CN100480176C - Wet-process two-stage phosphoric acid concentration method - Google Patents
Wet-process two-stage phosphoric acid concentration method Download PDFInfo
- Publication number
- CN100480176C CN100480176C CNB2006100399375A CN200610039937A CN100480176C CN 100480176 C CN100480176 C CN 100480176C CN B2006100399375 A CNB2006100399375 A CN B2006100399375A CN 200610039937 A CN200610039937 A CN 200610039937A CN 100480176 C CN100480176 C CN 100480176C
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- acid
- stage
- concentration
- sour
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses aprocess of two-stage condensing phosphoric acid with wet method. It comprises condensing phosphoric acid, clarifying, adsorbing with fluorine and water circulation system; and it employs a two-stage condensing course in series: adding diluted phosphoric acid into the first stage condensing closed circuit, heating with steam, steaming out of water in a short time invacuum condition to condense phosphoric acid into mediate acid, clarifying to remove part of suspending soild and getting clean acid A; putting acid A to the second condensing system to be condensed into diluted phosphoric acid, clarifying and getting clean acid B, that is the finished product. The left acid by clarifying in the two stages is used for preparing compound fertilizer or is recoveried after press filtration; the SiF4 and HF in steam is adsorbed through two-stage adverse current and is prepared into side product of fluosilicic acid. The invention smploys a two-stage condensing process, which improvese heat and mass transferring process, saves investment at the same production capability; reduces phosphoric acid circulation amount and circulating water consumption; reduces phosphoric acid viscosity and improves concentration and quality of finished product.
Description
Technical field
The invention belongs to the phosphoric acid production field, relate to a kind of Wet-process two-stage phosphoric acid concentration method.
Background technology
Phosphoric acid by wet process is the basic intermediates of multiple fertile industry of phosphorus and phosphate industry, has important status, is in great demand.China has formed about 5,000,000 tons of/year P at present
2O
5Throughput.In most cases, the post-treatment of phosphoric acid all requires to use strong phosphoric acid, and this just need carry the filtration grade dilute phosphoric acid dense by means of various concentration method.The method that extensively adopts is to adopt the pump circulation vacuum concentration method of single-stage concentration technique at present.
Single-stage concentrates from 24～26%P
2O
5Dilute phosphoric acid once concentration to 48～52% finished product strong phosphoric acid, it exists following shortcoming: heat transfer efficiency is low during the heating of round-robin strong phosphoric acid, and well heater need have bigger heating-surface area; The solubleness of impurity is little in the strong phosphoric acid, and crystallization is separated out easily, and in order to prevent fouling in the circulation loop, the phosphoric acid temperature rise of heating back should be controlled lowlyer, thereby sour internal circulating load is bigger, and watt consumption is bigger; Strong phosphoric acid boiling point height, if will keep lower boiling point, the pressure of flashing chamber then will be controlled lowlyer, under this pressure, the evaporation capacity of flashing chamber is also just lower; Specifications of equipment such as flashing chamber, well heater, recycle pump are bigger, invest more; When foreign matter content is high in the dilute phosphoric acid, can bring difficulty to concentration operation, finished product concentration of phosphoric acid and quality are reduced.
Summary of the invention
The objective of the invention is at above-mentioned technical problem provide that a kind of cost is low, the Wet-process two-stage phosphoric acid concentration method of save energy, raising phosphoric acid quality.
The objective of the invention is to realize by following technical measures:
A kind of Wet-process two-stage phosphoric acid concentration method, comprise that Phosphoric Acid Concentration, phosphoric acid storage clarification, fluorine absorb, circulating water system, this method adopts the two-stage series connection concentration flow path, dilute phosphoric acid is joined in the first step concentration systems circulation loop, use steam heating, flash evaporation moisture makes Phosphoric Acid Concentration become middle acid under vacuum state, the sour storage tank clarification through the centre, remove the part suspended solids, get sour clearly A; Clear sour A delivers in the concentration systems circulation loop of the second stage, use steam heating, flash evaporation moisture makes sour clearly A be condensed into strong phosphoric acid under vacuum state, again through storage tank clarify sour clearly B, clear sour B is finished product phosphoric acid, and the acid of becoming silted up of two-stage clarification gained is directly used in the processing compound manure or reclaims wherein phosphoric acid through press filtration;
The SiF that contains in the vaporised gas
4, the HF water absorbs through countercurrent washing, makes the byproduct silicofluoric acid, the silicofluoric acid that second stage concentration systems reclaims seals in first step concentration systems, with the generation that reduces silica gel with gather.
The spissated method of described Wet-process two-stage phosphoric acid, wherein the spissated technical parameter of the first step is: dilute phosphoric acid concentration 20～28%P
2O
5, solid content≤2.5%, middle acid concentration 38～40%P
2O
5, 80～85 ℃ of recycle acid temperature, temperature head is 5～6 ℃ before and after the flashing chamber pressure 20～25kPa, well heater, well heater heat transfer coefficient 5000～6000kJ/ (m
2H ℃), the clear sour A solid content in storage tank clarification back≤2.0% is sent in middle acid; The spissated technical parameter in the second stage is: clear sour A concentration 38～40%P
2O
5, solid content≤2.0%, gelled acid concentration 48～52%P
2O
5, 85～87 ℃ of recycle acid temperature, temperature head is 2.0～3.0 ℃ before and after the flashing chamber pressure 9～10kPa, well heater, heat transfer coefficient 4000～4800kJ/ (m
2H ℃), gelled acid send the clear sour B solid content in storage tank clarification back≤2.0%.
Described Wet-process two-stage phosphoric acid concentration method, wherein the byproduct silicofluoric acid is 12～22%H
2SiF
6
Beneficial effect of the present invention:
1, first step phosphoric acid concentration low viscosity is little, and thermal resistance is little during heat transfer, the heat transfer efficiency height, thereby the heat transfer coefficient of well heater is bigger, the heat transfer area that needs is less.And because the moisture major part in the phosphoric acid promptly evaporates when phosphoric acid concentration is low in the first step, because the heating and the moisture evaporation of phosphoric acid are all more convenient at this moment, evaporation institute thermal losses is also slightly low.
2, the first step is because the phosphoric acid concentration lower boiling is low, and its equilibrium pressure is higher at a certain temperature, so flashing chamber can be operated under elevated pressures.At this moment the specific volume of secondary steam (steam that material is evaporated) is less, and the steam specific volume is healed little evaporation capacity just more greatly under identical secondary steam linear velocity, so it is just less to evaporate the identical needed flashing chamber sectional area of moisture.
3, first step phosphoric acid concentration is low, and the solubleness of impurity is bigger, and be difficult for crystallization and separate out the dirty thing of formation, thus allow phosphoric acid heating back temperature rise higher, thereby the phosphoric acid internal circulating load is less, watt consumption is also less.
4, first step concentration systems working pressure is higher, allows the recirculated water return water temperature of barometric condenser high slightly, thereby can reduce the recirculated water consumption.
5, middle acid has been removed a part of suspended solid in advance through clarification, and the spissated phosphoric acid viscosity in the second stage is reduced, and has reduced operation easier, thereby can improve finished product concentration of phosphoric acid and quality.This is particularly important for the higher dilute phosphoric acid of foreign matter content.
6, because the influence of above-mentioned various factors makes first step concentration systems efficient improve the energy consumption reduction, the required equipment specification is less, invests less.
7, because equipment is little, the efficient height is used for large-scale plant and also can reduces the quantity that concentrates series, realizes that domestic manufacture of key equipment is also easier.
The spissated leading indicator of single-stage and two-stage is relatively as follows:
Unit single-stage method of enrichment two-stage method of enrichment (summation)
Phosphoric acid well heater total heating surface (THS) amasss m
21.000 0.581
Flashing chamber total sectional area m
21.000 0.636
Phosphoric Acid Circulating Pump total flux m
31.000 0.581
Total system invests 1.000 0.700
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The invention will be further elaborated by the following examples, but do not limit the present invention.
Embodiment 1
In conjunction with Figure of description and table 1,200,000 tons of/year P
2O
5Concentration systems adopts the two-stage series connection concentration flow path, and the first step concentrates: with concentration is 28%P
2O
5, solid content≤2.5% the filtration grade dilute phosphoric acid join in the pump circulation loop (forming) by flashing chamber, Phosphoric Acid Circulating Pump, well heater, phosphoric acid is heated with steam by well heater, temperature head is 5～6 ℃ before and after the well heater, well heater heat transfer coefficient 5000kJ/ (m
2H ℃), the recycle acid temperature is controlled at 80～85 ℃, and (to make Phosphoric Acid Concentration become concentration be 40%P to flash evaporation moisture in the pressure 20～25kPa) at flashing chamber under the vacuum state
2O
5In the middle of acid, the part suspended solids is removed in the clarification of sour storage tank through the centre, sour clearly A, clear sour A solid content≤2.0%; Clear sour A is delivered to second stage concentration systems, and the main device of second stage concentration systems is with first step concentration systems, and second stage concentration systems technical parameter is: middle acid (clear sour A) concentration 40%P
2O
5, solid content≤2.0%, gelled acid concentration 50%P
2O
5, 85～87 ℃ of recycle acid temperature, temperature head is 2.0～3.0 ℃ before and after the flashing chamber pressure 9～10kPa, well heater, heat transfer coefficient 4800KJ/ (m
2H ℃), gelled acid gets sour clearly B, clear sour B solid content≤2.0% after sending the storage tank clarification.40%P
2O
5In the middle of acid (clear sour A) flash evaporation moisture in flashing chamber to make Phosphoric Acid Concentration become concentration be 50%P
2O
5Strong phosphoric acid, again through storage tank clarification, sour clearly B, clear sour B is finished product phosphoric acid.The acid of becoming silted up of two-stage clarification gained can be directly used in the processing compound manure or reclaim wherein phosphoric acid through press filtration.
From the vaporised gas that flashing chamber comes out, contain SiF
4, HF, through scum dredger, absorb in two sections fluorine absorbers (respectively supporting circulation groove) water countercurrent washing, make 12～22%H
2SiF
6The silicofluoric acid byproduct, residual air is again through scum dredger, barometric condenser, be cooled with circulating water and condensation, (overwhelming majority is a water vapor to non-condensable gases in the gas after absorbing fluorine by the steam injector extraction at last, in barometric condenser, cool off and condensation the remaining non-condensable gases that has only minute quantity---air, CO with recirculated cooling water
2Deng, extract emptying out by steam injector).The silicofluoric acid that second stage concentration systems reclaims seals in the circulation groove of fluorine absorber in the first step concentration systems, and with the generation that reduces silica gel with gather, all the other steps are with first step concentration systems.
200,000 tons of/year P of table 1
2O
5Concentrating unit adopts single-stage and the spissated design of two-stage relatively
| Project | The existing device single-stage of certain engineering concentrates | Two-stage concentrates | Two-stage is saved than one-level |
| Produce series | Bi serie, every serial 100,000 tons of/year P 2O 5 | Single series, two-stage | |
| Product acid concentration | Be concentrated to 50%P by 28% 1 step 2O 5 | The first step is concentrated to 40% clarification separation by 28% and removes suspended substance; Second step was concentrated to 50% by 40% again | |
| Evaporator evaporation area and evaporation capacity | Two vaporizer total evaporation area: 2 * 32.15=64.3m 2Evaporation capacity: 723.4kgH 2O/(m 2·h) | First evaporator evaporation area: 16.61m 2Second stage evaporator evaporation area: 19.62m 2Total evaporation area 36.23m 2Average evaporation capacity: 1284kgH 2O/(m 2·h) | Save evaporation area 28.07m 2Account for 43.7% |
| The Phosphoric Acid Circulating Pump flow | Every Q=7315m of two recycle pumps 3/ h total flux 14630m 3/h | First step recycle pump Q=5000m 3/ h second stage recycle pump Q=4800m 3/ h total flux 9600m 3/h | Save phosphoric acid internal circulating load 5030m 3/ h accounts for 34.4% |
| Phosphoric acid well heater heat transfer area | Two every heat transfer area: F=568.2m 2Total area 1136.4m 2 | First level heater heat transfer area: F=380m 2Second stage well heater heat transfer area: F=320m 2Total area 700m 2 | Save heat transfer area 436.4m 2Account for 384% |
| Fluorine absorber | Tower of each series, sectional area: F=32.15m 2Total area 64.3m 2 | The long-pending 5.3m of two tower sections of each level 2Total area 21.22m 2 | Save the long-pending 43.08m of tower section 2Account for 66.9% |
| Quantity of circulating water | Total Water 5500m 3/h | Total Water 3800m 3/h | Save quantity of circulating water 1700m 3/h |
| Account for 31% | |||
| Plant investment | Comprehensively relatively make an appointment with and to save 30% |
Claims (2)
1. Wet-process two-stage phosphoric acid concentration method, comprise that Phosphoric Acid Concentration, phosphoric acid storage clarification, fluorine absorb, circulating water system, it is characterized in that this method adopts the two-stage series connection concentration flow path, dilute phosphoric acid is joined in the first step concentration systems circulation loop, use steam heating, flash evaporation moisture makes Phosphoric Acid Concentration become middle acid under vacuum state, the sour storage tank clarification through the centre, remove the part suspended solids, get sour clearly A; Clear sour A delivers in the concentration systems circulation loop of the second stage, use steam heating, flash evaporation moisture makes sour clearly A be condensed into strong phosphoric acid under vacuum state, again through storage tank clarify sour clearly B, clear sour B is finished product phosphoric acid, and the acid of becoming silted up of two-stage clarification gained is directly used in the processing compound manure or reclaims wherein phosphoric acid through press filtration;
The SiF that contains in the vaporised gas
4, the HF water absorbs through countercurrent washing, makes the byproduct silicofluoric acid, the silicofluoric acid that second stage concentration systems reclaims seals in first step concentration systems, with the generation that reduces silica gel with gather;
Wherein the spissated technical parameter of the first step is: dilute phosphoric acid concentration 20～28%P
2O
5, solid content≤2.5%, middle acid concentration 38～40%P
2O
5, 80～85 ℃ of recycle acid temperature, temperature head is 5～6 ℃ before and after the flashing chamber pressure 20～25kPa, well heater, well heater heat transfer coefficient 5000～6000kJ/ (m
2H ℃), clear sour A solid content≤2.0% after the storage tank clarification is sent in middle acid;
Wherein the spissated technical parameter in the second stage is: clear sour A concentration 38～40%P
2O
5, solid content≤2.0%, gelled acid concentration 48～52%P
2O
5, 85～87 ℃ of recycle acid temperature, temperature head is 2.0～3.0 ℃ before and after the flashing chamber pressure 9～10kPa, well heater, heat transfer coefficient 4000～4800KJ/ (m
2H ℃), gelled acid send clear sour B solid content≤2.0% after the storage tank clarification.
2, Wet-process two-stage phosphoric acid concentration method according to claim 1 is characterized in that the byproduct silicofluoric acid is 12～22%H
2SiF
6
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100399375A CN100480176C (en) | 2006-04-27 | 2006-04-27 | Wet-process two-stage phosphoric acid concentration method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100399375A CN100480176C (en) | 2006-04-27 | 2006-04-27 | Wet-process two-stage phosphoric acid concentration method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1843901A CN1843901A (en) | 2006-10-11 |
| CN100480176C true CN100480176C (en) | 2009-04-22 |
Family
ID=37062872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100399375A Active CN100480176C (en) | 2006-04-27 | 2006-04-27 | Wet-process two-stage phosphoric acid concentration method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100480176C (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445226B (en) * | 2008-11-27 | 2011-04-13 | 中国石化集团南京设计院 | Novel technology of two-effect evaporation of phosphoric acid with wet method |
| CN101474523B (en) * | 2008-12-26 | 2011-05-11 | 瓮福（集团）有限责任公司 | Absorption method of fluorine |
| CN101972584A (en) * | 2010-11-01 | 2011-02-16 | 山东聊城鲁西化工第四化肥有限公司 | Device and process for washing phosphoric acid tail gas and cogenerating sodium fluosilicate |
| CN102491295B (en) * | 2011-11-28 | 2014-03-12 | 安徽六国化工股份有限公司 | Method for producing monoammonium phosphate by utilizing sludge acid as raw material through slurry concentration process |
| CN102863267B (en) * | 2012-09-08 | 2014-03-26 | 湖北三宁化工股份有限公司 | Method for producing monoammonium phosphate and coproducing N-P binary compound fertilizer by using wet-process phosphoric acid |
| CN104211031B (en) * | 2013-06-04 | 2017-02-08 | 四川玖长科技有限公司 | Equipment and process for recovery of fluorine from flue gas of hydration absorption of phosphorus in kiln-method phosphoric acid technology |
| CN106064809B (en) * | 2016-05-27 | 2018-10-02 | 云南磷化集团有限公司 | A kind of high-temperature gas directly heats the method that concentrated wet-process phosphoric acid prepares peroxophosphoric acid |
| CN106006806A (en) * | 2016-07-22 | 2016-10-12 | 株洲三特环保节能有限公司 | Hot air and tubular heater combined waste acid concentration treatment method and device |
| CN107161965A (en) * | 2017-04-21 | 2017-09-15 | 宜昌东圣磷复肥有限责任公司 | A kind of wet-process phosphoric acid concentration waste gas recovering device and its technique |
| CN108101012B (en) * | 2018-01-25 | 2023-09-29 | 中国五环工程有限公司 | Wet phosphoric acid concentration production process and system |
| CN110562943A (en) * | 2019-09-05 | 2019-12-13 | 云南云天化以化磷业研究技术有限公司 | Method for continuously preparing superphosphoric acid |
| CN110510590B (en) * | 2019-10-08 | 2024-06-14 | 中化重庆涪陵化工有限公司 | Stable and efficient wet-process phosphoric acid production system and process |
| CN114314539B (en) * | 2020-09-27 | 2023-04-11 | 四川大学 | Method for multi-effect sectional concentration and fractional flash defluorination of wet-process phosphoric acid |
-
2006
- 2006-04-27 CN CNB2006100399375A patent/CN100480176C/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 大型湿法磷酸和磷复肥装置技术进步综述. 陈如玉.硫酸设计与粉体工程，第2005年第1期. 2005 |
| 大型湿法磷酸和磷复肥装置技术进步综述. 陈如玉.硫酸设计与粉体工程，第2005年第1期. 2005 * |
| 湿法磷酸浓缩装置的多级蒸发设计. 张沂圭，蒋国贤，孙菊萍.硫酸设计与粉体工程，第2004年第2期. 2004 |
| 湿法磷酸浓缩装置的多级蒸发设计. 张沂圭，蒋国贤，孙菊萍.硫酸设计与粉体工程，第2004年第2期. 2004 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1843901A (en) | 2006-10-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100480176C (en) | Wet-process two-stage phosphoric acid concentration method | |
| CN102616973B (en) | Method and device for processing high-saline organic wastewater | |
| CN104016317A (en) | Method and device for preparing high-concentration dilute nitric acid | |
| CN109432808B (en) | Energy-saving and environment-friendly DDGS waste heat evaporation system | |
| CN101704539B (en) | Method and device for evaporating mother liquid in aluminium oxide plant | |
| CN102249203A (en) | Phosphoric acid evaporation process and device thereof | |
| CN101643203A (en) | Method for recovering and utilizing steam condensate water in production of wet phosphoric acid | |
| CN103566605A (en) | Treatment equipment and treatment method of molasses alcohol waste liquid | |
| CN206680208U (en) | A kind of residual heat from boiler fume coupling evaporation concentrates desulfurization wastewater system | |
| CN101962813B (en) | Thermal-energy recycling system in spandex-spinning production process | |
| CN101445226B (en) | Novel technology of two-effect evaporation of phosphoric acid with wet method | |
| CN111717949A (en) | Low-temperature multi-effect evaporation sewage concentration device and process of finned heat pipe | |
| CN101982450B (en) | Method for recovering butanol-butyl acetate from waste acid water generated during antibiotic production through reduced pressure distillation | |
| CN101913669A (en) | Multi-effect energy-saving ammonia recovery process and device | |
| CN105967255A (en) | Landfill leachate treatment system and technology | |
| CN114229936B (en) | Ammonia water MVR stripping system and stripping method thereof | |
| CN104341084B (en) | For the energy-saving printing and dyeing sludge dehumidification system of cogeneration | |
| CN202030875U (en) | High-efficiency energy-saving flash evaporation device of viscose acid-bath system | |
| CN2726696Y (en) | Composite type Chinese medicinal liquid concentrating and alcohol reclaiming device | |
| CN209828291U (en) | Heat pump vacuum concentration system | |
| CN201787847U (en) | Heat recycling system in spinning production process of spandex | |
| CN208525852U (en) | A kind of energy-saving distilling equipment | |
| CN203736879U (en) | Extracted water evaporating and concentrating system | |
| CN212740792U (en) | Low-temperature multi-effect evaporation sewage concentration device with fin heat pipes | |
| CN206121197U (en) | A MVR vapor recompression device for PA6 polymerization monomer is retrieved |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: SINOPEC NANJING ENGINEERING COMPANY LIMITED Free format text: FORMER NAME: NANJING INST. OF DESIGN, SINOPEC |
|
| CP03 | Change of name, title or address |
Address after: 211100, No. 1189, Jian Jian Road, Dongshan Town, Jiangning District, Jiangsu, Nanjing Patentee after: Sinopec Nanjing Engineering & Construction Inc. Address before: 210048 Jiangsu Province, Nanjing city Liuhe District Dachang geguan Road No. 268 Patentee before: Nanjing Inst. of Design, SINOPEC |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: No. 3 horses horses Science Park Avenue in Qixia District of Nanjing City, Jiangsu province 210049 Patentee after: SINOPEC NANJING ENGINEERING & CONSTRUCTION Inc. Address before: 211100, No. 1189, Jian Jian Road, Dongshan Town, Jiangning District, Jiangsu, Nanjing Patentee before: SINOPEC NANJING ENGINEERING & CONSTRUCTION Inc. |