CN110963475A - Method for producing phosphate concentrate powder - Google Patents
Method for producing phosphate concentrate powder Download PDFInfo
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- CN110963475A CN110963475A CN201811148107.5A CN201811148107A CN110963475A CN 110963475 A CN110963475 A CN 110963475A CN 201811148107 A CN201811148107 A CN 201811148107A CN 110963475 A CN110963475 A CN 110963475A
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- Prior art keywords
- solution
- powder
- lime powder
- phosphate
- phosphate concentrate
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- 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
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/322—Preparation by neutralisation of orthophosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a production method for producing phosphate concentrate powder by using low-grade phosphate ore. The method comprises the following steps: step one, lime powder is used for neutralizing a mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration; secondly, performing solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure within about 1-2.0MPa to separate the solution from tricalcium phosphate solid phase to obtain a filter cake; and thirdly, stacking filter cakes obtained by filter pressing at one position for natural drying to obtain the phosphate concentrate powder. The production method has simple operation and high stability, and can save a large amount of energy.
Description
Technical Field
The invention relates to a production method for producing phosphate concentrate powder by using low-grade phosphate ore, in particular to a process for generating and extracting phosphate concentrate powder in a mixed solution and removing a phosphoric acid component in a whisker synthesis process.
Background
At present, when low-grade phosphate ore is used for producing calcium sulfate whiskers, clear liquid generated after filtration contains components such as phosphoric acid, calcium chloride and the like, sulfuric acid is added to synthesize the calcium sulfate whiskers, and the obtained by-product is a mixture of dilute phosphoric acid and dilute hydrochloric acid, and ammonium phosphate-magnesium chloride fertilizer is obtained after ammoniation and air flow drying.
When the fertilizer is produced, a large amount of heat energy needs to be provided for drying, a large amount of waste gas is generated, the fertilizer is difficult to sell in the market, and the economic benefit is low.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel production method which has low production cost and can generate phosphate concentrate powder without floatation. The process has simple starting and stopping procedures and strong digestion capability in the product market.
In order to solve the problems, the technical scheme of the invention is as follows: the method comprises the following steps of (1) carrying out acidolysis and filtration on low-grade phosphate ore by hydrochloric acid to obtain a mixed solution of dilute phosphoric acid and dilute calcium chloride, adding lime powder into the solution to enable phosphoric acid in the solution to generate tricalcium phosphate precipitate, filtering and separating to obtain a phosphate concentrate powder filter cake, naturally drying to obtain phosphate concentrate powder, and allowing a liquid phase to enter a synthesis process for continuous use, wherein the method comprises the following steps:
step one, lime powder is used for neutralizing a mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration, the mixed solution is reacted for about 3 to 6 hours at normal temperature, the mixed solution is continuously stirred during the neutralization reaction, and the final pH value is controlled between 4.5 and 5.0; the adding proportion of the lime powder is about 5-10% of the mass of the mixed solution;
secondly, performing solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure within about 1-2.0MPa to separate the solution from tricalcium phosphate solid phase to obtain a filter cake;
and thirdly, stacking filter cakes obtained by filter pressing at one position for natural drying to obtain the phosphate concentrate powder. The drying time depends on the weather condition, and is generally about 7-10 days.
Preferably, in the method for producing the phosphate concentrate powder, in the first step, the neutralization reaction is to gradually and slowly add the lime powder into the neutralization tank, the lime powder is added for 4 times, and 25 percent of the total weight of the lime powder is added every time, so that the wrapping is avoided.
Preferably, in the method for producing the phosphate concentrate powder, in the first step, the neutralization reaction is carried out in a neutralization tank under stirring, the stirring speed is controlled to be 15-23rpm, and the time of the neutralization reaction is about 2-4 hours, so that the materials are uniformly dispersed and the reaction is complete.
Preferably, the method for producing phosphate concentrate powder uses lime powder to precipitate tricalcium phosphate from phosphoric acid in the solution in the first step, and calcium chloride does not participate in the reaction.
Preferably, in the method for producing the phosphate concentrate powder, in the first step, during the neutralization of the solution and the lime powder, pH test paper is used for detecting the acid value of the solution every half hour, so that the pH value is finally controlled between 4.5 and 5.0.
Advantageous effects
The method provided by the invention mainly has the following advantages:
1. p in the phosphate rock powder can be separated by chemical ore dressing2O5The content of the compound is improved by about one time, and the economic benefit is increased. The low grade phosphate ore used at present contains P2O516.5 wt.%, the phosphate concentrate obtained contained P2O5At 31 wt.%.
2. Can make a small amount of hydrochloric acid in the mixed solution continue to react, increase the concentration of calcium chloride and is beneficial to improving the productivity of the next synthesis procedure.
3. After phosphoric acid is removed from the mixed solution, the interference in the synthesis of the calcium sulfate whisker is reduced, the synthesis time is shortened by about 4 hours, and the quality of the whisker product is improved.
4. The obtained phosphate concentrate powder can be naturally dried or directly sold, so that a large amount of energy can be saved, and a large amount of tail gas emission can be reduced.
5. The production operation is simple, and the production stability is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The adopted tubular reactor is purchased from Spiraria pernyi crown and bridge compound fertilizer scientific and technological service limited company with the model of WZDC-14, the mixed solution of the phosphoric acid and the calcium chloride obtained after the hydrochloric acid acidolysis for the raw material low-grade phosphate comes from Hubei Wayuxin material scientific and technological limited company, and the mass of the main chemical components in the mixed solution of the phosphoric acid and the calcium chloride obtained after the acidolysis filtrationFraction, P2O59% of CaCl214% of MgCl2The content was 10%.
Example 1
And (2) neutralizing the mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration by using lime powder, and gradually and slowly adding the lime powder into a neutralization tank, wherein the adding proportion of the lime powder is about 10 percent of the mass of the mixed solution, and the lime powder is added for 4 times, and the adding amount of the lime powder is 25 percent of the total amount of the lime powder. In order to avoid the wrapping phenomenon, stirring is carried out in a neutralization tank, the stirring speed is controlled at 23rpm, the neutralization time is about 4 hours at normal temperature, pH test paper is used for detecting the acid value of the solution every half hour, the final pH value is controlled at 4.5, the materials are uniformly dispersed, and the reaction is complete. The use of lime powder can make phosphoric acid in the solution form tricalcium phosphate precipitate, and calcium chloride does not participate in the reaction.
And (4) carrying out solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure to be about 2.0MPa to separate the solution from the tricalcium phosphate in a solid phase manner.
And stacking filter cakes obtained by filter pressing together for natural drying for about 7 days to obtain the phosphate concentrate powder.
The content test of the obtained phosphate concentrate powder shows that the mass fraction P of the main chemical components in the phosphate concentrate powder2O530.1% of MgO, 5.8% of Fe2O31.3% of Al2O31.0 percent, and meets the requirement of first grade II of GB/T1868 + 1995 phosphorite product standard.
Example 2
And (2) neutralizing the mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration by using lime powder, and gradually and slowly adding the lime powder into a neutralization tank, wherein the adding proportion of the lime powder is about 10 percent of the mass of the mixed solution, and the lime powder is added for 4 times, and the adding amount of the lime powder is 25 percent of the total amount of the lime powder. In order to avoid the wrapping phenomenon, stirring is carried out in a neutralization tank, the stirring speed is controlled at 23rpm, the neutralization time is about 4 hours at normal temperature, pH test paper is used for detecting the acid value of the solution every half hour, the final pH value is controlled at 5, the materials are uniformly dispersed, and the reaction is complete. The use of lime powder can make phosphoric acid in the solution form tricalcium phosphate precipitate, and calcium chloride does not participate in the reaction.
And (4) carrying out solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure to be about 2.0MPa to separate the solution from the tricalcium phosphate in a solid phase manner.
And stacking filter cakes obtained by filter pressing together for natural drying for about 10 days to obtain the phosphate concentrate powder.
The content test of the obtained phosphate concentrate powder shows that the mass fraction P of the main chemical components in the phosphate concentrate powder2O529.87% of MgO, 4.5% of Fe2O32.8% of Al2O31.1 percent, and meets the requirement of first grade II of GB/T1868-1995 phosphorite product standard.
Example 3
And (2) neutralizing the mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration by using lime powder, and gradually and slowly adding the lime powder into a neutralization tank, wherein the adding proportion of the lime powder is about 9 percent of the mass of the mixed solution, and the lime powder is added for 4 times, and the adding amount of the lime powder is 25 percent of the total amount of the lime powder. In order to avoid the wrapping phenomenon, stirring is carried out in a neutralization tank, the stirring speed is controlled at 23rpm, the neutralization time is about 4 hours at normal temperature, pH test paper is used for detecting the acid value of the solution every half hour, the final pH value is controlled at 4.5, the materials are uniformly dispersed, and the reaction is complete. The use of lime powder can make phosphoric acid in the solution form tricalcium phosphate precipitate, and calcium chloride does not participate in the reaction.
And stacking filter cakes obtained by filter pressing together for natural drying for about 10 days to obtain the phosphate concentrate powder.
The content test of the obtained phosphate concentrate powder shows that the mass fraction P of the main chemical components in the phosphate concentrate powder2O531.3% of MgO, 5.2% of Fe2O31.2% of Al2O3Is 0.7 percent, and meets the first-class requirement of GB/T1868-1995 phosphorite product standard.
Comparative example
And (2) neutralizing the mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration by using lime powder, gradually and slowly adding the lime powder into the neutralization tank, wherein the adding proportion of the lime powder is about 10 percent of the mass of the mixed solution, and adding the lime powder for 4 times. Adding 25% of the total amount of the lime powder each time. In order to avoid the wrapping phenomenon, stirring is carried out in a neutralization tank, the stirring speed is controlled at 23rpm, the neutralization time is about 4 hours at normal temperature, pH test paper is used for detecting the acid value of the solution every half hour, the final pH value is controlled at 7, the materials are uniformly dispersed, and the reaction is complete. The use of lime powder can make phosphoric acid in the solution form tricalcium phosphate precipitate, and calcium chloride does not participate in the reaction.
And (4) carrying out solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure to be about 2.0MPa to separate the solution from the tricalcium phosphate in a solid phase manner.
And stacking filter cakes obtained by filter pressing together for natural drying for about 10 days to obtain the phosphate concentrate powder.
The content test of the obtained phosphate concentrate powder shows that the mass fraction P of the main chemical components in the phosphate concentrate powder2O524.3% of MgO, 4.9% of Fe2O33.2% of Al2O32.1% P in phosphate concentrate powder, in comparison with the examples2O5The content is low.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A method for producing phosphate concentrate powder, comprising the steps of:
step one, lime powder is used for neutralizing a mixed solution of phosphoric acid and calcium chloride obtained after acidolysis and filtration;
secondly, performing solid-liquid separation on the neutralized suspension, conveying the solution into a plate-frame filter press by using a pump, and controlling the pressure within about 1-2.0MPa to separate the solution from tricalcium phosphate solid phase to obtain a filter cake;
thirdly, stacking filter cakes obtained by filter pressing at one position for natural drying or drying by utilizing a heat source to obtain phosphate concentrate powder, wherein P in the phosphate concentrate powder2O5The content is 28 wt.% to 38 wt.%.
2. The method of claim 1 wherein the lime powder is added in a proportion of about 5 to 10% by mass of the mixed solution.
3. The process according to claim 1, wherein in the first step, the neutralization reaction is carried out in a neutralization tank with stirring.
4. The method of claim 1, wherein the neutralization reaction is carried out at normal temperature for about 3 to 6 hours in the first step.
5. The method as claimed in claim 1, wherein the time for the natural drying in the third step is 7 to 10 days.
6. The method of claim 1, wherein in the third step, the heat source drying temperature is 110 ℃ to 200 ℃.
7. The method of claim 1, wherein in the first step, the acid value of the solution is measured using pH paper every half hour during the neutralization reaction.
8. The method of claim 3, wherein the rotation speed of the stirring is controlled to be 15-23rpm, and the time of the neutralization reaction is about 2-4 hours.
9. A method according to claim 3, characterized in that in the first step, the neutralization reaction is carried out by gradually and slowly adding lime powder into the neutralization tank, the addition being carried out in 4 portions, each of which adds 25% of the total weight of lime powder.
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| CN201811148107.5A CN110963475B (en) | 2018-09-29 | 2018-09-29 | Method for producing phosphate concentrate powder |
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Citations (9)
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|---|---|---|---|---|
| US3956464A (en) * | 1970-10-16 | 1976-05-11 | Pennzoil Company | Preparation of phosphates |
| CN101337657A (en) * | 2008-08-06 | 2009-01-07 | 黄明科 | Process for disassembling phosphate ore by mixed acid and coproducing potassium dihydrogen phosphate, hydrogen phosphate and combined fertilizer |
| CN101362594A (en) * | 2008-09-10 | 2009-02-11 | 云南天创科技有限公司 | Method for producing high-quality tricalcium phosphate |
| CN101380062A (en) * | 2008-08-26 | 2009-03-11 | 武汉凌派化工科技有限公司 | Method for producing feedstuff calcium hydrogen phosphate by decomposition of medium-low grade phosphate ore using hydrochloric acid |
| CN101456545A (en) * | 2008-12-25 | 2009-06-17 | 四川大学 | Method for producing triple superphosphate and co-producing calcium chloride by middle-low grade phosphate rock |
| CN101481105A (en) * | 2009-02-12 | 2009-07-15 | 上海彩凤饲料磷钙有限公司 | Process for preparing tricalcium phosphate |
| CN102583290A (en) * | 2012-02-18 | 2012-07-18 | 张黔生 | Low-grade phosphorite mineral dressing technology and method for producing by-product high-purity gypsum powder |
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2018
- 2018-09-29 CN CN201811148107.5A patent/CN110963475B/en active Active
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| US3956464A (en) * | 1970-10-16 | 1976-05-11 | Pennzoil Company | Preparation of phosphates |
| CN101337657A (en) * | 2008-08-06 | 2009-01-07 | 黄明科 | Process for disassembling phosphate ore by mixed acid and coproducing potassium dihydrogen phosphate, hydrogen phosphate and combined fertilizer |
| CN101380062A (en) * | 2008-08-26 | 2009-03-11 | 武汉凌派化工科技有限公司 | Method for producing feedstuff calcium hydrogen phosphate by decomposition of medium-low grade phosphate ore using hydrochloric acid |
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| CN101456545A (en) * | 2008-12-25 | 2009-06-17 | 四川大学 | Method for producing triple superphosphate and co-producing calcium chloride by middle-low grade phosphate rock |
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| CN102583290A (en) * | 2012-02-18 | 2012-07-18 | 张黔生 | Low-grade phosphorite mineral dressing technology and method for producing by-product high-purity gypsum powder |
| CN103496685A (en) * | 2013-10-14 | 2014-01-08 | 四川省化工设计院 | Method for continuously producing feed-grade dibasic calcium phosphate |
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