CN105502320A - Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite - Google Patents
Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite Download PDFInfo
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- CN105502320A CN105502320A CN201511024136.7A CN201511024136A CN105502320A CN 105502320 A CN105502320 A CN 105502320A CN 201511024136 A CN201511024136 A CN 201511024136A CN 105502320 A CN105502320 A CN 105502320A
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- phosphoric acid
- half water
- hemihydrated
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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
- C01B25/18—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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite, which comprises the following steps: by using medium/low-grade phosphorite as the raw material, grinding to prepare a phosphorite slurry, and carrying out floatation to remove partial impurities, thereby obtaining a medium/high-grade phosphorite concentrate; and by using the phosphorite concentrate and sulfuric acid as raw materials, carrying out phosphorite dissolution and crystallization reaction according to the conventional technological conditions for producing hemihydrated phosphoric acid, and filtering to prepare the high-concentration hemihydrated phosphoric acid. In the hemihydrated phosphoric acid slurry filtering process, the filter cake needs countercurrent washing three times, part of the secondary washing liquid is used as washing water of the primary washing procedure, and the rest secondary washing liquid is used as a raw material for producing feed-grade calcium hydrogen phosphate. The quantity of the washing water entering the hemihydrating reaction system is reduced, thereby ensuring the concentration of the hemihydrated phosphoric acid finished product. According to the method, part of the low-concentration higher-impurity secondary washing liquid is removed, thereby solving the problems that the high-concentration hemihydrated phosphoric acid can not be easily produced from the medium/low-grade phosphorite and the technical water in the hemihydrated phosphoric acid production process is difficult for balance.
Description
Technical field
The invention belongs to phosphoric acid chemical field, Wet-process Phosphoric Acid Production method and technology, be specifically related to a kind of method utilizing mid low grade phosphate rock to produce half water law phosphoric acid.
Background technology
The finished product phosphoric acid concentration produced due to half wet technology is high, can strong phosphoric acid, many-sided advantage such as half water material slurry intensity filter is large, product acid quality is good, energy consumption is low of direct production Vanadium Pentoxide in FLAKES concentration 38 ~ 45%, caused the great attention of phosphorous chemical industry enterprise in recent years, part phosphorous chemical industry enterprise builds and the half water law phosphoric acid production device that puts into operation.In order to ensure higher phosphoric acid concentration, dry ground phosphate rock must be raw material by the higher-grade of more than 28%, simultaneously in order to solve the balance total amount of production system process water, suitably must reduce the consumption of filter progress washing water, but reduce the washing effect that washing water consumption can have influence on half water phosphogypsum, cause the Washing ratio of filtration low.
Dilute phosphoric acid is that raw material carries out in two sections and the method for purification is produced in calcium hydrophosphate fodder process in a wet process, in wet method dilute phosphoric acid used, the concentration of Vanadium Pentoxide in FLAKES is generally about 5 ~ 10%, the too low then production efficiency of dilute phosphoric acid concentration is low, and dilute phosphoric acid excessive concentration then can reduce the yield of Vanadium Pentoxide in FLAKES.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, there is provided the production cost of a kind of reduction by half water phosphoric acid, improve half water phosphoric acid concentration, solve conventional half water law and produce the problem that process water in process phosphoric acid is difficult to balance, this method is applicable to all enterprises that two sections of neutralisations produce feed-grade calcium phosphate product salts.
The object of the invention is to realize by following technical solution.
Utilize mid low grade phosphate rock to produce a method for half water law phosphoric acid, comprise following process: produce higher-grade with low-grade phosphate ore by flotation and to wet phosphorus fine ore; With wet phosphorus fine ore and sulfuric acid for raw material, half water phosphoric acid production technique routinely produces half water phosphoric acid, in the filtration procedure of half water phosphatase reaction slip, two washing lotions of taking-up part lower concentration, high impurity are as the raw material producing calcium hydrophosphate fodder, remaining two washing lotions as a wash water, with a washing lotion as the dissolving and the crystallization reaction groove that return acid and enter half water phosphatase reaction; Half water phosphoric acid of obtained higher concentration after half water phosphoric acid material pulp filters.
Produce the raw material of half water phosphoric acid with mid low grade phosphate rock, the grade of phosphorus ore raw ore is 20 ~ 25%, after the impurity such as fragmentation, ball milling and reverse flotation remove portion magnesium, iron, aluminium, and high-grade wet phosphorus fine ore in obtained.
The present invention with the wet phosphorus fine ore of the phosphorus pentoxide content 24 ~ 30% of moisture content 9 ~ 15%, grade and phosphorus ore for raw material, according to half water phosphoric acid conventional production process as temperature of reaction, the reaction times, phosphorus ore dissolve and crystallizer tank in sulfate concentration, calcium ion concn etc. produce phosphoric acid.Present method reduces the oven dry link of phosphorus ore, can save coal consumption, power consumption, the productive expense such as artificial.
When the present invention's double water phosphoric acid material pulp filters, filter or turntable type filter etc. are filter plant as taped, and half water phosphogypsum filter cake needs through three countercurrent washings.When carrying out secondary washing, take out 10 ~ 50% of two washing filtrate total amounts, two washingss of phosphorus pentoxide content 5 ~ 12% are as the raw material producing calcium hydrophosphate fodder, two washing lotions of remaining 50 ~ 90% are then transported to one and wash operation, as the washing water that washes; Owing to decreasing two washing lotion consumptions of lower concentration, improve the concentration as returning Vanadium Pentoxide in FLAKES in a sour washing lotion, thus ensure that in half water phosphoric acid, Vanadium Pentoxide in FLAKES concentration reaches 40 ~ 45%.
The invention has the beneficial effects as follows, solve conventional half water law and produce the problem that process water in process phosphoric acid is difficult to balance, decrease the oven dry link of phosphorus ore, coal consumption, power consumption, the productive expense such as artificial can be saved.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
With the phosphorus ore raw ore of grade 21.6% for raw material, by broken, be milled to fineness and cross 100 orders and reach 93%, after the process of reverse flotation de-magging, filter flotation concentrate, obtain the wet phosphorus concentrate of grade 26.7%, moisture 9.3%.With the wet phosphorus concentrate after flotation and sulfuric acid for main raw material, carry out the solubilizing reaction of phosphorus ore and the crystallization reaction of half water phosphogypsum according to the common process condition of half water phosphoric acid production.At filter progress, take out 15% of two washing filtrate total amounts, the dilute phosphoric acid of phosphorus pentoxide content 7.9% for the production of the raw material of feed-grade calcium phosphate salt, the phosphorus pentoxide content of the finished product half water phosphoric acid finally obtained reaches 41.3%.
Embodiment 2
With the phosphorus ore raw ore of grade 21.2% for raw material, by broken, be milled to fineness and cross 100 orders and reach 91.5%, after the process of reverse flotation de-magging, filter flotation concentrate, obtain the wet phosphorus concentrate of grade 25.6%, moisture 10.5%.With the wet phosphorus concentrate after flotation and sulfuric acid for main raw material, carry out the solubilizing reaction of phosphorus ore and the crystallization reaction of half water phosphogypsum according to the common process condition of half water phosphoric acid production.At filter progress, take out 36% of two washing filtrate total amounts, the dilute phosphoric acid of phosphorus pentoxide content 10.1% for the production of the raw material of feed-grade calcium phosphate salt, the phosphorus pentoxide content of the finished product half water phosphoric acid finally obtained reaches 42.5%.
Embodiment 3
With the phosphorus ore raw ore of grade 20.8% for raw material, by broken, be milled to fineness and cross 100 orders and reach 92.6%, after the process of reverse flotation de-magging, filter flotation concentrate, obtain the wet phosphorus concentrate of grade 25.1%, moisture 13.5%.With the wet phosphorus concentrate after flotation and sulfuric acid for main raw material, carry out the solubilizing reaction of phosphorus ore and the crystallization reaction of half water phosphogypsum according to the common process condition of half water phosphoric acid production.At filter progress, take out 49% of two washing filtrate total amounts, the dilute phosphoric acid of phosphorus pentoxide content 15.1% for the production of the raw material of feed-grade calcium phosphate salt, the phosphorus pentoxide content of the finished product half water phosphoric acid finally obtained reaches 43.6%.
Claims (3)
1. utilize mid low grade phosphate rock to produce a method for half water law phosphoric acid, it is characterized in that, comprise following process: produce higher-grade with low-grade phosphate ore by flotation and to wet phosphorus fine ore; With wet phosphorus fine ore and sulfuric acid for raw material, half water phosphoric acid production technique routinely produces half water phosphoric acid, in the filtration procedure of half water phosphatase reaction slip, two washing lotions of taking-up part lower concentration, high impurity are as the raw material producing calcium hydrophosphate fodder, remaining two washing lotions as a wash water, with a washing lotion as the dissolving and the crystallization reaction groove that return acid and enter half water phosphatase reaction; Half water phosphoric acid of obtained higher concentration after half water phosphoric acid material pulp filters.
2. a kind of method utilizing mid low grade phosphate rock to produce half water law phosphoric acid according to claim 1, it is characterized in that: the phosphorus ore producing half water phosphoric acid is mid low grade phosphate rock, the grade of phosphorus ore raw ore is 20 ~ 25%, after the impurity such as reverse flotation remove portion magnesium, iron, aluminium, the wet phosphorus fine ore of obtained phosphorus pentoxide content 24 ~ 30%, moisture 9 ~ 13%.
3. a kind of method utilizing mid low grade phosphate rock to produce half water law phosphoric acid according to claim 1, it is characterized in that: in the filtration procedure of half water phosphoric acid material pulp, half water phosphogypsum filter cake needs through three countercurrent washings, take out 10 ~ 50% of two washing lotion total amounts, two washingss of phosphorus pentoxide content 5 ~ 12% are as the raw material producing calcium hydrophosphate fodder, two washing lotions of remaining 50 ~ 90% are then transported to one and wash operation, as the washing water that washes; Owing to decreasing two washing lotion consumptions of lower concentration, improve the concentration as returning Vanadium Pentoxide in FLAKES in a sour washing lotion, thus still can ensure that half water phosphoric acid Vanadium Pentoxide in FLAKES concentration reaches 40 ~ 45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511024136.7A CN105502320A (en) | 2015-12-30 | 2015-12-30 | Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511024136.7A CN105502320A (en) | 2015-12-30 | 2015-12-30 | Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite |
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| CN105502320A true CN105502320A (en) | 2016-04-20 |
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| CN201511024136.7A Pending CN105502320A (en) | 2015-12-30 | 2015-12-30 | Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110902665A (en) * | 2019-12-12 | 2020-03-24 | 昆明川金诺化工股份有限公司 | Method for improving semi-hydrated phosphoric acid concentration and washing rate |
| CN115959641A (en) * | 2022-12-13 | 2023-04-14 | 昆明川金诺化工股份有限公司 | Method for producing wet-process phosphoric acid from low-grade phosphate ore direct flotation phosphate tailings and application thereof |
| CN116768171A (en) * | 2023-06-28 | 2023-09-19 | 昆明川金诺化工股份有限公司 | Process for producing high-quality semi-aqueous wet-process phosphoric acid |
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| CN1669915A (en) * | 2005-02-01 | 2005-09-21 | 云南三环化工有限公司 | Method for improving property of dihydrate wet-process phosphoric acid reaction slurry |
| CN1789118A (en) * | 2004-12-17 | 2006-06-21 | 冯孝桂 | Method for producing feed calcium hydrogen phosphate using sulphuric acid method |
| CN1792776A (en) * | 2005-12-23 | 2006-06-28 | 中国石化集团南京设计院 | Process for producing wet method phosphoric acid by medium low grade phosphorus mine |
| CN1994870A (en) * | 2006-12-21 | 2007-07-11 | 四川大学 | Process for preparing high concentration phosphoric acid from middle-and low-grade phosphorus ore |
| CN103213960A (en) * | 2013-05-17 | 2013-07-24 | 成都川科化工有限公司 | Method for producing phosphoric acid by decomposing low-grade phosphate rock with wet-process phosphoric acid |
| CN103213964A (en) * | 2013-05-17 | 2013-07-24 | 成都川科化工有限公司 | Method for producing wet-process phosphoric acid by utilizing low-grade phosphorite |
-
2015
- 2015-12-30 CN CN201511024136.7A patent/CN105502320A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789118A (en) * | 2004-12-17 | 2006-06-21 | 冯孝桂 | Method for producing feed calcium hydrogen phosphate using sulphuric acid method |
| CN1669915A (en) * | 2005-02-01 | 2005-09-21 | 云南三环化工有限公司 | Method for improving property of dihydrate wet-process phosphoric acid reaction slurry |
| CN1792776A (en) * | 2005-12-23 | 2006-06-28 | 中国石化集团南京设计院 | Process for producing wet method phosphoric acid by medium low grade phosphorus mine |
| CN1994870A (en) * | 2006-12-21 | 2007-07-11 | 四川大学 | Process for preparing high concentration phosphoric acid from middle-and low-grade phosphorus ore |
| CN103213960A (en) * | 2013-05-17 | 2013-07-24 | 成都川科化工有限公司 | Method for producing phosphoric acid by decomposing low-grade phosphate rock with wet-process phosphoric acid |
| CN103213964A (en) * | 2013-05-17 | 2013-07-24 | 成都川科化工有限公司 | Method for producing wet-process phosphoric acid by utilizing low-grade phosphorite |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110902665A (en) * | 2019-12-12 | 2020-03-24 | 昆明川金诺化工股份有限公司 | Method for improving semi-hydrated phosphoric acid concentration and washing rate |
| CN110902665B (en) * | 2019-12-12 | 2022-11-15 | 昆明川金诺化工股份有限公司 | Method for improving semi-hydrated phosphoric acid concentration and washing rate |
| CN115959641A (en) * | 2022-12-13 | 2023-04-14 | 昆明川金诺化工股份有限公司 | Method for producing wet-process phosphoric acid from low-grade phosphate ore direct flotation phosphate tailings and application thereof |
| CN116768171A (en) * | 2023-06-28 | 2023-09-19 | 昆明川金诺化工股份有限公司 | Process for producing high-quality semi-aqueous wet-process phosphoric acid |
| CN116768171B (en) * | 2023-06-28 | 2024-07-02 | 昆明川金诺化工股份有限公司 | Process for producing high-quality semi-aqueous wet-process phosphoric acid |
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