CN101525130B - Technique for purifying and producing industrial phosphoric acid by wet-process phosphoric acid - Google Patents
Technique for purifying and producing industrial phosphoric acid by wet-process phosphoric acid Download PDFInfo
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- CN101525130B CN101525130B CN2009100615560A CN200910061556A CN101525130B CN 101525130 B CN101525130 B CN 101525130B CN 2009100615560 A CN2009100615560 A CN 2009100615560A CN 200910061556 A CN200910061556 A CN 200910061556A CN 101525130 B CN101525130 B CN 101525130B
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Abstract
The invention relates to the technique for purifying and producing industrial phosphoric acid by wet-process phosphoric acid, which comprises the following steps of: (1) desulfurization and defluorination sedimentation-filtration process; (2) the extraction of wet-process phosphoric acid after desulfurization and defluorination process; (3) the washing of organic phase after extraction; (4) the back extraction of the organic phase after washing; (5) the refining of aqueous phase after the back extraction; (6) concentrating till containing 85wt% H3PO4 and recycling organic solvent. The technique has the beneficial effects that (1) the wet-process phosphoric acid produced by adopting the existing sulfuric acid process does need to be preconcentrated; (2) compound extracting agent of the technique has good suitability for the extraction of the wet-process phosphoric acid; (3) the compound extracting agent has better separating effect on iron ions and other heavy metal ions; (4) emulsiongenerated by the organic phase in the washing process can be eliminated by a warming/stewing mode; (5) the technique adopts amidine fiber adsorption column to refine wet-process phosphoric acid and can effectively absorb trace metal ions, and the clearance of the metal ions can reach 99 wt%.
Description
Technical field
The present invention relates to a kind of technology of purifying and producing industrial phosphoric acid by wet-process phosphoric acid.
Background technology
The purification process of phosphoric acid by wet process mainly contains chemical precipitation method, crystallization process, ion exchange method, solvent precipitation, organic solvent extractionprocess, thickening-purification technology method, electroosmose process, present industrial general employing organic solvent extractionprocess, organic solvent extractionprocess mainly contains the Central-Liqueur flow process that French Luo Na-Rhone-Poulenc adopts the organic solvent extractionprocess purification of wet process phosphoric acid, the Phorex method of France APC company, Britain Albright Wilson method, Israel IMI Cleaning method, Japan Cao Da technology.Japan's Cao Da technology with pre-treatment after phosphoric acid and propyl carbinol carry out multi-stage counter current extraction, but its content to raw phosphoric acid has certain requirement, wherein P
2O
5% content is between 30～50%.The Phorex method of France APC company is characterized in isopropylcarbinol phosphoric acid being extracted merely, in the low concentration scope phosphoric acid is had extracting power, but it is bad and bad to the phosphoric acid extraction effect in high concentration range that negatively charged ion is removed effect.Britain Albright Wilson method, adopting mibk during its characteristics is extraction agent, but this extraction agent toxicity is bigger.Israel IMI Cleaning method, these method characteristics are to be extraction agent with the diisopropyl ether, raw phosphoric acid are had relatively high expectations P
2O
5% content is more than 50%, and decontamination effect improving is bad, and purifying phosphoric acid is fit to do fertilizer.The Central-Liqueur flow process of France Luo Na-Rhone-Poulenc, being characterized in adopting single tributyl phosphate is extraction agent, to raw phosphoric acid concentration requirement height, solvent is more expensive.
In recent years, China is in the purification research of phosphoric acid by wet process, also done a large amount of work, for example East China University of Science has carried out to mock with the dibutyl Asia and has been extraction agent Research on Purification of Wet Phosphoric Acid from nitric acid system, and be extraction agent Research on Purification of Wet Phosphoric Acid from hydrochloric acid system with S34E, it is extraction agent that Chengdu Univ. of Science ﹠ Technology has studied with propyl carbinol and primary isoamyl alcohol, the technology of purifying phosphoric acid from hydrochloric acid system, chemical engineering institute of East China University of Science has also adopted organic solvent deposit and organic solvent bonded method to come purification of wet process phosphoric acid, studied removing in advance of impurity before the extraction with acetone, and be extraction agent purified research etc. with MIBK.Simultaneously the production technique of organic solvent extractionprocess purification of wet process phosphoric acid some researchs and improvement have been done, No. 98800222.1, Chinese patent application " purification process of phosphoric acid by wet process " for example, extraction ability to multiple organic solvent compares, but selected organic solvent or certain toxicity is arranged, or the kind effect of extraction is also not intact, still can't industrial production.The ketone ester mixed extractant is adopted in No. 02133869.8, patent application " a kind of purification treatment method of wet-process phosphoric acid ", and phosphoric acid extraction is effective under high density, handles but extraction back phosphoric acid also need carry out the deep desulfuration defluorinate.No. 03117850.2, patent application " method for preparing PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid with phosphoric acid by wet process ", be characterized in adopting the mixed solvent of tributyl phosphate/kerosene to extract, solvent need not to reclaim separately, it is better that positively charged ion is removed effect, but can not effectively remove negatively charged ion, after the phosphoric acid by wet process extraction, need the deep desulfuration defluorinate, simultaneously the raw material phosphoric acid concentration is had certain requirement.No. 200410081600.1, patent application " a kind of production technique of purification of wet process phosphoric acid and equipment " is characterized in that extraction/washing/back extraction carries out in tower, extraction/washing/stripping efficiency height is provided with between washing/back extraction and falls emulsifying tank, increases facility investment.
Summary of the invention
Problem to be solved by this invention is the technology that a kind of purifying and producing industrial phosphoric acid by wet-process phosphoric acid is provided at above-mentioned prior art, to reduce the production cost of phosphoric acid, thereby improve the economic benefit of phosphoric acid deep processing, Technology of the present invention is effective, the industrial phosphoric acid that obtains, its every index are better than industrial phosphoric acid premium grads (with reference to thermal phosphoric acid GB/T2091-2008 standard).
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: a kind of technology of purifying and producing industrial phosphoric acid by wet-process phosphoric acid is characterized in that including the next coming in order step:
1) once desulfurization defluorinate sedimentation filtration treatment: the phosphoric acid by wet process that will make by sulfuric acid process adds the composite desulfate reagent of lime carbonate and ground phosphate rock by 120～140% of sulfate ion stoichiometric ratio, and wherein the mass ratio of lime carbonate and ground phosphate rock is 4～9: 1; Or press 140～160% composite desulfate reagent that add calcium oxide and ground phosphate rock of the stoichiometric ratio of sulfate ion, wherein the mass ratio of lime carbonate and ground phosphate rock is 4～9: 1, press 100～120% adding defluorinating agent yellow soda ash of the stoichiometric ratio of fluorion, add the activated silica auxiliary agent simultaneously, the activated silica add-on is a fluorion stoichiometric 0.15%; Or press fluorion stoichiometric ratio 100～120% add the defluorinating agent yellow soda ash, add the aluminium hydroxide auxiliary agent simultaneously, the aluminium hydroxide add-on is that fluorion is stoichiometric 0.10%, its reaction process parameter: temperature of reaction is 40～50 ℃; Mixing speed 200～250rpm; Reaction times is 210～240min, filters, and obtains filtrate;
2) extraction of back phosphoric acid by wet process is handled in the desulfurization defluorinate: the filtrate phosphoric acid by wet process that step 1) is obtained is with alcohol-ester mixed organic solvents counter-current extraction, extraction temperature is 55～60 ℃, extraction phase is an organic phase than by volume: water=2.5～4: 1, and the organic phase after obtaining extracting;
3) washing of extraction back organic phase: the organic phase that step 2) obtains is washed with washings, its reaction process parameter: wash temperature is 50～60 ℃, and mixing speed is 200～250rpm, reaction times 5～10min;
4) back extraction of washing back organic phase: the organic phase after the step 3) washing is stripped with reflux type with deionized water, reextraction is compared and is organic phase by volume: water=5～7: 1, water after the reextraction is dilute phosphoric acid, the reaction process parameter: temperature is 55～60 ℃;
5) the refining of back water of stripping: the step 4) water that obtains of stripping contains sulfate ion, and magnesium ion adds barium oxide by 100% of actual measurement sulfate ion stoichiometric ratio, and its reaction process parameter: temperature of reaction is 50～60 ℃; Mixing speed 200～250rpm; Reaction times is 15～30min, adopts amido fiber adsorption column through reacted water, obtains refining water;
6) concentrate: the refining aqueous phase solution that step 5) obtains concentrates, concentrate to adopt underpressure distillation, and vacuum tightness 125mmHg, 75～102 ℃ of temperature are concentrated into and contain 85wt%H
3PO
4And recovery organic solvent.
Press such scheme, the content of the described phosphoric acid by wet process of step 1) is 21～38wt%H
3PO
4
Press such scheme, step 2) alcohol-ester volume ratio is 7: 3～8: 2 in the described mixed organic solvents, and wherein alcohol is propyl carbinol or primary isoamyl alcohol, and ester is a tributyl phosphate.
Press such scheme, step 2) described organic phase ingress adding extraction promotor sulfuric acid, its add-on is 0.5～1% of the described phosphoric acid by wet process quality of step 1).
Press such scheme, the described washings of step 3) is the dilute solution of phosphoric acid, and wherein phosphorus acid content is 5～15wt%; Washing is compared and is organic phase by volume: water=3～6: 1.
Press such scheme, the structural formula of the described amido fiber of step 5) is:
Wherein: R is-CH
2NHCH
2NHCH
2-, Cell is a Mierocrystalline cellulose.
The present invention is provided with a desulfurization defluorinate subsider, sedimentation filter residue, step 2 in step 1)) extraction, the step 4) back extraction carries out in the impulse oscillation sieve-tray tower, adopts surge pump that organic phase is produced pulse, and the impulse oscillation frequency is at 20～45min
-1Between, the step 3) washing is carried out in steel basin, and groove installs heat insulation measure additional, and step 5) is made with extra care in refining subsider and is carried out.
As Fig. 2, the impulse oscillation sieve-tray tower adopts phosphoric acid by wet process (heavy phase) from top heavy phase import 1 charging among the present invention, and organic extractant (light phase) light phase import 2 chargings from the bottom are after the extraction phase-splitting, heavy phase is from 3 dischargings of bottom heavy out, gently from 4 dischargings of top light phase export.As Fig. 1, see extraction tower 6 and back extraction tower 7, organic extractant utilizes pulse and the density difference of himself upwards to flow rapidly, through sieve plate in the tower, fully contact extraction with the phosphoric acid by wet process that enters from top heavy phase import 1 by oscillating screen plate 5 apertures, to be extracted in the organic phase through the phosphoric acid by wet process that the desulfurization defluorinate is handled, the design of back extraction tower and principle of work are consistent with extraction tower, heavy phase enters from top heavy phase import 1, gently light phase import 2 enters from the bottom, phase-splitting after counter current contact is respectively from another outlet discharging.
Beneficial effect of the present invention is:
1) to adopt the phosphoric acid by wet process content of existing Production By Sulfuric Acid Process be 21～38% (H in the present invention
3PO
4Meter, wt%), phosphoric acid by wet process need not to carry out pre-concentration, can avoid concentrating back phosphoric acid by wet process concentration height, and viscosity causes the shortcoming of inferior separating effect greatly, can save the energy expenditure of bringing because of concentrating (about 15～20%);
2) composite extractant of the present invention is good to the adaptability of phosphoric acid by wet process extraction, and percentage extraction is 80～90%, adds extraction promotor (H in the organic solvent ingress
2SO
4), mass percent concentration is 75～85% o'clock, sulfate ion can with calcium ion generation precipitin reaction in the phosphoric acid by wet process, effectively remove calcium ion, make sulfate ion content＜0.002% (SO in the extracted organic phase
4 2-Meter, wt%), calcium ion content＜0.002%.(Ca
2+Meter, wt%);
3) among the present invention composite extractant to iron ion (Fe
2+), other heavy metal ion has separating effect preferably, after the extraction, iron ion (Fe in the organic phase
2+), heavy metal ion (As
3+, Pb
2+) content is low, iron ion content≤0.0001% (Fe
2+Meter, wt%), heavy metal ion content≤0.0001% (Pb
2+Meter, wt%).Unavoidably can contain the small amount of impurities ion in this technology extraction process and enter into extracted organic phase, as sulfate ion, little metal ion, therefore, obtain highly purified phosphoric acid by wet process, also must wash extracted organic phase, back extraction, treating process, remove above-mentioned foreign ion;
4) desulfurization defluorinate of the present invention is once carried out in desulfurization defluorinate subsider, desulfurization defluorinate groove in the technology, top is right cylinder, the bottom is a cone, and right cylinder is a desulfurization defluorination reaction main body, and centrum is the precipitation negative area, whipping appts is set in the groove, accelerate the desulfurization defluorinate treatment time, make wherein that impurity fully reacts rapid precipitation with the composite desulfate defluorinating agent, the sedimentation of centrum part energy accelerate precipitation;
5) the present invention's washing is carried out in steel basin, can effectively avoid and eliminate the emulsion that produces in the washing process, and the rinse bath of setting can be eliminated the emulsion that organic phase in the washing process produces by the mode that heats up/leave standstill;
6) the present invention adopts amido fiber adsorption column to make with extra care phosphoric acid by wet process, energy active adsorption trace metal ion, and the clearance of metal ion can reach 99wt%.
Description of drawings
Fig. 1 is extraction, washing and the back extraction synoptic diagram of wet phosphoric acid purifying;
The impulse oscillation sieve-tray tower structural representation that Fig. 2 uses for wet phosphoric acid purifying.
Embodiment
Further introduce the present invention below by embodiment, but embodiment can not be construed as limiting the invention.
Embodiment 1: phosphoric acid by wet process prepares industrial phosphoric acid
In the present embodiment, (wt%) composed as follows of phosphoric acid by wet process:
1, the desulfurization defluorinate is handled
The desulfurization defluorinate is handled and is carried out in desulfurization defluorinate subsider, and with the phosphoric acid by wet process of Production By Sulfuric Acid Process, content is 25.68% (H
3PO
4Meter wt%), need not to concentrate, and press the composite desulfate reagent of 120% adding lime carbonate and ground phosphate rock of the stoichiometric ratio of sulfate ion, and wherein the mass ratio of lime carbonate and ground phosphate rock is 6: 1; Press 100% adding yellow soda ash of the stoichiometric ratio of fluorion, add the activated silica auxiliary agent simultaneously, the activated silica add-on is a fluorion stoichiometric 0.15%.Temperature of reaction, 40 ℃, mixing speed, 250rpm, the reaction times, 240min, after filtration, solid content＜0.9wt% in the filtrate;
2, organic solvent extraction
Extraction is carried out in the impulse oscillation sieve-tray tower, with alcohol-ester mixed organic solvents counter-current extraction, alcohol in the mixed organic solvents-ester volume ratio is 8: 2, and wherein alcohol is propyl carbinol, and ester is a tributyl phosphate, extraction is in a ratio of organic phase: water=3: 1, add extraction promotor (sulfuric acid, mass concentration are 75%) at the organic phase inlet, add-on is the 0.5wt% of the described phosphoric acid by wet process quality of step 1), extraction temperature is 60 ℃, impulse oscillation frequency 35.
3, washing
Washing is carried out in steel basin, and washings is the dilute solution of phosphoric acid, and wherein phosphorus acid content is 5% (H
3PO
4Meter, wt%); Washing is in a ratio of organic phase: water=5: 1, wash temperature are 50 ℃, and mixing speed is 250rpm, and the reaction times is 5min.
4, back extraction
Back extraction is carried out in the impulse oscillation sieve-tray tower.Strip with reflux type with deionized water, strip and be in a ratio of organic phase: water=6: 1, temperature of reaction are 60 ℃, impulse oscillation frequency 30min
-1
5, refining
Make with extra care in refining subsider and carry out.By actual measurement sulfate ion (SO
4 2-) stoichiometric ratio 100% add barium oxide (BaO); Temperature of reaction, 50 ℃, mixing speed, 250rpm, reaction times, 30min.Reacted water is further refining by amido fiber adsorption column, and adopts 0.1%HNO
3(wt%) for washing fluid adsorption column is regenerated, the structural formula of described amido fiber is:
Wherein: R is-CH
2NHCH
2NHCH
2-, Cell is a Mierocrystalline cellulose.
6, concentrate
With the concentrated PHOSPHORIC ACID TECH.GRADE that is prepared into of the dilute phosphoric acid that obtains after refining.Concentrate and adopt underpressure distillation to concentrate vacuum tightness 125mmHg, temperature 75-102 ℃.
The prepared PHOSPHORIC ACID TECH.GRADE of present embodiment table composed as follows (wt%):
Embodiment 2: phosphoric acid by wet process prepares industrial phosphoric acid
In the above-mentioned processing step, except that desulfurization defluorinate treatment process, all the other operations are all identical with embodiment 1.
The desulfurization defluorinate is handled and is carried out in desulfurization defluorinate subsider, and with the phosphoric acid by wet process of Production By Sulfuric Acid Process, content is 25.68% (H
3PO
4Meter wt%), need not to concentrate, and press the composite desulfate reagent of 150% adding calcium oxide and ground phosphate rock of the stoichiometric ratio of sulfate ion, and wherein the mass ratio of calcium oxide and ground phosphate rock is 7: 1; Press 110% adding yellow soda ash of the stoichiometric ratio of fluorion, add the aluminium hydroxide auxiliary agent simultaneously, the aluminium hydroxide add-on is a fluorion stoichiometric 0.10%.Temperature of reaction, 45 ℃, mixing speed, 200rpm, reaction times, 230min.
The PHOSPHORIC ACID TECH.GRADE of present embodiment gained table composed as follows (wt%):
Embodiment 3: phosphoric acid by wet process prepares industrial phosphoric acid
In the above-mentioned processing step, except that extraction process, all the other operations are all identical with embodiment 1.
Extraction is carried out in the impulse oscillation sieve-tray tower, with alcohol-ester mixed organic solvents counter-current extraction, alcohol in the mixed organic solvents-ester volume ratio is 8: 2, and wherein alcohol is primary isoamyl alcohol, and ester is a tributyl phosphate, extraction is in a ratio of organic phase: water=3: 1, add extraction promotor (sulfuric acid, mass concentration are 75%) at the organic phase inlet, add-on is the 0.5wt% of the described phosphoric acid by wet process quality of step 1), extraction temperature is 60 ℃, impulse oscillation frequency 35.
The PHOSPHORIC ACID TECH.GRADE of present embodiment gained table composed as follows (wt%):
Embodiment 4: phosphoric acid by wet process prepares industrial phosphoric acid
In the above-mentioned processing step, except that desulfurization defluorinate treatment process, all the other operations are all identical with embodiment 3.
The desulfurization defluorinate is handled and is carried out in desulfurization defluorinate subsider, and with the phosphoric acid by wet process of Production By Sulfuric Acid Process, content is 25.68% (H
3PO
4Meter wt%), need not to concentrate, and press the composite desulfate reagent of 140% adding calcium oxide and ground phosphate rock of the stoichiometric ratio of sulfate ion, and wherein the mass ratio of calcium oxide and ground phosphate rock is 7: 1; Press 100% adding yellow soda ash of the stoichiometric ratio of fluorion, add the aluminium hydroxide auxiliary agent simultaneously, the aluminium hydroxide add-on is a fluorion stoichiometric 0.10%.Temperature of reaction, 40 ℃, mixing speed, 250rpm, reaction times, 240min.
The PHOSPHORIC ACID TECH.GRADE of present embodiment gained table composed as follows (wt%):
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of processing parameter of the present invention (as temperature, time etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (4)
1. the technology of purifying and producing industrial phosphoric acid by wet-process phosphoric acid is characterized in that including the next coming in order step:
1) once desulfurization defluorinate sedimentation filtration treatment: the phosphoric acid by wet process that will make by sulfuric acid process adds the composite desulfate reagent of lime carbonate and ground phosphate rock by 120～140% of sulfate ion stoichiometric ratio, and wherein the mass ratio of lime carbonate and ground phosphate rock is 4～9: 1; Or press 140～160% composite desulfate reagent that add calcium oxide and ground phosphate rock of the stoichiometric ratio of sulfate ion, wherein the mass ratio of lime carbonate and ground phosphate rock is 4～9: 1, press 100～120% adding defluorinating agent yellow soda ash of the stoichiometric ratio of fluorion, add the activated silica auxiliary agent simultaneously, the activated silica add-on is a fluorion stoichiometric 0.15%; Or press fluorion stoichiometric ratio 100～120% add the defluorinating agent yellow soda ash, add the aluminium hydroxide auxiliary agent simultaneously, the aluminium hydroxide add-on is that fluorion is stoichiometric 0.10%, its reaction process parameter: temperature of reaction is 40～50 ℃; Mixing speed 200～250rpm; Reaction times is 210～240min, filters, and obtains filtrate;
2) extraction of back phosphoric acid by wet process is handled in the desulfurization defluorinate: the filtrate phosphoric acid by wet process that step 1) is obtained is with alcohol-ester mixed organic solvents counter-current extraction, extraction temperature is 55～60 ℃, extraction phase is an organic phase than by volume: water=2.5～4: 1, organic phase after obtaining extracting, alcohol in the wherein said mixed organic solvents-ester volume ratio is 7: 3～8: 2, wherein alcohol is propyl carbinol or primary isoamyl alcohol, and ester is a tributyl phosphate;
3) washing of extraction back organic phase: the organic phase that step 2) obtains is washed with washings, its reaction process parameter: wash temperature is 50～60 ℃, mixing speed is 200～250rpm, reaction times 5～10min, wherein said washings is the dilute solution of phosphoric acid, and wherein phosphorus acid content is 5～15wt%; Washing is compared and is organic phase by volume: water=3～6: 1;
4) back extraction of washing back organic phase: the organic phase after the step 3) washing is stripped with reflux type with deionized water, reextraction is compared and is organic phase by volume: water=5～7: 1, water after the reextraction is dilute phosphoric acid, the reaction process parameter: temperature is 55～60 ℃;
5) the refining of back water of stripping: the step 4) water that obtains of stripping contains sulfate ion, and magnesium ion adds barium oxide by 100% of actual measurement sulfate ion stoichiometric ratio, and its reaction process parameter: temperature of reaction is 50～60 ℃; Mixing speed 200～250rpm; Reaction times is 15～30min, adopts amido fiber adsorption column through reacted water, obtains refining water;
6) concentrate: the refining aqueous phase solution that step 5) obtains concentrates, concentrate to adopt underpressure distillation, and vacuum tightness 125mmHg, 75～102 ℃ of temperature are concentrated into and contain 85wt%H
3PO
4And recovery organic solvent.
2. by the technology of the described purifying and producing industrial phosphoric acid by wet-process phosphoric acid of claim 1, the content that it is characterized in that the described phosphoric acid by wet process of step 1) is 21～38wt%H
3PO
4
3. by the technology of the described purifying and producing industrial phosphoric acid by wet-process phosphoric acid of claim 1, it is characterized in that step 2) described organic phase ingress adding extraction promotor sulfuric acid, its add-on is 0.5～1% of the described phosphoric acid by wet process quality of step 1).
4. by the technology of the described purifying and producing industrial phosphoric acid by wet-process phosphoric acid of claim 1, it is characterized in that the structural formula of the described amido fiber of step 5) is:
Wherein: R is-CH
2NHCH
2NHCH
2-, Cell is a Mierocrystalline cellulose.
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| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1769163A (en) * | 2005-09-19 | 2006-05-10 | 绵阳高新区精微新材料有限公司 | Method for preparing technical grade phosphoric acid, foodstuff grade phosphoric acid and phosphate using wet method and thin phosphoric acid |
| CN1792777A (en) * | 2005-10-31 | 2006-06-28 | 宜宾天原股份有限公司 | Process for purifying producing extracting solvent of food grade phosphoric acid by wet method phosphoric acid and extracting process thereof |
| 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 |
| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
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