CN109942118A - A kind of environment-friendly treatment method of trifluoroacetic acid waste liquid - Google Patents
A kind of environment-friendly treatment method of trifluoroacetic acid waste liquid Download PDFInfo
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- CN109942118A CN109942118A CN201910327207.2A CN201910327207A CN109942118A CN 109942118 A CN109942118 A CN 109942118A CN 201910327207 A CN201910327207 A CN 201910327207A CN 109942118 A CN109942118 A CN 109942118A
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Abstract
The invention belongs to hazardous waste processing technology fields, and in particular to a kind of environment-friendly treatment method of trifluoroacetic acid.After trifluoroacetic acid and hydroxide are carried out pretreatment neutralization by this method, lime white is added in reaction solution and forms calcium fluoride precipitate, is separated by filters pressing and send filtrate to rotary kiln high temperature incineration, landfill disposal after sludge is stabilized and solidified.The complete precipitation process of fluorine ion can be stabilized and be solidified land-fill method using specific, guarantee that processing is up to standard by this method；This method does not generate outer waste air during carrying out, all waste gases, which are collected, to be handled and is monitored using VOC on-line computing model, unqualified gas guarantees that waste gas containing fluoride close to zero-emission, realizes real environmental protection treatment by being recycled into reactor and as the gas source source of air stirring；This method is controlled by reaction details and parameter, guarantees the safety in treatment process.
Description
Technical field
The invention belongs to hazardous waste processing technology fields, and in particular to a kind of environment-friendly treatment method of trifluoroacetic acid.
Background technique
Trifluoroacetic acid is very widely used as organic compound or the fine solvent of organic reaction in Chemical Manufacture.Three
Fluoroacetic acid has acrid odors, is a kind of strong and non-oxidizing acid, can smoke, therefore generally be not easy to connect with air in processing
Touching.Trifluoroacetic acid is different from traditional such as concentrated sulfuric acid smoke strong acid, because bringing to environmental protection treatment tired containing fluorine ion
It is difficult.The prior art there is no the very good processing method for trifluoroacetic acid, small test or it is micro- it is anti-in, for trifluoroacetic acid
Waste liquid generallys use revolving removal, and this method is not fundamentally to remove, only a kind of palliative method, will
Trifluoroacetic acid revolving is evaporate into air, is easy to cause damages to air or water body, and then influence the health of human body；In addition real
Also have in the operation of border and the alkali such as trifluoroacetic acid and lime are done into simple neutralisation treatment, is then burned or solidified, trifluoroacetic acid
It can only simply be neutralized to related lye, fluorine ion can not be settled out completely and be solidified, or there are fluoride ion removings not to do
Only by entering atmosphere again after burning, the standard that dangerous waste is handled is not achieved.
Therefore, it is necessary to invent a kind of environment-friendly treatment method of trifluoroacetic acid waste liquid, fluorine ion is precipitated to solidification completely, and
And guarantee the environmental protection in treatment process and safety, additional waste gas containing fluoride is not generated.
Summary of the invention
The technical problems to be solved by the present invention are: in view of the above problems, providing a kind of environmental protection of trifluoroacetic acid
Processing method.
Scheme of the invention of the invention is as follows:
A kind of environment-friendly treatment method of trifluoroacetic acid waste liquid, comprising the following steps:
1) waste liquid pre-processes: trifluoroacetic acid waste liquid is stored in closing waste liquid barrel, it will according to certain speed using the pump housing
Trifluoroacetic acid is pumped into the reactor being stirred continuously for presetting sodium hydroxide or potassium hydroxide solution by feed pipe, control
The reaction temperature of trifluoroacetic acid waste liquid and sodium hydroxide or potassium hydroxide is no more than 60 DEG C, and control reaction end PH is 7, described anti-
Device is answered to be placed in confined reaction room, the gas extraction that the reaction chamber setting blower generates reaction carries out lye neutralization and absorption
Processing, unqualified tail gas are back in reaction chamber；
2) precipitating compression: the reaction solution pre-processed is transferred in collecting vessel from reactor, and lime white tune is added
PH is saved to meta-alkalescence, filters pressing after standing, gained filtrate, which is sent to rotary kiln high temperature incineration, to be burnt, sludge stabilize and solidification at
Reason；
3) filtrate is handled: filtrate being sent into rotary kiln high temperature incineration, rotary kiln is initial when control filtrate puts into rotary kiln
Temperature is 850 DEG C or more, and dual firing chamber's temperature that rotary kiln is controlled in treatment process is 1100-1150 DEG C；
4) Treatment of Sludge: sludge is mixed with stabilizer, adds water and curing agent stirring solidification, landfill is entered after solidification
Field landfill.
Trifluoroacetic acid waste liquid is reacted neutralization with sodium hydroxide or potassium hydroxide using pretreatment by this programme completely, generates fluorine
Change sodium or potassium fluoride and water, sodium fluoride or potassium fluoride add lime white and generate precipitating calcirm-fluoride, and wherein calcium fluoride precipitate is dirt
Mud carries out stabilisation and curing process, and liquid generated passes through high temperature incineration into exhaust emissions.Due to trifluoroacetic acid waste liquid
In be usually mixed with other organic solvents, and organic solvent can not directly carry out solidification landfill, therefore just be dissolved in filtrate together
It burns.Consider cost reason, pretreated lye is preferably sodium hydroxide.
Further, the feed pipe need to extend into the bottom of the preset aqueous slkali of reactor.Trifluoroacetic acid waste liquid is direct
It is extend into reactor bottom, avoids contacting smoke with large quantity of air, trifluoroacetic acid directly occurs with sodium hydroxide anti-under stiring
It answers.
Further, the reaction temperature of control trifluoroacetic acid waste liquid and sodium hydroxide or potassium hydroxide is no more than 60 DEG C.Instead
Settable temperature control in device is answered, reaction temperature is controlled, prevents reaction from excessively acutely making solution bumping and splash, simultaneously
It will lead to the tetrafluoroethene liner softening of reactor if temperature is excessively high.
Further, air stirrer can be installed additional in reactor bottom, the gas source of the air stirrer derives from
The air of reaction chamber where reactor.There is the unqualified tail gas of circulation in the air of reaction chamber, can be returned by air stirring
To reactor secondary response again, treating tail gas and stirring double action are realized, is killed two birds with one stone.Meanwhile stirring being arranged in bottom,
It can reinforce mixing with feed pipe arranged at the bottom, be conducive to the progress of reaction.
Further, in the step (1), the mass concentration of sodium hydroxide or potassium hydroxide solution is 30%, the alkali
The volume of liquid accounts for reactor no more than half height.Observable reacts violent situation and waste liquid speed is added to adjust, and guarantees reaction
Liquid does not splash out.Reaction continues stirring 5-15 minutes after reaching the terminal that PH is 7, guarantees fully reacting.
Further, in the step (1), react generation gas first pass through lye absorption, maintain lye PH be 10 with
On, gas after alkali cleaning is through VOC on-line computing model outlet after activated carbon adsorption, and unqualified to be partly refluxed to waste liquid pretreated
Between reaction, handled again through blower absorption.Since trifluoroacetic acid volatility is especially strong, contain in order to avoid generating during the reaction
Fluorine gas generates pollution to atmosphere, and reaction chamber keeps tiny structure, is equipped with pressure gauge observation；Wind is utilized in closed reaction chamber
The gas that machine generates reaction is extracted out, and through alkali cleaning and adsorption treatment, through the qualified then outlet of detection, unqualified, return continues to locate
Reason, accomplishes fluoro-gas zero-emission.
Further, in the step (2), lime white is added under the reaction solution stirring condition pre-processed, adjusts PH
It is 9, guarantees that calcium fluoride precipitate is complete, stands filters pressing processing again after abundant reaction in one hour.
Further, in the step (3), rotary kiln high temperature incineration temperature is needed to wait at 850 DEG C or so, determines operating condition
Waste liquid can be put into after stabilization, and is atomized and is sprayed into rotary kiln high temperature incineration.The moment is wanted to pay attention to kiln temperature, two during incineration disposal
The variation for firing room temperature, exhaust emissions index etc., makes corresponding adjustment in time.It is noted that fire prevention, is dressed in fill process
Appliances for labor protection, while carrying out charging safety and administration of the prevention and control.
Further, in the step (4), stabilizer uses thiocarbamide, and curing agent uses cement；First configuration volume fraction is
10% thiourea solution, stabilize and solidification proportion is according to sludge: 10% thiocarbamide: cement: water=1:0.01:0.2:0.01 is carried out,
First thiocarbamide and sludge are added in stirred tank, water is then continuously added and is mixed, mixing time is 5-10 minutes, after
Curing agent cement is added in stirred tank and is stirred for 3-5 minutes, the above material is then sent into landfill yard landfill.It is same with this
When, mixture can be sampled, Leaching analysis is done after 7 days, underproof return workshop is disposed again.
As the above scheme is adopted, beneficial effects of the present invention are as follows: the administering method phase with traditional trifluoroacetic acid
Than fluorine ion can be first transformed into salt from acid by this method completely by reasonable pre-reaction step, solved and used lime in the past
Not enough due to lime alkalinity, the fluorine ion in trifluoroacetic acid is limited by ionization equilibrium, and can not to form calcirm-fluoride completely heavy for one-step method
It forms sediment, so that there is also more fluorine ions in the mixing liquid in precipitating；This method is by trifluoroacetic acid and highly basic sodium hydroxide or hydrogen
Aoxidize nak response so that fluorine ion in highly basic in and after ionization as far as possible completely, add lime and carry out processing to having precipitated
Entirely；Other organic solvents are usually mixed in trifluoroacetic acid waste liquid, organic solvent carries out burning disposal, calcium fluoride precipitate in filtrate
Stabilized and solidification land-fill method using specific, guarantee the pollutant in each waste liquid match respectively suitable processing method and
It handles up to standard；This method does not generate outer waste air during carrying out, all waste gases, which are collected, to be handled and use VOC on-line computing model
Monitoring, unqualified gas guarantee waste gas containing fluoride close to zero by being recycled into reactor and as the gas source source of air stirring
Discharge, realizes real environmental protection treatment；This method is controlled by reaction details and parameter, guarantees the safety in treatment process.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Embodiment
A kind of environment-friendly treatment method of trifluoroacetic acid waste liquid, comprising the following steps:
1) waste liquid pre-processes: trifluoroacetic acid waste liquid being stored in closing waste liquid barrel, the hydrogen-oxygen for being 30% by mass concentration
Change sodium solution to be added in reactor, liquor capacity accounts for the half of reactor volume.Using diaphragm pump according to certain speed by three
Fluoroacetic acid is pumped into reactor bottom by feed pipe, and the bottom of reactor is provided with two rows and opens up foraminate stainless steel tube,
It will be passed through stainless steel tube after the gas compression between reaction using air driven pump, form air stirring in reaction chamber, automatic control is set
Reaction end PH=7 processed adjusts the speed that waste liquid is added according to violent situation is reacted, and guarantees that reaction liquid cannot splash out, controls
The temperature of reaction solution processed is no more than 60 DEG C；After being reacted to terminal, then it is passed through air 10 minutes；It is negative pressure between control reaction, gives up
The exhaust gas generated when liquid bucket and reaction sucks deacidification tank by the blower with pipeline on top between reaction, and deacidification tank lye absorbs tail
Sour gas in gas, the lye used in tank that deacidifies are provided by chemical tank, and the pH value of online PH instrument control pharmacy agent maintains PH=
10 or more, the tail gas after alkali cleaning enters absorbent charcoal adsorption tank, and the tail gas after activated carbon adsorption passes through VOC on-line computing model, qualified
Outlet, it is underproof to flow back between reaction, discharged after processing is qualified again；
2) it precipitating compression: by diaphragm pump by reaction solution extraction device, is fitted into collecting vessel outer between reacting, stone is added
It is 9 that mortar, which adjusts PH, filters pressing after standing one hour, and gained filtrate, which is sent to rotary kiln high temperature incineration, to be burnt, and sludge is stabilized
And curing process；
3) filtrate is handled: when incineration rotary kiln temperature is at 850 DEG C or so, waste liquid can be put into after determining stable conditions,
Waste liquid is pumped to spray gun by waste liquid, its atomization is sprayed by compressed air and carries out high temperature full combustion in rotary kiln, locating
It must assure that dual firing chamber's temperature between 1100-1150 DEG C during setting.The moment is wanted to pay attention to kiln temperature, two during incineration disposal
The variation for firing room temperature, exhaust emissions index etc., makes corresponding adjustment in time.It is noted that fire prevention, is dressed in fill process
Appliances for labor protection, while carrying out charging safety and administration of the prevention and control.
4) Treatment of Sludge: sludge is mixed with stabilizer, adds water and curing agent stirring solidification, landfill is entered after solidification
Field fills, and in the step (4), stabilizer uses thiocarbamide, and curing agent uses cement；First configuration volume fraction is that 10% thiocarbamide is molten
Liquid, stabilize and solidification proportion is according to sludge: 10% thiocarbamide: cement: water=1:0.01:0.2:0.01 carries out, first by thiocarbamide with
Sludge is added in stirred tank, is then continuously added water and is mixed, and mixing time is 5-10 minutes, after by curing agent water
Mud, which is added in stirred tank, to be stirred for 3-5 minutes, and the above material is then sent into landfill yard landfill.It in process of production can root
It according to regulating pondage ratio when solidification effect, is subject to and reaches optimized solidification state, enter after reaction is sufficiently stirred in the above material
Landfill yard landfill, samples simultaneously, Leaching analysis is done after 7 days, underproof return workshop is disposed again.
After being handled using this method, the Leaching analysis after incineration tail gas index and landfill reaches discharge mark
It is quasi-.
Wherein, incineration tail gas norm controlling is as follows:
Burning process index executes " dangerous waste incineration contamination control standard " GB-18484-2001, monitoring data result
As shown in table 1
Monitoring data after stabilization in the filtrate processing burning of 1 embodiment 1 of table
| Index name | Unit | Con trolling index | Monitoring data |
| HF | mg/Nm3 | < 7 | 1.0 |
| Hcl | mg/Nm3 | < 70 | 12 |
| SO2 | mg/Nm3 | < 300 | 38 |
| CO | mg/Nm3 | < 80 | 30 |
| NOX | mg/Nm3 | < 500 | 117 |
As seen from the above table, carrying out burning disposal to filtrate using this method makes each monitoring index be all satisfied national standard control
Range processed.
After Treatment of Sludge, leach toxicity test data are as shown in table 2:
Leaching analysis after the sludge curing of 2 embodiment 1 of table
| Serial number | Project | Stabilization Control limit value (mg/L) | Detection data |
| 1 | Organic mercury | 0.001 | It is not detected |
| 2 | Mercury and mercuric compounds (in terms of total mercury) | 0.25 | It is not detected |
| 3 | Lead (in terms of total lead) | 5 | 0.06 |
| 4 | Cadmium (in terms of total cadmium) | 0.50 | 0.002 |
| 5 | Total chromium | 12 | 0.05 |
| 6 | Cr VI | 2.50 | 0.008 |
| 7 | Copper and its compound (in terms of total copper) | 75 | 0.032 |
| 8 | Zinc and its compound (in terms of total zinc) | 75 | 0.06 |
| 9 | Beryllium and its compound (in terms of total beryllium) | 0.20 | 0.001 |
| 10 | Barium and its compound (in terms of total barium) | 150 | 0.65 |
| 11 | Nickel and its compound (in terms of total nickel) | 15 | 0.05 |
| 12 | Arsenic and its compound (in terms of total arsenic) | 2.5 | 0.02 |
| 13 | Inorganic fluoride (not including calcirm-fluoride) | 100 | 10.5 |
| 14 | Cyanide (in terms of CN) | 5 | 0.02 |
It is analyzed by upper table Leaching it is found that each Testing index after sludge curing is up to standard.
Comparative example
A kind of environment-friendly treatment method of trifluoroacetic acid waste liquid: trifluoroacetic acid waste liquid is stored in closing waste liquid barrel, by stone
Mortar solution is added in reactor, and liquor capacity accounts for the half of reactor volume.Using diaphragm pump according to certain speed by three
Fluoroacetic acid is pumped into reactor bottom by feed pipe, and the bottom of reactor is provided with two rows and opens up foraminate stainless steel tube,
It will be passed through stainless steel tube after the gas compression between reaction using air driven pump, form air stirring in reaction chamber, adjusts reaction eventually
Point PH is 9, adjusts the speed that waste liquid is added according to violent situation is reacted, and guarantees that reaction liquid cannot splash out, controls reaction solution
Temperature no more than 60 DEG C；After being reacted to terminal, then it is passed through air 10 minutes；After the completion of this method, can finally it generate
More dry mud, is unable to complete filters pressing, and through detecting, the liquid in mud does not sink containing the organic matter solvent in waste liquid and largely also
The fluorine ion in shallow lake can not be directly entered solidification landfill step；If passing through filters pressing after being diluted with water mashing, can make to be separated by solid-liquid separation,
Then since diluting effect improves the dissolubility of calcirm-fluoride, filtrate can only be made to increase more fluorine ions, is burned in filtrate
It will cause that fluoride is exceeded in processing, to be unable to reach the requirement of environmental protection treatment.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
1. a kind of environment-friendly treatment method of trifluoroacetic acid waste liquid, which comprises the following steps:
1) waste liquid pre-processes: trifluoroacetic acid waste liquid being stored in closing waste liquid barrel, using the pump housing according to certain speed by trifluoro
Acetic acid is pumped into the reactor being stirred continuously for presetting sodium hydroxide or potassium hydroxide solution by feed pipe, and trifluoro is controlled
The reaction temperature of acetic acid waste liquid and sodium hydroxide or potassium hydroxide is no more than 60 DEG C, and control reaction end PH is 7, the reactor
It is placed in confined reaction room, the gas extraction that the reaction chamber setting blower generates reaction carries out at lye neutralization and absorption
Reason, unqualified tail gas are back in reaction chamber；
2) precipitating compression: the reaction solution pre-processed is transferred in collecting vessel from reactor, and lime white is added and adjusts PH
To meta-alkalescence, filters pressing after standing, gained filtrate is sent to rotary kiln high temperature incineration, and sludge stabilize and curing process；
3) filtrate is handled: filtrate being sent into rotary kiln high temperature incineration, the initial temperature of rotary kiln when control filtrate puts into rotary kiln
It is 850 DEG C or more, dual firing chamber's temperature that rotary kiln is controlled in treatment process is 1100-1150 DEG C；
4) Treatment of Sludge: sludge is mixed with stabilizer, is added water and curing agent stirring solidification, is filled out after solidification into landfill yard
It buries.
2. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that the feed pipe and three
The closing waste liquid barrel of fluoroacetic acid waste liquid storage seals installation, and feed pipe need to extend into the bottom of the preset lye of reactor.
3. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 2, which is characterized in that in the step (1),
Air stirrer can be installed additional in reactor bottom, the gas source of the air stirrer is from the reaction chamber where reactor
Air.
4. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that in the step (1),
Reaction continues stirring 5-15 minutes after reaching the terminal that PH is 7.
5. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that in the step (2),
Lime white is added under the reaction solution stirring condition pre-processed, adjusting PH is 9, and standing one hour, filters pressing again is handled.
6. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that in the step (4),
Stabilizer uses thiocarbamide, and curing agent uses cement；First configuration volume fraction is 10% thiourea solution, stabilizes and solidification proportion is pressed
According to sludge: 10% thiocarbamide: cement: water=1:0.01:0.2:0.01 is carried out, and first thiocarbamide and sludge is added in stirred tank, so
After be continuously added water and be mixed, mixing time is 5-10 minute, after will be stirred in curing agent cement addition stirred tank
3-5 minutes, the above material is then sent into landfill yard landfill.
7. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that in the step (1),
The gas that reaction generates first passes through lye absorption, and maintaining lye PH is 10 or more, and the gas after alkali cleaning passes through after activated carbon adsorption
VOC on-line computing model outlet, it is unqualified to be partly refluxed between the pretreated reaction of waste liquid, it is handled again through blower absorption.
8. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1, which is characterized in that in the step (3),
Waste liquid can be put into after determining stable conditions, the filtrate can spray into rotary kiln high temperature by atomization and burn.
9. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 1-8, which is characterized in that the step
Suddenly in (1), the mass concentration of sodium hydroxide or potassium hydroxide solution is 30%, and the volume of sodium hydroxide or potassium hydroxide accounts for reaction
Device is no more than half height.
10. the environment-friendly treatment method of trifluoroacetic acid waste liquid according to claim 9, which is characterized in that the step (1)
In, control reaction chamber is tiny structure, and reaction indoor location pressure gauge is monitored.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114110623A (en) * | 2021-11-09 | 2022-03-01 | 上海天汉环境资源有限公司 | Ammonia fluoride waste liquid incineration treatment method and treatment device thereof |
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Application publication date: 20190628 |