CN103213964B - Low-grade phosphate ore is utilized to produce the method for phosphoric acid by wet process - Google Patents
Low-grade phosphate ore is utilized to produce the method for phosphoric acid by wet process Download PDFInfo
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- CN103213964B CN103213964B CN201310185467.3A CN201310185467A CN103213964B CN 103213964 B CN103213964 B CN 103213964B CN 201310185467 A CN201310185467 A CN 201310185467A CN 103213964 B CN103213964 B CN 103213964B
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- phosphoric acid
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Abstract
The invention discloses the method utilizing low-grade phosphate ore to produce phosphoric acid by wet process, be characterized in the method adopting two-step reaction, countercurrent washing, concrete steps are: in extraction tank, use phosphorolytic cleavage phosphorus ore during the first step reaction, obtain clear liquid through solid-liquid separation removing residue; Second step reaction will extract clear liquid and sulfuric acid reaction in the reactor, generates Crystallization of Gypsum (phosphogypsum) and phosphoric acid solution, obtain phosphoric acid solution and phosphogypsum through solid-liquid separation; Phosphoric acid solution part returns for decomposing phosphate rock, and part exports as finished product.Low-grade phosphate ore is utilized to produce higher concentration quality product matter phosphoric acid by wet process; Phosphoric acid yield is high; Meanwhile, obtaining can the white gypsum by-product of direct widespread use.The prospects for commercial application of the method is wide.<!--1-->
Description
Technical field
The present invention relates to a kind of method utilizing low-grade phosphate ore to produce phosphoric acid by wet process, belong to Wet-process Phosphoric Acid Production field.
Background technology
Phosphoric acid by wet process is one of important method of preparing phosphoric acid, is also the basic product of sulphur dioxide of phosphor chemical industry, and be widely used in the middle of phosphate industry and phosphate & compound fertilizer industry, demand is large.The production technique of phosphoric acid by wet process is mainly based on mineral acid (sulfuric acid) decomposing phosphate rock preparing phosphoric acid.The phosphate rock resource total amount of China is close to 50,000,000,000 t, and P in phosphorus ore
2o
5the rich ore of content more than 30% only accounts for about 8% of reserves, and the overwhelming majority is low grade ore, phosphorus ore P
2o
5average grade is only 16.85%, and is mostly collophanite, and selecting and purchasing difficulty is large, and enrichment cost is high.Utilize low-grade (P
2o
5﹤ 24%) future developing trend of phosphorus ore Ze Shi China sulphur dioxide of phosphor chemical industry.
Show from existing document and data, except not yet having industrialized unit without water law flow process, other technical process mainly contains two wet technologies and half wet technology.But the increase of reduction and foreign matter content gradually along with world phosphate grade, the adaptability of two water law flow processs to phosphorus ore and the reliability of technique, stability is comparatively strong, dominate in large-scale wet method phosphoric acid manufacture process.Wherein employing two water law of wet-process phosphoric acid production plant more than 80% is produced, the parts such as wet phosphoric acid by dihydrate production process mainly comprises reaction, filtrations, concentrates, washing tail gas, sour storage.Sulfuric acid and phosphorus ore carry out extractive reaction in a reactive tank, and the main phosphoric acid of production liquid phase, solid phase are mainly the phosphoric acid material pulp of phosphogypsum; Then by phosphoric acid material pulp filtering separation in filter, filtrate is dilute phosphoric acid product, and filter residue is phosphogypsum, stores up; Dilute phosphoric acid product, by concentrated, improves its concentration to 50% further; The tail gas of reactive moieties, by the repeatedly rear emptying of washing, meets environmental protection standard.
One of principal feature of low-grade phosphate ore is that acid non-soluble substance foreign matter content is high especially, and when adopting traditional phosphoric acid production method to generate phosphoric acid, it almost all enters in phosphogypsum, thus phosphogypsum quality is reduced greatly, causes its comprehensive utilization difficulty.And because in low-grade phosphate ore, foreign matter content is high, phosphorus ore often there will be that rate of decomposition is low, and Washing ratio is low, the calcium sulfate parcel that reaction generates makes reaction passivation, generates calcium hydrophosphate crystal and adds P
2o
5loss, crystal of calcium sulfate is difficult to be separated, the problem such as cause that finished product phosphoric acid quality is on duty mutually, thus cause production cost abnormal high, produce extremely unstable, thus agricultural diammonium phosphate and the agricultural monoammonium phosphate of excellent level cannot be produced.
Chinese patent CN9110859.7 " tower Wet-process Phosphoric Acid Production method and apparatus " mentions can being raw material production phosphoric acid by wet process with mid low grade phosphate rock, but its phosphorus ore grade P used
2o
5≤ 25%, available mid low grade phosphate rock scope is narrower; The mixed slurry of ground phosphate rock and recycled phosphoric acid is directly entered extraction tower and sulfuric acid reaction by this method, the impurity in phosphorus ore and phosphogypsum is not separated; And use the vitriol oil as extraction agent, cause local SO
4 2-concentration is large, makes reaction incomplete.
Chinese patent 200510022547.2 " utilizing mid low grade phosphate rock to produce the method for phosphoric acid by wet process " also mentions that its method can take mid low grade phosphate rock as raw material production phosphoric acid by wet process, but its phosphorus ore grade used is P
2o
5%:18 ~ 26%, and require MgO≤2.0wt%, Fe
2o
3+ Al
2o
3≤ 3.5wt%; It has the foreign matter content of phosphorus ore is comparatively strict with, and flow process is complicated simultaneously, reaction is complicated, two sections of reaction of high order, thus makes cost high, does not possess industrialization ubiquity; The method adopts multi-stage counter current extraction, and operating process is long, and production equipment requires high; Do not have the washing of residue, gypsum and wash water to utilize simultaneously, fail to realize the effective profit of industrialization of resource technique.Industrialization has sizable difficulty.
Summary of the invention
The object of the invention is for higher-grade phosphorus ore in China is rapidly exhausted that low-grade phosphate ore is relatively many and low-cost reality, but conventional wet phosphoric acid production method adopts during mid low grade phosphate rock exists shortcomings, and a kind of method 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.
Object of the present invention is realized by following technical measures, and wherein said raw material number, except specified otherwise, is parts by weight:
The method utilizing low-grade phosphate ore to produce phosphoric acid by wet process adopts two-step reaction, countercurrent washing flow process, and produce higher concentration quality product matter phosphoric acid by wet process and high-quality white colored stone cream by low-grade phosphate ore, concrete steps are as follows:
Step 1, use phosphorolytic cleavage low-grade phosphate ore ore pulp, obtain calcic extraction clear liquid and filter residue through solid-liquid separation I;
Step 2, by above-mentioned extraction clear liquid and sulfuric acid reaction, obtain phosphoric acid by wet process and phosphogypsum through solid-liquid separation II; Part phosphoric acid returns for decomposing phosphate rock, and part phosphoric acid exports as finished product;
Step 3, by above-mentioned filter residue through washing I, washing water be used for phosphorus ore slurrying; By above-mentioned phosphogypsum, obtain high-quality white phosphogypsum through washing II, washing water enter step I recycle.
The quality of described low-grade phosphate ore is: P
2o
5content is 20 ~ 23wt%, and other impurity is without particular requirement.
When described step 1 is reacted: be 25.5 ~ 36wt%P by concentration
2o
5phosphoric acid extraction phosphorus ore, extraction slip in liquid-solid ratio=22 ~ 27, temperature 35 ~ 57 DEG C reaction 3 ~ 8h.
Described calcic extraction clear liquid and 92 ~ 98wt% sulfuric acid reaction generate Crystallization of Gypsum, and sulfuric acid dosage is 109 ~ 120% of stoichiometric quantity, at temperature 80 ~ 95 DEG C reaction 3 ~ 6h; The concentration generating phosphoric acid is 24.5 ~ 35wt%P
2o
5.
Described solid-liquid separation adopts vacuum filtration, wash and add the separation method that auxiliary agent combines.
Described auxiliary agent is at least one in polyacrylamide, modified polyacrylamide, polymerization ferrous sulfate and polymerize aluminum chloride, and the addition of auxiliary agent is 2 ~ 50ppm.
Performance test
Adopt GB/T1871.1-1995 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-=1.42wt%, MgO=1.25wt%, Fe
2o
3=0.57wt%, Al
2o
3=0.78wt%, F=6325ppm.
2, product phosphoric acid quality: P
2o
5=33.76wt%, CaO=0.67wt%, SO
4 2-=1.75wt%, MgO=2.23wt%, Fe
2o
3=1.16wt%, Al
2o
3=0.94wt%, F=58630ppm.
The present invention compared with prior art has the following advantages:
1, can low-grade phosphate ore be used, to foreign matter content no requirement (NR)s such as magnesium iron in phosphorus ore, expand the universality of phosphorus ore source of supply and process industry;
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 ratio and P
2o
5high (the phosphorus ore P of the rate of recovery
2o
5percentage extraction>=95%, P
2o
5washing ratio>=98%, P
2o
5the rate of recovery>=95%), phosphoric acid concentration is 25 ~ 35%, is better than other method existing;
4, washing water efficiency utilization: phosphogypsum washing water return the washing for filter residue, its washing water finally enter ore grinding step, realize washing water efficiency utilization, improve the Washing ratio of Vanadium Pentoxide in FLAKES, can realize industrialization.
5, filter residue and phosphogypsum are separated, obtain high-quality white phosphogypsum product, improve the utility value of phosphogypsum;
6, sulphuric acid is 109 ~ 120% of reaction formula stoichiometric quantity, CaO, MgO, Fe in product phosphoric acid
2o
3, Al
2o
3content low, improve phosphoric acid quality.
Accompanying drawing explanation
Fig. 1 is the process flow sheet utilizing low-grade phosphate ore to produce phosphoric acid by wet process
1, ore grinding, 2, single step reaction, 3, be separated I, 4, two steps reactions, 5, be separated II, 6, washing I,
7, II is washed.
Embodiment
Be specifically described the present invention below by embodiment, what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention, 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 utilizing low-grade phosphate ore to produce phosphoric acid by wet process comprises the following steps:
Step 1: with low-grade phosphate ore (P
2o
5=23.00wt%, CaO=40.07wt%, MgO=3.20, Fe
2o
3=1.52wt%, Al
2o
3=0.55wt%) prepare phosphorus ore ore pulp, then with phosphoric acid (P
2o
5=25.83wt%) carry out single step reaction, temperature 42 DEG C ~ 50 DEG C, reaction 3h, liquid-solid ratio=27 in extraction slip, add polyacrylamide 20ppm, modified polyacrylamide 20ppm after completion of the reaction, polymerization ferrous sulfate 10ppm is extracted clear liquid and filter residue through being separated I operation, percentage extraction is 95.1%;
Step 2: add 1 portion of extraction clear liquid and 1.12 times of calculated amount sulfuric acid in special reactor, sulfuric acid=98wt%, temperature maintains 80 DEG C ~ 85 DEG C, reaction 3h.Reaction solution adds polyacrylamide 20ppm, modified polyacrylamide 20ppm, polymerization ferrous sulfate 10ppm after being separated II, and liquid is higher quality phosphoric acid by wet process (P
2o
5=24.94wt%), Vanadium Pentoxide in FLAKES yield is 99.12%; Solid is product white phosphogypsum.Wherein part phosphoric acid returns extraction tank for decomposing phosphate rock, and part phosphoric acid exports as finished product.
Step 3: the filter residue that step 1 is obtained by reacting is after washing I operation, and its washing water are used for phosphorus ore slurrying, and residual washing-out rate is 98.82%; Step 2 is obtained by reacting gypsum, and after washing II operation, obtain high-quality white phosphogypsum, its washing water enter washing I and reuse, and Washing ratio is 98.43%.
Embodiment 2:
The method utilizing low-grade phosphate ore to produce phosphoric acid by wet process comprises the following steps:
Step 1: with low-grade phosphate ore (P
2o
5=20.07wt%, CaO=43.13wt%, MgO=2.56, Fe
2o
3=1.23wt%, Al
2o
3=0.67wt%) prepare phosphorus ore ore pulp, then with phosphoric acid (P
2o
5=35.96wt%) carry out extractive reaction, temperature 35 DEG C ~ 42 DEG C, reaction 8h, liquid-solid ratio=25 in extraction slip, add polyacrylamide 10ppm after completion of the reaction, modified polyacrylamide 20ppm is extracted clear liquid and filter residue through lock out operation, percentage extraction is 96.12%;
Step 2: add 1 portion of extraction clear liquid and 1.20 times of calculated amount sulfuric acid in special reactor, sulfuric acid=92wt%, temperature maintains 85 DEG C ~ 90 DEG C, reaction 6h.Reaction solution adds polyacrylamide 10ppm, modified polyacrylamide 20ppm after being separated II, and liquid is higher quality phosphoric acid by wet process (P
2o
5=34.95wt%), Vanadium Pentoxide in FLAKES yield is 98.22%; Solid is product white phosphogypsum.Wherein part phosphoric acid returns extraction tank for decomposing phosphate rock, and part phosphoric acid exports as finished product.
Step 3: the filter residue that step 1 is obtained by reacting is after washing I operation, and its washing water are used for phosphorus ore slurrying, and residual washing-out rate is 98.14%; Step 2 is obtained by reacting gypsum, and after washing II operation, obtain high-quality white phosphogypsum, its washing water enter washing I and reuse, and Washing ratio is 98.82%.
Embodiment 3:
The method 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=1.19wt%, Al
2o
3=0.89wt%) prepare phosphorus ore ore pulp, then with phosphoric acid (P
2o
5=27.52wt%) carry out extractive reaction, temperature 48 DEG C ~ 57 DEG C, reaction 6h, liquid-solid ratio=22 in extraction slip, add polyacrylamide 2ppm after completion of the reaction and be extracted clear liquid and filter residue through lock out operation, percentage extraction is 95.67%;
Step 2: add 1 portion of extraction clear liquid and 1.09 times of calculated amount sulfuric acid in special reactor, sulfuric acid=96wt%, temperature maintains 90 DEG C ~ 95 DEG C, fully reacts 5h.Reaction solution adds polyacrylamide 2ppm after being separated II, and liquid is higher quality phosphoric acid by wet process (P
2o
5=26.27wt%), Vanadium Pentoxide in FLAKES yield is 98.87%; Solid is product white phosphogypsum.Wherein part phosphoric acid returns extraction tank for decomposing phosphate rock, and part phosphoric acid exports as finished product.
Step 3: the filter residue that step 1 is obtained by reacting is after washing I operation, and its washing water are used for phosphorus ore slurrying, and residual washing-out rate is 98.14%; Step 2 is obtained by reacting gypsum, and after washing II operation, obtain high-quality white phosphogypsum, its washing water enter washing I and reuse, and Washing ratio is 98.91%.
Claims (1)
1. utilize low-grade phosphate ore to produce the method for phosphoric acid by wet process, it is characterized in that, concrete steps are as follows:
Then step 1: prepare phosphorus ore ore pulp with low-grade phosphate ore is 35.96wt%P with concentration
2o
5phosphoric acid carry out extractive reaction, temperature 35 DEG C ~ 42 DEG C, reaction 8h, extraction slip in liquid-solid ratio=25, add polyacrylamide 10ppm, modified polyacrylamide 20ppm after completion of the reaction, be extracted clear liquid and filter residue through lock out operation;
Step 2: add 1 portion of extraction clear liquid and 1.20 times of calculated amount sulfuric acid in the reactor, h 2 so 4 concentration is 92%, and temperature maintains 85 DEG C ~ 90 DEG C, reaction 6h, reaction solution adds polyacrylamide 10ppm, modified polyacrylamide 20ppm after being separated, and liquid is concentration is 34.95wt%P
2o
5phosphoric acid, solid be product white phosphogypsum, wherein part phosphoric acid returns extraction tank for decomposing phosphate rock, and part phosphoric acid exports as finished product;
Step 3: the filter residue that step 1 is obtained by reacting is after washing I operation, and its washing water are used for phosphorus ore slurrying; Step 2 is obtained by reacting white phosphogypsum, and after washing II operation, obtain high-quality white phosphogypsum, its washing water enter washing I and reuse.
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Cited By (1)
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| CN109573972A (en) * | 2019-01-23 | 2019-04-05 | 山东鲁北企业集团总公司 | A kind of method of mid low grade phosphate rock production phosphoric acid and low silica cream |
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| CN103626143A (en) * | 2013-11-29 | 2014-03-12 | 晏明朗 | Method for wet production of phosphoric acid and byproduct, namely white gypsum |
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