CN113860277A - Dihydrate wet process phosphoric acid production technology - Google Patents
Dihydrate wet process phosphoric acid production technology Download PDFInfo
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- CN113860277A CN113860277A CN202111284329.1A CN202111284329A CN113860277A CN 113860277 A CN113860277 A CN 113860277A CN 202111284329 A CN202111284329 A CN 202111284329A CN 113860277 A CN113860277 A CN 113860277A
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- slurry
- reaction
- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 18
- 150000004683 dihydrates Chemical class 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 238000005516 engineering process Methods 0.000 title description 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 239000002367 phosphate rock Substances 0.000 claims abstract description 14
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000029087 digestion Effects 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000011574 phosphorus Substances 0.000 claims abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 7
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000012066 reaction slurry Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 claims abstract description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims abstract description 3
- 239000010440 gypsum Substances 0.000 claims abstract description 3
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 3
- 235000019691 monocalcium phosphate Nutrition 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000005496 eutectics Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- CKRORYDHXIRZCH-UHFFFAOYSA-N phosphoric acid;dihydrate Chemical compound O.O.OP(O)(O)=O CKRORYDHXIRZCH-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/223—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
- C01B25/225—Dihydrate process
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a dihydrate wet-process phosphoric acid production process, which comprises the following steps: when the total content of sesquioxide impurities in the phosphorite exceeds 2.3 percent, the free sulfate radical in the reaction slurry is increased from 25g/l to 30g/l to more than 35 g/l; in the crystal growing process of the digestion tank, part of slurry is taken from the reaction tank 1 chamber and added into the digestion tank A, so that calcium dihydrogen phosphate in the slurry reacts with excessive sulfate radicals to form calcium sulfate dihydrate gypsum, and the sulfate radical content in the filtrate is reduced; to ensure the material balance of the reaction system, a pipeline is added at the outlet of the filter feeding pump of the digestion tank C, and the excess slurry quantity which is equal to the quantity taken out from the reaction tank 1 chamber is returned to the reaction tank 1 chamber. The invention can realize the improvement of the decomposition rate of the phosphorite, and the content of the phosphorus insoluble in the phosphogypsum can be reduced by 0.1 percent. The method is beneficial to improving the yield of phosphorus and stabilizing the quality of the product diluted phosphoric acid, brings great economic benefit to enterprises, and is suitable for all enterprises producing wet-process phosphoric acid.
Description
Technical Field
The invention relates to the technical field of wet-process phosphoric acid production, in particular to a reaction system for producing phosphoric acid by a dihydrate wet process and a process for controlling the content of dilute phosphate radical of a product.
Background
The wet-process phosphoric acid dihydrate is a mature one in the current wet-process phosphoric acid production process, and is widely popularized due to the wide adaptability to mineral substances. Along with the continuous exploitation and consumption of phosphorite resources, the quality of phosphorite gradually slides down, wherein the more prominent expression is the increase of sesquioxide impurities. In general, the design of the phosphoric acid by the dihydrate wet method requires that 3% of excessive free sulfate radicals in a reaction system can ensure that the extraction rate of the phosphorite meets the requirement. When the content of the sesquioxide is increased, if the free sulfate radical is excessive and insufficient, partial phosphorite is not decomposed, and the extraction rate is reduced; when the sulfate radical is controlled to be too high, the sulfate radical in the product dilute phosphoric acid is too high, and the influence on downstream products can be caused.
The inventor has not found a patent specially aiming at controlling free sulfate radicals in reaction slurry of phosphoric acid by a dihydrate wet method and product diluted phosphoric acid on a Chinese patent network at present.
Disclosure of Invention
The invention aims to solve the technical problem of how to control the content of free sulfate radicals in reaction slurry and product diluted acid, improve the extraction rate of phosphorite and stabilize the product quality aiming at the quality reduction of phosphorite.
In order to further improve the extraction rate of the phosphorite under the condition of low-quality phosphorite, the inventor collects and arranges related data through multiple experiments and analysis. The invention discloses a production process for improving the extraction rate of phosphorite, which comprises the following steps:
when the total content of sesquioxide impurities in the phosphorite exceeds 2.3 percent, the free sulfate radical in the reaction slurry is increased from 25g/l to 30g/l to more than 35 g/l; ensure the excessive sulfate radical and reduce the loss of eutectic phosphorus.
Secondly, in the crystal growing process of the digestion tank, part of slurry is taken from a reaction tank 1 and added into a digestion tank A, calcium dihydrogen phosphate in the slurry reacts with excessive sulfate radicals to form calcium sulfate dihydrate gypsum, and the content of the sulfate radicals in the filtrate is further reduced;
and thirdly, in order to ensure the material balance of the reaction system, a pipeline is added at the outlet of the filtering and feeding pump of the digestion tank C, and the excess slurry quantity which is equal to the quantity of the excess slurry taken out from the reaction tank 1 chamber is returned to the reaction tank 1 chamber.
The inventor points out that: in the step 1 of the method, the free sulfate radical control amount is determined according to the impurity content of the phosphorite, and when the total content of the sesquioxide exceeds the design value of phosphoric acid by a dihydrate wet method by 2.3 percent, the sulfate radical control amount must be increased to more than 35g/l to prevent the phosphoric acid from reacting with the impurities.
In the step 2 of the method, the slurry added into the tank A of the digestion tank is required to be slurry in the chamber 1 of the reaction tank, and the content of sulfate radicals is greatly reduced because the slurry is added into the chamber 1 of the reaction tank.
In the step 2 of the method, slurry in the chamber 1 of the reaction tank must be added into a digestion tank A, and the slurry is separated from the reaction tank after entering a digestion system, so that only the subsequent product of dilute sulfate phosphate radical is influenced, and sufficient reaction time is provided for the subsequent reaction after the slurry is added into the tank A. The specific reaction equation is as follows:
5Ca(H2 PO4)2+5H2SO4+10H2O=5CaSO4.2H2O↓+10H3PO4
in the step 3 of the method, the redundant slurry must be returned to the reaction tank 1 chamber, so that the material balance of the reaction system is ensured, and the reaction system is not influenced.
The invention has the beneficial effects that: the decomposition rate of the phosphorus ore can be improved, and the content of the phosphorus insoluble in the phosphogypsum can be reduced by 0.1 percent. The method is beneficial to improving the yield of phosphorus and stabilizing the quality of the product diluted phosphoric acid, brings great economic benefit to enterprises, and is suitable for all enterprises producing wet-process phosphoric acid.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
Example 1: the reaction tank of the embodiment has 6 chambers, 500ml of slurry in the 6 chambers of the reaction tank is taken, the content of slurry sulfate radical is 39g/l, 20ml of slurry in the 1 chamber of the reaction tank is taken, the content of slurry sulfate radical is 9g/l, 1000ml of beaker is used for mixing the two slurries, the slurry sulfate radical in 1000ml of beaker is reduced to 35g/l after the continuous stirring for 10 minutes, the reaction of the two slurries is proved, and the purpose of reducing the free sulfate radical of the dilute phosphoric acid radical of the product is achieved.
Example 2: according to the change of the impurity content of the ore, the sulfate radical in the 6 chambers of the reaction tank is controlled to be 40 +/-2 g/l in a certain plant, so that the filtering effect of the filter is ensured. The slurry was pumped into the digestion tank A from the reaction tank 1 by an air pump at an amount of 20m3H; and (3) carrying out sulfate radical analysis on the sample, wherein the sulfate radical content of the slurry in the chamber 1 of the reaction tank is 7-8g/l, the sulfate radical content in the chamber 6 of the reaction tank is 41 g/l, and the sulfate radical content of the filtered acid is 28 g/l.
Claims (1)
1. A dihydrate wet-process phosphoric acid production process is characterized by comprising the following steps:
when the total content of sesquioxide impurities in the phosphorite exceeds 2.3 percent, the free sulfate radical in the reaction slurry is increased from 25g/l to 30g/l to more than 35 g/l; ensuring excessive sulfate radicals and reducing the loss of eutectic phosphorus;
secondly, in the crystal growing process of the digestion tank, part of slurry is taken from a reaction tank 1 and added into a digestion tank A, calcium dihydrogen phosphate in the slurry reacts with excessive sulfate radicals to form calcium sulfate dihydrate gypsum, and the content of the sulfate radicals in the filtrate is further reduced;
and thirdly, in order to ensure the material balance of the reaction system, a pipeline is added at the outlet of the filtering and feeding pump of the digestion tank C, and the excess slurry quantity which is equal to the quantity of the excess slurry taken out from the reaction tank 1 chamber is returned to the reaction tank 1 chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111284329.1A CN113860277A (en) | 2021-11-01 | 2021-11-01 | Dihydrate wet process phosphoric acid production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111284329.1A CN113860277A (en) | 2021-11-01 | 2021-11-01 | Dihydrate wet process phosphoric acid production technology |
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| Publication Number | Publication Date |
|---|---|
| CN113860277A true CN113860277A (en) | 2021-12-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111284329.1A Pending CN113860277A (en) | 2021-11-01 | 2021-11-01 | Dihydrate wet process phosphoric acid production technology |
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| Country | Link |
|---|---|
| CN (1) | CN113860277A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304041A (en) * | 2022-09-26 | 2022-11-08 | 瓮福（集团）有限责任公司 | Process for reducing insoluble phosphorus in phosphogypsum in production of phosphoric acid by dihydrate wet method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3726647A (en) * | 1971-02-11 | 1973-04-10 | R Somerville | Apparatus for the production of phosphoric acid |
| CN101125646A (en) * | 2007-09-26 | 2008-02-20 | 云南常青树化工有限公司 | Method for preparing high concentration phosphoric acid by directly reducing low and middle grade phosphorus ore |
| CN102701167A (en) * | 2012-06-13 | 2012-10-03 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing industrial ammonium dihydrogen phosphate |
| CN112299386A (en) * | 2020-10-31 | 2021-02-02 | 贵州开磷集团矿肥有限责任公司 | Method for removing sulfate radical in wet-process dilute phosphoric acid by using phosphate slurry |
-
2021
- 2021-11-01 CN CN202111284329.1A patent/CN113860277A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3726647A (en) * | 1971-02-11 | 1973-04-10 | R Somerville | Apparatus for the production of phosphoric acid |
| CN101125646A (en) * | 2007-09-26 | 2008-02-20 | 云南常青树化工有限公司 | Method for preparing high concentration phosphoric acid by directly reducing low and middle grade phosphorus ore |
| CN102701167A (en) * | 2012-06-13 | 2012-10-03 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing industrial ammonium dihydrogen phosphate |
| CN112299386A (en) * | 2020-10-31 | 2021-02-02 | 贵州开磷集团矿肥有限责任公司 | Method for removing sulfate radical in wet-process dilute phosphoric acid by using phosphate slurry |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304041A (en) * | 2022-09-26 | 2022-11-08 | 瓮福（集团）有限责任公司 | Process for reducing insoluble phosphorus in phosphogypsum in production of phosphoric acid by dihydrate wet method |
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