CN104803522B - A kind of processing method of high sodium fluoride waste - Google Patents

A kind of processing method of high sodium fluoride waste Download PDF

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CN104803522B
CN104803522B CN201510243481.3A CN201510243481A CN104803522B CN 104803522 B CN104803522 B CN 104803522B CN 201510243481 A CN201510243481 A CN 201510243481A CN 104803522 B CN104803522 B CN 104803522B
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sodium fluoride
processing
waste
fluoride waste
sedimentation
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CN104803522A (en
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李程文
廖志辉
王子龙
刘东晓
梁亚娟
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Hunan Non Ferrous Metal Investment Co., Ltd
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HUNAN NONFERROUS FLUORINE CHEMICAL TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The processing method of a kind of high sodium fluoride waste, comprises the following steps: prepared by (1) fluosilicic acid: added by powdered silica in waste water, and reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;(2) lime flocculation: adding calcium hydroxide powder in fluosilicic acid pretreatment fluid, it is 6 ~ 9 that terminal pH controls;Add polyacrylamide flocculant, after stirring reaction, standing sedimentation, takes out supernatant and is primary effluent;(3) advanced treating: adding degree of depth de-fluoridation adsorbent to primary effluent, standing sedimentation, bed mud reusable edible after sedimentation again after stirring reaction, supernatant is secondary effluent, and its Funing tablet can reach below 5mg/L.The present invention solves high sodium fluoride waste lime mud sedimentation difficulty, goes out the problem that shipwreck is up to standard, and its lime consumption is few, and solid waste discharge amount is little, and water outlet fluorine can stably be down to below 5mg/L, it is achieved standard water discharge is discharged.

Description

A kind of processing method of high sodium fluoride waste
Technical field
The present invention relates to the processing method of a kind of high sodium fluoride waste, be specifically related in a kind of optical glass production process the processing method of effective fluorine removal of the fluoride waste produced.
Background technology
Optical glass is when being processed, due to mechanically damaged, therefore inevitably there is the defect such as slight crack, thin seam, scraping in its surface, and these defects not only will result only in the change of optical glass material surface optical performance, and optical element even can be made the most damaged.Therefore, the optical glass producing later stage often can use the soda acid etch of various concentration to process to change its material surface performance.Conventional washing lotion mainly has HF, NaOH etc., adds other H more simultaneously2SO4、HNO3Or the auxiliary such as ammoniacal liquor, the silicon of glass surface can be transformed into H under the corrosion of HF2SiF6Enter in washes.The feature that this waste water highlights is that acidity is high, mainly with HF, H2SiF6It is main, its Na simultaneously+Content is the most at a relatively high, and (HF content is often beyond 20000mg/L, H2SiF6Content is often beyond 10000mg/L, Na+Often beyond 10000mg/L).
At present, fluoride waste produced by optical glass producer is typically with the traditional handicraft of lime flocculation and processes, but often it can be seen that lime flocculation effect of settling is poor in actual motion processing procedure, go out water fluoridation cannot steady decrease to below 10mg/L.It is at a relatively high that effect of settling difference is because total acidity in waste water, in order to ensure that water outlet pH and enough Ca/F then must be added to substantial amounts of lime, the solid-to-liquid ratio thus causing system raises, and during lime flocculation, the lime quantity of slag is quite big, and substantial amounts of calcirm-fluoride fine grained is difficult to settle down.Water outlet cannot be up to standard, and being because the solubility of calcirm-fluoride under normal temperature is 16.3 mg/L, it is converted to fluorine ion and is 7.9 mg/L, when in waste water containing substantial amounts of sodium salt, affected by the salt effect of strong electrolyte, the solubility of calcirm-fluoride can increase, thus fluorinion concentration can be caused to be more than 10mg/L.
In water, Oil repellent is too high not only results in fluorine in human bodies poisoning, causes fluorosis of bone, den tal fluorosis etc., animals and plants also can be made to be poisoned simultaneously, affect agriculture-stock production, cause serious environmental pollution.In existing " integrated wastewater discharge standard " regulation water, fluoride first discharge standard requires to reach below 10mg/L, and Chinese Ministry of Environmental Protection in 2014 has issued " Phos chemical industrial pollution thing discharge standard " (exposure draft), tighten up the discharge standard of every pollutant in Phos chemical industry waste water, waste gas further.This most just imply that following fluoride emission is by by stricter control, the newest " integrated wastewater discharge standard " tries, that is likely to fluoride first discharge standard can be reduced to 5mg/L, and the most many existing sewage-treatment plants will be unable to reach to process requirement.
CN104512973 discloses the processing method of a kind of fluoride waste, including: regulation wastewater pH is to less than 5, then is neutralized precipitation, and after after precipitation, waste water carries out flocculating setting, separation of solid and liquid obtains one-level filtrate;After one-level filtrate carries out coagulating sedimentation with aluminum contained compound, separation of solid and liquid obtains two grades of filtrates;Finally two grades of filtrates being carried out coagulant precipitation and obtain supernatant, it goes out water fluoridation can reach below 10mg/L.The method is suitable for F-、SO4 2-And Al3+The waste water that concentration is higher.
CN102070267 discloses a kind of method processing acid phosphorous fluoride waste, including: in waste water add calcium hydroxide, and control react pH be 12 ~ 14;In filtrate, add sulfuric acid after filtration again, regulate pH to 9 ~ 11, finally regulate pH to 6 ~ 7 with aluminum sulfate;After precipitate and separate, it goes out water fluoridation and can be reduced to below 10mg/L.
Above prior art is all by directly adding direct fluorine removal such as the precipitating reagent Han aluminium, calcic etc., the water fluoridation that goes out after it processes also is only capable of reaching below 10mg/L, it is difficult to meet the requirement of below 5mg/L.Process, according to prior art, the fluoride waste that optical glass industry contains sodium at high concentration ion, go out water fluoridation after process and be only capable of reaching about 20mg/L, it is difficult to be up to standard.
Summary of the invention
The technical problem to be solved is, prior art is overcome to be unsuitable for high sodium fluoride wastewater treatment, go out water fluoridation and be difficult to reach the defect of below 5mg/L, the processing method of a kind of high sodium fluoride waste is provided, it is particularly well-suited to the fluorine removal of the fluoride waste that optical glass industry produces, uses water fluoridation simultaneously and reach below 5mg/L.
The present invention solves its technical problem and the technical scheme is that the processing method of a kind of high sodium fluoride waste, comprises the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and it is 15 ~ 30g/L that silica addition controls, mixing speed 350 ~ 400r/min, mixing time 20 ~ 30min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide powder addition controls is 35 ~ 45g/L, and it is 6 ~ 9 that terminal pH controls, mixing speed 350 ~ 400r/min, mixing time 20 ~ 30min;After reaction terminates, adding polyacrylamide (PAM) solution (flocculant) that mass concentration is 0.5 ~ 1.0%, wherein PAM addition is 0.1 ~ 0.2g/L, mixing speed 150 ~ 200r/min, mixing time 2 ~ 3min;After reaction terminates, standing sedimentation 3 ~ 5min, it is achieved separation of solid and liquid, takes out supernatant and is primary effluent;Primary effluent Funing tablet is up to 30 ~ 50mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent (DFA) in step (2) gained primary effluent, wherein DFA addition is 1 ~ 4g/L, mixing speed 150 ~ 300r/min, mixing time 10 ~ 20min;After reaction terminates, standing sedimentation 3 ~ 5min, it is circulated utilization during bed mud can return to primary effluent after sedimentation;Supernatant is secondary effluent, and its Funing tablet can reach below 5mg/L, it is achieved standard water discharge is discharged;
Described degree of depth de-fluoridation adsorbent (DFA), JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.
Further, in step (1), it is 20 ~ 25g/L that silica addition controls.
Further, in step (2), it is 38 ~ 42g/L that calcium hydroxide addition controls.
Further, in step (3), degree of depth de-fluoridation adsorbent addition is 2 ~ 3g/L.
Further, in step (3), mixing speed 200 ~ 250r/min.
In step (3), after sedimentation, bed mud is circulated utilization in returning primary effluent, can use as degree of depth de-fluoridation adsorbent, but not reduce the follow-up addition of degree of depth de-fluoridation adsorbent.Recycle herein, can more preferable fluorine removal.
The present invention is by adding SiO2HF in waste water is made to be completely converted into H2SiF6, add Ca (OH)2, generate CaSiF6Precipitation.With CaF2Compare, CaSiF6Precipitation particle is bigger, it is easy to sedimentation separation, Ca (OH)2Consumption is lower, and the lime quantity of slag is less, decreases the discharge capacity of solid waste.F in waste water-It is completely converted into SiF6 2-, make total ion concentration in waste water reduce, interionic restraining function also can weaken, thus weaken Na+Salt effect, promote calcium fluosilicate Precipitation.Meanwhile, relative to little molecule F-, DFA is to big molecule SiF6 2-There is higher suction-operated, use water fluoridation and can be reduced to below 5mg/L.
The present invention is used to process high sodium fluoride waste, can effectively solve the problem that in conventional method, lime flocculation sedimentation difficulty, water outlet fluorine are difficult to reach 5mg/L problem below, using conventional method lime consumption to reach 70g/L, consumption of the present invention only needs 35 ~ 45g/L, and lime consumption can reduce by more than 30%.Present invention process is simple, and solid waste discharge amount is little, and water outlet fluorine can stably be down to below 5mg/L, it is achieved discharged wastewater met the national standard, it is to avoid environmental pollution.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The present embodiment comprises the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and silica addition controls as 15g/L, mixing speed 350r/min, mixing time 20min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide powder addition controls to control to be 6.5 for 35g/L, terminal pH, mixing speed 350r/min, mixing time 20min;After reaction terminates, adding the PAM solution that mass concentration is 0.5%, wherein PAM addition is 0.1g/L, mixing speed 150r/min, mixing time 2min;After reaction terminates, standing sedimentation 3min, separation of solid and liquid, take out supernatant and be primary effluent;Primary effluent Funing tablet is 48.2mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent (DFA) in step (2) gained primary effluent, wherein DFA addition is 1g/L, mixing speed 150r/min, mixing time 10min;After reaction terminates, standing sedimentation 3min, it is circulated utilization during bed mud can return to primary effluent after sedimentation;Supernatant is secondary effluent, and its Funing tablet is 4.8mg/L, it is achieved standard water discharge is discharged.
Described degree of depth de-fluoridation adsorbent (DFA), JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.
In the present invention, go out water fluoridation bioassay standard and carry out by " the mensuration ion selective electrode method of GBT 7484-87 water quality fluoride ".
Embodiment 2
The present embodiment comprises the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and silica addition controls as 20g/L, mixing speed 350r/min, mixing time 20min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide addition controls to control to be 7.4 for 38g/L, terminal pH, mixing speed 350r/min, mixing time 25min;After reaction terminates, adding polyacrylamide (PAM) solution of mass concentration 0.5%, wherein PAM addition is 0.1g/L, mixing speed 150r/min, mixing time 2min;After reaction terminates, standing sedimentation 4min, separation of solid and liquid, take out supernatant and be primary effluent;Primary effluent Funing tablet is 41.5mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent (DFA) in step (2) gained primary effluent, wherein DFA addition is 2g/L, mixing speed 200r/min, mixing time 15min;After reaction terminates, standing sedimentation 4min, it is circulated utilization during bed mud can return to primary effluent after sedimentation;Supernatant is secondary effluent, and its Funing tablet is 3.9mg/L, it is achieved standard water discharge is discharged.
Described degree of depth de-fluoridation adsorbent (DFA), JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.
Embodiment 3
The present embodiment comprises the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and silica addition controls as 25g/L, mixing speed 400r/min, mixing time 30min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide addition controls to control to be 7.8 for 42g/L, terminal pH, mixing speed 400r/min, mixing time 25min;After reaction terminates, adding the PAM solution of mass concentration 1.0%, wherein PAM addition is 0.2g/L, mixing speed 200r/min, mixing time 3min;After reaction terminates, standing sedimentation 4min, separation of solid and liquid, take out supernatant and be primary effluent;Primary effluent Funing tablet is 38.6mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent (DFA) to step (2) gained primary effluent, wherein DFA addition is 3g/L, mixing speed 250r/min, mixing time 20min;After reaction terminates, standing sedimentation 4min, it is circulated utilization during bed mud can return to primary effluent after sedimentation;Supernatant is secondary effluent, and its Funing tablet is 3.5mg/L, it is achieved standard water discharge is discharged.
Described degree of depth de-fluoridation adsorbent (DFA), JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.
Embodiment 4
The present embodiment comprises the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and silica addition controls as 30g/L, mixing speed 400r/min, mixing time 30min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide addition controls to control to be 8.6 for 45g/L, terminal pH, mixing speed 400r/min, mixing time 30min;After reaction terminates, adding the PAM solution of mass concentration 1.0%, wherein PAM addition is 0.2g/L, mixing speed 200r/min, mixing time 3min;After reaction terminates, standing sedimentation 5min, separation of solid and liquid, take out supernatant and be primary effluent;Primary effluent Funing tablet is 37.3mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent (DFA) to step (2) gained primary effluent, wherein DFA addition is 4g/L, mixing speed 300r/min, mixing time 20min;After reaction terminates, standing sedimentation 5min, it is circulated utilization during bed mud can return to primary effluent after sedimentation;Supernatant is secondary effluent, and its Funing tablet is 3.4mg/L, it is achieved standard water discharge is discharged.
Described degree of depth de-fluoridation adsorbent (DFA), JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.

Claims (6)

1. the processing method of one kind high sodium fluoride waste, it is characterised in that comprise the following steps:
(1) prepared by fluosilicic acid: added by powdered silica in waste water, and it is 15 ~ 30g/L that silica addition controls, mixing speed 350 ~ 400r/min, mixing time 20 ~ 30min;Reaction is filtered after terminating, and filtrate is fluosilicic acid pretreatment fluid;
(2) lime-flocculation: adding calcium hydroxide powder in step (1) gained fluosilicic acid pretreatment fluid, wherein calcium hydroxide powder addition controls is 35 ~ 45g/L, and it is 6 ~ 9 that terminal pH controls, mixing speed 350 ~ 400r/min, mixing time 20 ~ 30min;After reaction terminates, adding the polyacrylamide solution that mass concentration is 0.5 ~ 1.0%, wherein PAM addition is 0.1 ~ 0.2g/L, mixing speed 150 ~ 200r/min, mixing time 2 ~ 3min;After reaction terminates, standing sedimentation 3 ~ 5min, it is achieved separation of solid and liquid, takes out supernatant and is primary effluent;Primary effluent Funing tablet is up to 30 ~ 50mg/L;Bottom is that lime mud is as fixed-end forces;
(3) advanced treating: adding degree of depth de-fluoridation adsorbent in step (2) gained primary effluent, wherein degree of depth de-fluoridation adsorbent addition is 1 ~ 4g/L, mixing speed 150 ~ 300r/min, mixing time 10 ~ 20min;After reaction terminates, standing sedimentation 3 ~ 5min;Supernatant is secondary effluent, and its Funing tablet can reach below 5mg/L, it is achieved standard water discharge is discharged;
Described degree of depth de-fluoridation adsorbent, JNM-055 type, manufacturer is Environmental Protection Technology Co., Ltd of Jin Nuo alliance of Shenzhen.
The processing method of high sodium fluoride waste the most according to claim 1, it is characterised in that in step (1), it is 20 ~ 25g/L that silica addition controls.
The processing method of high sodium fluoride waste the most according to claim 1 and 2, it is characterised in that in step (2), it is 38 ~ 42g/L that calcium hydroxide addition controls.
The processing method of high sodium fluoride waste the most according to claim 1 and 2, it is characterised in that in step (3), degree of depth de-fluoridation adsorbent addition is 2 ~ 3g/L.
The processing method of high sodium fluoride waste the most according to claim 1 and 2, it is characterised in that in step (3), mixing speed 200 ~ 250r/min.
The processing method of high sodium fluoride waste the most according to claim 1 and 2, it is characterised in that in step (3), after reaction terminates, after sedimentation, bed mud is circulated utilization in returning primary effluent.
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CN105174236B (en) * 2015-08-11 2017-06-23 贵州师范学院 A kind of phosphoric acid by wet process prepares the method and apparatus of potassium phosphate
CN105174270A (en) * 2015-10-15 2015-12-23 湖南有色氟化学科技发展有限公司 Technology for preparing sodium fluorosilicate through fluoride-containing wastewater
CN108666644B (en) * 2018-05-23 2020-12-04 东莞市坤乾新能源科技有限公司 Method for recovering fluorine and lithium from waste electrolyte of lithium battery

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CN102276034A (en) * 2011-07-19 2011-12-14 上海电力学院 Process method for removing fluorides in high concentrations of fluoride-containing wastewater from thermal power plant

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