CN104556189A - Method for producing white gypsum being by-product of wet process phosphoric acid - Google Patents
Method for producing white gypsum being by-product of wet process phosphoric acid Download PDFInfo
- Publication number
- CN104556189A CN104556189A CN201410819001.9A CN201410819001A CN104556189A CN 104556189 A CN104556189 A CN 104556189A CN 201410819001 A CN201410819001 A CN 201410819001A CN 104556189 A CN104556189 A CN 104556189A
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- CN
- China
- Prior art keywords
- phosphoric acid
- wet process
- gypsum
- white gypsum
- reaction
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- 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
Abstract
The invention discloses a method for producing white gypsum being a by-product of wet process phosphoric acid and belongs to the technical field of production of phosphoric acid. The method comprises the following steps: (1) adding phosphorite powder into 15-25wt% of wet process phosphoric acid, controlling a liquid-solid ratio to be (12-15):1, controlling reaction temperature to be 75-90 DEG C, controlling reaction time to be 1-4 hours and filtering, wherein the content of phosphorus pentoxide in the phosphorite powder is 25-35wt%; (2) adding 93-98wt% of concentrated sulfuric acid into filtrate, stirring for reaction for 5-20 minutes, and carrying out solid-liquid separation to obtain white gypsum and phosphoric acid. A novel process of producing white phosphorous gypsum in the process of producing wet process phosphoric acid is developed; the production cost is reduced; the additional value is increased; the environmental pollution is reduced.
Description
Technical field
The invention belongs to phosphoric acid production technical field, particularly a kind of method of producing the white gypsum of phosphoric acid by wet process byproduct.
Background technology
The phosphogypsum that traditional Production By Sulfuric Acid Process phosphoric acid by wet process by-product is a large amount of, not only consumes a large amount of Sulphur ressource, and, often produce the phosphogypsum slag of one ton of phosphoric acid by wet process with regard to by-product about five tons.These phosphogypsum qualities are low can not be recycled, and depositing these phosphogypsums needs a large amount of funds and land resources, but also can cause environmental pollution, and therefore the exploitation of phosphogypsum slag are the urgent need to solve the problems that present each phosphoric acid production enterprise faces.
Summary of the invention
In order to solve the problem, realize the economic benefit of byproduct phosphogypsum, embodiments provide a kind of method of producing the white gypsum of phosphoric acid by wet process byproduct, the method comprises the following steps: ground phosphate rock joins in 15-25wt% phosphoric acid by wet process by (1), and controlling liquid-solid ratio is that 12-15:1(mL is to g, L is to Kg), temperature of reaction 75-90 DEG C, reaction times 1-4 hour, filter, wherein, in ground phosphate rock, the content of Vanadium Pentoxide in FLAKES is 25-35wt%.(2) in filtrate, add the vitriol oil of 93-98wt%, stirring reaction 5-20 minute, solid-liquid separation obtains white gypsum and phosphoric acid.Its reaction principle is:
The first step:
Ca
5F(PO
4)
3 + 7H
3PO
4+5H
2O —— 5Ca(H
2PO
4)
2.H
2O + HF↑
Second step:
Ca(H
2PO
4)
2.H
2O + H
2SO
4 + H
2O ——CaSO4.2H
2O↓ + 2H
3PO
4
Wherein, in the phosphoric acid by wet process in the embodiment of the present invention, the content of sulphur trioxide is less than 1.5wt%.
Preferably, in step (1), temperature of reaction is 80 DEG C, and the reaction times is 2 hours.
Preferably, in step (1), the liquid-solid ratio of phosphoric acid by wet process and ground phosphate rock is 12:1.
Preferably, in step (2), the concentration of the vitriol oil of use is 98wt%, stirring reaction 10 minutes.
Particularly, the method comprises the following steps:
(1) be that the ground phosphate rock of 25-35wt% joins the preferred 20wt% of 15-25wt%(by phosphorus pentoxide content) in phosphoric acid by wet process, controlling liquid-solid ratio is the preferred 12:1 of 12-15:1(), temperature of reaction 75-90 DEG C (preferably 80 DEG C), the 1-4 hour stirring reaction time (preferably 2 hours), stop stirring, leave standstill 5-20 minute (preferably 10 minutes), filter.
(2) vitriol oil (preferred 98wt%) of 93-98wt% is added in the filtrate obtained in step (1), stirring reaction 5-20 minute (preferably 10 minutes), stop stirring, leave standstill 20-60 minute (preferably 40 minutes), solid-liquid separation obtains white gypsum and phosphoric acid.Wherein, the phosphoric acid obtained can again for reacting as phosphoric acid by wet process and ground phosphate rock in step (1).
The method develops the novel process of producing white phosphogypsum in production phosphoric acid by wet process process, reduces production cost, improves pair value added, decreases environmental pollution.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below the present invention is described in further detail.
Embodiment 1
Get containing P
2o
520wt% phosphoric acid by wet process 400g, pulp 200g, add in 1000ml beaker simultaneously, when 80 DEG C, and 350r/min stirring reaction 2h.Stop stirring and leave standstill 10 minutes, filter gypsum tailings, gypsum tailings drying is weighed.Cross the vitriol oil 37g that cleaner liquid adds 98wt%, stir 10 minutes, leave standstill 40 minutes, filter white phosphogypsum, white phosphogypsum drying is weighed.Filtrate phosphoric acid is weighed to be detected.The parameter of phosphoric acid by wet process and breeze is as shown in table 1, and result data is as shown in table 2 and table 3:
Table 1
table 2
Table 3
As can be seen from above-mentioned data: phosphoric acid by wet process and breeze feed intake by 2:1, white gypsum average conversion only has about 9.5%, 20wt% phosphoric acid by wet process consumption inadequate, and breeze is excessive not to react completely too much.
Embodiment 2
Get containing P
2o
520wt% phosphoric acid by wet process 600g, pulp 100g, add in 1000ml beaker simultaneously, when 80 DEG C, and 350r/min stirring reaction 2h.Stop stirring and leave standstill 10 minutes, filter gypsum tailings, gypsum tailings drying is weighed.Cross the vitriol oil 30g that cleaner liquid adds 98wt%, stir 10 minutes, leave standstill 40 minutes, filter white phosphogypsum, white phosphogypsum drying is weighed.Filtrate phosphoric acid is weighed to be detected.The parameter of phosphoric acid by wet process and breeze is as shown in table 4, result data as shown in table 5 and table 6:
Table 4
table 5
Table 6
As can be seen from above-mentioned data: phosphoric acid by wet process and breeze feed intake by 6:1, white gypsum average conversion about 20.3%, phosphoric acid consumption reaches theoretical amount, and breeze is inexcessive, but breeze still has part not react.May be that monocalcium phosphate solubleness in phosphoric acid that reaction generates is little, a large amount of monocalcium phosphate be attached to breeze surface and have impact on reaction.
Embodiment 3
Get containing P
2o
520wt% phosphoric acid by wet process 600g, pulp 50g, add in 1000ml beaker simultaneously, when 80 DEG C, and 350r/min stirring reaction 2h.Stop stirring and leave standstill 10 minutes, filter gypsum tailings, gypsum tailings drying is weighed.Cross the vitriol oil 30g that cleaner liquid adds 98wt%, stir 10 minutes, leave standstill 40 minutes, filter white phosphogypsum, white phosphogypsum drying is weighed.Filtrate phosphoric acid is weighed to be detected.The parameter of phosphoric acid by wet process and breeze is as shown in table 7, and result data is as shown in table 8 and table 9:
Table 7
table 8
Table 9
As can be seen from above-mentioned data: phosphoric acid by wet process and breeze feed intake by 12:1, phosphoric acid consumption reaches 2 times of theoretical amount, in phosphoric acid, the content of sulphur trioxide is more than 2%, white gypsum transformation efficiency about 30%, in phosphoric acid, the content of sulphur trioxide is below 1.5%, white gypsum transformation efficiency about 36%, ground phosphate rock primitive reaction is complete.
Embodiment 4
Get containing P
2o
520wt% phosphoric acid by wet process 600g, pulp 40g, add in 1000ml beaker simultaneously, when 80 DEG C, and 350r/min stirring reaction 2h.Stop stirring and leave standstill 10 minutes, filter gypsum tailings, gypsum tailings drying is weighed.Cross the vitriol oil 30g that cleaner liquid adds 98wt%, stir 10 minutes, leave standstill 40 minutes, filter white phosphogypsum, white phosphogypsum drying is weighed.Filtrate phosphoric acid is weighed to be detected.The parameter of phosphoric acid by wet process and breeze is as shown in table 10, and result data is as shown in table 11 and table 12
Table 10
table 11
Table 12
As can be seen from above-mentioned data: phosphoric acid by wet process and breeze feed intake by 15:1, phosphoric acid consumption is excessive, and in phosphoric acid, the content of sulphur trioxide is more than 2%, white gypsum transformation efficiency about 35%, in phosphoric acid, the content of sulphur trioxide is below 1.5%, white gypsum average conversion about 40%.
Meanwhile, the present embodiment has also carried out phosphoric acid by wet process and breeze feeds intake by 18:1,20:1,22:1,24:1,25:1.Due to sulfur trioxide content in phosphoric acid by wet process about 2%, the dark plaster that the larger reaction of phosphoric acid consumption generates is more, and white gypsum transformation efficiency is more and more lower.
In addition, the present embodiment has also carried out amplification test to phosphoric acid by wet process and breeze in 12:1 ratio, the basis of lab scale amplifies 5 times, the transformation efficiency about 36% of white gypsum.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Various other that any technical conceive according to the present invention is made change and distortion accordingly, all should be included in the protection domain of the claims in the present invention.
Claims (4)
1. produce a method for the white gypsum of phosphoric acid by wet process byproduct, it is characterized in that: comprise the following steps:
(1) joined by ground phosphate rock in 15-25wt% phosphoric acid by wet process, control liquid-solid ratio is 12-15:1, temperature of reaction 75-90 DEG C, reaction times 1-4 hour, and filter, in described ground phosphate rock, the content of Vanadium Pentoxide in FLAKES is 25-35wt%;
(2) in filtrate, add the vitriol oil of 93-98wt%, stirring reaction 5-20 minute, solid-liquid separation obtains white gypsum and phosphoric acid.
2. the method for the white gypsum of production phosphoric acid by wet process byproduct according to claim 1, it is characterized in that, in described phosphoric acid by wet process, the content of sulphur trioxide is less than 1.5wt%.
3. the method for the white gypsum of production phosphoric acid by wet process byproduct according to claim 1, is characterized in that, in step (1), the liquid-solid ratio of phosphoric acid by wet process and ground phosphate rock is 12:1.
4. the method for the white gypsum of production phosphoric acid by wet process byproduct according to claim 1, is characterized in that, said method comprising the steps of:
(1) be that the ground phosphate rock of 25-35wt% joins in 15-25wt% phosphoric acid by wet process by phosphorus pentoxide content, control liquid-solid ratio is 12-15:1, temperature of reaction 75-90 DEG C, stirring reaction time 1-4 hour, stops stirring, and leaves standstill 5-20 minute, filters;
(2) in filtrate, add the vitriol oil of 93-98wt%, stirring reaction 5-20 minute, stop stirring, leave standstill 20-60 minute, solid-liquid separation obtains white gypsum and phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410819001.9A CN104556189A (en) | 2014-12-25 | 2014-12-25 | Method for producing white gypsum being by-product of wet process phosphoric acid |
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|---|---|---|---|
| CN201410819001.9A CN104556189A (en) | 2014-12-25 | 2014-12-25 | Method for producing white gypsum being by-product of wet process phosphoric acid |
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| CN104556189A true CN104556189A (en) | 2015-04-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154979A (en) * | 2015-09-18 | 2015-12-16 | 金正大诺泰尔化学有限公司 | Method for producing wet-process phosphoric acid and coproducing alpha-semi-hydrated gypsum whisker and high-purity high-whiteness alpha-semi-hydrated gypsum whisker |
| WO2017173717A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for directly using phosphogypsum decomposition gas in wet phosphoric acid production |
| CN113072046A (en) * | 2021-04-09 | 2021-07-06 | 郑州大学 | Method for removing impurities and improving whiteness of phosphogypsum through flotation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986394A (en) * | 2005-12-21 | 2007-06-27 | 张智新 | Production process of calcium dihydrogen phosphate |
| CN102001636A (en) * | 2010-09-26 | 2011-04-06 | 四川大学 | Method for producing broad-concentration phosphoric acid and clean plaster by middle-low grade phosphorus ore wet process |
| CN103626143A (en) * | 2013-11-29 | 2014-03-12 | 晏明朗 | Method for wet production of phosphoric acid and byproduct, namely white gypsum |
-
2014
- 2014-12-25 CN CN201410819001.9A patent/CN104556189A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986394A (en) * | 2005-12-21 | 2007-06-27 | 张智新 | Production process of calcium dihydrogen phosphate |
| CN102001636A (en) * | 2010-09-26 | 2011-04-06 | 四川大学 | Method for producing broad-concentration phosphoric acid and clean plaster by middle-low grade phosphorus ore wet process |
| CN103626143A (en) * | 2013-11-29 | 2014-03-12 | 晏明朗 | Method for wet production of phosphoric acid and byproduct, namely white gypsum |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154979A (en) * | 2015-09-18 | 2015-12-16 | 金正大诺泰尔化学有限公司 | Method for producing wet-process phosphoric acid and coproducing alpha-semi-hydrated gypsum whisker and high-purity high-whiteness alpha-semi-hydrated gypsum whisker |
| WO2017173717A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for directly using phosphogypsum decomposition gas in wet phosphoric acid production |
| CN113072046A (en) * | 2021-04-09 | 2021-07-06 | 郑州大学 | Method for removing impurities and improving whiteness of phosphogypsum through flotation method |
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Application publication date: 20150429 |
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