CN107721057A - A kind of method for treating copper-containing waste water based on magnetic adsorbent - Google Patents
A kind of method for treating copper-containing waste water based on magnetic adsorbent Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a kind of method for treating copper-containing waste water based on magnetic adsorbent, including carboxymethyl cellulose is placed in deionized water and dissolved, add the sugar of ring six, add NaOH, externally-applied magnetic field reaction；FeCl is added into above-mentioned solution3·6H2O、FeCl2·4H2O and Fe3O4, add atoleine；NaOH solution is added into above-mentioned solution, adds epichlorohydrin, casts out that to obtain gel after supernatant standby；Collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, natural sedimentation, obtained supernatant and precipitation；Adjust the pH value of supernatant；Gel is added into supernatant, externally-applied magnetic field continues to react；The copper ion in copper-containing wastewater has been adsorbed in gel.The method comprises the steps of firstly, preparing the gel with absorption heavy metal, then by gel as in the waste water containing copper, copper ion in copper-containing wastewater is adsorbed, the processing method of the present invention is simple, it is easy to operate, content of copper ion in industrial wastewater after being handled using treatment method is reduced, and reaches the discharge standard of national waste water.
Description
Technical field
The invention belongs to water-treatment technology field, more particularly to a kind of copper-containing wastewater processing side based on magnetic adsorbent
Method.
Background technology
Industrial wastewater（industrial wastewater ）Including production waste water, production waste and cooling water, refer to work
Caused waste water and waste liquid in industry production process, wherein containing outflow with water industrial production materials, intermediate product, byproduct with
And caused pollutant in production process.
Classify by the product and processing object of industrial enterprise, such as Metallurgical Waste Water, paper waste, coke-oven gas waste water, metal
Pickling waste waters, chemical fertilizer waste water, textile printing and dyeing wastewater, waste water from dyestuff, leather-making waste water, agricultural chemicals waste water, power station waste water etc..
One feature of industrial wastewater is water quality and water because of the difference of production technology and the mode of production and difference is very big；Work
Another feature of industry waste water is：In addition to indirect cooling water, all containing the relevant material of a variety of same raw material, and in waste water
Existing forms are often different.
Copper-containing wastewater is a kind of waste water as caused by the industry such as metallurgy, electronics, in the industry of production copper product, in waste water
Then have copper and other heavy metals.Copper content substantially exceeds the sewage drainage standard of national regulation in copper-containing wastewater, if directly
Discharge, can seriously pollute environment.Copper-containing wastewater is handled therefore, it is necessary to take the necessary measures.
The content of the invention
The invention provides a kind of method for treating copper-containing waste water based on magnetic adsorbent, to solve waste water in the prior art
Middle copper content exceedes the problem of sewage drainage standard of national regulation.
To achieve these goals, the present invention uses following technical scheme：
A kind of method for treating copper-containing waste water based on magnetic adsorbent, comprises the following steps：
Dissolved Step 1: carboxymethyl cellulose is placed in deionized water, 10-20min is stirred by ultrasonic, adds ring six
Sugar, 3-5min is stirred by ultrasonic, adds NaOH, 5-10min is stirred by ultrasonic, additional 0.8-1.2T magnetic field, continues to react 1-2h；
Step 2: add FeCl in the solution obtained to step 13·6H2O、FeCl2·4H2O and Fe3O4, 3- is stirred by ultrasonic
5min, 30-35 DEG C is again heated to, adds atoleine, be heated to 35-70 DEG C, 1-2min is stirred by ultrasonic；
Step 3: adding NaOH solution in the solution obtained to step 2,3-5min is stirred by ultrasonic, adds epichlorohydrin, ultrasound
3-4h is stirred, stands 5-7h, casts out that to obtain gel after supernatant standby；
Step 4: collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, stands 5-6h, natural sedimentation, what is obtained is upper
Clear liquid and precipitation；
Step 5: the pH value of regulation supernatant is to 6-8；
Step 6: the gel obtained in step 3 is added in the supernatant obtained into step 5,3-4h is stirred by ultrasonic, stands
1-2 hours, additional 0.8-1.2T magnetic field, continue to react 1-2h；
Step 7: the copper ion in copper-containing wastewater is adsorbed in gel.
Further, the mass ratio of carboxymethyl cellulose and the sugar of ring six is 0.3-2.0 in the step 1：1.
Further, the deionized water in the step 1 and the volume ratio of atoleine in the step 2 are 1：1.5-
3.5。
Further, the mass ratio of deionized water and carboxymethyl cellulose is 100 in the step 1：1-3.
Further, the FeCl3·6H2O、FeCl2·4H2O and Fe3O4Addition gross mass be solvent gross mass at that time
8-15%.
Further, the FeCl3·6H2O、FeCl2·4H2O and Fe3O4Between mass ratio be 1：1：5.
Further, the reaction temperature of the step 1 is 20-30 DEG C.
Further, the reaction temperature of the step 3 is 35-70 DEG C.
Further, the reaction temperature of the step 4 is 30-35 DEG C.
Further, the reaction temperature of the step 6 is 35-70 DEG C.
Further, the concentration of the NaOH solution in the step 3 is 1-3mol/L.
Compared with prior art, the invention has the advantages that：
The method comprises the steps of firstly, preparing the gel with absorption heavy metal, then gel is given up as in the waste water containing copper to cupric
Copper ion in water is adsorbed, and processing method of the invention is simple, easy to operate, the industry after being handled using treatment method
Content of copper ion in waste water substantially reduces, so as to reach the discharge standard of national waste water.
Embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
A kind of method for treating copper-containing waste water based on magnetic adsorbent, comprises the following steps：
Dissolved Step 1: carboxymethyl cellulose is placed in deionized water, 10-20min is stirred by ultrasonic, adds ring six
Sugar, 3min is stirred by ultrasonic, adds NaOH, 5min is stirred by ultrasonic, additional 0.8T magnetic field, continues to react 1h；
Step 2: add FeCl in the solution obtained to step 13·6H2O、FeCl2·4H2O and Fe3O4, 3min is stirred by ultrasonic,
30 DEG C are again heated to, adds atoleine, is heated to 35 DEG C, 1min is stirred by ultrasonic；
Step 3: adding NaOH solution in the solution obtained to step 2,3min is stirred by ultrasonic, adds epichlorohydrin, ultrasound is stirred
Mix 3h, stand 5h, cast out that to obtain gel after supernatant standby；
Step 4: collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, stands 5h, natural sedimentation, obtained supernatant
Liquid and precipitation；
Step 5: the pH value of regulation supernatant is to 6；
Step 6: the gel obtained in step 3 is added in the supernatant obtained into step 5,3h is stirred by ultrasonic, stands 1
Hour, additional 0.8T magnetic field, continue to react 1h；
Step 7: the copper ion in copper-containing wastewater is adsorbed in gel.
The mass ratio of carboxymethyl cellulose and the sugar of ring six is 0.3 in the step 1：1, the deionization in the step 1
The volume ratio of water and atoleine in the step 2 is 1：1.5, deionized water and carboxymethyl cellulose in the step 1
Mass ratio is 100：1.
The FeCl3·6H2O、FeCl2·4H2O and Fe3O4Addition gross mass be the 8% of solvent gross mass at that time, it is described
FeCl3·6H2O、FeCl2·4H2O and Fe3O4Between mass ratio be 1：1：5.
The reaction temperature of the step 1 is 20 DEG C, and the reaction temperature of the step 3 is 35 DEG C, the step 4 it is anti-
It is 30 DEG C to answer temperature, and the reaction temperature of the step 6 is 35 DEG C, and the concentration of the NaOH solution in the step 3 is 1mol/L.
Embodiment 2
A kind of method for treating copper-containing waste water based on magnetic adsorbent, comprises the following steps：
Dissolved Step 1: carboxymethyl cellulose is placed in deionized water, 105min be stirred by ultrasonic, add the sugar of ring six,
4min is stirred by ultrasonic, adds NaOH, 8min is stirred by ultrasonic, additional 1.0T magnetic field, continues to react 1-2h；
Step 2: add FeCl in the solution obtained to step 13·6H2O、FeCl2·4H2O and Fe3O4, 4min is stirred by ultrasonic,
33 DEG C are again heated to, adds atoleine, is heated to 50 DEG C, 1min is stirred by ultrasonic；
Step 3: adding NaOH solution in the solution obtained to step 2,4min is stirred by ultrasonic, adds epichlorohydrin, ultrasound is stirred
Mix 3h, stand 6h, cast out that to obtain gel after supernatant standby；
Step 4: collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, stands 5h, natural sedimentation, obtained supernatant
Liquid and precipitation；
Step 5: the pH value of regulation supernatant is to 7；
Step 6: the gel obtained in step 3 is added in the supernatant obtained into step 5,3h is stirred by ultrasonic, stands 1
Hour, additional 1.0T magnetic field, continue to react 1h；
Step 7: the copper ion in copper-containing wastewater is adsorbed in gel.
The mass ratio of carboxymethyl cellulose and the sugar of ring six is 1.5 in the step 1：1, the deionization in the step 1
The volume ratio of water and atoleine in the step 2 is 1：2.0, deionized water and carboxymethyl cellulose in the step 1
Mass ratio is 100：2.
The FeCl3·6H2O、FeCl2·4H2O and Fe3O4Addition gross mass be the 10% of solvent gross mass at that time, institute
State FeCl3·6H2O、FeCl2·4H2O and Fe3O4Between mass ratio be 1：1：5.
The reaction temperature of the step 1 is 25 DEG C, and the reaction temperature of the step 3 is 50 DEG C, the step 4 it is anti-
It is 33 DEG C to answer temperature, and the reaction temperature of the step 6 is 50 DEG C, and the concentration of the NaOH solution in the step 3 is 2mol/L.
Embodiment 3
A kind of method for treating copper-containing waste water based on magnetic adsorbent, comprises the following steps：
Dissolved Step 1: carboxymethyl cellulose is placed in deionized water, 20min is stirred by ultrasonic, added the sugar of ring six, surpass
Sound stirs 5min, adds NaOH, and 10min is stirred by ultrasonic, additional 1.2T magnetic field, continues to react 2h；
Step 2: add FeCl in the solution obtained to step 13·6H2O、FeCl2·4H2O and Fe3O4, 5min is stirred by ultrasonic,
35 DEG C are again heated to, adds atoleine, is heated to 70 DEG C, 2min is stirred by ultrasonic；
Step 3: adding NaOH solution in the solution obtained to step 2,5min is stirred by ultrasonic, adds epichlorohydrin, ultrasound is stirred
Mix 4h, stand 7h, cast out that to obtain gel after supernatant standby；
Step 4: collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, stands 6h, natural sedimentation, obtained supernatant
Liquid and precipitation；
Step 5: the pH value of regulation supernatant is to 8；
Step 6: the gel obtained in step 3 is added in the supernatant obtained into step 5,4h is stirred by ultrasonic, stands 2
Hour, additional 1.2T magnetic field, continue to react 2h；
Step 7: the copper ion in copper-containing wastewater is adsorbed in gel.
The mass ratio of carboxymethyl cellulose and the sugar of ring six is 2.0 in the step 1：1, the deionization in the step 1
The volume ratio of water and atoleine in the step 2 is 1：1.5-3.5, deionized water and carboxymethyl cellulose in the step 1
The mass ratio of element is 100： 3.
The FeCl3·6H2O、FeCl2·4H2O and Fe3O4Addition gross mass be the 15% of solvent gross mass at that time, institute
State FeCl3·6H2O、FeCl2·4H2O and Fe3O4Between mass ratio be 1：1：5.
The reaction temperature of the step 1 is 30 DEG C, and the reaction temperature of the step 3 is 70 DEG C, the step 4 it is anti-
It is 35 DEG C to answer temperature, and the reaction temperature of the step 6 is 70 DEG C, and the concentration of the NaOH solution in the step 3 is 3mol/L.
The method comprises the steps of firstly, preparing the gel with absorption heavy metal, then by gel as in the waste water containing copper, to containing
Copper ion in copper waste water is adsorbed, and processing method of the invention is simple, easy to operate, after being handled using treatment method
Content of copper ion in industrial wastewater reduces, and reaches the discharge standard of national waste water.
In waste water after the processing method processing for detecting embodiment 1-3, the clearance of copper is up to more than 99%, its
The effect of middle embodiment 2 is the most obvious, and the clearance of copper is up to 99.5%, and this illustrates processing method provided by the invention, really may be used
So that the copper in copper-containing wastewater to be removed, and positive effect.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method for treating copper-containing waste water based on magnetic adsorbent, it is characterised in that comprise the following steps：
Dissolved Step 1: carboxymethyl cellulose is placed in deionized water, 10-20min is stirred by ultrasonic, adds ring six
Sugar, 3-5min is stirred by ultrasonic, adds NaOH, 5-10min is stirred by ultrasonic, additional 0.8-1.2T magnetic field, continues to react 1-2h；
Step 2: add FeCl in the solution obtained to step 13·6H2O、FeCl2·4H2O and Fe3O4, 3- is stirred by ultrasonic
5min, 30-35 DEG C is again heated to, adds atoleine, be heated to 35-70 DEG C, 1-2min is stirred by ultrasonic；
Step 3: adding NaOH solution in the solution obtained to step 2,3-5min is stirred by ultrasonic, adds epichlorohydrin, ultrasound
3-4h is stirred, stands 5-7h, casts out that to obtain gel after supernatant standby；
Step 4: collect copper-containing wastewater：Used industrial copper-containing wastewater is reclaimed, stands 5-6h, natural sedimentation, what is obtained is upper
Clear liquid and precipitation；
Step 5: the pH value of regulation supernatant is to 6-8；
Step 6: the gel obtained in step 3 is added in the supernatant obtained into step 5,3-4h is stirred by ultrasonic, stands
1-2 hours, additional 0.8-1.2T magnetic field, continue to react 1-2h；
Step 7: the copper ion in copper-containing wastewater is adsorbed in gel.
2. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that the step
The mass ratio of carboxymethyl cellulose and the sugar of ring six is 0.3-2.0 in one：1.
3. the method for treating copper-containing waste water according to claim 2 based on magnetic adsorbent, it is characterised in that the step
Deionized water in one and the volume ratio of atoleine in the step 2 are 1：1.5-3.5.
4. the method for treating copper-containing waste water according to claim 3 based on magnetic adsorbent, it is characterised in that the step
The mass ratio of deionized water and carboxymethyl cellulose is 100 in one：1-3.
5. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that described
FeCl3·6H2O、FeCl2·4H2O and Fe3O4Addition gross mass for solvent gross mass at that time 8-15%.
6. the method for treating copper-containing waste water according to claim 5 based on magnetic adsorbent, it is characterised in that described
FeCl3·6H2O、FeCl2·4H2O and Fe3O4Between mass ratio be 1：1：5.
7. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that the step
Three reaction temperature is 35-70 DEG C.
8. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that the step
Four reaction temperature is 30-35 DEG C.
9. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that the step
Six reaction temperature is 35-70 DEG C.
10. the method for treating copper-containing waste water according to claim 1 based on magnetic adsorbent, it is characterised in that the step
The concentration of NaOH solution in rapid three is 1-3mol/L.
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| CN201711006877.1A CN107721057A (en) | 2017-10-25 | 2017-10-25 | A kind of method for treating copper-containing waste water based on magnetic adsorbent |
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| CN201711006877.1A CN107721057A (en) | 2017-10-25 | 2017-10-25 | A kind of method for treating copper-containing waste water based on magnetic adsorbent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903448A (en) * | 2016-05-09 | 2016-08-31 | 浙江海洋大学 | Method for preparing nanocrystalline cellulose magnetic particle adsorbent |
| CN106220866A (en) * | 2016-07-28 | 2016-12-14 | 东北林业大学 | A kind of preparation method that copper ion is had high adsorption magnetic hydrogel |
| CN106693920A (en) * | 2017-02-14 | 2017-05-24 | 上海工程技术大学 | Magnetic nano composite material and a preparation method and application thereof |
-
2017
- 2017-10-25 CN CN201711006877.1A patent/CN107721057A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903448A (en) * | 2016-05-09 | 2016-08-31 | 浙江海洋大学 | Method for preparing nanocrystalline cellulose magnetic particle adsorbent |
| CN106220866A (en) * | 2016-07-28 | 2016-12-14 | 东北林业大学 | A kind of preparation method that copper ion is had high adsorption magnetic hydrogel |
| CN106693920A (en) * | 2017-02-14 | 2017-05-24 | 上海工程技术大学 | Magnetic nano composite material and a preparation method and application thereof |
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