CN103213964A - Method for producing wet-process phosphoric acid by utilizing low-grade phosphorite - Google Patents
Method for producing wet-process phosphoric acid by utilizing low-grade phosphorite Download PDFInfo
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- CN103213964A CN103213964A CN2013101854673A CN201310185467A CN103213964A CN 103213964 A CN103213964 A CN 103213964A CN 2013101854673 A CN2013101854673 A CN 2013101854673A CN 201310185467 A CN201310185467 A CN 201310185467A CN 103213964 A CN103213964 A CN 103213964A
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Abstract
The invention discloses a method for producing wet-process phosphoric acid by utilizing low-grade phosphorite. The method is characterized by adopting a two-step reaction and backwashing method and specifically comprises the steps of: in first-step reaction, decomposing phosphorite with phosphoric acid in an extraction tank, and removing residues through solid-liquid separation to obtain clear liquid; and in the second-step reaction, reacting the extracted clear liquid with sulfuric acid in a reactor to generate calcium sulphate dihydrate crystal (ardealite) and phosphoric acid solution, and performing solid-liquid separation to obtain the phosphoric acid solution and the ardealite, returning a part of phosphoric acid solution to be used for decomposing phosphorite and a part of phosphoric acid solution to be used for outputting finished products. High-concentration high-quality wet-process phosphoric acid can be produced by utilizing the low-grade phosphorite; the phosphoric acid yield is high; and in addition, the white gypsum side product capable of being widely applied directly can be obtained. The method has wide industrial application prospects.
Description
Technical field
The present invention relates to a kind of method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process, belong to the Wet-process Phosphoric Acid Production field.
Background technology
Phosphoric acid by wet process is one of important method of producing phosphoric acid, also is the basic product of phosphorous chemical industry industry, is widely used in the middle of the multiple fertile industry of phosphate industry and phosphorus, and demand is big.The production technique of phosphoric acid by wet process mainly is to produce phosphoric acid based on mineral acid (sulfuric acid) decomposing phosphate rock.The phosphate rock resource total amount of China is near 50,000,000,000 t, and P in the phosphorus ore
2O
5The rich ore of content more than 30% only accounts for the about 8% of reserves, and the overwhelming majority is a low grade ore, phosphorus ore P
2O
5Average grade only is 16.85%, and mostly is collophanite greatly, and the selecting and purchasing difficulty is big, enrichment cost height.Utilize low-grade (P
2O
5﹤ 24%) phosphorus ore then is the future development trend of China's phosphorous chemical industry industry.
Show that from existing document and data except that no water law flow process does not have the industrialized unit as yet, other technical process mainly contains two wet technologies and half wet technology.But along with the reduction gradually of world's phosphorus ore grade and the increase of foreign matter content, two water law flow processs are to the adaptability of phosphorus ore and the reliability of technology, and stability is stronger, dominate in large-scale wet method phosphoric acid manufacture process.Parts such as the wherein employing two water law productions of wet-process phosphoric acid production plant more than 80%, wet phosphoric acid by dihydrate production process mainly comprise reaction, filtration, concentrate, washing tail gas, acid storage.Sulfuric acid and phosphorus ore carry out extractive reaction in a reactive tank, the main phosphoric acid of production liquid phase, solid phase are mainly the phosphoric acid material pulp of phosphogypsum; With phosphoric acid material pulp filtering separation in filter, filtrate is the dilute phosphoric acid product then, and filter residue is a phosphogypsum, stores up; The dilute phosphoric acid product further improves its concentration to 50% by concentrating; The tail gas of reactive moieties meets environmental protection standard by repeatedly washing back emptying.
One of principal feature of low-grade phosphate ore is that the acid non-soluble substance foreign matter content is high especially, and it almost all enters in the phosphogypsum when adopting traditional phosphoric acid production method to generate phosphoric acid, thereby the phosphogypsum quality is reduced greatly, causes its comprehensive utilization difficulty.And because foreign matter content height in the low-grade phosphate ore, it is low that rate of decomposition appears in phosphorus ore regular meeting, and the washing rate is low, and the calcium sulfate parcel that reaction generates makes the reaction passivation, and generating calcium hydrophosphate crystal has increased P
2O
5Loss, crystal of calcium sulfate is difficult to separate, problem such as cause that the finished product phosphoric acid quality is on duty mutually, thereby cause production cost high unusually, produce extremely unstable, thereby can't produce agricultural diammonium phosphate and the agricultural monoammonium phosphate of excellent level.
Chinese patent CN9110859.7 " tower Wet-process Phosphoric Acid Production method and apparatus " mentions being the raw material production phosphoric acid by wet process with mid low grade phosphate rock, but its used phosphorus ore grade P
2O
5≧ 25%, available mid low grade phosphate rock scope is narrower; This method directly enters extraction tower and sulfuric acid reaction with the mixed slurry of ground phosphate rock and recycled phosphoric acid, impurity in the phosphorus ore and phosphogypsum is not separated; And use the vitriol oil as extraction agent, cause local SO
4 2-Concentration is big, makes reaction not exclusively.
Chinese patent 200510022547.2 " utilizes mid low grade phosphate rock to produce the method for phosphoric acid by wet process " and mentions that also its method can be the raw material production phosphoric acid by wet process with the mid low grade phosphate rock, but its used phosphorus ore grade is P
2O
5%:18～26%, and require MgO ≦ 2.0wt%, Fe
2O
3+ Al
2O
3≦ 3.5wt%; Its foreign matter content to phosphorus ore has is strict with, while flow process complexity, complicated, the two sections reaction of high order of reaction, thus make the cost height, do not possess the industrialization ubiquity; This method adopts multi-stage counter current extraction, and operating process is long, and production equipment requires high; Do not have the washing and the wash water utilization of residue, gypsum simultaneously, fail to realize the effective profit of industrialization of resource technology.Industrialization has sizable difficulty.
Summary of the invention
The objective of the invention is at the rapid exhaustion of higher-grade phosphorus ore in China and low-grade phosphate ore is more relatively and low-cost reality, but there are many shortcomings in conventional wet phosphoric acid production method when adopting mid low grade phosphate rock, and a kind of method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process is provided, technical process is succinct, convenient, easy handling obtains high-quality white phosphogypsum simultaneously.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise:
The method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process is to adopt two-step reaction, countercurrent washing flow process, produces higher concentration quality product matter phosphoric acid by wet process and high-quality white gypsum by low-grade phosphate ore, and concrete steps are as follows:
Step 1, usefulness phosphorolytic cleavage low-grade phosphate ore ore pulp obtain calcic extraction clear liquid and filter residue through the solid-liquid separation I;
Step 2, with above-mentioned extraction clear liquid and sulfuric acid reaction, obtain phosphoric acid by wet process and phosphogypsum through the solid-liquid separation II; Part phosphoric acid returns and is used for decomposing phosphate rock, and part phosphoric acid is exported as finished product;
The quality of described low-grade phosphate ore is: P
2O
5Content is 20～23wt%, and other impurity does not have particular requirement.
When described step 1 was reacted: with concentration was 25.5～36wt%P
2O
5The phosphoric acid extraction phosphorus ore, liquid-solid ratio=22～27 in the extraction slip are at 35～57 ℃ of temperature reaction, 3～8h.
Described calcic extraction clear liquid and 92 ~ 98wt% sulfuric acid reaction generate the terra alba crystallization, and the sulfuric acid consumption is 109～120% of a stoichiometric quantity, at 80～95 ℃ of reactions of temperature, 3～6h; Generating concentration of phosphoric acid is 24.5～35 wt % P
2O
5
The separation method that described solid-liquid separation adopts vacuum filtration, washing and adding auxiliary agent to combine.
Described auxiliary agent is at least a in polyacrylamide, modified polyacrylamide, polymerization ferrous sulfate and the polymerize aluminum chloride, and the addition of auxiliary agent is 2～50ppm.
Performance test
Adopt GB/T 1871.1-1995 standard as follows to product phosphoric acid test result
1, product phosphoric acid quality: P
2O
5=26.58wt%, CaO=0.23wt%, SO
4 2-=1.42 wt%, MgO=1.25 wt%, Fe
2O
3=0.57 wt%, Al
2O
3=0.78wt%, F=6325ppm.
2, product phosphoric acid quality: P
2O
5=33.76wt%, CaO=0.67wt%, SO
4 2-=1.75 wt%, MgO=2.23wt%, Fe
2O
3=1.16 wt%, Al
2O
3=0.94wt%, F=58630ppm.
The present invention compared with prior art has the following advantages:
1, low-grade phosphate ore be can use,, phosphorus ore source of supply and the industrialized universality of technology enlarged foreign matter content no requirement (NR)s such as magnesium iron in the phosphorus ore;
2, directly use low-grade phosphate ore, simplify its phosphorus enrichment process, technical process is simple;
3, phosphorus ore percentage extraction of the present invention, washing rate and P
2O
5Rate of recovery height (phosphorus ore P
2O
5Percentage extraction 〉=95%, P
2O
5Washing rate 〉=98%, P
2O
5The rate of recovery 〉=95%), phosphoric acid concentration is 25～35%, is better than existing other method;
4, washing water efficiently utilize: the phosphogypsum washing water return the washing that is used for filter residue, and its washing water finally enter the ore grinding step, realize that washing water efficiently utilize, and improve the washing rate of Vanadium Pentoxide in FLAKES, can realize industrialization.
5, filter residue and phosphogypsum are separated, obtained high-quality white phosphogypsum product, improved the utility value of phosphogypsum;
6, the sulfuric acid add-on is 109～120% of a reaction formula stoichiometric quantity, the CaO in the product phosphoric acid, MgO, Fe
2O
3, Al
2O
3Content low, improved the phosphoric acid quality.
Description of drawings
Fig. 1 utilizes low-grade phosphate ore to produce the process flow sheet of phosphoric acid by wet process
1, ore grinding, 2, single step reaction, 3, separate I, the reaction of 4, two steps, 5, separate II, 6, the washing I,
7, washing II.
Embodiment
Below by embodiment the present invention is specifically described, be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified, but can not be interpreted as limiting the scope of the invention.The person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1:
The method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process may further comprise the steps:
Step 1: with low-grade phosphate ore (P
2O
5=23.00wt%, CaO=40.07wt%, MgO=3.20, Fe
2O
3=1.52 wt%, Al
2O
3=0.55 wt%) prepares the phosphorus ore ore pulp, then with phosphoric acid (P
2O
5=25.83wt%) carry out single step reaction, 42 ℃～50 ℃ of temperature, reaction 3h, liquid-solid ratio=27 in the extraction slip, reaction finishes, and the back adds polyacrylamide 20ppm, modified polyacrylamide 20ppm, polymerization ferrous sulfate 10ppm obtain extracting clear liquid and filter residue through separating the I operation, and percentage extraction is 95.1%;
Step 2: in special reactor, add 1 portion of extraction clear liquid and 1.12 times of calculated amount sulfuric acid, sulfuric acid=98wt%, temperature maintenance is reacted 3h at 80 ℃～85 ℃.Reaction solution adds polyacrylamide 20ppm, modified polyacrylamide 20ppm, polymerization ferrous sulfate 10ppm after separating II, and liquid is higher quality phosphoric acid by wet process (P
2O
5=24.94wt%), the Vanadium Pentoxide in FLAKES yield is 99.12%; Solid is a product white phosphogypsum.Wherein part phosphoric acid returns extraction tank and is used for decomposing phosphate rock, and part phosphoric acid is exported as finished product.
Step 3: after the filter residue that step 1 reaction obtains was operated through the washing I, its washing water were used for phosphorus ore slurrying, and the residual washing-out rate is 98.82%; Step 2 reaction obtains gypsum, and through obtaining high-quality white phosphogypsum after the operation of washing II, its washing water enter the washing I and reuse, and the washing rate is 98.43%.
Embodiment 2:
The method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process may further comprise the steps:
Step 1: with low-grade phosphate ore (P
2O
5=20.07wt%, CaO=43.13wt%, MgO=2.56, Fe
2O
3=1.23 wt%, Al
2O
3=0.67 wt%) prepares the phosphorus ore ore pulp, then with phosphoric acid (P
2O
5=35.96wt%) carry out extractive reaction, 35 ℃～42 ℃ of temperature, reaction 8h, liquid-solid ratio=25 in the extraction slip, add polyacrylamide 10ppm, modified polyacrylamide 20ppm after reaction finishes and obtain extracting clear liquid and filter residue through lock out operation, percentage extraction is 96.12%;
Step 2: in special reactor, add 1 portion of extraction clear liquid and 1.20 times of calculated amount sulfuric acid, sulfuric acid=92wt%, temperature maintenance is reacted 6h at 85 ℃～90 ℃.Reaction solution adds polyacrylamide 10ppm, modified polyacrylamide 20ppm after separating II, and liquid is higher quality phosphoric acid by wet process (P
2O
5=34.95wt%), the Vanadium Pentoxide in FLAKES yield is 98.22%; Solid is a product white phosphogypsum.Wherein part phosphoric acid returns extraction tank and is used for decomposing phosphate rock, and part phosphoric acid is exported as finished product.
Step 3: after the filter residue that step 1 reaction obtains was operated through the washing I, its washing water were used for phosphorus ore slurrying, and the residual washing-out rate is 98.14%; Step 2 reaction obtains gypsum, and through obtaining high-quality white phosphogypsum after the operation of washing II, its washing water enter the washing I and reuse, and the washing rate is 98.82%.
Embodiment 3:
The method of utilizing low-grade phosphate ore to produce phosphoric acid by wet process comprises the steps:
Step 1: with low-grade phosphate ore (P
2O
5=21.32wt%, CaO=39.67wt%, MgO=3.18, Fe
2O
3=1.19 wt%, Al
2O
3=0.89 wt%) prepares the phosphorus ore ore pulp, then with phosphoric acid (P
2O
5=27.52wt%) carry out extractive reaction, 48 ℃～57 ℃ of temperature, reaction 6h, liquid-solid ratio=22 in the extraction slip add polyacrylamide 2ppm after reaction finishes and obtain extracting clear liquid and filter residue through lock out operation, and percentage extraction is 95.67%;
Step 2: in special reactor, add 1 portion of extraction clear liquid and 1.09 times of calculated amount sulfuric acid, sulfuric acid=96wt%, temperature maintenance is fully reacted 5h at 90 ℃～95 ℃.Reaction solution adds polyacrylamide 2ppm after separating II, and liquid is higher quality phosphoric acid by wet process (P
2O
5=26.27wt%), the Vanadium Pentoxide in FLAKES yield is 98.87%; Solid is a product white phosphogypsum.Wherein part phosphoric acid returns extraction tank and is used for decomposing phosphate rock, and part phosphoric acid is exported as finished product.
Step 3: after the filter residue that step 1 reaction obtains was operated through the washing I, its washing water were used for phosphorus ore slurrying, and the residual washing-out rate is 98.14%; Step 2 reaction obtains gypsum, and through obtaining high-quality white phosphogypsum after the operation of washing II, its washing water enter the washing I and reuse, and the washing rate is 98.91%.
Claims (6)
1. utilize low-grade phosphate ore to produce the method for phosphoric acid by wet process, it is characterized in that this method is to adopt two-step reaction, countercurrent washing flow process, produce higher concentration quality product matter phosphoric acid by wet process and high-quality white gypsum by low-grade phosphate ore, concrete steps are as follows:
Step 1, usefulness phosphorolytic cleavage low-grade phosphate ore ore pulp obtain calcic extraction clear liquid and filter residue through the solid-liquid separation I;
Step 2, with above-mentioned extraction clear liquid and sulfuric acid reaction, obtain phosphoric acid by wet process and phosphogypsum through the solid-liquid separation II; Part phosphoric acid returns and is used for decomposing phosphate rock, and part phosphoric acid is exported as finished product;
Step 3, with above-mentioned filter residue through the washing I, washing water are used for phosphorus ore slurrying; With above-mentioned phosphogypsum, obtain high-quality white phosphogypsum through the washing II, washing water enter the recycle of step I.
2. according to the described method of utilizing low-grade phosphate ore to produce phosphoric acid of claim 1, it is characterized in that the quality of low-grade phosphate ore is: P
2O
5Content is 20～23wt%, and other impurity does not have particular requirement.
3. according to the described method of utilizing low-grade phosphate ore to produce phosphoric acid of claim 1, when it is characterized in that step 1 reaction: with concentration is 25.5～36wt%P
2O
5The phosphoric acid extraction phosphorus ore, liquid-solid ratio=22～27 in the extraction slip are at 35～57 ℃ of temperature reaction, 3～8h.
4. according to the described method of utilizing low-grade phosphate ore to produce phosphoric acid of claim 1, it is characterized in that calcic extraction clear liquid and 92 ~ 98wt% sulfuric acid reaction generate the terra alba crystallization, the sulfuric acid consumption is 109～120% of a stoichiometric quantity, at 80～95 ℃ of reactions of temperature, 3～6h; Generating concentration of phosphoric acid is 24.5～35 wt % P
2O
5
5. according to the described method of utilizing low-grade phosphate ore to produce phosphoric acid of claim 1, it is characterized in that the separation method that solid-liquid separation adopts vacuum filtration, washing and adding auxiliary agent to combine.
6. according to claim 1 or the 5 described methods of utilizing low-grade phosphate ore to produce phosphoric acid, it is characterized in that auxiliary agent is at least a in polyacrylamide, modified polyacrylamide, polymerization ferrous sulfate and the polymerize aluminum chloride, the addition of auxiliary agent is 2～50ppm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626143A (en) * | 2013-11-29 | 2014-03-12 | 晏明朗 | Method for wet production of phosphoric acid and byproduct, namely white gypsum |
| CN103803517A (en) * | 2014-02-27 | 2014-05-21 | 龚家竹 | Method for producing byproduct low-silicon ardealite by using high-silicon phosphorite |
| CN105502320A (en) * | 2015-12-30 | 2016-04-20 | 昆明川金诺化工股份有限公司 | Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite |
| CN105523533A (en) * | 2016-01-22 | 2016-04-27 | 贵州能矿织金磷化工有限公司 | Method for preparing high-quality phosphoric acid and high-quality phosphogypsum by leaching rare-earth-containing phosphorite with reproducible phosphoric acid |
| CN106044730A (en) * | 2016-06-03 | 2016-10-26 | 四川宏达股份有限公司 | Method for producing wet-process phosphoric acid from high-grade phosphate ore |
| CN106564925A (en) * | 2016-11-01 | 2017-04-19 | 昆明理工大学 | Method for preparing calcium sulfate whisker and phosphate compound fertilizer by coupling inorganic acid and sulfate and decomposing phosphate rock |
| CN109748252A (en) * | 2019-03-19 | 2019-05-14 | 济南大学 | A method of half water phosphoric acid by wet process is prepared using the controllable acidolysis of mid low grade phosphate rock |
| CN110548317A (en) * | 2019-09-20 | 2019-12-10 | 瓮福达州化工有限责任公司 | Flocculating agent and impurity sedimentation system suitable for wet-process phosphoric acid production |
| CN111362651A (en) * | 2020-04-03 | 2020-07-03 | 沈阳促晋科技有限公司 | High-performance autoclaved aerated concrete block prepared from graphite tailings and phosphorus tailings and preparation method thereof |
| CN112408346A (en) * | 2020-11-23 | 2021-02-26 | 中国科学院过程工程研究所 | Method for preparing low-impurity wet-process phosphoric acid and calcium sulfate by controlled acidolysis and synchronous extraction of phosphorite |
| CN113651300A (en) * | 2021-08-16 | 2021-11-16 | 四川绵竹市盘龙矿物质有限责任公司 | Method for improving phosphorus yield by using phosphorite with high calcium-phosphorus ratio for wet-process phosphoric acid purification |
| CN114804061A (en) * | 2021-01-19 | 2022-07-29 | 中国科学院过程工程研究所 | Device system and method for preparing wet-process phosphoric acid by synchronously extracting and separating impurities in acid splitting of phosphorite |
| CN115504440A (en) * | 2022-10-29 | 2022-12-23 | 山东联盟磷复肥有限公司 | Double-circulation wet-process phosphoric acid production method |
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| CN109573972B (en) * | 2019-01-23 | 2021-05-28 | 山东鲁北企业集团总公司 | Method for producing phosphoric acid and low-silicon gypsum from medium-low grade phosphorite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626143A (en) * | 2013-11-29 | 2014-03-12 | 晏明朗 | Method for wet production of phosphoric acid and byproduct, namely white gypsum |
| CN103803517A (en) * | 2014-02-27 | 2014-05-21 | 龚家竹 | Method for producing byproduct low-silicon ardealite by using high-silicon phosphorite |
| CN103803517B (en) * | 2014-02-27 | 2015-11-18 | 龚家竹 | The method of the low silicon ardealite of high silicon Phosphate Rock acid by-product |
| CN105502320A (en) * | 2015-12-30 | 2016-04-20 | 昆明川金诺化工股份有限公司 | Method for producing hemihydrated phosphoric acid from medium/low-grade phosphorite |
| CN105523533B (en) * | 2016-01-22 | 2017-12-15 | 贵州能矿织金磷化工有限公司 | The method for producing high-quality phosphoric acid and high-quality ardealite containing rare earth phosphate rock with regeneration phosphoric acid leaching |
| CN105523533A (en) * | 2016-01-22 | 2016-04-27 | 贵州能矿织金磷化工有限公司 | Method for preparing high-quality phosphoric acid and high-quality phosphogypsum by leaching rare-earth-containing phosphorite with reproducible phosphoric acid |
| CN106044730B (en) * | 2016-06-03 | 2018-05-18 | 四川宏达股份有限公司 | Utilize the method for high-grade phosphorus ore production phosphoric acid by wet process |
| CN106044730A (en) * | 2016-06-03 | 2016-10-26 | 四川宏达股份有限公司 | Method for producing wet-process phosphoric acid from high-grade phosphate ore |
| CN106564925A (en) * | 2016-11-01 | 2017-04-19 | 昆明理工大学 | Method for preparing calcium sulfate whisker and phosphate compound fertilizer by coupling inorganic acid and sulfate and decomposing phosphate rock |
| CN109748252A (en) * | 2019-03-19 | 2019-05-14 | 济南大学 | A method of half water phosphoric acid by wet process is prepared using the controllable acidolysis of mid low grade phosphate rock |
| CN110548317A (en) * | 2019-09-20 | 2019-12-10 | 瓮福达州化工有限责任公司 | Flocculating agent and impurity sedimentation system suitable for wet-process phosphoric acid production |
| CN111362651A (en) * | 2020-04-03 | 2020-07-03 | 沈阳促晋科技有限公司 | High-performance autoclaved aerated concrete block prepared from graphite tailings and phosphorus tailings and preparation method thereof |
| CN112408346A (en) * | 2020-11-23 | 2021-02-26 | 中国科学院过程工程研究所 | Method for preparing low-impurity wet-process phosphoric acid and calcium sulfate by controlled acidolysis and synchronous extraction of phosphorite |
| CN114804061A (en) * | 2021-01-19 | 2022-07-29 | 中国科学院过程工程研究所 | Device system and method for preparing wet-process phosphoric acid by synchronously extracting and separating impurities in acid splitting of phosphorite |
| CN114804061B (en) * | 2021-01-19 | 2024-01-26 | 中国科学院过程工程研究所 | Device system and method for preparing wet-process phosphoric acid by synchronously extracting and separating impurities through acidolysis of phosphorite |
| CN113651300A (en) * | 2021-08-16 | 2021-11-16 | 四川绵竹市盘龙矿物质有限责任公司 | Method for improving phosphorus yield by using phosphorite with high calcium-phosphorus ratio for wet-process phosphoric acid purification |
| CN115504440A (en) * | 2022-10-29 | 2022-12-23 | 山东联盟磷复肥有限公司 | Double-circulation wet-process phosphoric acid production method |
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