CN104310330A - Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct - Google Patents
Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct Download PDFInfo
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- CN104310330A CN104310330A CN201410477886.9A CN201410477886A CN104310330A CN 104310330 A CN104310330 A CN 104310330A CN 201410477886 A CN201410477886 A CN 201410477886A CN 104310330 A CN104310330 A CN 104310330A
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- dihydrogen phosphate
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 72
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title claims abstract description 38
- 235000019837 monoammonium phosphate Nutrition 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000006227 byproduct Substances 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 title abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 40
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000004202 carbamide Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000012452 mother liquor Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000000706 filtrate Substances 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims description 80
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 239000002002 slurry Substances 0.000 claims description 33
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 32
- 239000011777 magnesium Substances 0.000 claims description 32
- 229910052749 magnesium Inorganic materials 0.000 claims description 32
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims description 29
- 229910052700 potassium Inorganic materials 0.000 claims description 29
- 239000011591 potassium Substances 0.000 claims description 29
- DZHMRSPXDUUJER-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;dihydrogen phosphate Chemical compound NC(N)=O.OP(O)(O)=O DZHMRSPXDUUJER-UHFFFAOYSA-N 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 claims description 16
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 235000013619 trace mineral Nutrition 0.000 claims description 16
- 239000011573 trace mineral Substances 0.000 claims description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052698 phosphorus Inorganic materials 0.000 claims description 14
- 239000011574 phosphorus Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011575 calcium Substances 0.000 claims description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 12
- 229910052791 calcium Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000013522 chelant Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 241000675108 Citrus tangerina Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000003112 potassium compounds Chemical class 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Fertilizers (AREA)
Abstract
Description
技术领域 technical field
本发明涉及肥料技术领域，具体涉及一种制备磷酸二氢铵副产橘子树专用复合肥的方法。 The invention relates to the technical field of fertilizers, in particular to a method for preparing ammonium dihydrogen phosphate by-product special compound fertilizer for orange trees. the
背景技术 Background technique
橘子树为灌木至小乔木。分枝较多，枝扩展或略下垂，刺较少。单身复叶.翼叶通常狭窄，或仅有痕迹，叶片披针形。椭圆形或阔卵形，大小变异较大。顶端常有凹口，中脉由基部至凹口附近成叉状分枝，叶缘至少上半段通常有钝或圆裂齿，很少全缘。橘子树结出的果实叫橘子，橘子常与柑子一起被统称为柑橘，颜色鲜艳，酸甜可口，一般呈橘黄色，也有青色或其他颜色，是人们生活中最常见的水果之一，果皮可入药。而高品质的橘子离不开良好的肥料，橘子树吸收的主要营养元素是氮、磷、钾、硼、镁等，但普通肥料中氮磷钾的利用率很低，一般复合肥中氮利用率为20％-40％，磷只有20％左右，钾可达30％以上。由此可知，磷的当季利用率最低，氮、钾的利用率相当。普通肥料存在元素流失高，土壤环境污染大，成本高等问题，所以针对作物的不同，复合肥的专用性具有重要的意义。 Orange trees are shrubs to small trees. There are many branches, the branches are extended or slightly drooping, and the thorns are few. Single compound leaves. Wing leaves are usually narrow, or have only traces, and the leaves are lanceolate. Oval or broadly ovate, with large variations in size. Apex often notched, midrib branched from base to near notch, leaf margin usually has blunt or rounded teeth on at least the upper half, rarely entire. The fruit of the orange tree is called tangerine. Oranges are often collectively referred to as citrus together with tangerines. They are brightly colored, sweet and sour, generally orange in color, and also have blue or other colors. They are one of the most common fruits in people’s lives. The peel can be Used as medicine. And high-quality oranges are inseparable from good fertilizers. The main nutrients absorbed by orange trees are nitrogen, phosphorus, potassium, boron, magnesium, etc., but the utilization rate of nitrogen, phosphorus and potassium in ordinary fertilizers is very low. The rate is 20%-40%, phosphorus is only about 20%, and potassium can reach more than 30%. It can be seen that the utilization rate of phosphorus is the lowest in the current season, and the utilization rate of nitrogen and potassium is equal. Ordinary fertilizers have problems such as high element loss, large soil environmental pollution, and high cost. Therefore, the specificity of compound fertilizers is of great significance for different crops. the
目前针对农作物还有混合复合肥的制备技术，但是没有在相关专利文件和公开文献中发现针对农作物品种的不同通过对作物所需元素的研究，将元素进行搭配的化合态的复合肥的技术方案存在，也没有发现在制备磷酸二氢铵过程中副产橘子树专用复合肥的技术方案出现。 At present, there is also a preparation technology for compound fertilizers for crops, but no technical solutions for compound fertilizers in a compound state that match elements according to the research on the elements required by crops for different crop varieties have not been found in relevant patent documents and open literature Exist, also do not find the technical scheme that by-product special compound fertilizer for orange trees occurs in the process of preparing ammonium dihydrogen phosphate. the
因此，本发明人通过大量的研究和实践从橘子树所需元素搭配为 主，在提高磷酸制备磷酸二氢铵产品的纯度的同时针对作物对所需元素的吸收率调整整个生产工艺和参数副产出适用于橘子树的专用高效复合肥。 Therefore, the present inventor mainly adjusts the whole production process and parameter side effects to the absorption rate of required elements by crops while improving the purity of ammonium dihydrogen phosphate product prepared from orange tree through a large amount of research and practice. Produces a special high-efficiency compound fertilizer suitable for orange trees. the
发明内容 Contents of the invention
为解决上述技术问题，本发明提供了一种元素流失少、环境污染低、元素搭配合理、在提高磷酸二氢铵产品纯度的同时副产能使橘子树对元素进行充分的吸收的橘子树专用复合肥的制备方法。 In order to solve the above-mentioned technical problems, the present invention provides a special composite compound for orange trees, which has less element loss, low environmental pollution, reasonable element mix, and improves the purity of ammonium dihydrogen phosphate products while the secondary production capacity enables orange trees to fully absorb elements. Fertilizer preparation method. the
本发明是通过以下技术方案予以实现的： The present invention is achieved through the following technical solutions:
一种制备磷酸二氢铵副产橘子树专用复合肥的方法，该方法包括以下步骤： A method for preparing ammonium dihydrogen phosphate by-product orange tree special compound fertilizer, the method comprises the following steps:
a、原料制备：先将磷酸与尿素按摩尔比为2:1.3～1.7的比例混合，磷酸浓度为69～75％，按升温速度为5℃/min升至85-125℃，搅拌反应25min，制得料浆，分离得到磷酸脲； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.3-1.7, the concentration of phosphoric acid is 69-75%, rise to 85-125°C at a heating rate of 5°C/min, and stir for 25 minutes. Obtain slurry, separate and obtain urea phosphate;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.1～3.7并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value of 3.1 to 3.7 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer. Filter and separate to obtain ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液； c, filtrate element addition: add potassium element and the trace element compound required by orange tree to the filtrate obtained by separation to obtain the mother liquor of special compound fertilizer for orange tree;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥。 d, drying: the mother liquor is placed in a drier, the temperature is controlled at 35° C., after drying for 25 minutes, the water content is controlled to be 4% to obtain a special fertilizer for orange trees. the
所述步骤a中磷酸与尿素的反应为磷酸溶液与尿素固体的反应，磷酸与尿素按摩尔比为2:1.5的比例混合，磷酸的浓度为73％。 The reaction of phosphoric acid and urea in the step a is the reaction of phosphoric acid solution and urea solid, the molar ratio of phosphoric acid and urea is 2:1.5, and the concentration of phosphoric acid is 73%. the
所述步骤c中微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为 8.5％、钙元素为4.2％、镁元素为4.5％。 In the step c, the trace element compound is a chelate of calcium and magnesium, and the content of nitrogen in the mother liquor of the special compound fertilizer for orange trees is 15.6%, phosphorus pentoxide is 7.6%, potassium is 8.5%, and calcium is 4.2%, magnesium is 4.5%. the
所述步骤d中橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 In the step d, the nitrogen element content of the special compound fertilizer for orange trees is 15.3%, the calcium element content is 3.9%, the magnesium element content is 4.2%, the phosphorus pentoxide content is 7.3%, and the potassium element content is 8.2%. . the
所述步骤d中橘子树专用复合肥为化合态复混肥。 The special compound fertilizer for orange trees in the step d is a compound fertilizer in a chemical state. the
所述步骤d中橘子树专用复合肥其成分中含有以下氮磷钾化合态 In the step d, the special compound fertilizer for orange trees contains the following nitrogen, phosphorus and potassium compound state in its composition
结构式： Structural formula:
其中，碳原子与氧原子之间的虚线表示C原子与O原子之间存在配位键。 Wherein, the dotted line between the carbon atom and the oxygen atom indicates that there is a coordination bond between the C atom and the O atom.
本发明的有益效果在于：通过磷酸与尿素反应制备出高纯度的磷酸二氢铵的同时剩下的料浆还可以通过元素添加，干燥等工艺制备成橘子树所需的专用复合肥，母液得到了充分的利用，降低了成本，针对橘子树所需的元素含量及橘子树对元素的吸收率的研究和分析，制备出来的化合态复合肥在最大程度上的符合橘子树的要求，减少了元素的浪费，避免了复合肥的残留引起的土壤污染问题。 The beneficial effects of the present invention are that: while the high-purity ammonium dihydrogen phosphate is prepared by the reaction of phosphoric acid and urea, the remaining slurry can also be prepared into the special compound fertilizer required by orange trees through processes such as element addition and drying, and the mother liquor can be obtained In order to make full use of it and reduce the cost, according to the research and analysis of the element content required by the orange tree and the absorption rate of the element by the orange tree, the prepared compound fertilizer meets the requirements of the orange tree to the greatest extent, reducing the The waste of elements avoids the soil pollution problem caused by the residue of compound fertilizer. the
具体实施方式 Detailed ways
以下结合实施例对本发明的技术方案作进一步描述，但要求保护的范围并不局限于所述。 The technical solution of the present invention will be further described below in conjunction with the examples, but the scope of protection is not limited to the description. the
反应原理说明： Description of the reaction principle:
首先通过对磷酸与尿素反应参数的调整，制备出磷酸脲，磷酸脲能够继续与磷酸发生反应形成H2NCONH3 +和H2PO4 -，H2NCONH3 +在 含有磷酸的环境下，在温度为85～120℃时形成中间离子和磷酸二氢根，加入过量的铵根离子后，磷酸二氢根与铵根离子反应生成磷酸二氢铵析出，加入钾离子后和中间离子中的铵根离子反应形成然后加入钙元素和镁元素的螯合物，形成化合态复合肥，经过干燥处理后即得到橘子树专用复合肥。上述反应原理的反应方程式如下： First, by adjusting the reaction parameters of phosphoric acid and urea, urea phosphate was prepared . Urea phosphate can continue to react with phosphoric acid to form H 2 NCONH 3 + and H 2 PO 4 - . Formed at a temperature of 85-120°C Intermediate ion and dihydrogen phosphate, after adding excess ammonium ion, dihydrogen phosphate reacts with ammonium ion to form ammonium dihydrogen phosphate, which is precipitated, and reacts with ammonium ion in the intermediate ion after adding potassium ion to form Then add calcium and magnesium chelates to form a compound fertilizer, which is then dried to obtain a special compound fertilizer for orange trees. The reaction equation of above-mentioned reaction principle is as follows:
化学反应方程式一： Chemical reaction equation one:
H2PO3+CO(NH2)2—CO(NH2)2·H3PO4 H 2 PO 3 +CO(NH 2 ) 2 —CO(NH 2 ) 2 ·H 3 PO 4
化学反应方程式二： Chemical reaction equation two:
CO(NH2)2·H3PO4—H2NCONH3 ++H2PO4 - CO(NH 2 ) 2 ·H 3 PO 4 —H 2 NCONH 3 + +H 2 PO 4 -
化学反应方程式三： Chemical reaction equation three:
H2PO4 -+NH4 +—NH4H2PO4 H 2 PO 4 - +NH 4 + —NH 4 H 2 PO 4
化学反应方程式四： Chemical reaction equation four:
化学反应方程式五： Chemical reaction equation five:
下面结合具体实施例对本发明做进一步的阐述。 The present invention will be further elaborated below in conjunction with specific embodiments. the
实施例一 Embodiment one
a、原料制备：先将磷酸与尿素按摩尔比为2:1.3的比例混合，磷酸浓度为69％，按升温速度为5℃/min升至85℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.3, the concentration of phosphoric acid is 69%, rise to 85°C at a heating rate of 5°C/min, stir and react for 25min, and prepare a slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制 PH值为3.1并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.1 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: mother liquor is placed in drier, temperature is controlled at 35 ℃, after drying 25min, control moisture content to be 4% and obtain orange tree special fertilizer, the nitrogen element content of the orange tree special compound fertilizer is 15.3%, calcium element content The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
实施例二 Example two
a、原料制备：先将磷酸与尿素按摩尔比为2:1.4的比例混合，磷酸浓度为70％，按升温速度为5℃/min升至90℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.4, the concentration of phosphoric acid is 70%, rise to 90°C at a heating rate of 5°C/min, stir and react for 25min, and prepare a slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.2并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.2 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min 后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: the mother liquor is placed in a drier, the temperature is controlled at 35 ° C, and after drying for 25 minutes, the water content is controlled to be 4% to obtain a special fertilizer for orange trees. The nitrogen content of the special compound fertilizer for orange trees is 15.3%, and the content of calcium elements The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
实施例三 Embodiment three
a、原料制备：先将磷酸与尿素按摩尔比为2:1.5的比例混合，磷酸浓度为71％，按升温速度为5℃/min升至95℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.5, the concentration of phosphoric acid is 71%, rise to 95°C at a heating rate of 5°C/min, stir and react for 25min to prepare a slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.3并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.3 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: mother liquor is placed in drier, temperature is controlled at 35 ℃, after drying 25min, control moisture content to be 4% and obtain orange tree special fertilizer, the nitrogen element content of the orange tree special compound fertilizer is 15.3%, calcium element content The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
实施例四 Embodiment four
a、原料制备：先将磷酸与尿素按摩尔比为2:1.6的比例混合，磷酸浓度为72％，按升温速度为5℃/min升至100℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.6, the concentration of phosphoric acid is 72%, rise to 100°C at a heating rate of 5°C/min, stir and react for 25min to obtain a slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.4并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.4 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: mother liquor is placed in drier, temperature is controlled at 35 ℃, after drying 25min, control moisture content to be 4% and obtain orange tree special fertilizer, the nitrogen element content of the orange tree special compound fertilizer is 15.3%, calcium element content The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
实施例五 Embodiment five
a、原料制备：先将磷酸与尿素按摩尔比为2:1.6的比例混合，磷酸浓度为70％，按升温速度为5℃/min升至105℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.6, the concentration of phosphoric acid is 70%, rise to 105°C at a heating rate of 5°C/min, stir and react for 25min, and prepare a slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.6并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.6 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: mother liquor is placed in drier, temperature is controlled at 35 ℃, after drying 25min, control moisture content to be 4% and obtain orange tree special fertilizer, the nitrogen element content of the orange tree special compound fertilizer is 15.3%, calcium element content The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
实施例六 Embodiment six
a、原料制备：先将磷酸与尿素按摩尔比为2:1.7的比例混合，磷酸浓度为75％，按升温速度为5℃/min升至125℃，搅拌反应25min，制得料浆，分离得到磷酸脲，磷酸与尿素的反应为磷酸溶液与尿素固体的反应； a. Raw material preparation: first mix phosphoric acid and urea in a molar ratio of 2:1.7, the concentration of phosphoric acid is 75%, rise to 125°C at a heating rate of 5°C/min, stir and react for 25min, and prepare slurry, separate Obtain urea phosphate, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
b、制备磷酸二氢铵：往含有磷酸脲的料浆中缓慢加入氨水控制PH值为3.7并充分搅拌得到含有氮、磷的料浆，料浆经冷却结晶机中降温至25℃、过滤、分离得到磷酸二氢铵； b. Preparation of ammonium dihydrogen phosphate: Slowly add ammonia water to the slurry containing urea phosphate to control the pH value to 3.7 and fully stir to obtain a slurry containing nitrogen and phosphorus. The slurry is cooled to 25°C in a cooling crystallizer, filtered, Separation obtains ammonium dihydrogen phosphate;
c、滤液元素添加：往分离得到的滤液中加入钾元素及橘子树所需的微量元素化合物得到橘子树专用复合肥的母液，微量元素化合物为钙、镁的螯合物，橘子树专用复合肥的母液中氮元素的含量为15.6％、五氧化二磷为7.6％、钾元素为8.5％、钙元素为4.2％、镁元素为4.5％； c, filtrate element addition: in the filtrate obtained by separation, add potassium element and the required trace element compound of orange tree to obtain the mother liquor of the special compound fertilizer for orange tree, the trace element compound is the chelate compound of calcium and magnesium, and the special compound fertilizer for orange tree The content of nitrogen element in the mother liquor is 15.6%, phosphorus pentoxide is 7.6%, potassium element is 8.5%, calcium element is 4.2%, magnesium element is 4.5%;
d、干燥：将母液置于干燥机中，温度控制在35℃，干燥25min后，控制含水量为4％得到橘子树专用肥，橘子树专用复合肥的氮元素含量为15.3％、钙元素含量为3.9％、镁元素的含量为4.2％、五氧化二磷的含量为7.3％、钾元素的含量为8.2％。 d, drying: mother liquor is placed in drier, temperature is controlled at 35 ℃, after drying 25min, control moisture content to be 4% and obtain orange tree special fertilizer, the nitrogen element content of the orange tree special compound fertilizer is 15.3%, calcium element content The content of magnesium element is 3.9%, the content of magnesium element is 4.2%, the content of phosphorus pentoxide is 7.3%, and the content of potassium element is 8.2%. the
下面结合具体实验例对本发明的产品和技术效果作进一步的说明。 The products and technical effects of the present invention will be further described below in conjunction with specific experimental examples. the
实验例一 Experimental example one
本发明实施例一、实施例二、实施例三、实施例四、实施例五、实施例六中制备出的磷酸二氢铵产品按GB25569—2010的标准进行检测， The ammonium dihydrogen phosphate product prepared in the embodiment of the present invention one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six is detected by the standard of GB25569-2010,
检测结果如表1所示： The test results are shown in Table 1:
表1 Table 1
本发明磷酸二氢铵产品纯度检测 The purity detection of ammonium dihydrogen phosphate product of the present invention
由表1中可以看出，本发明的技术方案生产出来的磷酸二氢铵不仅达到了合格标准，而且产品的纯度也较高，说明本方法制备磷酸二氢铵产品具有显著的进步。 As can be seen from Table 1, the ammonium dihydrogen phosphate produced by the technical solution of the present invention has not only reached the qualified standard, but also has a higher purity of the product, which shows that the method has significantly improved the ammonium dihydrogen phosphate product. the
实验例二 Experimental example two
根据橘子树对元素含量的吸收和橘子树的生长情况，对橘子树专用复合肥与普通复合肥作对比试验。以9棵橘子树为试验对象，分别标号为A、B、C、D、E、F、G、H、I、对A、B、C三个标号的橘子树施用普通肥料，对D、E、F、G、H、I等六个标号的橘子树分别施用实施例一、实施例二、实施例三、实施例四、实施例五、实施例六中所制备出的橘子树专用肥，对比实验结果如表2所示： According to the absorption of the element content by the orange tree and the growth of the orange tree, the special compound fertilizer for the orange tree and the common compound fertilizer are tested in comparison. Take 9 orange trees as test objects, respectively marked as A, B, C, D, E, F, G, H, I, apply common fertilizer to the orange trees with three labels of A, B, and C, and apply common fertilizer to the orange trees with three labels, D, E , F, G, H, I and other six signs of orange trees are applied respectively in embodiment one, embodiment two, embodiment three, embodiment four, embodiment five, the prepared orange tree special fertilizer in embodiment six, The results of the comparative experiments are shown in Table 2:
表2施用普通复合肥与橘子树专用复合肥对橘子树元素吸收率的对比及对橘子树生长的影响 Table 2 The comparison of the application of ordinary compound fertilizer and the special compound fertilizer for orange trees on the absorption rate of orange trees and the effect on the growth of orange trees
由上表可以看出本发明制备的橘子树专用复合肥能够被橘子树充分的吸收，并且还富含Ca、Me等橘子树所需的营养元素，对橘子树的正常生长提供了保障，改善了橘子树的长势，增加了橘子的产量，从而提高了经济效益。 As can be seen from the above table, the special compound fertilizer for orange trees prepared by the present invention can be fully absorbed by orange trees, and is also rich in nutrients required for orange trees such as Ca and Me, which guarantees the normal growth of orange trees and improves Improve the growth of orange trees, increase the output of oranges, thereby improving economic benefits. the
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| CN108046226A (en) * | 2017-12-22 | 2018-05-18 | 贵阳开磷化肥有限公司 | A kind of production method of PHOSPHORIC ACID TECH.GRADE dihydro coproducing ammonium Water soluble fertilizer |
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| WO2000055104A1 (en) * | 1999-03-18 | 2000-09-21 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
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| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
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| GB1191635A (en) * | 1966-07-27 | 1970-05-13 | Marchon Products Ltd | Improvements in the manufacture of Orthophosphates |
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| WO2000055104A1 (en) * | 1999-03-18 | 2000-09-21 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
| CN1583681A (en) * | 2004-05-24 | 2005-02-23 | 陈天骏 | Agricultural composite manure and preparing method thereof |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
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