CN1178192A - Optimized wet process for production of sulphuric acid - Google Patents
Optimized wet process for production of sulphuric acid Download PDFInfo
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- CN1178192A CN1178192A CN 96117727 CN96117727A CN1178192A CN 1178192 A CN1178192 A CN 1178192A CN 96117727 CN96117727 CN 96117727 CN 96117727 A CN96117727 A CN 96117727A CN 1178192 A CN1178192 A CN 1178192A
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Abstract
An optimized wet process for preparing phosphoric acid features that a settling step is additionally used between acidolysis step and liquid-solid seqaration step. The material from acidolysis tank is first settled and most materials extracted from different settled layer come into liquid-solid separation step. Its advantages are low solid content and high quality of the finished phosphoric acid ,high recovery rate of P2O5, and increasing the production power of liquid-solid separator by 20% or more.
Description
The present invention relates to the phosphoric acid production method, particularly relate to phosphate fertilizer industry wet method phosphoric acid manufacture process flow process.
The Wet-process Phosphoric Acid Production flow process of prior art is: Rock Phosphate (72Min BPL) and the sulfuric acid pulverized are generated phosphoric acid material pulp at acidolysis groove internal reaction; The phosphoric acid material pulp that comes out from the acidolysis groove is regardless of level and directly enters the isolated by vacuum filtration device successively the time and carry out liquid-solid separation, and the liquid phase of separating is a finished product phosphoric acid, and solid phase is a phosphogypsum; The solid phase phosphogypsum of separating is washed the back discharges; The washings of phosphogypsum mixes with about 2/3rds finished product phosphoric acid and turns back to the acidolysis groove and recycle.The Production Flow Chart of this phosphoric acid by wet process is adopted by manufacturing enterprise both domestic and external for many years, is traditional classical flow process.But the weak point of this flow process is directly to enter filtering separation device when the phosphoric acid material pulp that the acidolysis groove comes out is regardless of the level priority, has brought many disadvantageous consequences.The first, the tiny crystalline particle in the slip solid phase very easily stops up filter cloth (filtration medium) hole and filter cake layer passage, causes filtration resistance to increase, and the phosphogypsum moisture content increases, and washing effect, intensity filter and filter throughput descend, and the phosphoric acid productive rate is low.It two is, tiny crystalline particle easily penetrates filter cloth in the slip solid phase, and the solids content in the finished product phosphoric acid is increased, and the quality of product reduces.It three is, phosphoric acid material pulp all enters in the separating obtained finished product phosphoric acid of filtration unit major part and returns the circulation of acidolysis groove again, has strengthened the filter load, has increased production cost, has reduced throughput.
The objective of the invention is to overcome the weak point of prior art, a kind of liquid-solid separation device throughput in the production process of phosphoric acid is improved and disclose, the phosphoric acid by wet process optimization production technical process that liquid phase finished product phosphoric acid solid content of separating and solid phase phosphogypsum water capacity are all low.
Invention thought of the present invention is to increase pre-sedimentation operation before liquid-solid separation circuit, improving the working conditions of liquid-solid separation device, thereby realizes goal of the invention.
The objective of the invention is by taking following concrete technical measures to realize:
1. Rock Phosphate (72Min BPL) and sulfuric acid generate phosphoric acid material pulp in the reaction of acidolysis groove;
2. the phosphoric acid material pulp that comes out from the acidolysis groove enters sedimentation device and carries out sedimentation, and material is drawn respectively from different settled layer;
3. the material that extracts from sedimentation device is that major part enters liquid-solid separation device and carries out liquid-solid separation at least, and the liquid phase of separating is a phosphoric acid, and solid phase is a phosphogypsum.
4. the solid phase phosphogypsum of separating is washed, washings mixes with the liquid phase phosphoric acid of separating to small part and returns the acidolysis groove and recycle.
Sedimentation device in the sedimentation operation can be the gravity settling device, also can be the centrifugal force sedimentation device, or other sedimentation devices.Liquid-solid separation device can be a filtering separation device, as the formula that turns over, desk-top, belt equal vacuum filter, adding pressure type filter, centrifugal filter and other forms of filter; Also can be the decanter type tripping device, as helical-conveyer centrifugal etc.
Slip is in the settling process of sedimentation device, and the part that solid phase particles is big forms the thick slurry layer of bottom, and the part that particle is little forms the thin pulp layer.Slip is in filtering separation device, solid phase particles is thicker in the thick slurry, not only on filtration medium, form filter cake layer easily, and the loose porous crack of filter cake layer that forms, the solid content in the thin pulp is low, solid phase particles is more tiny, its particle had both penetrated filtration medium easily and had entered parting liquid, was difficult for forming filter cake layer, the hole in easy again blocking filtering medium and the filter cake layer, filtration resistance is increased, reduced the throughput of filtration unit.
When liquid-solid separation device is the filtering type tripping device, the phosphoric acid material pulp that comes out from the acidolysis groove can carry out the rough classification sedimentation earlier, i.e. not sedimentation goes out clear layer, sedimentation goes out thick slurry layer and thin pulp layer, the slip of drawing from thick slurry layer is introduced into filtering separation device, forms after the filter cake layer on filtration medium, and the slip of drawing from the thin pulp layer enters filtering separation device again, the solid phase of separating is a phosphogypsum, discharges by washing the back.The liquid phase of separating is a finished product phosphoric acid, and wherein most of the mixing with the washings of solid phase phosphogypsum returned the acidolysis groove and recycle.The phosphoric acid material pulp that comes out from the acidolysis groove also can compare sufficient sedimentation, sedimentation goes out clear layer, the clear liquid of drawing from clear layer is a finished product phosphoric acid, and remaining settled layer can divide thick slurry layer to draw respectively with the thin pulp layer again, enters filtering separation device by above-mentioned method steps classification again.Parting liquid can all mix with the solid phase washings and returns the acidolysis groove and recycle.Remaining settled layer also can no longer be divided thick slurry layer and thin pulp layer, enter liquid-solid filtering separation device in the lump and carry out liquid-solid separation, when liquid-solid separation device is settling separation device, as helical-conveyer centrifugal, the phosphoric acid material pulp that comes out from the acidolysis groove, generally to compare sufficient sedimentation, sedimentation goes out clear layer, the clear liquid of drawing from clear layer is a finished product phosphoric acid, remaining sedimentation slip preferably enters settling separation device in the lump, and the liquid phosphoric acid of separating can all mix with the solid phase phosphogypsum washings of separating and turns back to the acidolysis groove and recycle.In order to make slip be easier to sedimentation, can in the sedimentation operation of slip, add flocculation agent.The adding method of flocculation agent can add in the sedimentation of slip, also can add before slip enters sedimentation device, or join in the slip and go entering sedimentation device ingress.
Accompanying drawing 1 is the process flow sheet of one embodiment of the invention.
Accompanying drawing 2 is process flow sheets of an alternative embodiment of the invention.
Provide embodiments of the invention below in conjunction with description of drawings, and the present invention is described in further detail by embodiment.
Embodiment 1:
Sedimentation device is a gravity settling tank, and liquid-solid separation device is a vacuum filter.Technical process as shown in Figure 1.
(1) Rock Phosphate (72Min BPL) through pulverizing 1 joins the acidolysis groove with sulfuric acid 2 and carries out acidolysis reaction, generates phosphoric acid material pulp;
(2) phosphoric acid material pulp 3 that comes out from the acidolysis groove joins gravity settling tank and carries out rough classification, i.e. not sedimentation goes out clear layer;
(3) slip 4 that thick slurry layer is drawn from the subsider bottom (slip that promptly contains big crystalline particle part) joins vacuum filter earlier, form after the filter cake layer on the medium to be filtered, the slip 5 of drawing from subsider top thin pulp layer joins filter again, filter operation finishes, filtered liquid is a finished product phosphoric acid 7, and filter residue is a phosphogypsum 9;
(4) add washing water 6 to filter, the filter residue phosphogypsum is washed.Filter residue phosphogypsum 9 after washing is discharged;
(5) washings 8 mixes with part filtrate 7 and returns the acidolysis groove and recycle.
Present embodiment is specially adapted to the transformation of the phosphoric acid production technical process of existing vacuum filtration technology.
Embodiment 2:
Sedimentation device is a gravity settling tank, and liquid-solid separation device is the sedimentation helical-conveyer centrifugal.Technical process as shown in Figure 2.
(1) Rock Phosphate (72Min BPL) through pulverizing 1 joins the acidolysis groove with sulfuric acid 2 and carries out acidolysis reaction, generates phosphoric acid material pulp;
(2) phosphoric acid material pulp 3 that comes out from the acidolysis groove joins gravity settling tank, in subsider, add flocculation agent 10 simultaneously, slip carries out sufficient sedimentation in subsider, form clear layer, the clear liquor 11 of drawing from clear layer, be finished product phosphoric acid, finished product phosphoric acid accounts for about 1/3 of slip liquid phase total amount;
(3) slip except that clear liquor 12 adds the sedimentation helical-conveyer centrifugal in the lump and carries out liquid-solid separation, and the liquid phase of discharge is a phosphoric acid 7, and the solid phase sediment is a phosphogypsum 9;
(4) add 6 pairs of phosphogypsums of Xian Di water and wash, the phosphogypsum 9 behind washing dehydration is discharged, and washings 8 mixes with parting liquid 7 and returns the acidolysis groove.
The present invention compared with prior art, its relatively outstanding advantage is:
1. work as phosphoric acid material pulp through the rough classification sedimentation, contain than after the thick slurry of crystalline particle joins liquid-solid filtering separation device earlier and forms filter cake layer greatly, the thin pulp that will contain less crystalline particle again adds liquid-solid filtering separation device, finishes the liquid-solid separation of phosphoric acid material pulp.Because the solid-phase crystallization particle in the thick slurry is bigger, forms filter cake layer easily, the loose porous again crack of the filter cake layer of formation makes filtration resistance reduce, i.e. the intensity filter of filtering separation device (phosphogypsum kg (doing)/m
2H) improve, will be regardless of level from the phosphoric acid material pulp that the acidolysis groove comes out with prior art and successively directly add filtering separation device in the lump and compare, intensity filter can improve more than 20%, filters throughput accordingly and also can improve more than 20%.This that is to say, adopts technology of the present invention, under the condition that does not change existing liquid-solid filtering separation device, can improve whole phosphoric acid plant throughput more than 20%.In addition, because the solid-phase crystallization particle is difficult for penetrating filtration medium more greatly in the thick slurry, the filter cake layer that forms is equivalent to construct the new filtration medium of one deck again on filtration medium, promptly improved the filtration capacity of filtration medium, make tiny crystalline particle in the slip be difficult for penetrating filtration medium and enter liquid phase, tiny crystalline particle penetration coefficient in the slip can reduce more than 50%, and corresponding finished product phosphoric acid solid content reduces greatly, and the quality of finished product phosphoric acid has obtained improving greatly.
2. when the fully sedimentation of phosphoric acid material pulp warp, make about about 1/3 liquid phase clarification in the slip, directly draw from sedimentation device and obtain finished product phosphoric acid.This not only can obtain high-quality finished product phosphoric acid, and has correspondingly reduced the processing load of liquid-solid separation device.Because the liquid phase after separating is returned the acidolysis groove, allow liquid phase that certain solid content is arranged, thereby reduced requirements for liquid solid separation again, make the process optimization of the liquid-solid sepn process of phosphoric acid phosphogypsum.So both improve the phosphoric acid product quality, reduced the phosphoric acid production cost again.
3. at present both at home and abroad the phosphoric acid production technical process of phosphoric acid production enterprise is substantially all taked, and will be regardless of level from the phosphoric acid material pulp that the acidolysis groove comes out and successively directly enter vacuum filter in the lump and carry out liquid-solid separation.With the present invention existing phosphoric acid production flow process is transformed, only needing increases a subsider or swirler, sets up several transport pipes, the plant investment expense increases under few situation, just can improve throughput more than 20%, and the quality of phosphoric acid improves greatly, also improved P simultaneously
2O
5The rate of recovery.
Of the present invention open, traditional Wet-process Phosphoric Acid Production technology has been pushed ahead major step.
The invention is not restricted to the described mode of embodiment, also can be designed to other embodiments according to its invention thought.
Claims (4)
1. optimized wet process for production of sulphuric acid, process step is successively: (1) Rock Phosphate (72Min BPL) and sulfuric acid generate phosphoric acid material pulp in the reaction of acidolysis groove, (2) phosphoric acid material pulp enters liquid-solid separation device and carries out liquid-solid phase and separate, liquid phase is a phosphoric acid, solid phase is a phosphogypsum, (3) the solid phase phosphogypsum of separating is washed, washings mixes with Partial Liquid Phase phosphoric acid at least and returns the acidolysis groove and recycle, it is characterized in that after hydrolysis procedure, set up the sedimentation operation before the liquid-solid separation circuit, the phosphoric acid material pulp that comes out from the acidolysis groove carries out sedimentation earlier, draws respectively from different settled layer then, wherein is the liquid-solid separation circuit that part enters down the road at least.
2. optimized wet process for production of sulphuric acid according to claim 1, it is characterized in that phosphoric acid material pulp carries out the rough classification sedimentation earlier, draw respectively from its thick slurry layer and thin pulp layer, after a thick slurry layer slip of drawing enters filtering separation device formation filter cake layer, the slip of drawing from the thin pulp layer enters filtering separation device again, liquid phase is a finished product phosphoric acid, and wherein a part is mixed with the washings of filter residue and to be returned the acidolysis groove and recycle.
3. optimized wet process for production of sulphuric acid according to claim 1, it is characterized in that phosphoric acid material pulp carries out sufficient sedimentation earlier, form clear layer and stiff layer, draw respectively then, the clarified liq of being drawn by clear layer is a finished product phosphoric acid, the material of drawing from the stiff layer enters equipment for separating liquid from solid, and the liquid phase of separating is mixed with the washings of solid phase phosphogypsum and returned the acidolysis groove and recycle.
4. according to claim 1 or 2 or 3 described optimized wet process for production of sulphuric acid, it is characterized in that phosphoric acid material pulp when carrying out sedimentation, can add flocculation agent, to accelerate settling process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117727A CN1052702C (en) | 1996-09-27 | 1996-09-27 | Optimized wet process for production of sulphuric acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117727A CN1052702C (en) | 1996-09-27 | 1996-09-27 | Optimized wet process for production of sulphuric acid |
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| CN1178192A true CN1178192A (en) | 1998-04-08 |
| CN1052702C CN1052702C (en) | 2000-05-24 |
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| CN96117727A Expired - Fee Related CN1052702C (en) | 1996-09-27 | 1996-09-27 | Optimized wet process for production of sulphuric acid |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321057C (en) * | 2005-02-01 | 2007-06-13 | 云南三环化工有限公司 | Improved wet dihydrate phosphoric acid producing process |
| CN100439239C (en) * | 2006-10-12 | 2008-12-03 | 贵州宏福实业开发有限总公司 | Method of reducing rare earth content in phosphoric acid |
| CN102284463A (en) * | 2011-06-08 | 2011-12-21 | 湖北三宁化工股份有限公司 | Treatment method and device for wet discharging and dry stacking of ardealite |
| CN102583284A (en) * | 2012-02-09 | 2012-07-18 | 昆明川金诺化工股份有限公司 | Method for removing slag before solvent extraction in process of producing industrial-grade phosphoric acid by wet-process phosphoric acid |
| CN103420350A (en) * | 2013-09-04 | 2013-12-04 | 安徽新中远化工科技有限公司 | Method for removing impurities in phosphoric acid |
| CN103520993A (en) * | 2013-10-16 | 2014-01-22 | 瓮福紫金化工股份有限公司 | Filtering cloth washing water filtering system in wet-process phosphoric acid production |
| CN104860288A (en) * | 2015-05-07 | 2015-08-26 | 深圳市芭田生态工程股份有限公司 | Method for preparing phosphoric acid by using wet method |
| CN105883743A (en) * | 2016-04-13 | 2016-08-24 | 四川绵竹市盘龙矿物质有限责任公司 | Method for increasing yield of defluorinated phosphorus in feed grade calcium hydrogen phosphate |
| CN106395775A (en) * | 2016-08-31 | 2017-02-15 | 郝付勇 | Method for filtering phosphoric acid extraction slurry |
| CN111977624A (en) * | 2020-09-02 | 2020-11-24 | 瓮福（集团）有限责任公司 | High-valued clean production process for reducing phosphorus loss of phosphogypsum by wet-process phosphoric acid device |
| CN113148968A (en) * | 2021-05-24 | 2021-07-23 | 云南云天化股份有限公司 | Method for producing alpha-semi-hydrated gypsum by wet-process phosphorus processing |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876204B (en) * | 2006-07-06 | 2010-07-07 | 上海南化水处理技术工程有限公司 | Ardealite innocent treatment method |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2929777A (en) * | 1958-12-11 | 1960-03-22 | Int Minerals & Chem Corp | Clarification of acidic phosphatic solutions |
| US3099622A (en) * | 1960-10-25 | 1963-07-30 | Int Minerals & Chem Corp | Production of clarified acidic phosphatic solutions |
| US3129170A (en) * | 1960-10-25 | 1964-04-14 | Int Minerals & Chem Corp | Process for the clarification of an acidic inorganic phosphatic solution |
| CN1043213C (en) * | 1994-06-01 | 1999-05-05 | 龚家竹 | Method for extracting phosphoric acid by hydrochloric acid method |
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- 1996-09-27 CN CN96117727A patent/CN1052702C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321057C (en) * | 2005-02-01 | 2007-06-13 | 云南三环化工有限公司 | Improved wet dihydrate phosphoric acid producing process |
| CN100439239C (en) * | 2006-10-12 | 2008-12-03 | 贵州宏福实业开发有限总公司 | Method of reducing rare earth content in phosphoric acid |
| CN102284463A (en) * | 2011-06-08 | 2011-12-21 | 湖北三宁化工股份有限公司 | Treatment method and device for wet discharging and dry stacking of ardealite |
| CN102583284A (en) * | 2012-02-09 | 2012-07-18 | 昆明川金诺化工股份有限公司 | Method for removing slag before solvent extraction in process of producing industrial-grade phosphoric acid by wet-process phosphoric acid |
| CN103420350B (en) * | 2013-09-04 | 2016-03-02 | 安徽新中远化工科技有限公司 | The minimizing technology of impurity in a kind of phosphoric acid |
| CN103420350A (en) * | 2013-09-04 | 2013-12-04 | 安徽新中远化工科技有限公司 | Method for removing impurities in phosphoric acid |
| CN103520993A (en) * | 2013-10-16 | 2014-01-22 | 瓮福紫金化工股份有限公司 | Filtering cloth washing water filtering system in wet-process phosphoric acid production |
| CN104860288A (en) * | 2015-05-07 | 2015-08-26 | 深圳市芭田生态工程股份有限公司 | Method for preparing phosphoric acid by using wet method |
| CN105883743A (en) * | 2016-04-13 | 2016-08-24 | 四川绵竹市盘龙矿物质有限责任公司 | Method for increasing yield of defluorinated phosphorus in feed grade calcium hydrogen phosphate |
| CN105883743B (en) * | 2016-04-13 | 2018-04-20 | 四川绵竹市盘龙矿物质有限责任公司 | A kind of method that defluorinate phosphrus reagent is improved in calcium hydrophosphate fodder production technology |
| CN106395775A (en) * | 2016-08-31 | 2017-02-15 | 郝付勇 | Method for filtering phosphoric acid extraction slurry |
| CN111977624A (en) * | 2020-09-02 | 2020-11-24 | 瓮福（集团）有限责任公司 | High-valued clean production process for reducing phosphorus loss of phosphogypsum by wet-process phosphoric acid device |
| CN111977624B (en) * | 2020-09-02 | 2022-12-23 | 瓮福（集团）有限责任公司 | High-valued clean production process for reducing phosphorus loss of phosphogypsum by wet-process phosphoric acid device |
| CN113148968A (en) * | 2021-05-24 | 2021-07-23 | 云南云天化股份有限公司 | Method for producing alpha-semi-hydrated gypsum by wet-process phosphorus processing |
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| CN1052702C (en) | 2000-05-24 |
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