CN105399179B - Promote the method for charcoal absorption removal water body intermediate ion liquid using phosphate - Google Patents
Promote the method for charcoal absorption removal water body intermediate ion liquid using phosphate Download PDFInfo
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- CN105399179B CN105399179B CN201510909745.4A CN201510909745A CN105399179B CN 105399179 B CN105399179 B CN 105399179B CN 201510909745 A CN201510909745 A CN 201510909745A CN 105399179 B CN105399179 B CN 105399179B
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Abstract
The present invention relates to a kind of method for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, belong to field of water pollution control.This method is：Phosphate is added into the water body containing ionic liquid, fully mixes and dissolves；With the ionic liquid in charcoal absorption water body, after adsorption equilibrium or adsorption saturation is reached, first with acidic elution agent elution ionic liquid, then with alkaline solution activated carbon pH is adjusted back to alkalescent, activated carbon is re-used in next round absorption.Compared with prior art, the present invention has been obviously improved the ability of charcoal absorption removal ionic liquid using phosphate.The present invention need not carry out other operation bidirectional processing, obvious to the Adsorption effect promoting of ionic liquid, and activated carbon is reusable repeatedly, has preferable popularizing application prospect.
Description
Technical field
The present invention relates to a kind of ionic liquid processing method, promotes charcoal absorption using phosphate more particularly, to one kind
The method for removing water body intermediate ion liquid, belongs to field of water pollution control.
Background technology
Ionic liquid refers to be in a liquid state at room temperature, the fused salt compound being made up of completely zwitterion.It is waved with difficulty
The features such as sending out, be stable to water and air, be superior to many kinds of substance solubility property, therefore it is referred to as " green solvent ", extensively should
For fields such as chemical industry, medicine, biotechnology, agricultural and food.Ionic liquid into environment water is not easy by Institute of Micro-biology
Degraded, all has certain toxicity to animal, plant and microorganism.Therefore, it is necessary to the ionic liquid contained in industrial water body
Carry out rationally effective disposal.
Mainly there are two class methods to the treatment measures of ionic liquid solution at present, one kind is the structure progress to ionic liquid
Destroy, ionic liquid is changed into other harmless or less toxic small molecules.Related measure includes pyrolysis, chemical oxidation and biology
Processing etc.；This kind of method can not carry out effectively resource reclaim to the ionic liquid in water body.Another kind of method is by ionic liquid
Body is effectively separated recovery from water body, and major measure includes vacuum distillation, crystallization, extraction and absorption etc..Wherein, depressurize
Distillation, crystallization and the method extracted simultaneously are not suitable for handling the water body containing ionic liquid on a large scale.Therefore, absorption is the side recommended
Method.Although there is the document report using charcoal absorption processing ionic liquid water body at present, charcoal absorption ionic liquid
Ability is universal very low, if being subject to commercial Application with prior art parameter, processing cost will be caused to remain high.
The content of the invention
What the present invention needed to solve is that adsorbance is not high on the activated carbon for ionic liquid (particularly hydrophilic ionic-liquid)
The problem of.Improved method main at present is to improve activated carbon dosage increase, and this will cause processing cost to be lifted.The present invention passes through
A small amount of phosphate is added in water body, under conditions of other technical parameters are not changed, activated carbon can be realized to ionic liquid
Body adsorption capacity is obviously improved.
The purpose of the present invention can be achieved through the following technical solutions：
Promote the method for charcoal absorption removal water body intermediate ion liquid using phosphate, to the water body containing ionic liquid
Middle addition phosphate, fully mixes and dissolves；With the ionic liquid in charcoal absorption water body, reaching adsorption equilibrium or absorption
After saturation, first with acidic elution agent elution ionic liquid, then with alkaline solution activated carbon pH is adjusted back to the weak base for being more than 8.0
Property, activated carbon is re-used in next round absorption.
Ionic liquid in water body includes glyoxaline ion liquid, pyridine ionic liquid, quaternary ammonium ionic liquid, season phosphine
Class ionic liquid, pyrrolidines ionic liquid or piperidines ionic liquid.
Described phosphate includes sodium phosphate, potassium phosphate or ammonium phosphate.
After adding phosphate, the ratio of phosphatic molar concentration and ionic liquid molar concentration maintains 1/ in water body
In the range of 500 to 1/50.
Described acidic elution agent includes pH=1-3 hydrochloric acid or sulfuric acid solution.
Described alkaline solution includes pH=11-13 sodium hydroxide or potassium hydroxide aqueous solution.
The mode of ionic liquid in charcoal absorption water body is static balancing absorption mode or dynamic column absorption mode.
Static balancing absorption mode is：A small amount of phosphate is added into a certain amount of water body containing ionic liquid, is further thrown
Add the activated carbon of certain mass, fully vibration causes charcoal absorption ionic liquid to reach balance, and activated carbon is filtered and taken out, is put
Enter in acidic elution agent, the ionic liquid being tightly held by activated carbon will be desorbed into acidic elution agent, then by activated carbon from acidity
Take out, be placed in alkaline solution in eluant, eluent, activated carbon pH is adjusted to alkalescent, reuses activated carbon.
Dynamic column absorption mode is：In cylinder fill certain mass activated carbon, under the conditions of flow velocity is stablized, with containing from
Sub- liquid and a small amount of phosphatic water body flow through activated carbon packed column and carry out post absorption, and absorption drains water body after reaching saturation,
Adsorption column is eluted with 1 bed volume acidic elution agent, then the distillation water elution adsorption column with 1 bed volume, ionic liquid reach
Desorption is complete, further elutes adsorption column with the alkaline solution of 1 bed volume, activated carbon pH is recalled to alkalescent, makes activity
Charcoal reuses.
The adsorption conditionses of static balancing absorption mode or dynamic column absorption mode may be referred to conventional activated carbon absorbing process.
The present invention principle be：Trivalent phosphate has salting-out effect, can be hydrated strongly by electrostatic interaction freely molten
The hydrone of agent, so as to effectively reduce the aquation of hydrone and ionic liquid, and then reduce the molten of water body intermediate ion liquid
Xie Du.
Compared with prior art, the present invention only need to add a small amount of phosphate solution in water body, so that it may greatly promote work
Property charcoal is to the adsorption effect of ionic liquid, and cost is cheap, significant effect.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1：
Sodium phosphate promotes activated carbon Static Adsorption ionic liquid (1- ethyl-3-methylimidazoles tetrafluoroborate)
【Add sodium phosphate experiment】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazole tetrafluoro boron
A small amount of sodium phosphate is added in acid salt aqueous solution, the concentration of sodium phosphate is 0.01mmol/L after stablizing.Further add a certain amount of
Powder merchandise active carbon vibrate 24h, it is to be adsorbed reach balance after, measure activated carbon to 1- ethyl-3-methylimidazole tetrafluoro boric acids
The saturated extent of adsorption of salt is 40.6mg/g.Insert in pH=1 hydrochloric acid solution, 1- ethyl-3-methylimidazole tetrafluoroborates can
It is desorbed completely by acid solution.Activated carbon is placed in pH=13 sodium hydrate aqueous solution, activated carbon pH can be adjusted to 10 it is weak
Alkalescence.Activated carbon is reusable repeatedly.
【Sodium phosphate contrast experiment is not added】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazoles
Add a certain amount of powder merchandise active carbon in tetrafluoro boric acid saline solution, vibrate 24h, it is to be adsorbed reach balance after, measure work
Property charcoal is 16.2mg/g to the saturated extent of adsorption of 1- ethyl-3-methylimidazole tetrafluoroborates, is then taken out activated carbon, with steaming
Distilled water is cleaned.Insert in pH=1 hydrochloric acid solution, the ionic liquid of absorption is all desorbed into acid solution.
Compare the adsorbance for adding activated carbon before and after sodium phosphate, add front and rear activated carbon and the adsorbance of ionic liquid is lifted
About 2.5 times, it was demonstrated that phosphate can effectively facilitate absorption of the activated carbon to ionic liquid.
Embodiment 2：
Ammonium phosphate promotes activated carbon Static Adsorption ionic liquid (N- butyl -3- picolines hexafluorophosphate)
【Add ammonium phosphate experiment】Concretely comprise the following steps：To pending 1mmol/L N- butyl -3- picoline hexafluoro phosphorus
A small amount of ammonium phosphate is added in acid salt aqueous solution, the concentration of ammonium phosphate is 0.01mmol/L after stablizing.Further adding will be a certain amount of
Powder merchandise active carbon vibration 24h, it is to be adsorbed reach balance after, measure activated carbon to N- butyl -3- picoline hexafluoro phosphorus
The saturated extent of adsorption of hydrochlorate is 56.6mg/g.Insert in pH=1 sulfuric acid solution, N- butyl -3- picoline hexafluorophosphates
It can be desorbed completely by acid solution.Activated carbon is placed in pH=13 potassium hydroxide aqueous solution, it is weak activated carbon pH can be adjusted to 9.5
Alkalescence.Activated carbon is reusable repeatedly.
【Ammonium phosphate contrast experiment is not added】Concretely comprise the following steps：To pending 1mmol/L N- butyl -3- picolines
Add a certain amount of powder merchandise active carbon in hexafluorophosphoric acid saline solution, vibrate 24h, it is to be adsorbed reach balance after, measure work
Property charcoal is 29.0mg/g to the saturated extent of adsorption of N- butyl -3- picoline hexafluorophosphates, is then taken out activated carbon, with steaming
Distilled water is cleaned.Insert in pH=1 sulfuric acid solution, the ionic liquid of absorption is all desorbed into acid solution.
Compare the adsorbance for adding activated carbon before and after ammonium phosphate, add front and rear activated carbon and the adsorbance of ionic liquid is lifted
About 2.0 times, it was demonstrated that phosphate can effectively facilitate absorption of the activated carbon to ionic liquid.
Embodiment 3：
Activated-charcoal column Dynamic Adsorption ionic liquid (1- ethyl-3-methylimidazoles hexafluorophosphate)
【Add potassium phosphate experiment】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazole hexafluoro phosphorus
A small amount of potassium phosphate is added in acid salt aqueous solution, the concentration of potassium phosphate is 0.01mmol/L after stablizing.10g granular activated carbons are taken to load
Internal diameter 1cm, high 10cm glass column.Under the conditions of stablizing under flow velocity, above-mentioned solution is flowed through into activated carbon packed column and carries out post suction
It is attached, measure that to reach the accessible liquor capacity of adsorption saturation be 1600ml.Solution in post is drained, adds 1 bed volume pH
=1 hydrochloric acid solution is eluted, then the distillation water elution adsorption column with 1 bed volume, 1- ethyl-3-methylimidazole hexafluoro phosphorus
Hydrochlorate can be desorbed completely.1 bed volume pH=13 potassium hydroxide aqueous solution is added, activated carbon pH can be adjusted to 9.0
Alkalescent.Activated carbon is reusable repeatedly.
【Potassium phosphate contrast experiment is not added】Concretely comprise the following steps：Do not add potassium phosphate, other processing operations with【Add phosphoric acid
Sodium is tested】It is identical, measure that to reach the accessible liquor capacity of adsorption saturation be 500ml.
Compare and add solution treating capacity before and after phosphate, it is 500ml to add pre-treatment water, adds post processing water and is
1600ml, adsorption treatment amount lift about 3.2 times.
Embodiment 4：
Activated-charcoal column Dynamic Adsorption ionic liquid (chlorination N- butyl -3- picolines)
【Add sodium phosphate experiment】Concretely comprise the following steps：Chlorination N- butyl -3- picoline water to pending 1mmol/L
A small amount of sodium phosphate is added in solution, the concentration of sodium phosphate is 0.01mmol/L after stablizing.10g granular activated carbons are taken to load internal diameter
1cm, high 10cm glass column.Under the conditions of stablizing under flow velocity, above-mentioned solution is flowed through into activated carbon packed column and carries out post absorption, is surveyed
It is 2000ml that the accessible liquor capacity of adsorption saturation, which must be reached,.Solution in post is drained, 1 bed volume pH=1's of addition
Sulfuric acid solution is eluted, then the distillation water elution adsorption column with 1 bed volume, and N- butyl -3- picolines can be taken off completely
It is attached.1 bed volume pH=13 sodium hydrate aqueous solution is added, activated carbon pH can be adjusted to pH9.5 alkalescent.Activated carbon
It is reusable multiple.
【Sodium phosphate contrast experiment is not added】Concretely comprise the following steps：Do not add sodium phosphate, other processing operations with【Add phosphoric acid
Sodium is tested】It is identical, measure that to reach the accessible liquor capacity of adsorption saturation be 600ml.
Compare and add solution treating capacity before and after phosphate, it is 600ml to add pre-treatment water, adds post processing water and is
2000ml, adsorption treatment amount lift 3.3 times.
Embodiment 5
Promote the method for charcoal absorption removal water body intermediate ion liquid using phosphate,
Sodium phosphate promotes activated carbon Static Adsorption ionic liquid (1- ethyl-3-methylimidazoles tetrafluoroborate)
【Add sodium phosphate experiment】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazole tetrafluoro boron
A small amount of sodium phosphate is added in acid salt aqueous solution, the concentration of sodium phosphate is 0.002mmol/L after stablizing.Further add a certain amount of
Powder merchandise active carbon vibrate 24h, it is to be adsorbed reach balance after, measure activated carbon to 1- ethyl-3-methylimidazole tetrafluoro boric acids
The saturated extent of adsorption of salt is 28.8mg/g.Insert in pH=3 sulfuric acid solution, 1- ethyl-3-methylimidazole tetrafluoroborates can
It is desorbed completely by acid solution.Activated carbon is placed in pH=13 potassium hydroxide aqueous solution, activated carbon pH can be adjusted to 10 it is weak
Alkalescence.Activated carbon is reusable repeatedly.
【Sodium phosphate contrast experiment is not added】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazoles
Add a certain amount of powder merchandise active carbon in tetrafluoro boric acid saline solution, vibrate 24h, it is to be adsorbed reach balance after, measure work
Property charcoal is 16.2mg/g to the saturated extent of adsorption of 1- ethyl-3-methylimidazole tetrafluoroborates, is then taken out activated carbon, with steaming
Distilled water is cleaned.Insert in pH=3 sulfuric acid solution, the ionic liquid of absorption is all desorbed into acid solution.
Compare the adsorbance for adding activated carbon before and after sodium phosphate, add front and rear activated carbon and the adsorbance of ionic liquid is lifted
About 1.8 times, it was demonstrated that phosphate can effectively facilitate absorption of the activated carbon to ionic liquid.
Embodiment 6
Promote the method for charcoal absorption removal water body intermediate ion liquid using phosphate,
Sodium phosphate promotes activated carbon Static Adsorption ionic liquid (1- ethyl-3-methylimidazoles tetrafluoroborate)
【Add sodium phosphate experiment】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazole tetrafluoro boron
A small amount of sodium phosphate is added in acid salt aqueous solution, the concentration of sodium phosphate is 0.002mmol/L after stablizing.Further add a certain amount of
Powder merchandise active carbon vibrate 24h, it is to be adsorbed reach balance after, measure activated carbon to 1- ethyl-3-methylimidazole tetrafluoro boric acids
The saturated extent of adsorption of salt is 50.5mg/g.Insert in pH=2 hydrochloric acid solution, 1- ethyl-3-methylimidazole tetrafluoroborates can
It is desorbed completely by acid solution.Activated carbon is placed in pH=12 sodium hydrate aqueous solution, activated carbon pH can be adjusted to 10 it is weak
Alkalescence.Activated carbon is reusable repeatedly.
【Sodium phosphate contrast experiment is not added】Concretely comprise the following steps：To pending 1mmol/L 1- ethyl-3-methylimidazoles
Add a certain amount of powder merchandise active carbon in tetrafluoro boric acid saline solution, vibrate 24h, it is to be adsorbed reach balance after, measure work
Property charcoal is 16.2mg/g to the saturated extent of adsorption of 1- ethyl-3-methylimidazole tetrafluoroborates, is then taken out activated carbon, with steaming
Distilled water is cleaned.Insert in pH=2 hydrochloric acid solution, the ionic liquid of absorption is all desorbed into acid solution.
Compare the adsorbance for adding activated carbon before and after sodium phosphate, add front and rear activated carbon and the adsorbance of ionic liquid is lifted
About 3.1 times, it was demonstrated that phosphate can effectively facilitate absorption of the activated carbon to ionic liquid.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel do not depart from improvement that scope made and modification all should be the present invention's according to the announcement of the present invention
Within protection domain.
Claims (7)
1. promote the method that charcoal absorption removes water body intermediate ion liquid using phosphate, it is characterised in that to containing ion
Phosphate is added in the water body of liquid, fully mixes and dissolves；
With the ionic liquid in charcoal absorption water body, after adsorption equilibrium or adsorption saturation is reached, first with acidic elution agent
Elution ionic liquid, then activated carbon pH is adjusted back to the alkalescent scope for being more than 8.0 with alkaline solution, it is re-used in activated carbon
In next round absorption；
After adding phosphate, the ratio of phosphatic molar concentration and ionic liquid molar concentration is 1/500 to 1/50 in water body；
The mode of ionic liquid in charcoal absorption water body is static balancing absorption mode or dynamic column absorption mode.
2. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, the ionic liquid in water body includes glyoxaline ion liquid, pyridine ionic liquid, quaternary ammonium ionic liquid, season
Phosphine ionic liquid, pyrrolidines ionic liquid or piperidines ionic liquid.
3. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, described phosphate includes sodium phosphate, potassium phosphate or ammonium phosphate.
4. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, described acidic elution agent includes pH=1-3 hydrochloric acid or sulfuric acid solution.
5. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, described alkaline solution includes pH=11-13 sodium hydroxide or potassium hydroxide aqueous solution.
6. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, static balancing absorption mode is：A small amount of phosphate is added into a certain amount of water body containing ionic liquid, is further thrown
Add the activated carbon of certain mass, fully vibration causes charcoal absorption ionic liquid to reach balance, and activated carbon is filtered and taken out, is put
Enter in acidic elution agent, the ionic liquid being tightly held by activated carbon will be desorbed into acidic elution agent, then by activated carbon from acidity
Take out, be placed in alkaline solution in eluant, eluent, activated carbon pH is adjusted to the alkalescent more than 8.0, reuses activated carbon.
7. the method according to claim 1 for promoting charcoal absorption to remove water body intermediate ion liquid using phosphate, its
It is characterised by, dynamic column absorption mode is：In cylinder fill certain mass activated carbon, under the conditions of flow velocity is stablized, with containing
Ionic liquid and a small amount of phosphatic water body flow through activated carbon packed column and carry out post absorption, and absorption takes out water body after reaching saturation
It is dry, adsorption column is eluted with 1 bed volume acidic elution agent, then the distillation water elution adsorption column with 1 bed volume, ionic liquid reach
It is complete to desorption, adsorption column further is eluted with the alkaline solution of 1 bed volume, activated carbon pH is recalled to weak more than 8.0
Alkalescence, reuse activated carbon.
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