CN110117037A - The processing method of one metal ion species type sewage - Google Patents
The processing method of one metal ion species type sewage Download PDFInfo
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- CN110117037A CN110117037A CN201910410558.XA CN201910410558A CN110117037A CN 110117037 A CN110117037 A CN 110117037A CN 201910410558 A CN201910410558 A CN 201910410558A CN 110117037 A CN110117037 A CN 110117037A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The present invention relates to organically-modified and technical field of sewage.The present invention provides the processing method of a metal ion species type sewage, this method is modified montmorillonite by cationic and anionic surfactant, and makes efficient long chain cation surfactant and environmentally friendly glucose-type anionic surfactant by oneself.Raw material sources needed for this method are extensive, are easy to get, the sewage treatment route industrialization easy to accomplish being related to.By composite modified to the male-female ion of montmorillonite, montmorillonite is increased to the adsorption capacity of metal ion, the metal ion being more advantageous in processing waste water.
Description
Technical field
The present invention relates to organically-modified and technical field of sewage, and in particular to the processing of a metal ion species type sewage
Method.
Background technique
Montmorillonite also known as montmorillonite, be it is a kind of with dilatancy, in layer structure containing a small amount of alkali and alkaline earth gold
The hydrous alumino silicates mineral of category, molecular formula: Al2(OH)2Si4O10；Molecular weight 360；English language Chemical name:
montmorillonite。
Montmorillonite is 2:1 type layered clay mineral, and unit cell is a piece of by pressing from both sides in two panels apex angle Si-O tetrahedron inwardly
Al-O or Mg-O octahedron forms a structure sheaf.Montmorillonite due to its large specific surface area, the characteristics such as porosity is high, polarity is strong and it is right
The heavy metals harmful pollutants such as Pb, Zn, Cd, Cr, Hg in water has adsorption capacity, is the harmful member of removal heavy metal in waste water
The ideal Low Cost Sorbents of element.
By the modified adsorption capacity that montmorillonite can be enhanced, common modification mode be it is organically-modified, it is organically-modified
Although montmorillonite can adsorb organic matter, because to have hydrophobicity weaker to the adsorption capacity of heavy metal for it.
Quaternary ammonium salt is typical cationic surfactant, there are the problem of: the surface of water cannot be reduced well
Power reduces wetting ability, cannot effectively adsorb organic matter to be difficult to form micella.Anionic surfactant generally with
It based on sodium n-alkylbenzenesulfonate, however the production of sodium alkyl benzene sulfonate, uses and discharges, get worse the pollution of water body.
Summary of the invention
In view of the above-mentioned problems in the prior art, the present invention provides the processing methods of a metal ion species type sewage.
The following technical solution is employed by the present invention:
The processing method of one metal ion species type sewage, which is characterized in that handle waste water solution, institute using modified montmorillonoid
It states modified montmorillonoid and montmorillonite is modified by cationic and anionic surfactant, the modification procedure includes the following steps:
Step 1: synthesis long chain cation surfactant
By octadecyl bromo hydrocarbon, dimethylaminoethanol and dehydrated alcohol are added in reaction flask, heating stirring 8h.Ice
Cooling crystallization under water-bath, obtains crude product；It is recrystallized again with the mixed solvent of acetone and methanol, obtains white crystal, vacuum
It is dry, obtain target product, N- octadecyl-N- (2- ethoxy)-N, N- ditallowdimethyl ammonium bromide.
Specific reaction equation is as follows:
Step 2: synthesis N- lauryl glucoside amine
Lauryl amine and glucose are added in the three-necked flask for filling methanol, it is cooling after being stirred to react 6h at 60 DEG C
It to room temperature and moves in ice-water bath, sodium borohydride (excess) then is added, continues to stir, until reaction system is at pellucidity；
There is white crystal precipitation after room temperature stands 3h with the pH of hydrochloric acid regulation system, reaction solution is being filtered, by filter cake dehydrated alcohol
Repeatedly after washing, it is placed in the mixed solution of sodium hydroxide solution and methanol after temperature rising reflux 8h, it is cooling, white precipitate is precipitated,
Suction filtration obtains crude product, N- lauryl glucoside amine.
Specific reaction equation is as follows:
Step 3: synthesis of glucose type anionic surfactant
The N- lauryl glucoside amine and glyoxalic acid of synthesis are added in the three-necked flask for filling methanol, in 60 DEG C
After being stirred to react 5h, at 80~85 DEG C, the glyoxalic acid for steaming methanol with Rotary Evaporators and not answering obtains the sticky shape Portugal of yellow
Grape sugar-type anionic surfactant.
Specific reaction equation is as follows:
Step 4: sodium
It weighs montmorillonite to be add to deionized water with sodium hydroxide, heating stirring, after 2h, filters reaction solution, it is dry
Filter cake, then filter cake is crushed, obtain sodium-based montmorillonite.
Step 5: male-female ion is composite modified
It weighs sodium-based montmorillonite to be add to deionized water with long chain cation surfactant, heating stirring, 2h
Afterwards, complexones is added, continues after stirring 2h, filters reaction solution, dry cake, as modified montmorillonite.
Step 6: absorption
Cu will be contained2+、Pb2+And Cd2+The modified montmorillonite in a reservoir, is poured into container by the sewage dress of ion
In, oscillation.Specifically, container is put on the oscillator, vibrates 1h at room temperature, then be centrifuged 10min on centrifuge, takes supernatant
With the residual concentration of heavy metal ion in atomic absorption spectrophotometer measurement filtrate.
Further, in the first step, the mixed volume ratio of acetone and methanol is 2:1.
Further, in the second step, the concentration of hydrochloric acid is 2mol/L.
Further, in the second step, the pH value for adjusting reaction solution is 2~3.
Further, in the second step, in the mixed solution of sodium hydroxide solution and methanol, in sodium hydroxide solution,
The mass fraction of sodium hydroxide is 5%, and the volume ratio of sodium hydroxide solution and methanol is 5:1.
Further, in the 4th step, original montmorillonoid soil comes from Inner Mongol Chifeng, SiO in montmorillonoid sample2Quality point
Number is 66.7%；Al2O3Mass fraction is 28.5%；H2O mass fraction is 5%.
Further, in the 4th step, the filter cake is crushed, and particle size is 0.074mm after crushing.
Compared with the conventional method, the invention has the advantages that:
(1) by introducing ethoxy on quaternary ammonium salt hydrophilic head base, surfactant is improved in the tension of solution surface,
There is better wettability.
(2) glycosyl surfactant active is most representative one kind in green surfactant, synthesizes glycosyl surface-active
Agent meets the theory of " Green Chemistry ".
(3) by N- octadecyl-N- (2- ethoxy)-N, N- ditallowdimethyl ammonium bromide cationic surfactant is de- to covering
Soil it is organically-modified on the basis of, glucose-type anionic surfactant is re-introduced into, so that after male-female ion is composite modified
Montmorillonite can adsorb organic matter, moreover it is possible to better adsorbing metal ions.
(4) present invention is using montmorillonite as starting material, and raw material is cheap and easy to get, and reaction condition is mildly easily-controllable, and route is easy real
Now industrialize.
Specific embodiment
The present invention is specifically described combined with specific embodiments below:
Embodiment 1
The processing method of one metal ion species type sewage is as follows:
(a) long chain cation surfactant is synthesized
Weigh 10g (0.03mol) octadecyl bromo hydrocarbon, 2.7g (0.03mol) dimethylaminoethanol and 50ml's is anhydrous
Ethyl alcohol is added in reaction flask, is warming up to 65 DEG C, stirs 8h.Cooling crystallization 2h or so under ice-water bath, suction filtration reaction solution, which obtains, slightly to be produced
Product；Crude product is recrystallized with the mixed solvent 30ml of acetone and methanol again, obtains white crystal, is dried in vacuo, obtains mesh
Mark product, N- octadecyl-N- (2- ethoxy)-N, N- ditallowdimethyl ammonium bromide (note THDAB) 11.6g, yield: 92%.
Specific reaction equation is as follows:
(b) N- lauryl glucoside amine is synthesized
It weighs 13g (0.07mol) lauryl amine and 12.6g (0.07mol) glucose is added to and fills three mouthfuls of 60ml methanol
It in flask, after being stirred to react 6h at 60 DEG C, is cooled to room temperature and moves in ice-water bath, 5.7g (0.15mol) boron is then added
Sodium hydride continues to stir, until reaction system is at pellucidity；With pH=2~3 of the hydrochloric acid regulation system of 2mol/L, room temperature
After standing 3h, there is white crystal precipitation, is filtering reaction solution, after filter cake is repeatedly washed with dehydrated alcohol, be placed on the hydrogen of 60ml
It is cooling after temperature rising reflux 8h in the mixed solution of sodium hydroxide solution and methanol, white precipitate is precipitated, suction filtration obtains crude product, N-
Lauryl glucoside amine 22.7g, yield: 93%.
Specific reaction equation is as follows:
(c) synthesis of glucose type anionic surfactant
The glyoxalic acid for weighing the N- lauryl glucoside amine 17g (0.05mol) and 7.4g (0.1mol) of synthesis is added to
In the three-necked flask for filling 20ml methanol, after 60 DEG C are stirred to react 5h, at 80~85 DEG C, methanol is steamed with Rotary Evaporators
The glyoxalic acid that do not answer obtains the sticky shape glucose-type anionic surfactant of yellow (note GTAS) 19.5g, yield: 96%；
Specific reaction equation is as follows:
(d) sodium
100g montmorillonite (note Bent) is weighed, with 10g sodium hydroxide, is added in the deionized water of 500ml, is warming up to 80
DEG C, after insulated and stirred 2h, reaction solution, dry cake are filtered, then filter cake is crushed, 0.074 mm screening obtains sodium-based montmorillonite.
(e) male-female ion is composite modified
Weigh sodium-based montmorillonite 30g, and 2g long chain cation surfactant (THDAB), be added to 300ml go from
In sub- water, 60 DEG C are warming up to, after stirring 2h, then 1g synthesis of glucose type anionic surfactant is added into reaction solution
(GTAS), after continuing insulated and stirred 2h, reaction solution, dry cake are filtered, as modified montmorillonite is denoted as THDAB-GTAS
Bent。
(f) preparation of waste water
The CuCl of 20mg is weighed respectively2、PbCl2、CdCl2, it is added and goes in the deionized water of 100ml, is made into 0.2mg/ml's
Cu2+、Pb2+、Cd2+Heavy metal solution.
(g) it adsorbs
Prepared Cu is taken respectively2+、Pd2+、Cd2+Waste water solution 100ml is in two conical flasks, respectively by montmorillonite
1mg and it is composite modified after montmorillonite 1mg pour into conical flask, then conical flask is put on the oscillator, vibrates 1h at room temperature, then
With centrifuge with 4200rmin-1Revolving speed be centrifuged 10min, take supernatant atomic absorption spectrophotometer measurement filtrate in weight
The residual concentration of metal ion.
Adsorbance q (mgmg is calculated by formula (1) and (2)-1) and removal rate Y.
Q=V (C0-Ce)/m (1)
Y=[(C0-Ce)/C0] × 100% (2)
In formula, V is the volume (ml) of heavy metal solution；M is the dosage (mg) of clay mineral；C0、CeFor an absorption front and back huge sum of money
Belong to the concentration (mgml of ion-1)。
To sum up, modified montmorillonite is to the adsorption effect of metal ion, far better than common montmorillonite to metal ion
Adsorptivity.
Embodiment 2
The processing method of one metal ion species type sewage is as follows:
(a) long chain cation surfactant is synthesized
Weigh 10g (0.03mol) octadecyl bromo hydrocarbon, 2.7g (0.03mol) dimethylaminoethanol and 50ml's is anhydrous
Ethyl alcohol is added in reaction flask, is warming up to 65 DEG C, stirs 8h.Cooling crystallization 2h or so under ice-water bath, suction filtration reaction solution, which obtains, slightly to be produced
Product；Crude product is recrystallized with the mixed solvent 30ml of acetone and methanol again, obtains white crystal, is dried in vacuo, obtains mesh
Mark product, N- octadecyl-N- (2- ethoxy)-N, N- ditallowdimethyl ammonium bromide (note THDAB) 11.5g, yield: 91%.
Specific reaction equation is as follows:
(b) N- lauryl glucoside amine is synthesized
It weighs 13g (0.07mol) lauryl amine and 12.6g (0.07mol) glucose is added to and fills three mouthfuls of 60ml methanol
It in flask, after being stirred to react 6h at 60 DEG C, is cooled to room temperature and moves in ice-water bath, 5.7g (0.15mol) boron is then added
Sodium hydride continues to stir, until reaction system is at pellucidity；With pH=2~3 of the hydrochloric acid regulation system of 2mol/L, room temperature
After standing 3h, there is white crystal precipitation, is filtering reaction solution, after filter cake is repeatedly washed with dehydrated alcohol, be placed on the hydrogen of 60ml
It is cooling after temperature rising reflux 8h in the mixed solution of sodium hydroxide solution and methanol, white precipitate is precipitated, suction filtration obtains crude product, N-
Lauryl glucoside amine 23g, yield: 93%.
Specific reaction equation is as follows:
(c) synthesis of glucose type anionic surfactant
The glyoxalic acid for weighing the N- lauryl glucoside amine 17g (0.05mol) and 7.4g (0.1mol) of synthesis is added to
In the three-necked flask for filling 20ml methanol, after 60 DEG C are stirred to react 5h, at 80~85 DEG C, methanol is steamed with Rotary Evaporators
The glyoxalic acid that do not answer obtains the sticky shape glucose-type anionic surfactant of yellow (note GTAS) 19.4g, yield: 95%；
Specific reaction equation is as follows:
(d) sodium
100g montmorillonite (note Bent) is weighed, with 10g sodium hydroxide, is added in the deionized water of 500ml, is warming up to 80
DEG C, after insulated and stirred 2h, reaction solution, dry cake are filtered, then filter cake is crushed, 0.074 mm screening obtains sodium-based montmorillonite.
(e) male-female ion is composite modified
Weigh sodium-based montmorillonite 30g, and 2g long chain cation surfactant (THDAB), be added to 300ml go from
In sub- water, 60 DEG C are warming up to, after stirring 2h, then 1g synthesis of glucose type anionic surfactant is added into reaction solution
(GTAS), after continuing insulated and stirred 2h, reaction solution, dry cake are filtered, as modified montmorillonite is denoted as THDAB-GTAS
Bent。
(f) preparation of waste water
The CuCl of 20mg is weighed respectively2、PbCl2、CdCl2, it is added and goes in the deionized water of 100ml, is made into 0.2mg/ml's
Cu2+、Pb2+、Cd2+Heavy metal solution.
(g) it adsorbs
Prepared Cu is taken respectively2+、Pd2+、Cd2+Waste water solution 100ml is in two conical flasks, respectively by montmorillonite
1mg and it is composite modified after montmorillonite 1mg pour into conical flask, then conical flask is put on the oscillator, vibrates 1h at room temperature, then
With centrifuge with 4200rmin-1Revolving speed be centrifuged 10min, take supernatant atomic absorption spectrophotometer measurement filtrate in weight
The residual concentration of metal ion.
Adsorbance q (mgmg is calculated by formula (1) and (2)-1) and removal rate Y.
Q=V (C0-Ce)/m (1)
Y=[(C0-Ce)/C0] × 100% (2)
In formula, V is the volume (ml) of heavy metal solution；M is the dosage (mg) of clay mineral；C0、CeFor an absorption front and back huge sum of money
Belong to the concentration (mgml of ion-1)。
To sum up, modified montmorillonite is to the adsorption effect of metal ion, far better than common montmorillonite to metal ion
Adsorptivity.
Certainly, the above description is not a limitation of the present invention, and the present invention is also not limited to the example above, this technology neck
The variations, modifications, additions or substitutions that the technical staff in domain is made within the essential scope of the present invention also should belong to of the invention
Protection scope.
Claims (7)
1. the processing method of a metal ion species type sewage, which is characterized in that waste water solution is handled using modified montmorillonoid, it is described
Modified montmorillonoid is modified montmorillonite by cationic and anionic surfactant, and the modification procedure includes the following steps:
Step 1: synthesis long chain cation surfactant
By octadecyl bromo hydrocarbon, dimethylaminoethanol and dehydrated alcohol are added in reaction flask, after heating stirring, cooling analysis
Crystalline substance recrystallizes, and vacuum drying obtains target product, N- octadecyl-N- (2- ethoxy)-N, N- ditallowdimethyl ammonium bromide；
Specific reaction equation is as follows:
Step 2: synthesis N- lauryl glucoside amine
Lauryl amine and glucose are added in the flask for filling methanol, is stirred to react, is cooled to room temperature simultaneously at 55~65 DEG C
It moves in ice-water bath, excess sodium borohydrate is added, continues to stir, until reaction system is at pellucidity；The pH of regulation system, it is quiet
It postpones, filters, wash filter cake, and filter cake is placed in solution after temperature rising reflux, it is cooling, white precipitate is precipitated, suction filtration obtains thick
Product, N- lauryl glucoside amine；
Specific reaction equation is as follows:
Step 3: synthesis of glucose type anionic surfactant
N- lauryl glucoside amine and glyoxalic acid that above-mentioned second step synthesizes are added in the flask for filling methanol, stirring is anti-
Ying Hou, the glyoxalic acid for steaming methanol with Rotary Evaporators and not answering, obtains glucose-type anionic surfactant；
Specific reaction equation is as follows:
Step 4: sodium
It weighs montmorillonite to be add to deionized water with sodium hydroxide, heating stirring, suction filtration reaction solution, dry cake, then will
Filter cake crushes, and obtains sodium-based montmorillonite；
Step 5: male-female ion is composite modified
The sodium-based montmorillonite for weighing above-mentioned 4th step preparation respectively, the long chain cation surface-active with the preparation of the above-mentioned first step
Agent is added in deionized water, heating stirring, adds the glucose-type anionic surfactant of above-mentioned third step preparation, after
After continuous stirring, reaction solution, dry cake, as modified montmorillonite are filtered；
Step 6: absorption
Cu will be contained2+、Pb2+And Cd2+The sewage dress of ion in a reservoir, the modified montmorillonite is poured into container, is shaken
It swings.
2. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the first step
In, recrystallization uses the mixed solvent of acetone and methanol, and the mixed volume ratio of the acetone and methanol is 2:1.
3. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the second step
In, there is salt acid for adjusting pH, the concentration of the hydrochloric acid is 2mol/L.
4. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the second step
In, the pH value for being adjusted to reaction solution is 2~3.
5. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the second step
In, flow back the mixed solution used, and the mixed solution is made by sodium hydroxide solution and methanol, the sodium hydroxide solution
In, the mass fraction of sodium hydroxide is 5%, and the volume ratio of sodium hydroxide solution and methanol is 5:1.
6. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the 4th step
In, each component and mass fraction are respectively as follows: SiO in montmorillonite266.7%；Al2O328.5%；H2O 5%.
7. the processing method of metal ion species type sewage according to claim 1, which is characterized in that the 4th step
In, montmorillonite particle size is 0.074mm in the crushing.
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