CN1305946A - Process for preparing feed-class calcium dihydrogen phosphate and high-phosphorus products - Google Patents
Process for preparing feed-class calcium dihydrogen phosphate and high-phosphorus products Download PDFInfo
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- CN1305946A CN1305946A CN 01107205 CN01107205A CN1305946A CN 1305946 A CN1305946 A CN 1305946A CN 01107205 CN01107205 CN 01107205 CN 01107205 A CN01107205 A CN 01107205A CN 1305946 A CN1305946 A CN 1305946A
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Abstract
A process for preparing feed-class calcium dihydrogen phosphate and high-P products includes decomposing phosphorus ore with sulfuric acid, filter, neutralizing with calcium carbonate, separating out impurities, neutralizing with calcium hydroxide, separating to obtain solution of calcium dihydrogen phosphate, concentrating, adding calcium and drying. Its advantages are low content of impurities, high water solubility and simple preparing process.
Description
The present invention belongs to a method for producing feed-grade dihydrogen phosphate or high-phosphorus product with low impurity by using wet-process phosphoric acid and limestone as raw material.
The existing production method of feed-grade dihydrogen phosphate mainly adopts two methods of thermal phosphoric acid purification and wet phosphoric acid purification. The method for taking thermal phosphoric acid as a raw material comprises the following steps: 1. a one-step no-return method (such as Chinese patent application No. 93110806.3) for generating calcium dihydrogen phosphate by reacting hot phosphoric acid with limestone (or lime); 2. fluidized phosphoric acid spraying one-step method (such as Chinese patent application No. 98112087.3) using hot phosphoric acid and lime or limestone powder as raw materials; 3. the production method of calcium hydrophosphate with high effective phosphorus, which is characterized in that lime powder and powdery calcium phosphate or calcium hydrophosphate or the mixture of the lime powder and the powdery calcium phosphate or the calcium hydrophosphate are uniformly mixed and then are strongly stirred and mixed with phosphoric acid to react to generate calcium dihydrogen phosphate (for example, the Chinese patent application number is 97111341.6); 4. the method for producing calcium dihydrogen phosphate by the reaction of hot phosphoric acid and calcium hydrogen phosphate (for example, Chinese patent application No. 96116482.4) is adopted. The wet phosphoric acid is used as raw material to remove arsenic, lead, fluorine and other impurities in the wet phosphoric acid by adopting a wet phosphoric acid purification process to obtain 30-60% of purified phosphoric acid, and then the purified phosphoric acid is used for producing feed-grade monocalcium phosphate (such as Chinese patent application No. 96100337.5).
By combining the methods, the production method taking the hot-process phosphoric acid as the raw material adopts the hot-process phosphoric acid with high price, although the feed-grade monocalcium phosphate with low impurity content can be obtained, the product cost is high, the arsenic and lead contents in the raw material hot-process phosphoric acid are generally high, and the phosphoric acid with low arsenic and lead contents needs to be selected or the phosphoric acid is subjected to dearsenification and lead treatment to reach the feed grade; the method for producing feed-grade monocalcium phosphate by adopting a wet-process phosphoric acid purification process is difficult to stably produce purified phosphoric acid according to the currently mastered data, cannot ensure the product quality, has high impurities and low water solubility in the product, and is difficult to achieve the best animal feeding effect.
The high-phosphorus product is a calcium phosphate salt product with the phosphorus content of 19-22%, contains calcium dihydrogen phosphate and calcium hydrogen phosphate, is characterized by containing water-soluble phosphorus higher than calcium hydrogen phosphate, and is suitable for being mixed with animal feeds of different types and different ages.
The invention aims to provide a production method for producing feed-grade calcium dihydrogen phosphate or high-phosphorus products by using wet-process phosphoric acid as a raw material, which has stable process and low impurity content of the products and can make up for the defects in the prior art.
The purpose of the invention is realized as follows: decomposing phosphorite with sulfuric acid, filtering, neutralizing phosphoric acid with calcium carbonate, separating to obtain impurities, neutralizing filtrate with calcium hydroxide, separating to obtain calcium dihydrogen phosphate solution, concentrating, adding calcium, and drying, or directly adding calcium and drying to obtain calcium dihydrogen phosphate or high-phosphorus product.
Wherein: the main process steps of the invention are characterized in that:
A. decomposing and filtering phosphorite by sulfuric acid
The extraction reaction temperature is 70-95 ℃, the optimal temperature is 85 ℃, the extraction reaction time is 2-8 hours, and the optimal extraction reaction time is 4 hours.
B. Neutralizing and separating impurities with calcium carbonate for filtering phosphoric acid
With CaCO3Reacting with wet-process phosphoric acid, and removing most impurities in the wet-process phosphoric acid through solid-liquid separation to obtain a solution containing phosphoric acid and calcium dihydrogen phosphate, wherein the main chemical reaction is as follows:
the extracted phosphoric acid is 10-30% phosphoric acid. Preferably 15-20%.
C. Neutralizing the filtrate with calcium hydroxide, and separating to obtain calcium dihydrogen phosphate solution
Mixing the solution of phosphoric acid and calcium dihydrogen phosphate obtained in the previous step with Ca (OH)2Neutralizing the solution to the end point, separating and removing impurities to obtain the calcium dihydrogen phosphate solution meeting the feed-grade requirement, wherein the main chemical reaction comprises the following steps:
D. concentrating calcium dihydrogen phosphate solution, adding calcium, and drying, or directly adding calcium and drying to obtain calcium dihydrogen phosphate or high-phosphorus product
Wherein: the calcium is added with a certain amount of calcium hydrophosphate and calcium oxide.
The drying method comprises centrifugal spray drying and pressure spray drying.
The high-phosphorus product refers to a calcium phosphate product with the phosphorus content of 19-22%.
The product of the invention has stable quality, low impurity content, high water solubility and simple process, and is characterized by containing water-soluble phosphorus higher than calcium hydrophosphate and being suitable for being mixed with animal feeds of different types and ages.
The following figures of the invention are given
FIG. 1 is a process flow diagram of the present invention
The invention is further illustrated by the following figures and examples.
Example 1:with 1kg (32% P)2O5、46％CaO) ground phosphate rock, 98% sulfuric acid 0.85kg, water 0.4kg, and acid returning 8% (P)2O5)2.25kg, extracted at 85 ℃ for 4 hours, separated reaction slurry, and filtered phosphoric acid 15.5% (P)2O5)2kg of the filtrate was neutralized with 170g of calcium carbonate for 30 minutes under stirring, the residue was separated and removed, and 14.4% (P) of the filtrate was obtained2O5) Neutralizing 1.67kg with 8% lime milk 200g, and separating to obtain 12% (P)2O5)1.8kg, concentrating the filtrate to 0.76kg, adding 98g feed grade calcium hydrophosphate, and drying the slurry by a spray drying tower to obtain a feed grade calcium biphosphate product.
Example 2: with 1kg (32% P)2O546 percent of CaO), 0.85kg of 98 percent of sulfuric acid, 0.4kg of water and 8 percent of acid returning (P)2O5)2.25kg, extracted at 85 ℃ for 4 hours, separated reaction slurry, and filtered phosphoric acid 15.5% (P)2O5)2kg of the filtrate was neutralized with 170g of calcium carbonate for 30 minutes under stirring, the residue was separated and removed, and 14.5% (P) of the filtrate was obtained2O5) Neutralizing 1.67kg with 8% lime milk 200g, and separating to obtain 12% (P)2O5)1.8kg, concentrating the filtrate to 0.76kg, adding 14.3g of lime powder, and drying the slurry by a spray drying tower to obtain a feed-grade calcium dihydrogen phosphate product.
Example 3: with 1kg (32% P)2O546 percent of CaO), 0.85kg of 98 percent of sulfuric acid, 0.4kg of water and 8 percent of acid returning (P)2O5)2.25kg, extracted at 85 ℃ for 4 hours, separated reaction slurry, and filtered phosphoric acid 15.5% (P)2O5)2kg of the filtrate was neutralized with 170g of calcium carbonate for 30 minutes under stirring, the residue was separated and removed, and 14.5% (P) of the filtrate was obtained2O5) Neutralizing 1.67kg with 8% lime milk 200g, and separating to obtain 12% (P)2O5)1.8kg, concentrating the filtrate to 0.76kg, adding 245g feed grade calcium hydrogen phosphate, and drying the slurry with spray drying tower to obtain feed grade high phosphorus product (21% P).
Example 4: with 1kg (32% P)2O546 percent of CaO), 0.85kg of 98 percent of sulfuric acid, 0.4kg of water and 8 percent of acid returning (P)2O5)2.25kg, extracted at 85 ℃ for 4 hours, separated reaction slurry, and filtered phosphoric acid 15.5% (P)2O5)2kg of the filtrate was neutralized with 170g of calcium carbonate for 30 minutes under stirring, the residue was separated and removed, and 14.5% (P) of the filtrate was obtained2O5) Neutralizing 1.67kg with 8% lime milk 200g, and separating to obtain 12% (P)2O5)1.8kg, concentrating the filtrate to 0.76kg, adding 29g of lime powder, and drying the slurry by a spray drying tower to obtain a feed grade high phosphorus product (21% P).
The product of the invention has stable quality, low impurity content, high water solubility and simple process, and is characterizedby containing water-soluble phosphorus higher than calcium hydrophosphate and being suitable for being mixed with animal feeds of different types and ages.
Claims (9)
1. A method of producing a feed grade monocalcium phosphate or high phosphorus product, comprising: decomposing phosphorite with sulfuric acid, filtering, neutralizing phosphoric acid with calcium carbonate, separating to obtain impurities, neutralizing filtrate with calcium hydroxide, separating to obtain calcium dihydrogen phosphate solution, concentrating, adding calcium, and drying, or directly adding calcium and drying to obtain calcium dihydrogen phosphate or high-phosphorus product.
2. The method of claim 1, wherein the feed grade monocalcium phosphate or high phosphorus product comprises: the extracted phosphoric acid is 10-30% phosphoric acid.
3. The method of claim 1, wherein the feed grade monocalcium phosphate or high phosphorus product comprises: the calcium is added with a certain amount of calcium hydrophosphate and calcium oxide.
4. The method of claim 1, wherein the feed grade monocalcium phosphate or high phosphorus product comprises: the drying method comprises centrifugal spray drying and pressure spray drying.
5. The method of claim 1, wherein the feed grade monocalcium phosphate or high phosphorus product comprises: the high-phosphorus product refers to a calcium phosphate product with the phosphorus content of 19-22%.
6. A method of producing a feed grade monocalcium phosphate or high phosphorusproduct according to claim 1 or 2, characterized in that: the extracted phosphoric acid is 15-20% phosphoric acid.
7. The method of claim 1, wherein the feed grade monocalcium phosphate or high phosphorus product comprises: in the process of decomposing and filtering phosphorite by sulfuric acid, the extraction reaction temperature is 70-95 ℃, and the extraction reaction time is 2-8 hours.
8. A method of producing a feed grade monocalcium phosphate or high phosphorus product according to claim 1 or 7, wherein: in the process of decomposing and filtering phosphorite by sulfuric acid, the optimum temperature of the extraction reaction is 85 ℃.
9. A method of producing a feed grade monocalcium phosphate or high phosphorus product according to claim 1 or 7, wherein: in the sulfuric acid decomposition and filtration of the phosphorite, the optimal extraction reaction time is 4 hours.
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| CN 01107205 CN1305946A (en) | 2001-03-28 | 2001-03-28 | Process for preparing feed-class calcium dihydrogen phosphate and high-phosphorus products |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643204B (en) * | 2008-08-05 | 2011-07-20 | 北京紫光英力化工技术有限公司 | Novel process for cleanly producing phosphate ammoniate fertilizer in the processing of phosphate rock powder |
| CN103864042A (en) * | 2014-02-28 | 2014-06-18 | 昆明川金诺化工股份有限公司 | Method for lowering free acid of feed grade monocalcium phosphate |
| CN105417516A (en) * | 2015-12-18 | 2016-03-23 | 瓮福（集团）有限责任公司 | Production method for feed-grade monocalcium phosphate |
| CN105921259A (en) * | 2016-05-09 | 2016-09-07 | 贵州省冶金化工研究所 | Method for producing feed grade monocalcium phosphate through medium and low grade mixed phosphate ore |
| CN106853962A (en) * | 2016-12-18 | 2017-06-16 | 贵州越都化工有限公司 | A kind of feed-level calcium biphosphate and preparation method thereof |
| WO2017151015A1 (en) | 2016-03-03 | 2017-09-08 | Mineral And Chemical Company Eurochem, Joint Stock Company | Phosphorus-potassium-nitrogen-containing npk-fertilizer and method for the preparation of granulated phosphorus-potassium-nitrogen-containing npk-fertilizer |
| WO2017151017A1 (en) | 2016-03-03 | 2017-09-08 | Mineral And Chemical Company Eurochem, Joint Stock Company | Phosphorus-potassium-nitrogen-containing npk-fertilizer and a method for the preparation of granulated phosphorus-potassium-nitrogen-containing npk-fertilizer |
| CN108455545A (en) * | 2018-02-01 | 2018-08-28 | 连云港西都生化有限公司 | A kind of preparation method of calcium dihydrogen phosphate |
| CN108751154A (en) * | 2018-06-04 | 2018-11-06 | 中化化肥有限公司成都研发中心 | The preparation method of calcium dihydrogen phosphate |
-
2001
- 2001-03-28 CN CN 01107205 patent/CN1305946A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643204B (en) * | 2008-08-05 | 2011-07-20 | 北京紫光英力化工技术有限公司 | Novel process for cleanly producing phosphate ammoniate fertilizer in the processing of phosphate rock powder |
| CN103864042A (en) * | 2014-02-28 | 2014-06-18 | 昆明川金诺化工股份有限公司 | Method for lowering free acid of feed grade monocalcium phosphate |
| CN105417516A (en) * | 2015-12-18 | 2016-03-23 | 瓮福（集团）有限责任公司 | Production method for feed-grade monocalcium phosphate |
| WO2017151015A1 (en) | 2016-03-03 | 2017-09-08 | Mineral And Chemical Company Eurochem, Joint Stock Company | Phosphorus-potassium-nitrogen-containing npk-fertilizer and method for the preparation of granulated phosphorus-potassium-nitrogen-containing npk-fertilizer |
| WO2017151017A1 (en) | 2016-03-03 | 2017-09-08 | Mineral And Chemical Company Eurochem, Joint Stock Company | Phosphorus-potassium-nitrogen-containing npk-fertilizer and a method for the preparation of granulated phosphorus-potassium-nitrogen-containing npk-fertilizer |
| CN105921259A (en) * | 2016-05-09 | 2016-09-07 | 贵州省冶金化工研究所 | Method for producing feed grade monocalcium phosphate through medium and low grade mixed phosphate ore |
| CN105921259B (en) * | 2016-05-09 | 2018-07-31 | 贵州省冶金化工研究所 | The method for producing feed-level calcium biphosphate using middle-low grade mixing rock phosphate in powder |
| CN106853962A (en) * | 2016-12-18 | 2017-06-16 | 贵州越都化工有限公司 | A kind of feed-level calcium biphosphate and preparation method thereof |
| CN108455545A (en) * | 2018-02-01 | 2018-08-28 | 连云港西都生化有限公司 | A kind of preparation method of calcium dihydrogen phosphate |
| CN108455545B (en) * | 2018-02-01 | 2021-09-10 | 连云港西都食品配料有限公司 | Preparation method of monocalcium phosphate |
| CN108751154A (en) * | 2018-06-04 | 2018-11-06 | 中化化肥有限公司成都研发中心 | The preparation method of calcium dihydrogen phosphate |
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