CN103979510A - Dearsenization method in production of phosphoric acid - Google Patents
Dearsenization method in production of phosphoric acid Download PDFInfo
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- CN103979510A CN103979510A CN201410169485.7A CN201410169485A CN103979510A CN 103979510 A CN103979510 A CN 103979510A CN 201410169485 A CN201410169485 A CN 201410169485A CN 103979510 A CN103979510 A CN 103979510A
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- phosphoric acid
- sulfide
- arsenic
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- hydrogen sulfide
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Abstract
The invention belongs to the technical field of the production of phosphoric acid in inorganic chemical industry, and relates to a dearsenization method in the production of phosphoric acid by a hot process. In the method, sulfide is used as adearsenization agent, and all the sulphur is wholly used for dearsenization and is fully utilized; at the same time, a sulfuretted hydrogen recovery facility does not need to be manufactured and mounted, so that the cost is reduced in various aspects, the production safety is improved, and the pollution of sulfuretted hydrogen to environment is reduced. The main implemented process sequences comprise that yellow phosphorus and air are combusted in a combustion furnace to generate phosphorus pentoxide flue gas, then the phosphorus pentoxide flue gas enters a hydration tower for reaction so as to generate phosphoric acid, the sulfide is firstly made into sulfuretted hydrogen gas which then enters a dearsenization reactor to be reacted with the phosphoric acid from the hydration tower to generate a mixture containing arsenic sulfide precipitates, the mixture is filtered, the obtained phosphoric acid enters a degassing groove for aeration, the sulfuretted hydrogen after the aeration is wholly fed into the hydration tower for reaction with the phosphoric acid, a part of arsenic sulfide is initially generated, the generated arsenic sulfide then enters the dearsenization reactor for further dearsenization, and then colour modulation treatment and acid regulation treatment are carried out on the phosphoric acid after the aeration, so that finished products are manufactured.
Description
Technical field:
The invention belongs to the phosphoric acid production technical field in inorganic chemistry industry, relate to a kind of arsenic removing method in thermal phosphoric acid production.
Background technology:
Phosphoric acid is important industrial chemicals and intermediate, and the production method of phosphoric acid mainly contains wet method and Re Fa, and kiln-process phosphoric acid is in exploitation.The mode of production of phosphoric acid by wet process is to make phosphoric acid with mineral acid and Rock Phosphate (72Min BPL) decomposition reaction, and the concentration of phosphoric acid by wet process is low, impurity is many, is mainly used in the production of phosphate fertilizer for agricultural, has also occurred now that some purification of wet process phosphoric acid are with the good phosphoric acid of the quality of production.Thermal phosphoric acid has that product concentration is high, purity advantages of higher, and in hi-tech, the meticulous phosphorous chemical industry of high added value, purposes is more and more wider.The production technique of thermal phosphoric acid is mainly divided into three relatively independent operations such as yellow phosphorus burning, Vanadium Pentoxide in FLAKES hydration, industrial phosphoric acid dearsenification purification, and thermal phosphoric acid is often divided into technical grade, food grade, electronic-grade by purity.The impurity such as the arsenic in phosphoric acid, lead are harmful to human body, and arsenic is a kind of protoplasma poisonous substance, has very high toxicity, and the toxicity of its compound is also very violent, so the arsenic of removing in phosphoric acid is very important.Food grade and electron-level phosphoric acid all need the impurity height such as the arsenic in industrial phosphoric acid, lead to remove.The chemical state of arsenic in phosphoric acid also do not have consistent saying at present, but most people is thought to exist with forms such as arsenic acid or arsenus acid.
The method of phosphoric acid dearsenification mainly contains following several
1. sulphide precipitation: by add certain precipitation agent in phosphate raw material, make it produce indissoluble or insoluble compound is separated out, then obtain low-arsenic phosphorus acid by filtering separation.With P
2s
5doing its reaction principle of dearsenic agent is:
P
4S
10+16H
2O＝4H
3PO
4+10H
2S↑
H
3AsO
4+H
2S＝H
3AsO
3+H
2O+S↓
2H
3A
sO
3+3H
2S＝6H
2O+A
s2S
3↓
Pb
2++S
2-＝PbS↓
2. solvent extration: dissolve in arsenic impurities in organic acid based on phosphoric acid and be extracted out, thereby make its separation.
3. ion exchange method: process phosphoric acid with strong-acid ion exchange resin, thereby remove arsenic impurities.
Solvent extraction and ion exchange method due to equipment and processing cost too high, do not possess the feasibility of large-scale commercial production.
4. halogenide dearsenification method: Japanese Toyo Boseki K.K invention, patent publication No. CN1332698A, CN1817790A the method is by pass into hydrogen halide in polyphosphoric acid, or add and can under acidic conditions, form iron, the copper of hydrogen halide, the muriate of tin carrys out dearsenification, arsenic is converted into the gaseous substance that volatilization point is not high, separated by the mode of heating evaporation.This method shortcoming: high containing arsenide tail gas danger, intractability is large, processing cost is high, in this normal direction polyphosphoric acid, introduce haloid element impurity, polyphosphoric acid quality product is had to considerable influence, under chlorion effect, thereby the corrodibility of polyphosphoric acid also greatly increases and causes this technique, in the process of industrialization, equipment material is required to raising, and production cost improves.
In above several method, the most frequently used with sulphide precipitation.Step and equipment that this method is required are simple, and dearsenification is effective.In with Publication about Document, there is the discussion of pair sulphide precipitation:
< < chemical engineering design > > the 4th phase in 1997 " is brief talked the design of food grade phosphoric acid dearsenification after-treatment device " and has introduced the dearsenification reactor of practical enamel glass material, 100 ℃ of left and right, add P2S5 reaction 1 hour, cooling-sedimentation to a 50 ℃ left and right enters filter and filters.And analyzed respectively flame filter press, continuous horizontal vacuum band-type filter machine, centrifugal filter and pre-coating drum filter relative merits separately.
" the dearsenification experiment of the hot method industrial phosphoric acid " design of < < phosphate industry > > the 4th phase of calendar year 2001 adds P2S5 to carry out dearsenification reaction in the reactor of sealing, after finishing, dearsenification reaction filters that (filtrate is diatomite or quartz sand, use vacuum pump filtration under diminished pressure), phosphoric acid after filtration, through degassed, purify and finally obtains low-arsenic phosphorus acid.
< < phosphate industry > > the 1st phase in 2003 " discussion of low-arsenic phosphorus acid product development technology " has introduced and has used P2S5 to do the dearsenicating technology flow process of dearsenic agent.
The design of < < sulphur phosphorus " is produced food grade phosphoric acid by industrial phosphoric acid operate continuously " with powder technology > > the 6th phase in 2005 and has been introduced the arsenic in removal industrial phosphoric acid, sulfide, the continuous production processes of readily oxidizable substance and decolouring.
Above document has just been discussed the method for phosphoric acid dearsenification, but the equipment and process flow process that dearsenification is needed does not have detailed explanation, so be difficult to realize in actual production.
Meanwhile, current report with P
2s
5sulfides is done in the dearsenicating technology flow process of dearsenic agent, when dearsenification, always having some hydrogen sulfide excessive, that unreacted is complete is mixed in phosphoric acid, this to product be have dysgenic, therefore dearsenification filter after Production Flow Chart have the operation that aeration is removed unnecessary hydrogen sulfide in degassing vessel together.Due to hydrogen sulfide be toxic substance, environmental administration forbids directly discharge now, therefore manufacturing enterprise all needs the hydrogen sulfide recvery facility of installing to reclaim degassing vessel aeration hydrogen sulfide out now, wherein conventional is recycle of alkali liquor tower, with sodium hydroxide lye circulated sprinkling, absorb degassing vessel aeration hydrogen sulfide out, and the sodium sulfide solution of producing after reclaiming needs to be sent to relevant chemical plant and further processes.Therefore there are 2 defects: the one, in order to guarantee that dearsenification reaches the specification of quality that arsenic content is very low, dearsenic agent is all forced to can be excessive more, causes waste, cost larger; The 2nd, to more hydrogen sulfide excessive, that unreacted is complete, need to install back receiving apparatus, waste equipment, power, liquid medicine, reclaiming liquid still needs further processing, has all increased cost.
Summary of the invention
Therefore in order to overcome P in the past
2s
5the dearsenic agent that sulfides is done the dearsenicating technology existence of dearsenic agent is forced to the defects such as excessive, hydrogen sulfide need to reclaim, and the present patent application people spy has proposed arsenic removing method new in a kind of phosphoric acid production, and technical scheme of the present invention is achieved in that
An arsenic removing method in phosphoric acid production, is primarily characterized in that, the main technological steps of its enforcement comprises: the first step, and yellow phosphorus and air generate Vanadium Pentoxide in FLAKES flue gas after entering roasting kiln generation combustion reactions; Second step, Vanadium Pentoxide in FLAKES flue gas enters into the hydration of hydration tower and generates phosphoric acid, and phosphoric acid is suitably lowered the temperature by interchanger, and a small amount of Vanadium Pentoxide in FLAKES flue gas and surplus air that hydration has not absorbed enter exhaust gas recovery system; The 3rd step, sulfide as dearsenic agent is made hydrogen sulfide in hydrogen sulfide generator, hydrogen sulfide enters dearsenification reactor, gives birth to and reacts with the phosphoric acid hybrid concurrency of the tentatively generating portion red arsenic that come from hydration tower, more arsenic is combined with sulphur and generates throw out; The 4th step, the mixture forming after dearsenification reaction enters header tank, after enter again flame filter press and remove by filter containing arsenic sulfide precipitation; The 5th step, after filtering, gained phosphoric acid enters degassing vessel aeration, degassing vessel aeration hydrogen sulfide is out sent into hydration tower and is reacted with phosphoric acid counter current contact hybrid concurrency is raw, the mixture of preliminary generating portion red arsenic and phosphoric acid, this mixture enters further dearsenification of dearsenicator as described in the 3rd step, phosphoric acid after aeration is processed through toning, acid adjustment, makes finished product.
The present invention compares with original technology, improves with advantage and is:
P in the past
2s
5sulfides is done in the dearsenicating technology of dearsenic agent, in order to guarantee that dearsenification reaches the specification of quality that arsenic content is very low, dearsenic agent is all forced to can be excessive more, cause cost larger, dearsenification needs aeration after filtering, degassing vessel aeration hydrogen sulfide out also needs to send into recycle of alkali liquor tower and reclaims, and exists dearsenic agent to be forced to 2 excessive, hydrogen sulfide need to reclaim defects.And the present invention no longer sends into recycle of alkali liquor tower to degassing vessel aeration hydrogen sulfide out, but introduce hydration tower, react with phosphoric acid counter current contact hybrid concurrency is raw, mixture with preliminary generating portion red arsenic and phosphoric acid, the excessive hydrogen sulfide of dearsenicator is drawn and sent toward the hydration tower of technique leading portion, be used to the effect of preliminary dearsenification, effective sulphur in all like this sulfide dearsenic agents is all for dearsenification, obtained maximum utilization, do not need fabrication and installation hydrogen sulfide recvery facility simultaneously, many-side has reduced cost, and hydrogen sulfide of the present invention is closed circuit conveying and use, production system for the poisonous hydrogen sulfide of this use has improved production security greatly, reduce the pollution of hydrogen sulfide to environment.
Accompanying drawing explanation
Accompanying drawing is technological process of production sketch of the present invention.
Embodiment
Below in conjunction with specific embodiment, implementation step of the present invention is done to further detail explanation, be beneficial to the more well-known the object, technical solutions and advantages of the present invention of understanding.Be necessary to be pointed out that at this; described specific embodiment is only for further illustrating that the present invention is carried out below; 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 or equipment component is replaced with similar equipment according to the invention described above content, and embodiment is as follows:
The first step, yellow phosphorus at the uniform velocity stably enters roasting kiln, under the large blower fan draft effect that natural air is installed at production system rear portion, also enter continuously and stably roasting kiln, after reacting with air combustion with yellow phosphorus in the roasting kiln of water-cooling jacket heat exchange, generate Vanadium Pentoxide in FLAKES flue gas simultaneously; Second step, Vanadium Pentoxide in FLAKES flue gas enters into the hydration of hydration tower and generates phosphoric acid, phosphoric acid is suitably lowered the temperature by sheet frame interchanger, to control sour temperature in hydration tower, remain between 80 ℃ to 100 ℃, a small amount of Vanadium Pentoxide in FLAKES flue gas and surplus air that hydration has not absorbed enter exhaust gas recovery system, degassing vessel aeration hydrogen sulfide out in process system rear portion is sent into the phosphoric acid counter current contact of hydration tower and hydration generation and is reacted, the mixture of preliminary generating portion red arsenic and phosphoric acid; The 3rd step, sulfide as dearsenic agent is made hydrogen sulfide in hydrogen sulfide generator, hydrogen sulfide enters dearsenification reactor, gives birth to and reacts 10 to 30 minutes with the phosphoric acid hybrid concurrency of the tentatively generating portion red arsenic that come from hydration tower, more arsenic is combined with sulphur and generates throw out; The 4th step, the phosphoric acid and the red arsenic mixture that after dearsenification reaction, form enter header tank, after enter again flame filter press and remove by filter containing arsenic sulfide precipitation; The 5th step, after filtering, gained phosphoric acid enters degassing vessel, at phosphoric acid liquid, heated to 90 ℃ to 120 ℃ states, the air blasting continuously makes the excess hydrogen sulfide desorption of gases dissolving in acid and is taken away by air, degassing vessel aeration hydrogen sulfide is out sent into hydration tower and is reacted with phosphoric acid counter current contact hybrid concurrency is raw, the mixture of preliminary generating portion red arsenic and phosphoric acid, this mixture enters further dearsenification of dearsenicator as described in the 3rd step, phosphoric acid after aeration is processed through toning, acid adjustment, makes the phosphoric acid for food finished product complying with the national standard requirements.
Claims (2)
1. the arsenic removing method in phosphoric acid production, is primarily characterized in that, the main technological steps of its enforcement comprises: the first step, and yellow phosphorus and air generate Vanadium Pentoxide in FLAKES flue gas after entering roasting kiln generation combustion reactions; Second step, Vanadium Pentoxide in FLAKES flue gas enters into the hydration of hydration tower and generates phosphoric acid, and phosphoric acid is suitably lowered the temperature by interchanger, and a small amount of Vanadium Pentoxide in FLAKES flue gas and surplus air that hydration has not absorbed enter exhaust gas recovery system; The 3rd step, sulfide as dearsenic agent is made hydrogen sulfide in hydrogen sulfide generator, hydrogen sulfide enters dearsenification reactor, gives birth to and reacts with the phosphoric acid hybrid concurrency of the tentatively generating portion red arsenic that come from hydration tower, more arsenic is combined with sulphur and generates throw out; The 4th step, the mixture forming after dearsenification reaction enters header tank, after enter again flame filter press and remove by filter containing arsenic sulfide precipitation; The 5th step, after filtering, gained phosphoric acid enters degassing vessel aeration, degassing vessel aeration hydrogen sulfide is out sent into hydration tower and is reacted with phosphoric acid counter current contact hybrid concurrency is raw, the mixture of preliminary generating portion red arsenic and phosphoric acid, this mixture enters further dearsenification of dearsenicator as described in the 3rd step, phosphoric acid after aeration is processed through toning, acid adjustment, makes finished product.
2. the arsenic removing method in a kind of phosphoric acid production according to claim 1, it is characterized in that, adopt sulfide to do dearsenic agent, after production process, degassing vessel aeration hydrogen sulfide out is all sent into hydration tower and phosphatase reaction, the mixture of preliminary generating portion red arsenic and phosphoric acid, effective sulphur in all sulfide dearsenic agents is all for dearsenification, obtained maximum utilization, do not need fabrication and installation hydrogen sulfide recvery facility simultaneously, many-side has reduced cost, has improved production security, has reduced the pollution of hydrogen sulfide to environment.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271150A (en) * | 2015-10-22 | 2016-01-27 | 昆明理工大学 | Method for removing arsenic through industrial phosphoric acid |
| CN108910850A (en) * | 2018-09-25 | 2018-11-30 | 湖北兴福电子材料有限公司 | A kind of thermal method electron-level phosphoric acid arsenic removing method |
| CN109607502A (en) * | 2019-01-16 | 2019-04-12 | 中州新材料(杭州)有限公司 | A kind of energy-saving and environment-friendly phosphorus pentoxide production technology |
| CN111689618A (en) * | 2020-07-08 | 2020-09-22 | 北京中科沃特膜科技有限公司 | Safe and efficient arsenic removal device and process for strong-acid wastewater integrated membrane |
| CN112225188A (en) * | 2020-10-15 | 2021-01-15 | 中国五环工程有限公司 | Process for removing arsenic from phosphoric acid by wet method |
| CN115057419A (en) * | 2022-06-07 | 2022-09-16 | 瓮福（集团）有限责任公司 | Industrial-grade wet-process phosphoric acid dearsenification method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271150A (en) * | 2015-10-22 | 2016-01-27 | 昆明理工大学 | Method for removing arsenic through industrial phosphoric acid |
| CN105271150B (en) * | 2015-10-22 | 2017-10-27 | 昆明理工大学 | A kind of method of industrial phosphoric acid arsenic removal |
| CN108910850A (en) * | 2018-09-25 | 2018-11-30 | 湖北兴福电子材料有限公司 | A kind of thermal method electron-level phosphoric acid arsenic removing method |
| CN109607502A (en) * | 2019-01-16 | 2019-04-12 | 中州新材料(杭州)有限公司 | A kind of energy-saving and environment-friendly phosphorus pentoxide production technology |
| CN111689618A (en) * | 2020-07-08 | 2020-09-22 | 北京中科沃特膜科技有限公司 | Safe and efficient arsenic removal device and process for strong-acid wastewater integrated membrane |
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| CN112225188B (en) * | 2020-10-15 | 2022-04-29 | 中国五环工程有限公司 | Process for removing arsenic from phosphoric acid by wet method |
| CN115057419A (en) * | 2022-06-07 | 2022-09-16 | 瓮福（集团）有限责任公司 | Industrial-grade wet-process phosphoric acid dearsenification method |
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Address after: 538004, the Guangxi Zhuang Autonomous Region Fangchenggang Port District Bus Industrial Park, Sha Road, southeast side Applicant after: FANGCHENGGANG BOSEN CHEMICAL TECHNOLOGY CO., LTD. Address before: 538004 phosphorus chemical industry park, Lingang Industrial Park, southwest port area, Fangchenggang, the Guangxi Zhuang Autonomous Region Applicant before: Fangchenggang Bosen Chemical Co., Ltd. |
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Application publication date: 20140813 |