CN1239705A - Wet phosphoric acid producing process - Google Patents

Wet phosphoric acid producing process Download PDF

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Publication number
CN1239705A
CN1239705A CN 98112089 CN98112089A CN1239705A CN 1239705 A CN1239705 A CN 1239705A CN 98112089 CN98112089 CN 98112089 CN 98112089 A CN98112089 A CN 98112089A CN 1239705 A CN1239705 A CN 1239705A
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phosphoric acid
extraction
reaction
tank
sif
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吴昭强
余祥鑫
曾德仁
高新成
林顺芝
许辰寿
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PHOSPHOROUS CALCIUM FERTILIZER PLANT WEIYUAN COUNTY
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PHOSPHOROUS CALCIUM FERTILIZER PLANT WEIYUAN COUNTY
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Priority to CN 98112089 priority Critical patent/CN1239705A/en
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Abstract

The wet phosphoric acid producing process includes steps, i. e., the continuous reaction step of pre-mixing to reduce acid and remove inpurity, total mixing, extration and crystallizing, the enclosed waste water circulation; and the production of Na2SiF6. The process has low power and acid consumption, high yield and high efficiency.

Description

Novel method for producing phosphoric acid by wet process
The invention relates to the technical field of phosphoric acid production, in particular to a novel method for producing phosphoric acid by a wet process.
The phosphoric acid process matched with the process for annual production of thirty thousand tons of ammonium phosphate and thirty thousand tons of feed grade calcium hydrophosphate in China has high energy consumption, and the power consumption reaches 210-2O5Sulfuric acid consumption 3.0-3.2 ton/TP2O5Water consumption of 30-50m3The phosphorus yield is only 91-92%, and the final production cost is high.
The invention aims to overcome the defects and provide a novel wet-process phosphoric acid production method which is low in power consumption, water consumption, sulfuric acid consumption, phosphorus yield and final production cost.
The purpose of the invention is realized as follows: the method comprises the following process steps: A. premixing, deacidifying and removing impurities; B. total mixing, extracting and growing crystalContinuing the reaction; C. closed circulation of system sewage and waste water and production of Na2SiF6
A. Pre-mixing, deacidifying and removing impurities: the working principle of the process is as follows:
……①
Figure A9811208900041
……③
……④
the working procedure can lead CaO in phosphorite to enter finished phosphoric acid product, and lead CaO in the ore to be reduced, thereby saving sulfuric acid consumption in the extraction process, and 5 percent of H in the phosphoric acid2SO4At ②, ③,④ reaction process, the H in the finished phosphoric acid product is made2SO4The consumption of sulfuric acid is reduced, and gypsum which is not beneficial to decomposition in phosphorite is crystallized and removed, so that the phosphorite is purified, and the method plays an extremely important role in easily reacting and generating thick and uniform crystals in the extraction and crystal growing process of ores.
And (3) process control: the temperature of the premixing tank is 60-70 ℃, the liquid-solid ratio is 5-8: 1, the retention time is 1 hour, and the settling time is 1 hour.
B. Total mixing, extraction and crystal growing continuous reaction: the working principle of the process is as follows:
……⑤
……⑦
the total mixing tank is reaction ⑤, namely, the dilute phosphoric acid reacts with the mineral powder to generate CaH2(PO4)2Avoiding the ore powder and H2SO4The direct contact forms the color failure, and the extraction rate is improved by 1 percent.
The extraction is reaction ⑥, and the crystal growth is reaction ⑦;
the total mixing tank not only plays a role of a reactor, but also takes away heat in advance, the diluted phosphoric acid reacts with the mineral powder and then enters the extraction tank, meanwhile, sulfuric acid is added for full reaction, and the diluted phosphoric acid is continuously precipitated to the crystal growing tank and is continuously filtered in the crystal growing tank; the retention time of slurry in the whole process is 2 and a half hours, the retention time is reduced by a half compared with that of a common reaction device, the viscosity of the slurry is reduced, and the liquid-solid ratio is reduced to 2-2.5: 1.
And (3) process control:
total mixing tank: the temperature is 60 ℃, and the pressure is-50 to 100 Pa;
an extraction tank: the temperature is 85-95 ℃, P2O518~22,SO346~50mg/L
The liquid-solid ratio is 2.0-2.5: 1, and the pressure is-50 Pa to-100 Pa;
growing the crystal in the crystal groove: the temperature is 65-75 ℃, and the pressure is-50 Pa to-100 Pa
C. Closed circulation of system sewage and waste water and production of Na2SiF6: washing the tail gas at 6-8 n/h3By using NaSO4With washing liquid H2SiF6Reaction to produce Na2SiF6With dilute H2SO4,Na2SiF6Separating and drying to obtain the finished product, and finally feeding the dilute sulfuric acid into an extraction tank. Compared with the prior art, the invention has the following advantages:
1. low power consumption and acid consumption, greatly reduced production cost, and power consumption of 120-2O5Acid consumption 2.4 ton/ton P2O5
2. The yield of the phosphorus is improved, and the yield of the phosphorus reaches 93.5 percent by adopting a new process;
3. the production efficiency is improved by more than 50%.
The present invention will be described in further detail with reference to the following examples:
the method comprises the following process steps: A. premixing, deacidifying and removing impurities; B. carrying out total mixing, extraction and crystal growing continuous reaction; C. closed circulation of system sewage and waste water and production of Na2SiF6
A. Pre-mixing, deacidifying and removing impurities: the working principle of the process is as follows:
……①
Figure A9811208900061
……③
……④
the working procedure can lead CaO in phosphorite to enter finished phosphoric acid product, and lead CaO in the ore to be reduced, thereby saving sulfuric acid consumption in the extraction process, and 5 percent of H in the phosphoric acid2SO4In the ②, ③ and ④ reaction process, H in the finished phosphoric acid is reacted2SO4Reduce the consumption of sulfuric acid, remove gypsum crystal which is not beneficial to decomposition in phosphorite, purify the phosphorite and have great importance for easy reaction and generation of thick and uniform crystal of ore in the process of extracting and growing crystalAnd (4) acting.
And (3) process control: the temperature of the premixing tank is 60-70 ℃, the liquid-solid ratio is 5-8: 1, the retention time is 1 hour, and the settling time is 1 hour.
B. Total mixing, extraction and crystal growing continuous reaction: the working principle of the process is as follows:
……⑤
……⑦
the total mixing tank is reaction ⑤, namely, the dilute phosphoric acid reacts with the mineral powder to generate CaH2(PO4)2Avoiding the ore powder and H2SO4The direct contact forms the color failure, and the extraction rate is improved by 1 percent.
The extraction is reaction ⑥, and the crystal growth is reaction ⑦;
the total mixing tank not only plays a role of a reactor, but also takes away heat in advance, the diluted phosphoric acid reacts with the mineral powder and then enters the extraction tank, meanwhile, sulfuric acid is added for full reaction, and the diluted phosphoric acid is continuously precipitated to the crystal growing tank and is continuously filtered in the crystal growing tank; the retention time of slurry in the whole process is 2 and a half hours, the retention time is reduced by a half compared with that of a common reaction device, the viscosity of the slurry is reduced, and the liquid-solid ratio is reduced to 2-2.5: 1.
And (3) process control:
total mixing tank: the temperature is 60 ℃, and the pressure is-50 to 100 Pa;
an extraction tank: the temperature is 85-95 ℃, P2O518~22,SO346~50mg/L
The liquid-solid ratio is 2.0-2.5: 1, and the pressure is-50 Pa to-100 Pa;
growing the crystal in the crystal groove: the temperature is 65-75 ℃, and the pressure is-50 Pa to-100 Pa
C. Closed circulation of system sewage and waste water and production of Na2SiF6: washing the tail gas at 6-8 n/h3By using NaSO4With washing liquid H2SiF6Reaction to produce Na2SiF6With dilute H2SO4,Na2SiF6Separating and drying to obtain the finished product, and finally feeding the dilute sulfuric acid into an extraction tank.
The invention has low power consumption and acid consumption, greatly reduces the production cost, and has the power consumption of 120-2O5Acid consumption 2.4 ton/ton P2O5(ii) a The yield of the phosphorus is improved, and the yield of the phosphorus reaches 93.5 percent by adopting a new process; the production efficiency is improved by more than 50%.

Claims (1)

1. A novel method for producing phosphoric acid by a wet process comprises the following process steps: A. premixing, deacidifying and removing impurities; B. carrying out total mixing, extraction and crystal growing continuous reaction; C. closed circulation of system sewage and waste water and production of Na2SiF6The method is characterized in that:
A. pre-mixing, deacidifying and removing impurities: the working principle of the process is as follows:
……①
……③
……④
the working procedure can lead CaO in phosphorite to enter finished phosphoric acid product, and lead CaO in the ore to be reduced, thereby saving sulfuric acid consumption in the extraction process, and 5 percent of H in the phosphoric acid2SO4In the ②, ③ and ④ reaction process, H in the finished phosphoric acid is reacted2SO4The consumption of sulfuric acid is reduced, and gypsum which is not beneficial to decomposition in phosphorite is crystallized and removed,so that the phosphorite is purified, and the method plays an extremely important role in easily reacting ores and generating coarse and uniform crystals in the extraction and crystal growing process;
and (3) process control: the temperature of the premixing tank is 60-70 ℃, the liquid-solid ratio is 5-8: 1, the retention time is 1 hour, and the settling time is 1 hour;
B. total mixing, extraction and crystal growing continuous reaction: the working principle of the process is as follows:
……⑤
Figure A9811208900022
……⑦
the total mixing tank is reaction ⑤, namely, the dilute phosphoric acid reacts with the mineral powder to generate CaH2(PO4)2Avoiding the ore powder and H2SO4The direct contact forms the color failure, and the extraction rate is improved by 1 percent;
the extraction is reaction ⑥, and the crystal growth is reaction ⑦;
the total mixing tank not only plays a role of a reactor, but also takes away heat in advance, the diluted phosphoric acid reacts with the mineral powder and then enters the extraction tank, meanwhile, sulfuric acid is added for full reaction, and the diluted phosphoric acid is continuously precipitated to the crystal growing tank and is continuously filtered in the crystal growing tank; the retention time of slurry in the whole process is 2 and half hours, the retention time is reduced by half compared with that of a common reaction device, the viscosity of the slurry is reduced, and the liquid-solid ratio is reduced to 2-2.5: 1;
and (3) processcontrol:
total mixing tank: the temperature is 60 ℃, and the pressure is-50 to 100 Pa;
an extraction tank: the temperature is 85-95 ℃, P2O518~22,SO346~50mg/L
The liquid-solid ratio is 2.0-2.5: 1, and the pressure is-50 Pa to-100 Pa;
growing the crystal in the crystal groove: the temperature is 65-75 ℃, and the pressure is-50 Pa to-100 Pa
C. Closed circulation of system sewage and waste water and production of Na2SiF6: washing the tail gas at 6-8 n/h3By using NaSO4With washing liquid H2SiF6Reaction to produce Na2SiF6With dilute H2SO4,Na2SiF6Separating and drying to obtain a finished product, and finally feeding dilute sulfuric acid into an extraction tank;
CN 98112089 1998-06-18 1998-06-18 Wet phosphoric acid producing process Pending CN1239705A (en)

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CN 98112089 CN1239705A (en) 1998-06-18 1998-06-18 Wet phosphoric acid producing process

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1317183C (en) * 2005-12-23 2007-05-23 中国石化集团南京设计院 Process for producing wet method phosphoric acid by medium low grade phosphorus mine
CN102390821A (en) * 2011-08-08 2012-03-28 云南云天化国际化工股份有限公司 Method for producing dihydrate wet-process phosphoric acid
CN104495770A (en) * 2014-12-24 2015-04-08 金正大诺泰尔化学有限公司 Method for purifying wet process phosphoric acid by crystallization in extraction process
CN106395774A (en) * 2016-09-09 2017-02-15 安徽六国化工股份有限公司 Gradient technology method for wet process phosphoric acid production

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1317183C (en) * 2005-12-23 2007-05-23 中国石化集团南京设计院 Process for producing wet method phosphoric acid by medium low grade phosphorus mine
CN102390821A (en) * 2011-08-08 2012-03-28 云南云天化国际化工股份有限公司 Method for producing dihydrate wet-process phosphoric acid
CN104495770A (en) * 2014-12-24 2015-04-08 金正大诺泰尔化学有限公司 Method for purifying wet process phosphoric acid by crystallization in extraction process
CN104495770B (en) * 2014-12-24 2017-12-29 金正大诺泰尔化学有限公司 A kind of method of purging by crystallization phosphoric acid by wet process in extraction process
CN106395774A (en) * 2016-09-09 2017-02-15 安徽六国化工股份有限公司 Gradient technology method for wet process phosphoric acid production

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