CN111892032A - Defoaming and feeding control method and device for wet-process phosphoric acid extraction reaction - Google Patents
Defoaming and feeding control method and device for wet-process phosphoric acid extraction reaction Download PDFInfo
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- CN111892032A CN111892032A CN202010824645.2A CN202010824645A CN111892032A CN 111892032 A CN111892032 A CN 111892032A CN 202010824645 A CN202010824645 A CN 202010824645A CN 111892032 A CN111892032 A CN 111892032A
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- 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
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Abstract
The invention discloses a defoaming and feeding control method and a defoaming and feeding control device for wet-process phosphoric acid extraction reaction, and relates to the technical field of wet-process phosphoric acid production. The sulfuric acid which is respectively added into the reaction tank 2# and the reaction tank 3# chambers in the original production is changed into the sulfuric acid which is mostly adjusted and added into a pipeline at the outlet of a reaction slurry circulating pump, and the sulfuric acid is quickly diluted by the slurry to release a large amount of heat. Therefore, the heat removed by gasification is released by the reaction of phosphate rock under the original process condition, and is changed into reaction heat release and sulfuric acid dilution heat, the heat to be removed is greatly increased, the gasification degree in unit time is enhanced, the foam volume in the circulating slurry under the vacuum condition required by the process is doubled and increased compared with that before modification, the foam wall becomes thinner, the stability is poor and the foam is continuously broken, and a large amount of foam is eliminated in a flash cooler. Thereby achieving the purpose of defoaming without adding a defoaming agent.
Description
Technical Field
The invention relates to the technical field of wet-process phosphoric acid production, in particular to a defoaming and feeding control method and a defoaming and feeding control device for wet-process phosphoric acid extraction reaction.
Background
Although the reserves of phosphorite resources are abundant in China, the reserves of high-grade phosphorite only account for about 30 percent of the total reserves, and most of the high-grade phosphorite is the medium-grade and low-grade silico-calcium collophanite. Along with the continuous consumption of high-grade phosphate ore, the high-grade phosphate ore reserves are less and less, and production enterprises using a large amount of phosphate ore have to obtain ore pulp meeting the raw material requirements through the flotation of medium-low grade phosphate ore.
At present, 30 ten thousand tons of wet-process phosphoric acid mostly use the extraction tank of square multislot, it is common that the extraction tank comprises 6 reaction tanks (1# -6 #) and 3 digestion tanks (7# -9 #), as shown in figure 1, be provided with the phosphorus ore thick liquid import on the 1# groove, 2#, 3# reaction tank are provided with the sulphuric acid import, the 6# inslot is provided with the circulating pump, the circulating pump passes through the pipeline and flashes cold system one end intercommunication, flash cold system other end and 1# groove intercommunication. The production process of the wet-process phosphoric acid is to inject the phosphorite slurry into the No. 1 tank, because the bottoms of the No. 1 to No. 6 tanks are communicated, the ore slurry enters each tank along with the circulating slurry, the sulfuric acid enters the extraction tank through the No. 2 and the No. 3 to be mixed with the phosphorite slurry, and the ore slurry and the sulfuric acid react in the extraction tank to prepare the phosphoric acid.
Because the ore pulp contains organic matters and carbonate, a large amount of carbon dioxide is released when the phosphate ore reacts with sulfuric acid, generated bubbles continuously rise under the stirring action, and the liquid phase contains organic residues for foaming and collecting in the flotation process, and the existence of the surfactants enables foams to be generated more easily and stably without breaking. The foam layer on the upper part of the extraction tank is continuously thickened, the space on the upper part of the tank is reduced, the heat released by reaction cannot be quickly removed due to the blocked gas flow, so that the rubber plate on the top of the reaction tank is damaged, the concrete on the top of the tank is corroded, the extraction tank has to be stopped for discharging and repairing, the production cost is increased, and the operation rate of the extraction tank is reduced.
In order to ensure the normal operation of production, different defoaming methods are adopted for defoaming in production. There are many common defoaming methods, and physical defoaming, mechanical defoaming, chemical defoaming and natural defoaming can be classified according to the principle. In the wet-process phosphoric acid production, defoaming pulp is generally adopted for mechanical defoaming, defoaming by adding a defoaming agent and defoaming by spraying water, and the mechanical defoaming of the defoaming pulp is only suitable for high-quality phosphorus ores and ores with low organic matter and carbonate content in the ores, but is difficult to find large-batch high-quality raw ores for use along with the increasing use amount of the phosphorus ores. Although the defoaming agent can be added for better defoaming, the defoaming agent is high in price, the production cost is increased, the workload is increased, and the labor intensity of workers is increased, so that the method is not an optimal defoaming method. The broken bubble of shower water has certain effect when the foam volume is not big, nevertheless because water enters into the ground paste, leads to filtering the washing water volume to reduce, influences the promotion of gypsum washing rate, when the foaming is serious, can't satisfy the production requirement.
Disclosure of Invention
The invention aims to provide a defoaming and feeding control method and a defoaming and feeding control device for wet-process phosphoric acid extraction reaction, and solves the problems that the prior defoaming technology is difficult to meet the production requirement of producing wet-process phosphoric acid by using low-grade phosphate ore, so that the defoaming effect in the extraction reaction process is not obvious, and a reaction tank is often corroded.
In order to solve the technical problems, the invention adopts the following technical scheme: a defoaming and feeding control method for wet-process phosphoric acid extraction reaction is characterized by comprising the following steps:
(1) adding the phosphorite slurry into a No. 1 reaction tank of the extraction tank;
(2) adding sulfuric acid with the concentration of 98% into No. 2 and No. 3 reaction tanks, wherein the amount of the added sulfuric acid is 30-40% of the total amount of the sulfuric acid required by the reaction with the phosphoric ore pulp in the step (1);
(3) and (2) adding sulfuric acid with the concentration of 98% into a pipeline communicating a circulating pump and a flash evaporator, wherein the added amount of the sulfuric acid is 60% -70% of the total amount of the sulfuric acid required by the reaction of the sulfuric acid and the phosphoric ore pulp in the step (1).
The further technical scheme is that the vacuum degree in the flash evaporator is controlled to be 35-45 kPa.
The invention also relates to a defoaming and charging control device for wet-process phosphoric acid extraction reaction, which is characterized in that: the extraction tank is composed of a 1# to 6# reaction tank and a 7# to 9# digestion tank, the 1# to 6# reaction tank is communicated in sequence, the 6# reaction tank overflows to the 7# digestion tank, the 7# digestion tank is communicated with the 8# digestion tank, and the 8# digestion tank overflows to the 9# digestion tank; be provided with the circulating pump in the 6# reaction tank, the circulating pump export is passed through pipeline and flash vessel one end intercommunication, and the flash vessel other end and 1# reaction tank intercommunication are provided with the phosphorus ore thick liquid entry on the 1# reaction tank, are provided with the sulphuric acid entry on 2#, the 3# reaction tank, are provided with the sulphuric acid entry on the pipeline.
The further technical proposal is that the extraction tanks are distributed in a grid of squared figures, and stirring devices are arranged in the 1# to 6# reaction tank and the 7# to 9# digestion tank.
The reaction mechanism is as follows: the sulfuric acid which is respectively added into the reaction tank 2# and the reaction tank 3# chambers in the original production is changed into the sulfuric acid which is mostly adjusted and added into a pipeline at the outlet of a reaction slurry circulating pump, and the sulfuric acid is quickly diluted by the slurry to release a large amount of heat. Therefore, the heat removed by gasification is released by the reaction of phosphate rock under the original process condition, and is changed into reaction heat release and sulfuric acid dilution heat, the heat to be removed is greatly increased, the gasification degree in unit time is enhanced, the foam volume in the circulating slurry under the vacuum condition required by the process is doubled and increased compared with that before modification, the foam wall becomes thinner, the stability is poor and the foam is continuously broken, and a large amount of foam is eliminated in a flash cooler. Thereby achieving the purpose of defoaming without adding a defoaming agent.
Compared with the prior art, the invention has the beneficial effects that: through increasing sulphuric acid addition point on the pipeline at reaction slurry circulating pump export, about 70% sulphuric acid adjustment is added to this point, under vacuum and thermal power composite condition, the bubble increases fast and breaks and realizes the defoaming to need not to add the defoaming agent again and carry out the defoaming, like this per ton P2O5The product can reduce the production cost by 1.5 yuan, can reduce the consumption of the defoaming agent by 45 tons every year, and reduce the production cost by 45 ten thousand yuan.
Drawings
FIG. 1 is a schematic diagram of a wet-process phosphoric acid extraction reaction device in the prior art.
FIG. 2 is a schematic diagram of a wet-process phosphoric acid extraction reaction device according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Fig. 2 shows: a defoaming and feeding control device for wet-process phosphoric acid extraction reaction comprises an extraction tank 101 and a flash evaporator 102, wherein the extraction tank 101 is composed of a 1# to 6# reaction tank and a 7# to 9# digestion tank, the 1# to 6# reaction tank is communicated in sequence, the 6# reaction tank overflows to the 7# digestion tank, the 7# digestion tank is communicated with a 8# digestion tank, and the 8# digestion tank overflows to the 9# digestion tank; be provided with circulating pump 103 in the 6# reaction tank, circulating pump 103 export is through pipeline 104 and flash vessel 102 one end intercommunication, and the flash vessel 102 other end and 1# reaction tank intercommunication are provided with the phosphorus ore thick liquid entry on the 1# reaction tank, are provided with the sulphuric acid entry on 2#, the 3# reaction tank, are provided with the sulphuric acid entry on the pipeline 104. The extraction tank 101 is arranged in a grid, and stirring devices are arranged in the 1# to 6# reaction tank and the 7# to 9# digestion tank.
Example 2
(1) Adding the phosphorite slurry into a No. 1 reaction tank of the extraction tank 101;
(2) adding sulfuric acid with the concentration of 98% into No. 2 and No. 3 reaction tanks, wherein the added amount of the sulfuric acid is 30% of the total amount of the sulfuric acid required by the reaction with the phosphorite pulp in the step 1;
(3) sulfuric acid with the concentration of 98% is added into a pipeline 104 communicating a circulating pump 103 and a flash evaporator 102, and the added amount of the sulfuric acid is 70% of the total amount of the sulfuric acid required for the reaction with the phosphorite pulp in the step 1. The vacuum in the flash vessel 102 was controlled at 35kPa absolute.
Example 3
(1) Adding the phosphorite slurry into a No. 1 reaction tank of the extraction tank 101;
(2) adding sulfuric acid with the concentration of 98% into No. 2 and No. 3 reaction tanks, wherein the added amount of the sulfuric acid is 35% of the total amount of the sulfuric acid required by the reaction with the phosphorite pulp in the step 1;
(3) sulfuric acid with the concentration of 98% is added into a pipeline 104 communicating a circulating pump 103 and a flash evaporator 102, and the added amount of the sulfuric acid is 65% of the total amount of the sulfuric acid required for the reaction with the phosphorite pulp in the step 1. The vacuum in the flash vessel 102 was controlled to 40kPa absolute.
Example 4
(1) Adding the phosphorite slurry into a No. 1 reaction tank of the extraction tank 101;
(2) adding sulfuric acid with the concentration of 98% into No. 2 and No. 3 reaction tanks, wherein the added amount of the sulfuric acid is 40% of the total amount of the sulfuric acid required by the reaction with the phosphorite pulp in the step 1;
(3) sulfuric acid with the concentration of 98% is added into a pipeline 104 communicating a circulating pump 103 and a flash evaporator 102, and the added amount of the sulfuric acid is 60% of the total amount of the sulfuric acid required by the reaction with the phosphorite pulp in the step 1. The vacuum in the flash vessel 102 was controlled at 45kPa absolute.
Example 5
(1) Continuously adding phosphate rock slurry with the solid content of 63% into the No. 1 reaction tank of the extraction tank 101 according to 256.1 t/h;
(2) correspondingly, 125.5t of 98 percent sulfuric acid is continuously added in each hour, wherein 37.6t is averagely added into the No. 2 and No. 3 reaction tanks; 87.9t was fed into a conduit 104 connecting the circulation pump 103 with the flash vessel 102.
(3) The vacuum in the flash vessel 102 was controlled at 42 kPa.
According to observation, under the condition that the quality of ore pulp is stable, after a sulfuric acid adding point is added, a defoaming agent is not required to be added into a reaction tank. The upper space of the reaction tank reached 1.4m during the production. Before the sulphuric acid addition point is not increased, the space height when defoaming by adding the defoaming agent is still increased by about 0.4m, the reaction tail gas flows smoothly, the whole extraction tank is in micro negative pressure, the reaction tail gas cannot emerge from the tank top to cause air pollution, and the production environment is good. The production cost of each ton of phosphoric acid product is reduced by 1.5 yuan.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. In addition to variations and modifications in the component parts or arrangements, other uses will also be apparent to those skilled in the art.
Claims (4)
1. A defoaming and feeding control method for wet-process phosphoric acid extraction reaction is characterized by comprising the following steps:
(1) adding the phosphorite slurry into a No. 1 reaction tank of the extraction tank (101);
(2) adding sulfuric acid with the concentration of 98% into No. 2 and No. 3 reaction tanks, wherein the amount of the added sulfuric acid is 30-40% of the total amount of the sulfuric acid required by the reaction with the phosphoric ore pulp in the step (1);
(3) and (2) adding sulfuric acid with the concentration of 98% into a pipeline (104) communicating a circulating pump (103) and a flash evaporator (102), wherein the added amount of the sulfuric acid is 60% -70% of the total amount of the sulfuric acid required by the reaction with the phosphoric ore pulp in the step (1).
2. The defoaming feeding control method for wet-process phosphoric acid extraction reaction according to claim 1, characterized in that: and controlling the vacuum degree in the flash evaporator to be 35-45 kPa.
3. The utility model provides a defoaming feeding control device of wet process phosphoric acid extraction reaction which characterized in that: the extraction device comprises an extraction tank (101) and a flash evaporator (102), wherein the extraction tank (101) is composed of a 1# to 6# reaction tank and a 7# to 9# digestion tank, the 1# to 6# reaction tank is communicated in sequence, the 6# reaction tank overflows to the 7# digestion tank, the 7# digestion tank is communicated with the 8# digestion tank, and the 8# digestion tank overflows to the 9# digestion tank; be provided with circulating pump (103) in the 6# reaction tank, circulating pump (103) export is through pipeline (104) and flash vessel (102) one end intercommunication, and flash vessel (102) other end and 1# reaction tank intercommunication are provided with the phosphorus ore thick liquid entry on the 1# reaction tank, are provided with the sulphuric acid entry on 2#, the 3# reaction tank, are provided with the sulphuric acid entry on pipeline (104).
4. The defoaming feeding control device for wet-process phosphoric acid extraction reaction according to claim 3, characterized in that: the extraction tank (101) is arranged in a squared figure, and stirring devices are arranged in the 1# to 6# reaction tank and the 7# to 9# digestion tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010824645.2A CN111892032A (en) | 2020-08-17 | 2020-08-17 | Defoaming and feeding control method and device for wet-process phosphoric acid extraction reaction |
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| CN202010824645.2A CN111892032A (en) | 2020-08-17 | 2020-08-17 | Defoaming and feeding control method and device for wet-process phosphoric acid extraction reaction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4382184A1 (en) | 2022-12-06 | 2024-06-12 | Yara International ASA | System for breaking a liquid foam and method of operating thereof |
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| JPH07257914A (en) * | 1994-03-22 | 1995-10-09 | Mitsui Toatsu Chem Inc | Method for reforming wet-process phosphoric acid |
| FR2859921A1 (en) * | 2003-09-18 | 2005-03-25 | Seppic Sa | Low-foaming, surface-active composition for modifying crystallization in wet process phosphoric acid production, containing (poly)oxyalkylenated alcohol or amine, carboxylic acid and water |
| CN103449391A (en) * | 2013-08-30 | 2013-12-18 | 云南三环中化化肥有限公司 | Method for adding sulfuric acid into reaction system during wet-process production of phosphoric acid |
| CN105329866A (en) * | 2015-11-27 | 2016-02-17 | 安徽六国化工股份有限公司 | Defoaming method and device for wet process phosphoric acid extracting reaction |
| CN108394880A (en) * | 2018-05-15 | 2018-08-14 | 武汉工程大学 | A method of eliminating phosphoric acid by wet process extraction reaction foam |
| CN108455543A (en) * | 2018-02-07 | 2018-08-28 | 四川绵竹市盘龙矿物质有限责任公司 | A kind of the defoaming charging process and its device of phosphoric acid by wet process extraction reaction |
| CN110510589A (en) * | 2019-09-10 | 2019-11-29 | 湖北祥云(集团)化工股份有限公司 | A kind of Wet-process Phosphoric Acid Production method and production system |
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2020
- 2020-08-17 CN CN202010824645.2A patent/CN111892032A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07257914A (en) * | 1994-03-22 | 1995-10-09 | Mitsui Toatsu Chem Inc | Method for reforming wet-process phosphoric acid |
| FR2859921A1 (en) * | 2003-09-18 | 2005-03-25 | Seppic Sa | Low-foaming, surface-active composition for modifying crystallization in wet process phosphoric acid production, containing (poly)oxyalkylenated alcohol or amine, carboxylic acid and water |
| CN103449391A (en) * | 2013-08-30 | 2013-12-18 | 云南三环中化化肥有限公司 | Method for adding sulfuric acid into reaction system during wet-process production of phosphoric acid |
| CN105329866A (en) * | 2015-11-27 | 2016-02-17 | 安徽六国化工股份有限公司 | Defoaming method and device for wet process phosphoric acid extracting reaction |
| CN108455543A (en) * | 2018-02-07 | 2018-08-28 | 四川绵竹市盘龙矿物质有限责任公司 | A kind of the defoaming charging process and its device of phosphoric acid by wet process extraction reaction |
| CN108394880A (en) * | 2018-05-15 | 2018-08-14 | 武汉工程大学 | A method of eliminating phosphoric acid by wet process extraction reaction foam |
| CN110510589A (en) * | 2019-09-10 | 2019-11-29 | 湖北祥云(集团)化工股份有限公司 | A kind of Wet-process Phosphoric Acid Production method and production system |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4382184A1 (en) | 2022-12-06 | 2024-06-12 | Yara International ASA | System for breaking a liquid foam and method of operating thereof |
| WO2024121192A1 (en) | 2022-12-06 | 2024-06-13 | Yara International Asa | System for breaking a liquid foam and method of operating thereof |
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