CN110240164A - The method and device of fluosilicic acid concentration - Google Patents
The method and device of fluosilicic acid concentration Download PDFInfo
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- CN110240164A CN110240164A CN201910559094.9A CN201910559094A CN110240164A CN 110240164 A CN110240164 A CN 110240164A CN 201910559094 A CN201910559094 A CN 201910559094A CN 110240164 A CN110240164 A CN 110240164A
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- fluosilicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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Abstract
The present invention relates to a kind of method and devices of fluosilicic acid concentration, which solve existing fluosilicic acid concentration is relatively low, the high technical problem of impurity content, it is equipped with for separating the silica gel separation equipment in fluosilicic acid, the heating equipment for heating air, for fluosilicic acid concentrator to be concentrated and for arsenic removal and except the cleaning equipment of mechanical admixture, concentrator front end is respectively communicated with separation equipment and heating equipment, and concentrator rear end is connected to cleaning equipment.The present invention should can be recycled in low dose fluoride silicic acid concentrate extensively.
Description
Technical field
The present invention relates to the method for concentration and device of a kind of siliceous, fluorine and the compound of other elements, more particularly to one
The concentration and recovery or other industry low dose fluoride silicic acid concentrate of kind Phosphoric Acid production process by-product fluosilicic acid with low concentration return
It receives.
Background technique
During Wet-process Phosphoric Acid Production, containing the fluorine of 2.5-3.0% in phosphorus ore used, in the process of concentrated acid decomposing phosphate rock
Middle generation silicon tetrafluoride gas, the overwhelming majority is directly absorbed by reaction liquid phase generates a variety of fluorides, enters phosphoric acid,diluted or phosphorus
In gypsum.About 10% silicon tetrafluoride gas can be escaped from reaction liquid phase, and it is low that 5-25% is generated after multi-level water washing absorption
Concentration fluosilicic acid, for downstream product such as production prodans, most producers have directly returned to again and have not given recycling in phosphoric acid,diluted
It utilizes.Fluosilicic acid returns in phosphoric acid, will cause the aggravation of prodan, potassium fluosilicate fouling, when with this phosphoric acid production phosphate fertilizer
Production process can also adversely affect, the quality and total content of final phosphate fertilizer product also will receive larger impact.
For a long time, the low dose fluoride silicic acid of phosphate fertilizer by-product, only a small number of producers are used to produce the products such as prodan, but
, economy bad factor limited by market dosage restricts, and comprehensive utilization ratio is very low.The low dose fluoride silicic acid of phosphate fertilizer by-product is dense because of its
Spend relatively low, and substances, other industry containing silica gel, phosphorus etc. are difficult to directly utilize.And the high concentration fluosilicic acid greater than 40% is answered extensively
For being fluorinated the numerous areas such as work, metallurgical electrolysis plating, economy is one of the direction of comprehensive utilization also superior to by-product villiaumite.
Fluosilicic acid thermal stability is poor, and heating is easily decomposed into ocratation and hydrogen fluoride gas, and 50 DEG C are increased to 80 DEG C of fluorine silicon
Sour resolution ratio increases 10-37 times；108.5 degrees Celsius of fluosilicic acid boiling point, it is completely decomposed into silicon tetrafluoride gas and hydrogen fluoride gas.
The vapor removed is flashed in silicon tetrafluoride gas and gas to react and generate a large amount of silica gel.With the raising of fluosilicic acid concentration,
Decomposition temperature is lower, and 30% concentration fluosilicic acid decomposes acutely at 70 DEG C, therefore Conventional concentration condition concentrate is to 40% or more high
Concentration is difficult to realize.There are mainly two types of existing patented technologies, is heated to 60-80 DEG C one is fluosilicic acid, low under vacuum conditions
Moisture flashes in concentration fluosilicic acid, realizes concentration；Such technique decomposes the silicon tetrafluoride gas of generation when vacuum flashing is concentrated
It can be reacted rapidly in gas phase pipeline with the vapor in flashed vapour and generate silica gel, cause line clogging, need frequently to clear up pipe
Road, the device utilization of capacity is low, and high concentration fluosilicic acid yield is also low；Another kind is that the concentrated sulfuric acid decomposes the dilute fluosilicic acid generation tetrafluoride in part
Then silicon gas is absorbed again with dilute fluosilicic acid and improves concentration；Such technique is while sulfuric acid decomposition generates silicon tetrafluoride gas
It is anti-with the water in liquid phase when also having vapor generation, and low dose fluoride silicic acid being recycled to absorb the silicon tetrafluoride gas generated
Ying Junhui generates a large amount of silica gel.Therefore, both techniques not can avoid in actual moving process and generate because fluosilicic acid decomposes
Silicon tetrafluoride gas reacts the problem of generating silica gel, leading to equipment, line clogging with water, and the device utilization of capacity is low, yield is low.
Summary of the invention
The present invention is relatively low in order to solve existing fluosilicic acid concentration, the high technical problem of impurity content, provide a kind of high concentration,
The low temperature method for concentration and device of high-purity fluorine silicic acid.
The present invention provides a kind of device of fluosilicic acid concentration, equipped with for separating the silica gel separation equipment in fluosilicic acid, using
In the heating equipment of heating air, for fluosilicic acid concentrator to be concentrated and for arsenic removal and except the cleaning equipment of mechanical admixture,
Concentrator front end is respectively communicated with separation equipment and heating equipment, and concentrator rear end is connected to cleaning equipment, and concentrator includes
Concentration tower, circulating pump and spray equipment are recycled, it is dense from recycling by spray equipment that circulating pump extracts fluosilicic acid in circulation concentration tower
The outflow of contracting tower top, circulation concentration tower are additionally provided with gas vent, and circulating pump can also extract fluosilicic acid in circulation concentration tower and flow into
Cleaning equipment, cleaning equipment include purification tank and accurate filter, and purification tank is equipped with agitating device.
Preferably, separation equipment includes natural subsidence equipment, plate and frame filter press, vertical type blotter press and centrifuge.
Preferably, heating equipment is equipped with air blower and heater, and heater can be added by low-pressure steam, hot water or hot wind
Hot-air.
The present invention provides a kind of method of fluosilicic acid concentration comprising following steps:
The first step separates the silica gel in fluosilicic acid；
Second step, circulation extract fluosilicic acid and hot air, take away moisture in fluosilicic acid using hot-air, improve fluorine silicon
Acid is to required concentration；
Third step, eliminating arsenic by fluosilicic acid and remove mechanical admixture, obtain finished product fluosilicic acid.
Preferably, hot air temperature is 40-80 DEG C in second step, and fluosilicic acid temperature is 20-40 DEG C in second step.
Preferably, third step eliminating arsenic by fluosilicic acid is passed through stink damp precursor reactant arsenic removal under agitation.
The invention has the advantages that being concentrated using low-temperature circulating, the saturated water of water in fluosilicic acid under cryogenic conditions is utilized
Steam is high, and this very low difference of the saturated vapor of fluosilicic acid and ocratation, and circulation realizes the steaming of moisture under cryogenic
Hair, the concentration of fluosilicic acid；Fluosilicic acid temperature of the present invention is 20-40 DEG C, avoids the temperature condition of fluosilicic acid decomposition completely, practical
There is no silica gel generation in, device totally continuous can be run；By the pretreatment and post-processing to fluosilicic acid, go respectively
In addition to the silica gel and other impurities of its mixing, meet properties of product requirement.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Accompanying drawings symbol description:
100. separation equipment；101. low dose fluoride silicic acid entrance；102. silica gel exports；200. heater；210. air blower；
211. air intake；300. circulation concentration towers；301. liquid inlet；302. gas access；303. gas vent；304. liquid discharge
Mouthful；310. circulating pump；311. spray equipment；400. purification tank；401. high concentration fluosilicic acid entrances；402. hydrogen sulfide entrances；
410. self-fractionating pump；500. accurate filter；600. finished product storage tank；610. discharge pump；611. product outlet.
Specific embodiment
With reference to the accompanying drawings and examples to can the present invention be described further so that the skill of the technical field of the invention
Art personnel can be easy to implement the present invention.
As shown in Figure 1, the present invention provides a kind of device of fluosilicic acid concentration, for dense to phosphate fertilizer by-product low dose fluoride silicic acid
Contracting obtains the fluosilicic acid product of high concentration, and the present invention includes the concentrator being sequentially communicated, cleaning equipment and stores equipment, dense
Contracting front equipment end is also respectively communicated with separation equipment 100 and heating equipment.
For low dose fluoride silicic acid pretreatment separation silica gel, low dose fluoride silicic acid entrance 101 is passed through low dense separation equipment 100
Fluosilicic acid is spent, the separation of silica gel in low dose fluoride silicic acid is realized by equipment such as centrifuges, then passes through the entrance of liquid inlet 301
300 stored in liquid phase space of concentration tower is recycled, provides condition for subsequent concentration；Isolated silica gel is divided by 102 discharge of silica gel outlet
Equipment from silica gel can also take other separation equipments such as natural subsidence, plate and frame filter press, vertical type blotter press.
Heating equipment includes heater 200 and air blower 210, and for heating to air, air is from air intake 211
Into in air blower 210, heater 200 uses the media such as low-pressure steam, hot water or hot wind for heat source, will blow from air blower 210
Air out is heated to 40-80 DEG C, is blown into circulation 300 gas-phase space of concentration tower by gas access 302.
Concentrator is the capital equipment to the concentration of low dose fluoride silicic acid low-temperature circulating comprising circulation concentration tower 300 follows
Ring pump 310 and spray equipment 311, circulation concentration tower 300 can be divided into stored in liquid phase space and gas-phase space, stored in liquid phase space with
Liquid outlet 304 is connected to, and liquid outlet 304 is connected to circulating pump 310, and the low dose fluoride silicic acid of no silica gel is from liquid inlet 301
Into after stored in liquid phase space, the spray equipment 311 of circulation 300 upper end of concentration tower, no silica gel can be entered by circulating pump 310
Low dose fluoride silicic acid be opened and closed from the uniformly dispersion landing of spray equipment 311, or by control valve from high concentration fluosilicic acid
Entrance 401 enters cleaning equipment；Circulation 300 gas-phase space of concentration tower is respectively communicated with gas access 302 and gas vent 303, gas
Body outlet 303 is located at 300 top of circulation concentration tower, and the hot-air blown from air blower 210 enters circulation 300 lower part gas of concentration tower
Phase space, hot-air are contacted with spray without silica gel low dose fluoride silicic acid, realize mass-and heat-transfer, the low dose fluoride silicic acid of no silica gel
20-40 DEG C of circulating temperature after absorption heat, the moisture in liquid phase enters under filament saturation vapour pressure effect with successive
Gas taken out of outside circulating absorption tower from gas vent 303, moisture is constantly reduced, and low dose fluoride silicic acid concentration is gradually increased, most
Final concentration reaches 40%-50%.
Cleaning equipment is mainly used for eliminating arsenic by fluosilicic acid except impurity comprising purification tank 400 and precision with agitating device
Filter 500, the fluosilicic acid for reaching predetermined concentration enter purification tank 400 from high concentration fluosilicic acid entrance 401, under agitation
It is passed through stink damp precursor reactant arsenic removal from hydrogen sulfide entrance 402, the fluosilicic acid after arsenic removal is transferred to precision by self-fractionating pump 410
Filter 500 filters off the insoluble matter impurity in deacidification and the vulcanization arsenic of arsenic removal generation, finally obtains the finished product of 40%-50%
Fluosilicic acid product.
Storage equipment is mainly used for storing finished product fluosilicic acid comprising finished product storage tank 600 and discharge pump 610, finished product storage tank
600 receive by the filtered finished product fluosilicic acid of accurate filter 500, are gone out finished product fluosilicic acid by finished product by discharge pump 610
Mouth 611 flows out.
The present invention also provides a kind of method of fluosilicic acid concentration, concrete measures are as follows:
The first step, low dose fluoride silicic acid pretreatment separation silica gel.Can with natural subsidence, plate and frame filter press, vertical type blotter press,
The equipment such as centrifuge realize the separation of silica gel in low dose fluoride silicic acid, provide condition for subsequent concentration.
Second step, low-temperature circulating concentration.Setting is by air blower 210, heater 200, circulation concentration tower 300, circulating pump 310
Etc. equipment constitute low-temperature circulating enrichment facility.It is empty that low dose fluoride silicic acid is directly entered circulation 300 lower liquid phase of concentration tower storage
Between, which is extracted by circulating pump 310, by tower top spray equipment 311, realizes continuous circulation.Heater 200 is using low
Pressing the media such as steam, hot water or hot wind is heat source, and the air of air blower 210 is heated to 40-80 DEG C, is blown into circulation concentration tower
300 lower part gas-phase spaces, hot-air are contacted with the fluosilicic acid of spray, realize that mass-and heat-transfer, fluosilicic acid absorb circulation warm after heat
20-40 DEG C is spent, the moisture in liquid phase is taken circulation out of with the gas successively entered and inhaled under filament saturation vapour pressure effect
It receives outside tower, moisture is constantly reduced, and fluosilicic acid concentration is gradually increased, and ultimate density reaches 40%-50%.
Third step, the post-processing of high concentration fluosilicic acid.It post-processes mainly eliminating arsenic by fluosilicic acid and removes mechanical admixture.High concentration fluorine
Silicic acid is passed through stink damp precursor reactant arsenic removal under agitation, and high concentration fluosilicic acid recycles precision filtration equipment after arsenic removal
500 filter off the insoluble matter impurity in deacidification and the vulcanization arsenic of arsenic removal generation, finally obtain the finished product fluosilicic acid of 40%-50%
Product.
Fluosilicic acid method for concentration and device of the present invention, cardinal principle are concentrated using low-temperature circulating, and utilization is low
The saturated steam of water is high in fluosilicic acid under the conditions of temperature, and this very low difference of the saturated vapor of fluosilicic acid and ocratation,
The evaporation of circulation realization moisture under cryogenic conditions, the concentration of fluosilicic acid, and significantly because of low temperature (20-40 DEG C, normal pressure) of the invention
Lower than previous cryogenic vacuum concentration aspect the used cryogenic vacuum condition of patent (general 60-80 DEG C, vacuum -0.06~-
0.09MPa), the temperature condition of fluosilicic acid decomposition is avoided completely, does not have silica gel generation in practice, device can connect completely
Continuous operation.The pretreatment and post-processing of fluosilicic acid, the impurity in silica gel and impurity removal process mixed respectively for it,
It is the necessary means in order to meet its properties of product.
The above is not intended to restrict the invention, only to the preferred embodiment of the present invention for the skill of this field
For art personnel, the invention may be variously modified and varied.It is all to be limited in range in claim of the invention, it is done
Any modification, equivalent substitution, improvement and etc., should all be within protection scope of the present invention.
Claims (6)
1. a kind of device of fluosilicic acid concentration, characterized in that equipped with for separating the silica gel separation equipment in fluosilicic acid, being used to add
The heating equipment of hot-air, for fluosilicic acid concentrator to be concentrated and for arsenic removal and except the cleaning equipment of mechanical admixture, it is described
Concentrator front end is respectively communicated with the separation equipment and heating equipment, and the concentrator rear end is connected to the cleaning equipment,
The concentrator includes circulation concentration tower, circulating pump and spray equipment, and the circulating pump extracts fluorine in the circulation concentration tower
Silicic acid is flowed out by the spray equipment from the circulation concentration tower top, and the circulation concentration tower is additionally provided with gas vent, institute
The fluosilicic acid inflow cleaning equipment in the circulation concentration tower can also be extracted by stating circulating pump, and the cleaning equipment includes purification
Slot and accurate filter, the purification tank are equipped with agitating device.
2. the device of fluosilicic acid concentration according to claim 1, which is characterized in that the separation equipment includes natural subsidence
Equipment, plate and frame filter press, vertical type blotter press and centrifuge.
3. the device of fluosilicic acid according to claim 1 concentration, which is characterized in that the heating equipment be equipped with air blower and
Heater, the heater can pass through low-pressure steam, hot water or Hot-blast Heating air.
4. a kind of method of fluosilicic acid concentration, characterized in that include the following steps:
The first step separates the silica gel in fluosilicic acid；
Second step, circulation extract the fluosilicic acid and hot air, take away moisture in the fluosilicic acid using the hot-air,
The fluosilicic acid is improved to required concentration；
Third step, the eliminating arsenic by fluosilicic acid and remove mechanical admixture, obtain finished product fluosilicic acid.
5. the method for fluosilicic acid concentration according to claim 7, which is characterized in that hot air temperature is in the second step
40-80 DEG C, fluosilicic acid temperature is 20-40 DEG C in the second step.
6. the method for fluosilicic acid concentration according to claim 7, which is characterized in that the third step eliminating arsenic by fluosilicic acid is stirring
Stink damp precursor reactant arsenic removal is passed through under the conditions of mixing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910559094.9A CN110240164A (en) | 2019-06-26 | 2019-06-26 | The method and device of fluosilicic acid concentration |
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| CN201910559094.9A CN110240164A (en) | 2019-06-26 | 2019-06-26 | The method and device of fluosilicic acid concentration |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510591A (en) * | 2019-09-27 | 2019-11-29 | 瓮福达州化工有限责任公司 | A kind of high purity phosphorus hydrochlorate concentration technology |
| CN112717443A (en) * | 2020-12-22 | 2021-04-30 | 四川大学 | Concentration process of fluosilicic acid |
| CN113800524A (en) * | 2021-10-21 | 2021-12-17 | 贵州川恒化工股份有限公司 | Concentration method of fluosilicic acid |
| CN116425167A (en) * | 2023-04-19 | 2023-07-14 | 贵州瓮福蓝天氟化工股份有限公司 | Concentration method and system of fluosilicic acid solution |
| CN116462200A (en) * | 2023-04-24 | 2023-07-21 | 中国五环工程有限公司 | Fluosilicic acid concentration method based on vacuum membrane distillation method |
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| CN1376633A (en) * | 2002-05-09 | 2002-10-30 | 四川龙蟒集团有限责任公司 | Process for concentrating diluted sulfuric acid and removing impurities |
| CN101049920A (en) * | 2007-05-14 | 2007-10-10 | 湖北三新磷酸有限公司 | Method for absorbing and extracting phosphor and fluorin from phosphoric acid produced in kiln method |
| CN101323435A (en) * | 2008-06-26 | 2008-12-17 | 瓮福（集团）有限责任公司 | Method for extracting iodine from iodine-containing fluosilicic acid |
| CN109678159A (en) * | 2019-01-23 | 2019-04-26 | 瓮福（集团）有限责任公司 | A kind of fluosilicic acid cleaning method for concentration |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1376633A (en) * | 2002-05-09 | 2002-10-30 | 四川龙蟒集团有限责任公司 | Process for concentrating diluted sulfuric acid and removing impurities |
| CN101049920A (en) * | 2007-05-14 | 2007-10-10 | 湖北三新磷酸有限公司 | Method for absorbing and extracting phosphor and fluorin from phosphoric acid produced in kiln method |
| CN101323435A (en) * | 2008-06-26 | 2008-12-17 | 瓮福（集团）有限责任公司 | Method for extracting iodine from iodine-containing fluosilicic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510591A (en) * | 2019-09-27 | 2019-11-29 | 瓮福达州化工有限责任公司 | A kind of high purity phosphorus hydrochlorate concentration technology |
| CN112717443A (en) * | 2020-12-22 | 2021-04-30 | 四川大学 | Concentration process of fluosilicic acid |
| CN113800524A (en) * | 2021-10-21 | 2021-12-17 | 贵州川恒化工股份有限公司 | Concentration method of fluosilicic acid |
| CN116425167A (en) * | 2023-04-19 | 2023-07-14 | 贵州瓮福蓝天氟化工股份有限公司 | Concentration method and system of fluosilicic acid solution |
| CN116462200A (en) * | 2023-04-24 | 2023-07-21 | 中国五环工程有限公司 | Fluosilicic acid concentration method based on vacuum membrane distillation method |
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