangzheng Information Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C5/00Fertilisers containing other nitrates
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention relates to the technical field of crop fertilizers, and provides a method for producing a Gly-containing water-soluble fertilizer, which purifies a glycine concentrated mother solution by an electrodialysis method, and enables refined glycine prepared by purification to react with calcium nitrate tetrahydrate to prepare glycine chelated calcium, so that the condition that calcium salt and nutrient elements such as phosphorus, sulfur and the like form precipitates can be prevented, the stability of plant cell membranes can be enhanced through the action of the glycine chelated calcium, and the Gly-containing water-soluble fertilizer can participate in the regulation and control of the physiological and biochemical processes and the enzyme activity of plants, and is beneficial to the growth of plants; and secondly, the compound amino acid chelated zinc is prepared from compound amino acid prepared by mixing various amino acids and zinc sulfate heptahydrate, trace elements and various amino acid components can be provided for plants, and while a nitrogen source is provided for plant growth through the compound amino acid, the interference of soil and metal ion antagonism can be resisted through the trace element zinc, so that a stable growth environment is provided for the plants.

Description

一种含Gly水溶肥料生产的方法A kind of method that contains Gly water-soluble fertilizer production

技术领域technical field

本发明涉及农作物肥料技术领域,具体涉及一种含Gly水溶肥料生产的方法。The invention relates to the technical field of crop fertilizers, in particular to a method for producing Gly-containing water-soluble fertilizers.

背景技术Background technique

水溶肥料易被农作物吸收,吸收利用率相对较高,是一个速效肥料,可以让种植者较快地看到肥料的效果和表现,随时可以根据作物不同长势对肥料配方作出调整;而且水溶肥料可以应用于喷滴灌等设施农业,实现水肥一体化,达到省水省肥省工的效能。现有的水溶肥料大多是通过中量元素和微量元素混合制得,部分水溶肥料还有指定种类的氨基酸,但是现有水溶肥料中的金属离子大都是以金属盐的形式存在,在施肥的过程中容易与土壤中的磷、硫等元素形成沉淀,从而降低植物的吸收率,而且现有的水溶肥料中含有的氨基酸种类较少,无法使植物的营养成分得到全面保证,因此,如何研制一种营养成分较为全面且有利于植物吸收的水溶肥料,成为了本领域技术人员亟待解决的技术问题。Water-soluble fertilizers are easily absorbed by crops, and their absorption and utilization rate is relatively high. It is applied to facility agriculture such as drip irrigation, realizes the integration of water and fertilizer, and achieves the efficiency of saving water, fertilizer and labor. Most of the existing water-soluble fertilizers are made by mixing medium and trace elements. Some water-soluble fertilizers also have specified types of amino acids, but most of the metal ions in the existing water-soluble fertilizers exist in the form of metal salts. During the fertilization process It is easy to form precipitation with phosphorus, sulfur and other elements in the soil, thereby reducing the absorption rate of plants, and the existing water-soluble fertilizers contain fewer amino acids, which cannot fully guarantee the nutritional content of plants. Therefore, how to develop a fertilizer A kind of water-soluble fertilizer which has more comprehensive nutritional components and is beneficial to plant absorption has become a technical problem to be solved urgently by those skilled in the art.

发明内容Contents of the invention

解决的技术问题Technical issues resolved

针对现有技术的不足,本发明提供了一种含Gly水溶肥料生产的方法,使生产的水溶肥料在保证植物营养成分全面补充的同时,还能够提高营养成分的吸收利用率,从而提高水溶肥料的应用前景。Aiming at the deficiencies in the prior art, the present invention provides a method for producing water-soluble fertilizers containing Gly, so that the water-soluble fertilizers produced can also improve the absorption and utilization rate of nutrients while ensuring the comprehensive supplementation of plant nutrients, thereby improving the production efficiency of water-soluble fertilizers. application prospects.

技术方案Technical solutions

为实现以上目的,本发明通过以下技术方案予以实现:To achieve the above object, the present invention is achieved through the following technical solutions:

一种含Gly水溶肥料生产的方法,所述方法包括以下步骤:A kind of method that contains Gly water-soluble fertilizer production, described method comprises the following steps:

Step1、量取100重量份甘氨酸浓缩母液备用,接着使用等量的甲醇对甘氨酸浓缩母液进行稀释,稀释结束后过滤去掉杂质,将所得溶液加入至电渗析器的淡室料桶中,并向电渗析器的浓室料桶中加入蒸馏水,经电渗析分离后得到淡室溶液和浓室溶液,将淡室溶液在70-100℃的温度下加热浓缩,直至甘氨酸结晶析出,将结晶物通过过滤与母液分离,干燥后既得精品甘氨酸,结晶过滤后的母液可循环使用;Step1, measure 100 parts by weight of glycine concentrated mother liquor for later use, then use an equal amount of methanol to dilute the glycine concentrated mother liquor, filter to remove impurities after dilution, add the resulting solution to the dilute chamber material tank of the electrodialyzer, and send to the electrodialyzer Distilled water is added to the thick chamber barrel of the dialyzer, and the light chamber solution and the concentrated chamber solution are obtained after separation by electrodialysis. The light chamber solution is heated and concentrated at a temperature of 70-100°C until glycine crystallizes, and the crystals are filtered through Separated from the mother liquor, dried to obtain high-quality glycine, and the mother liquor after crystallization and filtration can be recycled;

Step2、按照2:3的摩尔比称取四水硝酸钙和Step1中的精品甘氨酸与去离子水进行混合,以300-400r/min的速度搅拌5-10min后制成混悬液,使用盐酸或氨水将混悬液pH调至5.5并将温度加热至50℃,然后将混悬液倒入高压流体纳米磨中进行处理,直至混悬液变清为止,对变清后的混悬液进行低温减压干燥,再用100-200目筛网过滤成细粉,所得记作甘氨酸螯合钙;Step2. Weigh calcium nitrate tetrahydrate and the high-quality glycine in Step1 and deionized water according to the molar ratio of 2:3, mix them with deionized water, stir at a speed of 300-400r/min for 5-10min to make a suspension, use hydrochloric acid or Ammonia water adjusts the pH of the suspension to 5.5 and heats the temperature to 50°C, then pours the suspension into a high-pressure fluid nanomill for processing until the suspension becomes clear, and then cools the clear suspension Dry under reduced pressure, then filter into fine powder with 100-200 mesh sieve, and the gained is recorded as glycine chelated calcium;

Step3、称取一定量的复合氨基酸溶解于重量为其2-3倍的去离子水中,过滤去除不溶物后使用氢氧化钠溶液调节pH至5,接着加入重量为复合氨基酸20-30%的七水硫酸锌,在60℃的水浴温度中反应30min,反应后加热浓缩并进行冷却结晶,对结晶物进行过滤和干燥,所得记作复合氨基酸螯合锌;Step3. Weigh a certain amount of compound amino acid and dissolve it in deionized water 2-3 times its weight. After removing the insoluble matter by filtration, use sodium hydroxide solution to adjust the pH to 5, and then add 20-30% of the weight of the compound amino acid. Zinc sulfate water, reacted in a water bath temperature of 60°C for 30 minutes, heated and concentrated after the reaction, cooled and crystallized, filtered and dried the crystals, and the obtained was recorded as compound amino acid chelated zinc;

Step4、按照重量份计称取58-60份取甘氨酸浓缩母液、8-9份六水硝酸镁、5-8份中量元素、3-5份微量元素、15-18份Step2中的甘氨酸螯合钙、4-5份Step3中的复合氨基酸螯合锌和85-90份去离子水备用;Step4, take 58-60 parts by weight to get concentrated glycine mother liquor, 8-9 parts of magnesium nitrate hexahydrate, 5-8 parts of medium elements, 3-5 parts of trace elements, 15-18 parts of glycine chelate in Step2 Calcium complex, 4-5 parts of compound amino acid chelated zinc in Step3 and 85-90 parts of deionized water are standby;

Step5、将Step4中的甘氨酸浓缩母液与去离子水中的一半进行混合,搅拌均匀后加入上述重量份的甘氨酸螯合钙和复合氨基酸螯合锌,并进行再次搅拌,所得记作第一组分;Step5. Mix the glycine concentrated mother liquor in Step4 with half of the deionized water, stir evenly, add the above-mentioned glycine chelated calcium and compound amino acid chelated zinc, and stir again, and the obtained is recorded as the first component;

Step6、将Step4中的六水硝酸镁、中量元素、微量元素和余量的去离子水进行混合,搅拌均匀后所得记作第二组分;Step6, the magnesium nitrate hexahydrate in Step4, middle element, trace element and the deionized water of surplus are mixed, after stirring, the gained is recorded as the second component;

Step7、将第一组分和第二组分进行混合,搅拌均匀后过滤去除杂质,接着加热浓缩至原体积的一半,所得即为含Gly水溶肥料。Step7. Mix the first component and the second component, stir evenly, filter to remove impurities, then heat and concentrate to half of the original volume, and the obtained water-soluble fertilizer containing Gly.

更进一步地,所述甘氨酸浓缩母液的制备方法包括以下步骤:Further, the preparation method of the concentrated glycine mother liquor comprises the following steps:

步骤1、向反应器中倒入氯乙酸、甲醇和乌洛托品,搅拌溶解后缓慢通入液氨,在58-60℃的温度条件下进行合成反应2h,在反应的过程中维持反应体系的pH为7-8,其中,氯乙酸、甲醇和乌洛托品的摩尔比为1:7.5:0.2;Step 1. Pour chloroacetic acid, methanol and urotropine into the reactor, stir and dissolve, then slowly feed liquid ammonia, carry out the synthesis reaction at a temperature of 58-60°C for 2 hours, and maintain the reaction system during the reaction The pH is 7-8, wherein the molar ratio of chloroacetic acid, methanol and urotropine is 1:7.5:0.2;

步骤2、步骤1的反应结束后继续保温直至有晶体析出,接着冷却至室温并离心过滤,离心后得到母液和结晶物,使用少量甲醇对结晶物洗涤2次,将洗涤所得的洗液与上述母液进行混合,所得记作循环反应溶剂;Step 2, after the reaction of step 1, continue to keep warm until crystals are precipitated, then cool to room temperature and centrifugally filter, obtain mother liquor and crystals after centrifugation, use a small amount of methanol to wash the crystals twice, and wash the obtained lotion with the above-mentioned The mother liquor is mixed, and the gained is recorded as the circulating reaction solvent;

步骤3、将步骤2中的循环反应溶剂作为反应介质供下次循环反应使用,直到最后一次循环反应结束后得到母液和结晶物;Step 3, using the circulating reaction solvent in step 2 as the reaction medium for the next circulating reaction, until the last circulating reaction ends to obtain mother liquor and crystals;

步骤4、使用甲醇对步骤3中的结晶物进行洗涤2次,洗涤后的洗液与步骤3中的母液进行混合,混合后进行简单蒸馏,所得即为甘氨酸浓缩母液。Step 4, washing the crystals in step 3 twice with methanol, mixing the washed lotion with the mother liquor in step 3, and performing simple distillation after mixing to obtain concentrated glycine mother liquor.

更进一步地,所述步骤1中的搅拌速度为500-600r/min,所述步骤2中的离心转速为7000-8000r/min。Furthermore, the stirring speed in the step 1 is 500-600r/min, and the centrifugal speed in the step 2 is 7000-8000r/min.

更进一步地,所述步骤3中循环反应的次数为3-4次。Furthermore, the number of cyclic reactions in the step 3 is 3-4 times.

更进一步地,所述Step1的加热浓缩需要不断搅拌的情况下进行。Furthermore, the heating and concentration of Step 1 needs to be carried out under the condition of constant stirring.

更进一步地,所述Step2中去离子水的量为四水硝酸钙和精品甘氨酸总量的3-4倍。Further, the amount of deionized water in the Step2 is 3-4 times of the total amount of calcium nitrate tetrahydrate and refined glycine.

更进一步地,所述Step3中复合氨基酸的制备方法为:按照重量份计称取17-18份赖氨酸、1-2份谷氨酸、0.3-0.5份丙氨酸、0.03-0.05份缬氨酸和0.1-0.3份苯丙氨酸进行混合,混合均匀后即为复合氨基酸。Further, the preparation method of the compound amino acid in the Step3 is: weigh 17-18 parts of lysine, 1-2 parts of glutamic acid, 0.3-0.5 parts of alanine, 0.03-0.05 parts of valeric acid in parts by weight Amino acid and 0.1-0.3 parts of phenylalanine are mixed, and the compound amino acid is obtained after mixing evenly.

更进一步地,所述Step4中的中量元素为水合硅酸钠。Furthermore, the middle element in the Step4 is hydrated sodium silicate.

更进一步地,所述Step4中的微量元素为硼酸和硫酸亚铁按同等重量比混合制得。Furthermore, the trace elements in Step4 are obtained by mixing boric acid and ferrous sulfate in equal weight ratios.

更进一步地,所述Step5和Step6中的搅拌速度为600-800r/min。Further, the stirring speed in Step5 and Step6 is 600-800r/min.

有益效果Beneficial effect

本发明提供了一种含Gly水溶肥料生产的方法,与现有公知技术相比,本发明的具有如下有益效果:The invention provides a method for producing Gly-containing water-soluble fertilizers. Compared with the prior known technology, the invention has the following beneficial effects:

本发明通过电渗析法对甘氨酸浓缩母液进行提纯,并使提纯制得的精品甘氨酸与四水硝酸钙进行反应制得甘氨酸螯合钙,能够防止钙盐与磷、硫等营养元素形成沉淀的情况发生,通过甘氨酸螯合钙的作用能够增强植物细胞膜的稳定性,还能够参与植物生理生化过程及酶活性的调控,有利于植物的生长;其次,以多种氨基酸混合制得的复合氨基酸和七水硫酸锌制成复合氨基酸螯合锌,能够向植物提供微量元素及多种氨基酸成分,在通过复合氨基酸为植物生长提供氮源的同时,还能够通过微量元素锌来抵抗土壤的干扰、缓解金属离子拮抗,为植物提供稳定的生长环境;最后,通过六水硝酸镁、中量元素以及微量元素的加入,能够为植物提供更充足的养分,从而使本发明生产的含Gly水溶肥料具有更好的应用前景。The present invention purifies the concentrated glycine mother liquor by electrodialysis, and reacts the purified refined glycine with calcium nitrate tetrahydrate to prepare glycine chelated calcium, which can prevent calcium salt from forming precipitation with phosphorus, sulfur and other nutrient elements Glycine chelated calcium can enhance the stability of plant cell membranes, and can also participate in the regulation of plant physiological and biochemical processes and enzyme activities, which is beneficial to the growth of plants; secondly, compound amino acids and seven Zinc sulfate water is made of compound amino acid chelated zinc, which can provide plants with trace elements and a variety of amino acid components. While providing nitrogen sources for plant growth through compound amino acids, it can also resist soil interference and relieve metal stress through the trace element zinc. Ion antagonism provides a stable growth environment for plants; finally, through the addition of magnesium nitrate hexahydrate, medium elements and trace elements, more sufficient nutrients can be provided for plants, so that the Gly-containing water-soluble fertilizer produced by the present invention has better application prospects.

具体实施方式detailed description

为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of them. the embodiment. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.

实施例1:Example 1:

本实施例的一种含Gly水溶肥料生产的方法,方法包括以下步骤:A kind of method that contains Gly water-soluble fertilizer production of the present embodiment, the method comprises the following steps:

Step1、量取100重量份甘氨酸浓缩母液备用,接着使用等量的甲醇对甘氨酸浓缩母液进行稀释,稀释结束后过滤去掉杂质,将所得溶液加入至电渗析器的淡室料桶中,并向电渗析器的浓室料桶中加入蒸馏水,经电渗析分离后得到淡室溶液和浓室溶液,将淡室溶液在70℃的温度下加热浓缩,直至甘氨酸结晶析出,将结晶物通过过滤与母液分离,干燥后既得精品甘氨酸,结晶过滤后的母液可循环使用;Step1, measure 100 parts by weight of glycine concentrated mother liquor for later use, then use an equal amount of methanol to dilute the glycine concentrated mother liquor, filter to remove impurities after dilution, add the resulting solution to the dilute chamber material tank of the electrodialyzer, and send to the electrodialyzer Distilled water is added to the thick chamber barrel of the dialyzer, and the light chamber solution and the concentrated chamber solution are obtained after separation by electrodialysis. The light chamber solution is heated and concentrated at a temperature of 70°C until glycine crystals are precipitated, and the crystals are filtered and mixed with the mother liquor. After separation and drying, high-quality glycine is obtained, and the mother liquor after crystallization and filtration can be recycled;

Step2、按照2:3的摩尔比称取四水硝酸钙和Step1中的精品甘氨酸与去离子水进行混合,以300r/min的速度搅拌5min后制成混悬液,使用盐酸或氨水将混悬液pH调至5.5并将温度加热至50℃,然后将混悬液倒入高压流体纳米磨中进行处理,直至混悬液变清为止,对变清后的混悬液进行低温减压干燥,再用100目筛网过滤成细粉,所得记作甘氨酸螯合钙;Step2. Weigh calcium nitrate tetrahydrate and the high-quality glycine in Step1 and deionized water according to the molar ratio of 2:3, mix them with deionized water, stir at a speed of 300r/min for 5min to make a suspension, and use hydrochloric acid or ammonia water to dissolve the suspension The pH of the solution is adjusted to 5.5 and the temperature is heated to 50°C, then the suspension is poured into a high-pressure fluid nanomill for processing until the suspension becomes clear, and the clear suspension is dried under reduced pressure at low temperature, Filter it into a fine powder with a 100-mesh sieve, and the gained is recorded as glycine chelated calcium;

Step3、称取一定量的复合氨基酸溶解于重量为其2倍的去离子水中,过滤去除不溶物后使用氢氧化钠溶液调节pH至5,接着加入重量为复合氨基酸20%的七水硫酸锌,在60℃的水浴温度中反应30min,反应后加热浓缩并进行冷却结晶,对结晶物进行过滤和干燥,所得记作复合氨基酸螯合锌;Step3, take a certain amount of compound amino acid and dissolve it in deionized water twice its weight, filter and remove insoluble matter, use sodium hydroxide solution to adjust the pH to 5, then add zinc sulfate heptahydrate whose weight is 20% of compound amino acid, React in a water bath temperature of 60°C for 30 minutes, heat and concentrate after the reaction, and carry out cooling and crystallization, filter and dry the crystals, and the obtained is recorded as the compound amino acid chelated zinc;

Step4、按照重量份计称取58份取甘氨酸浓缩母液、8份六水硝酸镁、5份中量元素、3份微量元素、15份Step2中的甘氨酸螯合钙、4份Step3中的复合氨基酸螯合锌和85份去离子水备用;Step4, take 58 parts by weight to take concentrated glycine mother liquor, 8 parts of magnesium nitrate hexahydrate, 5 parts of medium elements, 3 parts of trace elements, 15 parts of glycine chelated calcium in Step2, 4 parts of compound amino acids in Step3 Chelated zinc and 85 parts of deionized water are standby;

Step5、将Step4中的甘氨酸浓缩母液与去离子水中的一半进行混合,搅拌均匀后加入上述重量份的甘氨酸螯合钙和复合氨基酸螯合锌,并进行再次搅拌,所得记作第一组分;Step5. Mix the glycine concentrated mother liquor in Step4 with half of the deionized water, stir evenly, add the above-mentioned glycine chelated calcium and compound amino acid chelated zinc, and stir again, and the obtained is recorded as the first component;

Step6、将Step4中的六水硝酸镁、中量元素、微量元素和余量的去离子水进行混合,搅拌均匀后所得记作第二组分;Step6, the magnesium nitrate hexahydrate in Step4, middle element, trace element and the deionized water of surplus are mixed, after stirring, the gained is recorded as the second component;

Step7、将第一组分和第二组分进行混合,搅拌均匀后过滤去除杂质,接着加热浓缩至原体积的一半,所得即为含Gly水溶肥料。Step7. Mix the first component and the second component, stir evenly, filter to remove impurities, then heat and concentrate to half of the original volume, and the obtained water-soluble fertilizer containing Gly.

甘氨酸浓缩母液的制备方法包括以下步骤:The preparation method of glycine concentrated mother liquor comprises the following steps:

步骤1、向反应器中倒入氯乙酸、甲醇和乌洛托品,搅拌溶解后缓慢通入液氨,在58℃的温度条件下进行合成反应2h,在反应的过程中维持反应体系的pH为7,其中,氯乙酸、甲醇和乌洛托品的摩尔比为1:7.5:0.2;Step 1. Pour chloroacetic acid, methanol and urotropine into the reactor, stir and dissolve, then slowly feed liquid ammonia, carry out the synthesis reaction at a temperature of 58°C for 2 hours, and maintain the pH of the reaction system during the reaction is 7, wherein the molar ratio of chloroacetic acid, methanol and urotropine is 1:7.5:0.2;

步骤2、步骤1的反应结束后继续保温直至有晶体析出,接着冷却至室温并离心过滤,离心后得到母液和结晶物,使用少量甲醇对结晶物洗涤2次,将洗涤所得的洗液与上述母液进行混合,所得记作循环反应溶剂;Step 2, after the reaction of step 1, continue to keep warm until crystals are precipitated, then cool to room temperature and centrifugally filter, obtain mother liquor and crystals after centrifugation, use a small amount of methanol to wash the crystals twice, and wash the obtained lotion with the above-mentioned The mother liquor is mixed, and the gained is recorded as the circulating reaction solvent;

步骤3、将步骤2中的循环反应溶剂作为反应介质供下次循环反应使用,直到最后一次循环反应结束后得到母液和结晶物;Step 3, using the circulating reaction solvent in step 2 as the reaction medium for the next circulating reaction, until the last circulating reaction ends to obtain mother liquor and crystals;

步骤4、使用甲醇对步骤3中的结晶物进行洗涤2次,洗涤后的洗液与步骤3中的母液进行混合,混合后进行简单蒸馏,所得即为甘氨酸浓缩母液。Step 4, washing the crystals in step 3 twice with methanol, mixing the washed lotion with the mother liquor in step 3, and performing simple distillation after mixing to obtain concentrated glycine mother liquor.

步骤1中的搅拌速度为500r/min,步骤2中的离心转速为7000r/min。The stirring speed in step 1 is 500r/min, and the centrifugal speed in step 2 is 7000r/min.

步骤3中循环反应的次数为3次。The number of cycle reactions in step 3 is 3 times.

Step1的加热浓缩需要不断搅拌的情况下进行。The heating concentration of Step1 needs to be carried out under the condition of constant stirring.

Step2中去离子水的量为四水硝酸钙和精品甘氨酸总量的3倍。The amount of deionized water in Step2 is 3 times of the total amount of calcium nitrate tetrahydrate and high-quality glycine.

Step3中复合氨基酸的制备方法为:按照重量份计称取17份赖氨酸、1份谷氨酸、0.3份丙氨酸、0.03份缬氨酸和0.1份苯丙氨酸进行混合,混合均匀后即为复合氨基酸。The preparation method of the compound amino acid in Step3 is: weigh 17 parts of lysine, 1 part of glutamic acid, 0.3 part of alanine, 0.03 part of valine and 0.1 part of phenylalanine in parts by weight and mix them evenly After that is the compound amino acid.

Step4中的中量元素为水合硅酸钠。The middle element in Step4 is hydrated sodium silicate.

Step4中的微量元素为硼酸和硫酸亚铁按同等重量比混合制得。Trace elements in Step4 are obtained by mixing boric acid and ferrous sulfate in equal weight ratios.

Step5和Step6中的搅拌速度为600r/min。The stirring speed in Step5 and Step6 is 600r/min.

实施例2:Example 2:

本实施例的一种含Gly水溶肥料生产的方法,方法包括以下步骤:A kind of method that contains Gly water-soluble fertilizer production of the present embodiment, the method comprises the following steps:

Step1、量取100重量份甘氨酸浓缩母液备用,接着使用等量的甲醇对甘氨酸浓缩母液进行稀释,稀释结束后过滤去掉杂质,将所得溶液加入至电渗析器的淡室料桶中,并向电渗析器的浓室料桶中加入蒸馏水,经电渗析分离后得到淡室溶液和浓室溶液,将淡室溶液在100℃的温度下加热浓缩,直至甘氨酸结晶析出,将结晶物通过过滤与母液分离,干燥后既得精品甘氨酸,结晶过滤后的母液可循环使用;Step1, measure 100 parts by weight of glycine concentrated mother liquor for later use, then use an equal amount of methanol to dilute the glycine concentrated mother liquor, filter to remove impurities after dilution, add the resulting solution to the dilute chamber material tank of the electrodialyzer, and send to the electrodialyzer Distilled water is added to the thick chamber barrel of the dialyzer, and the light chamber solution and the concentrated chamber solution are obtained after separation by electrodialysis. The light chamber solution is heated and concentrated at a temperature of 100°C until glycine crystallizes, and the crystals are filtered and mixed with the mother liquor. After separation and drying, high-quality glycine is obtained, and the mother liquor after crystallization and filtration can be recycled;

Step2、按照2:3的摩尔比称取四水硝酸钙和Step1中的精品甘氨酸与去离子水进行混合,以400r/min的速度搅拌10min后制成混悬液,使用盐酸或氨水将混悬液pH调至5.5并将温度加热至50℃,然后将混悬液倒入高压流体纳米磨中进行处理,直至混悬液变清为止,对变清后的混悬液进行低温减压干燥,再用200目筛网过滤成细粉,所得记作甘氨酸螯合钙;Step2. Weigh calcium nitrate tetrahydrate and the high-quality glycine in Step1 and deionized water according to the molar ratio of 2:3, mix them with deionized water, stir at a speed of 400r/min for 10min to make a suspension, and use hydrochloric acid or ammonia water to dissolve the suspension The pH of the solution is adjusted to 5.5 and the temperature is heated to 50°C, then the suspension is poured into a high-pressure fluid nanomill for processing until the suspension becomes clear, and the clear suspension is dried under reduced pressure at low temperature, Filter it into a fine powder with a 200-mesh sieve, and the gained is recorded as glycine chelated calcium;

Step3、称取一定量的复合氨基酸溶解于重量为其3倍的去离子水中,过滤去除不溶物后使用氢氧化钠溶液调节pH至5,接着加入重量为复合氨基酸30%的七水硫酸锌,在60℃的水浴温度中反应30min,反应后加热浓缩并进行冷却结晶,对结晶物进行过滤和干燥,所得记作复合氨基酸螯合锌;Step3, take a certain amount of compound amino acid and dissolve it in deionized water whose weight is 3 times, filter and remove insoluble matter, use sodium hydroxide solution to adjust the pH to 5, then add zinc sulfate heptahydrate whose weight is 30% of compound amino acid, React in a water bath temperature of 60°C for 30 minutes, heat and concentrate after the reaction, and carry out cooling and crystallization, filter and dry the crystals, and the obtained is recorded as the compound amino acid chelated zinc;

Step4、按照重量份计称取60份取甘氨酸浓缩母液、9份六水硝酸镁、8份中量元素、5份微量元素、18份Step2中的甘氨酸螯合钙、5份Step3中的复合氨基酸螯合锌和90份去离子水备用;Step4, take by weight 60 parts of concentrated glycine mother liquor, 9 parts of magnesium nitrate hexahydrate, 8 parts of medium elements, 5 parts of trace elements, 18 parts of glycine chelated calcium in Step2, 5 parts of compound amino acids in Step3 Chelated zinc and 90 parts of deionized water are standby;

Step5、将Step4中的甘氨酸浓缩母液与去离子水中的一半进行混合,搅拌均匀后加入上述重量份的甘氨酸螯合钙和复合氨基酸螯合锌,并进行再次搅拌,所得记作第一组分;Step5. Mix the glycine concentrated mother liquor in Step4 with half of the deionized water, stir evenly, add the above-mentioned glycine chelated calcium and compound amino acid chelated zinc, and stir again, and the obtained is recorded as the first component;

Step6、将Step4中的六水硝酸镁、中量元素、微量元素和余量的去离子水进行混合,搅拌均匀后所得记作第二组分;Step6, the magnesium nitrate hexahydrate in Step4, middle element, trace element and the deionized water of surplus are mixed, after stirring, the gained is recorded as the second component;

Step7、将第一组分和第二组分进行混合,搅拌均匀后过滤去除杂质,接着加热浓缩至原体积的一半,所得即为含Gly水溶肥料。Step7. Mix the first component and the second component, stir evenly, filter to remove impurities, then heat and concentrate to half of the original volume, and the obtained water-soluble fertilizer containing Gly.

甘氨酸浓缩母液的制备方法包括以下步骤:The preparation method of glycine concentrated mother liquor comprises the following steps:

步骤1、向反应器中倒入氯乙酸、甲醇和乌洛托品,搅拌溶解后缓慢通入液氨,在60℃的温度条件下进行合成反应2h,在反应的过程中维持反应体系的pH为8,其中,氯乙酸、甲醇和乌洛托品的摩尔比为1:7.5:0.2;Step 1. Pour chloroacetic acid, methanol and urotropine into the reactor, stir and dissolve, then slowly feed liquid ammonia, carry out the synthesis reaction at 60°C for 2 hours, and maintain the pH of the reaction system during the reaction is 8, wherein the molar ratio of chloroacetic acid, methanol and urotropine is 1:7.5:0.2;

步骤2、步骤1的反应结束后继续保温直至有晶体析出,接着冷却至室温并离心过滤,离心后得到母液和结晶物,使用少量甲醇对结晶物洗涤2次,将洗涤所得的洗液与上述母液进行混合,所得记作循环反应溶剂;Step 2, after the reaction of step 1, continue to keep warm until crystals are precipitated, then cool to room temperature and centrifugally filter, obtain mother liquor and crystals after centrifugation, use a small amount of methanol to wash the crystals twice, and wash the obtained lotion with the above-mentioned The mother liquor is mixed, and the gained is recorded as the circulating reaction solvent;

步骤3、将步骤2中的循环反应溶剂作为反应介质供下次循环反应使用,直到最后一次循环反应结束后得到母液和结晶物;Step 3, using the circulating reaction solvent in step 2 as the reaction medium for the next circulating reaction, until the last circulating reaction ends to obtain mother liquor and crystals;

步骤4、使用甲醇对步骤3中的结晶物进行洗涤2次,洗涤后的洗液与步骤3中的母液进行混合,混合后进行简单蒸馏,所得即为甘氨酸浓缩母液。Step 4, washing the crystals in step 3 twice with methanol, mixing the washed lotion with the mother liquor in step 3, and performing simple distillation after mixing to obtain concentrated glycine mother liquor.

步骤1中的搅拌速度为600r/min,步骤2中的离心转速为8000r/min。The stirring speed in step 1 is 600r/min, and the centrifugal speed in step 2 is 8000r/min.

步骤3中循环反应的次数为4次。The number of cycle reactions in step 3 is 4 times.

Step1的加热浓缩需要不断搅拌的情况下进行。The heating concentration of Step1 needs to be carried out under the condition of constant stirring.

Step2中去离子水的量为四水硝酸钙和精品甘氨酸总量的4倍。The amount of deionized water in Step2 is 4 times of the total amount of calcium nitrate tetrahydrate and high-quality glycine.

Step3中复合氨基酸的制备方法为:按照重量份计称取18份赖氨酸、2份谷氨酸、0.5份丙氨酸、0.05份缬氨酸和0.3份苯丙氨酸进行混合,混合均匀后即为复合氨基酸。The preparation method of the compound amino acid in Step3 is: weigh 18 parts of lysine, 2 parts of glutamic acid, 0.5 part of alanine, 0.05 part of valine and 0.3 part of phenylalanine in parts by weight and mix them evenly After that is the compound amino acid.

Step4中的中量元素为水合硅酸钠。The middle element in Step4 is hydrated sodium silicate.

Step4中的微量元素为硼酸和硫酸亚铁按同等重量比混合制得。Trace elements in Step4 are obtained by mixing boric acid and ferrous sulfate in equal weight ratios.

Step5和Step6中的搅拌速度为600r/min。The stirring speed in Step5 and Step6 is 600r/min.

实施例3:Example 3:

本实施例的一种含Gly水溶肥料生产的方法,方法包括以下步骤:A kind of method that contains Gly water-soluble fertilizer production of the present embodiment, the method comprises the following steps:

Step1、量取100重量份甘氨酸浓缩母液备用,接着使用等量的甲醇对甘氨酸浓缩母液进行稀释,稀释结束后过滤去掉杂质,将所得溶液加入至电渗析器的淡室料桶中,并向电渗析器的浓室料桶中加入蒸馏水,经电渗析分离后得到淡室溶液和浓室溶液,将淡室溶液在80℃的温度下加热浓缩,直至甘氨酸结晶析出,将结晶物通过过滤与母液分离,干燥后既得精品甘氨酸,结晶过滤后的母液可循环使用;Step1, measure 100 parts by weight of glycine concentrated mother liquor for later use, then use an equal amount of methanol to dilute the glycine concentrated mother liquor, filter to remove impurities after dilution, add the resulting solution to the dilute chamber material tank of the electrodialyzer, and send to the electrodialyzer Distilled water is added to the thick chamber barrel of the dialyzer, and the light chamber solution and the concentrated chamber solution are obtained after separation by electrodialysis. The light chamber solution is heated and concentrated at a temperature of 80°C until glycine crystals are precipitated, and the crystals are filtered and mixed with the mother liquor. After separation and drying, high-quality glycine is obtained, and the mother liquor after crystallization and filtration can be recycled;

Step2、按照2:3的摩尔比称取四水硝酸钙和Step1中的精品甘氨酸与去离子水进行混合,以400r/min的速度搅拌8min后制成混悬液,使用盐酸或氨水将混悬液pH调至5.5并将温度加热至50℃,然后将混悬液倒入高压流体纳米磨中进行处理,直至混悬液变清为止,对变清后的混悬液进行低温减压干燥,再用200目筛网过滤成细粉,所得记作甘氨酸螯合钙;Step2. Weigh calcium nitrate tetrahydrate and the high-quality glycine in Step1 and deionized water according to the molar ratio of 2:3 and mix them with deionized water. Stir at a speed of 400r/min for 8 minutes to make a suspension. Use hydrochloric acid or ammonia water to dissolve the suspension The pH of the solution is adjusted to 5.5 and the temperature is heated to 50°C, then the suspension is poured into a high-pressure fluid nanomill for processing until the suspension becomes clear, and the clear suspension is dried under reduced pressure at low temperature, Filter it into a fine powder with a 200-mesh sieve, and the gained is recorded as glycine chelated calcium;

Step3、称取一定量的复合氨基酸溶解于重量为其3倍的去离子水中,过滤去除不溶物后使用氢氧化钠溶液调节pH至5,接着加入重量为复合氨基酸25%的七水硫酸锌,在60℃的水浴温度中反应30min,反应后加热浓缩并进行冷却结晶,对结晶物进行过滤和干燥,所得记作复合氨基酸螯合锌;Step3, take a certain amount of compound amino acid and dissolve it in deionized water whose weight is 3 times, filter and remove insoluble matter, use sodium hydroxide solution to adjust the pH to 5, then add zinc sulfate heptahydrate whose weight is 25% of compound amino acid, React in a water bath temperature of 60°C for 30 minutes, heat and concentrate after the reaction, and carry out cooling and crystallization, filter and dry the crystals, and the obtained is recorded as the compound amino acid chelated zinc;

Step4、按照重量份计称取59份取甘氨酸浓缩母液、9份六水硝酸镁、7份中量元素、4份微量元素、16份Step2中的甘氨酸螯合钙、5份Step3中的复合氨基酸螯合锌和88份去离子水备用;Step4, take by weight 59 parts of glycine concentrated mother liquor, 9 parts of magnesium nitrate hexahydrate, 7 parts of medium elements, 4 parts of trace elements, 16 parts of glycine chelated calcium in Step2, 5 parts of compound amino acids in Step3 Chelated zinc and 88 parts of deionized water are standby;

Step5、将Step4中的甘氨酸浓缩母液与去离子水中的一半进行混合,搅拌均匀后加入上述重量份的甘氨酸螯合钙和复合氨基酸螯合锌,并进行再次搅拌,所得记作第一组分;Step5. Mix the glycine concentrated mother liquor in Step4 with half of the deionized water, stir evenly, add the above-mentioned glycine chelated calcium and compound amino acid chelated zinc, and stir again, and the obtained is recorded as the first component;

Step6、将Step4中的六水硝酸镁、中量元素、微量元素和余量的去离子水进行混合,搅拌均匀后所得记作第二组分;Step6, the magnesium nitrate hexahydrate in Step4, middle element, trace element and the deionized water of surplus are mixed, after stirring, the gained is recorded as the second component;

Step7、将第一组分和第二组分进行混合,搅拌均匀后过滤去除杂质,接着加热浓缩至原体积的一半,所得即为含Gly水溶肥料。Step7. Mix the first component and the second component, stir evenly, filter to remove impurities, then heat and concentrate to half of the original volume, and the obtained water-soluble fertilizer containing Gly.

甘氨酸浓缩母液的制备方法包括以下步骤:The preparation method of glycine concentrated mother liquor comprises the following steps:

步骤1、向反应器中倒入氯乙酸、甲醇和乌洛托品,搅拌溶解后缓慢通入液氨,在59℃的温度条件下进行合成反应2h,在反应的过程中维持反应体系的pH为8,其中,氯乙酸、甲醇和乌洛托品的摩尔比为1:7.5:0.2;Step 1. Pour chloroacetic acid, methanol and urotropine into the reactor, stir and dissolve, then slowly feed liquid ammonia, carry out the synthesis reaction at 59°C for 2 hours, and maintain the pH of the reaction system during the reaction is 8, wherein the molar ratio of chloroacetic acid, methanol and urotropine is 1:7.5:0.2;

步骤2、步骤1的反应结束后继续保温直至有晶体析出,接着冷却至室温并离心过滤,离心后得到母液和结晶物,使用少量甲醇对结晶物洗涤2次,将洗涤所得的洗液与上述母液进行混合,所得记作循环反应溶剂;Step 2, after the reaction of step 1, continue to keep warm until crystals are precipitated, then cool to room temperature and centrifugally filter, obtain mother liquor and crystals after centrifugation, use a small amount of methanol to wash the crystals twice, and wash the obtained lotion with the above-mentioned The mother liquor is mixed, and the gained is recorded as the circulating reaction solvent;

步骤3、将步骤2中的循环反应溶剂作为反应介质供下次循环反应使用,直到最后一次循环反应结束后得到母液和结晶物;Step 3, using the circulating reaction solvent in step 2 as the reaction medium for the next circulating reaction, until the last circulating reaction ends to obtain mother liquor and crystals;

步骤4、使用甲醇对步骤3中的结晶物进行洗涤2次,洗涤后的洗液与步骤3中的母液进行混合,混合后进行简单蒸馏,所得即为甘氨酸浓缩母液。Step 4, washing the crystals in step 3 twice with methanol, mixing the washed lotion with the mother liquor in step 3, and performing simple distillation after mixing to obtain concentrated glycine mother liquor.

步骤1中的搅拌速度为500r/min,步骤2中的离心转速为8000r/min。The stirring speed in step 1 is 500r/min, and the centrifugal speed in step 2 is 8000r/min.

步骤3中循环反应的次数为3次。The number of cycle reactions in step 3 is 3 times.

Step1的加热浓缩需要不断搅拌的情况下进行。The heating concentration of Step1 needs to be carried out under the condition of constant stirring.

Step2中去离子水的量为四水硝酸钙和精品甘氨酸总量的3倍。The amount of deionized water in Step2 is 3 times of the total amount of calcium nitrate tetrahydrate and high-quality glycine.

Step3中复合氨基酸的制备方法为:按照重量份计称取18份赖氨酸、1份谷氨酸、0.4份丙氨酸、0.04份缬氨酸和0.2份苯丙氨酸进行混合,混合均匀后即为复合氨基酸。The preparation method of the compound amino acid in Step3 is: weigh 18 parts of lysine, 1 part of glutamic acid, 0.4 part of alanine, 0.04 part of valine and 0.2 part of phenylalanine in parts by weight and mix them evenly After that is the compound amino acid.

Step4中的中量元素为水合硅酸钠。The middle element in Step4 is hydrated sodium silicate.

Step4中的微量元素为硼酸和硫酸亚铁按同等重量比混合制得。Trace elements in Step4 are obtained by mixing boric acid and ferrous sulfate in equal weight ratios.

Step5和Step6中的搅拌速度为700r/min。The stirring speed in Step5 and Step6 is 700r/min.

对比例:Comparative example:

于市面上随机抽取的一种含氨基酸水溶肥料。A water-soluble fertilizer containing amino acids randomly selected from the market.

性能检测performance testing

在实验田中随机划分4块3米×10米的试验田,并按照同样的种植方式种植同一品种的番茄,留取一块试验田不喷施肥料记作为空白组,其余四块分别喷施实施例1-3和对比例中的水溶肥料,并将其记作为实施例1、实施例2、实施例3和对比例,对不同试验田的番茄产量进行记录,记录数据如下表所示:Randomly divide 4 test fields of 3 meters × 10 meters in the test field, and plant tomatoes of the same variety according to the same planting method, keep a piece of test field without spraying fertilizer and record it as a blank group, and the remaining four blocks are sprayed with Example 1- 3 and the water-soluble fertilizer in the comparative example, and it is recorded as embodiment 1, embodiment 2, embodiment 3 and comparative example, the tomato output of different experimental fields is recorded, and the record data is shown in the following table:

试验田Test field 实施例1Example 1 实施例2Example 2 实施例3Example 3 对比例comparative example 空白组blank group 平均亩产量(公斤)Average yield per mu (kg) 45364536 43294329 45984598 27212721 18151815

通过上表的数据显示可知,试验田施例1-3的番茄亩产量明显高于对比例和空白组的亩产量,从而表示本发明实施例1-3生产的含Gly水溶肥料有助于提高农作物的产量;因此,本发明制得的含Gly水溶肥料具有更好的应用前景和市场推广价值。Shown by the data in the table above, it can be known that the yield per mu of tomato in Experimental Field Example 1-3 is significantly higher than that of comparative example and blank group, thereby showing that the Gly-containing water-soluble fertilizer produced by Embodiment 1-3 of the present invention helps to improve crops Therefore, the Gly-containing water-soluble fertilizer prepared by the present invention has better application prospects and market promotion value.

需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is a relationship between these entities or operations. There is no such actual relationship or order between them. Furthermore, the term "comprises", "comprises" or any other variation thereof is intended to cover a non-exclusive inclusion such that a process, method, article or apparatus comprising a set of elements includes not only those elements, but also includes elements not expressly listed. other elements of or also include elements inherent in such a process, method, article, or device. Without further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of additional identical elements in the process, method, article or apparatus comprising said element.

以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: it can still be described in the foregoing embodiments Modifications are made to the recorded technical solutions, or equivalent replacements are made to some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for producing a Gly-containing water-soluble fertilizer is characterized by comprising the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using methanol with the same amount, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a concentrated chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain a dilute chamber solution and a concentrated chamber solution, heating and concentrating the dilute chamber solution at the temperature of 70-100 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the crystallized and filtered mother liquor;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture for 5 to 10 minutes at the speed of 300 to 400r/min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the suspension to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension becomes clear, drying the clear suspension at a low temperature under reduced pressure, filtering the suspension into fine powder by using a 100 to 200-mesh screen, and obtaining the fine powder which is recorded as glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 2-3 times of the weight of the compound amino acid, filtering to remove insoluble substances, adjusting the pH to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight of 20-30% of the compound amino acid, reacting for 30min at the water bath temperature of 60 ℃, heating, concentrating, cooling, crystallizing, filtering and drying crystals to obtain the compound amino acid chelated zinc;
step4, weighing 58-60 parts by weight of concentrated glycine mother liquor, 8-9 parts by weight of magnesium nitrate hexahydrate, 5-8 parts by weight of medium elements, 3-5 parts by weight of trace elements, 15-18 parts by weight of calcium glycine chelate in Step2, 4-5 parts by weight of zinc amino acid complex chelate in Step3 and 85-90 parts by weight of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the glycine chelated calcium and the compound amino acid chelated zinc in parts by weight, and stirring again to obtain a first component;
step6, mixing magnesium nitrate hexahydrate, secondary elements, trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
2. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the method for preparing the mother solution of concentrated glycine comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 58-60 ℃, and maintaining the pH of a reaction system to be 7-8 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to obtain mother liquor and a crystal until the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
3. The method for producing the Gly-containing water-soluble fertilizer according to claim 2, wherein the stirring speed in the step1 is 500-600r/min, and the centrifugal rotation speed in the step2 is 7000-8000r/min.
4. The method for producing the Gly-containing water-soluble fertilizer according to claim 2, wherein the number of the circulating reactions in the step3 is 3-4.
5. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein Step1 is heated and concentrated under the condition of continuous stirring.
6. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the amount of the deionized water in Step2 is 3-4 times of the total amount of the calcium nitrate tetrahydrate and the refined glycine.
7. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the method for preparing the compound amino acid in Step3 comprises the following steps: weighing 17-18 parts of lysine, 1-2 parts of glutamic acid, 0.3-0.5 part of alanine, 0.03-0.05 part of valine and 0.1-0.3 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
8. The process for producing a Gly-containing water-soluble fertilizer according to claim 1, wherein the medium element in Step4 is sodium silicate hydrate.
9. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the trace element in Step4 is boric acid and ferrous sulfate which are mixed according to the same weight ratio.
10. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the stirring speed in Step5 and Step6 is 600-800r/min.
CN202211424128.1A 2022-11-15 2022-11-15 Method for producing Gly-containing water-soluble fertilizer Pending CN115594545A (en)

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