CN106629889B - Preparation method of glucose-based carbon microsphere imprinted material - Google Patents
Preparation method of glucose-based carbon microsphere imprinted material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 40
- 239000004005 microsphere Substances 0.000 title claims abstract description 38
- 239000008103 glucose Substances 0.000 title claims abstract description 33
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 11
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 11
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 34
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001431 copper ion Inorganic materials 0.000 abstract description 9
- 239000008367 deionised water Substances 0.000 abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 239000000178 monomer Substances 0.000 abstract description 5
- 229910000831 Steel Inorganic materials 0.000 abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 4
- 239000010959 steel Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 2
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 229910021645 metal ion Inorganic materials 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- 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
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
Abstract
The invention relates to AlCl prepared from glucose3A preparation method of a imprinting material which takes carbon microspheres synthesized by a catalyst as a functional monomer and Cu (II) as a template. The preparation process comprises the following steps: mixing glucose with AlCl3Adding the mixture into a water solution, stirring and dissolving the mixture, then putting the mixture into a steel reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for a certain time. Repeatedly washing the reacted product with distilled water, then putting the product into a reaction kettle again, adding a proper amount of tetraethylenepentamine and a copper sulfate solution with a certain concentration, and continuing the hydrothermal reaction of the mixed substances for a certain time. And finally, repeatedly soaking and washing the obtained product by using a sodium hydroxide solution and a hydrochloric acid solution, and repeatedly washing the product by using deionized water until copper ions can not be detected in the washing liquid. And drying the sample at low temperature to obtain the glucose-based carbon microsphere imprinted material. The material has good removal capability on copper ions in water.
Description
Technical Field
The invention belongs to the field of water treatment, and particularly relates to preparation and application of a glucose-based carbon microsphere imprinted material for removing metal ions Cu (II) in a water body.
Background
In the biomass pyrolysis and hydrothermal processes, a large amount of biochar is generated, the coke has the advantages of strong adsorption capacity, stable chemical properties, strong regenerability and the like, and has developed pore structures, higher specific surface area, stable aromatic structures and abundant surface functional groups. Glucose can generate intermolecular dehydration reaction under slightly acidic hydrothermal conditions to generate linear or dendritic oligomers, further polymerization can form carbon materials with higher oxygen content, and the surface of the carbon materials can keep a part of functional groups such as hydroxyl, carbonyl and the like. The hydrothermal method is an ideal method for preparing the carbon microspheres due to simple operation and pure products. The surface of the carbon microsphere prepared by the hydrothermal method has a large number of oxygen-containing functional groups, and the carbon microsphere can be bonded with metal ions so as to achieve the purpose of removing the metal ions. Liu Guxin and the like take commercial activated carbon and glucose as raw materials, a carbon sphere-activated carbon composite material with the surface and the pores loaded with nano carbon spheres is obtained through a hydrothermal process, the surface of the carbon sphere in the material is rich in active functional groups, and the adsorption capacity of the composite material on metal ions is detected by taking Cr (VI) as a model substance. It can be known that the adsorption capacity of the composite material to Cr (VI) is increased by 94 times and 3 times respectively compared with the traditional activated carbon [ inorganic materials bulletin, 2009, 24(6):1132 and 1136 ]. The metal ion imprinting technology is a method for preparing a high molecular functional material with selective adsorption performance on metal ions of a template by using the metal ions as the template and adopting the molecular imprinting technical principle. Functional monomers are important raw materials for preparing imprinted polymers. The functional monomer is basically porous organic polymer, which can be polycondensate or addition polymer, more crosslinked vinyl polymer, and inorganic carrier such as silica gel can be used as functional mother material. The metal ion imprinted material adopting biomass carbon as a functional monomer is rare.
Disclosure of Invention
The invention relates to a Cu (II) imprinted material, AlCl, using glucose as a carbon source3As a catalyst and a functional agent in the synthesis process of the carbon microsphere, tetraethylenepentamine is used as the functional agent of the Cu (II) imprinted material to increase the amino group on the surface of the material and strengthen the combination between Cu (II) and the carbon microsphere. The synthesized carbon microsphere imprinted material has uniform particles and good effect of removing Cu (II).
The preparation method of the imprinting material comprises the following steps:
carrying out hydrothermal reaction on a mixed solution of glucose and aluminum trichloride for a certain time to obtain carbon microspheres, mixing the carbon microspheres with a tetraethylene anhydrous and copper sulfate solution, continuing carrying out hydrothermal reaction, washing template ions of the obtained carbon microsphere material with a sodium hydroxide solution and a hydrochloric acid solution, and drying at a low temperature to obtain the Cu (II) carbon microsphere imprinting material.
The mass ratio range of the glucose to the aluminum trichloride is 1: 2-3: 1, the temperature of the hydrothermal reaction of glucose and aluminum trichloride is 160-180 ℃; the reaction time is 20-22 h.
The volume percentage of the tetraethylene non-amine is 12.5-25% (V/V).
The ratio of the carbon microspheres to the tetraethylenepentamine is 50:1-200:1(g/L), the volume ratio of the tetraethylenepentamine to the copper sulfate solution is 1:2-1:3, and the hydrothermal reaction time is 8-10 h.
The concentration of the copper sulfate solution is 1.0g/L,
and the elution of the Cu (II) is alternately eluted by using a sodium hydroxide solution and a hydrochloric acid solution.
The drying temperature is 45-60 ℃, and the drying time is 20-30 h.
The invention has the advantages and characteristics that:
the addition of a catalyst aluminum trichloride promotes the formation of the carbon microsphere, simultaneously, metal hydrated hydroxyl groups are added on the surface of the carbon microsphere, and the addition of tetraethylene amine-free increases amino groups on the surface of the imprinting material, so that the removal capability of the imprinting material on Cu (II) is enhanced. The preparation method is simple and has good effect of removing Cu (II). The invention synthesizes the metal ion imprinting material by taking the carbon microspheres hydrothermally synthesized by glucose as functional monomers and taking Cu (II) as a template, and has the advantages of wide raw material source, environmental friendliness, simple preparation process and easy control of conditions.
Drawings
FIG. 1 is an electron microscope scanning picture of a glucose-based carbon microsphere imprinted material.
FIG. 2 shows the different AlCls in example 33Compared with the effect of removing Cu (II) by the glucose-based carbon microsphere imprinting material prepared by the addition amount of (2).
FIG. 3 is a graph showing the adsorption effect of glucose-based carbon microsphere imprinted material of example 1 on Cu (II) with an initial concentration of 50ml and 100mg/L under different contact time conditions.
Detailed Description
Example 1:
0.02mol/L glucose and 0.01mol/L aluminum chloride were weighed into a small beaker containing about 40ml deionized water. Stirring with glass rod, dissolving, and sealing in steel reactor with PTFE lining. The reaction kettle is put into an oven with the temperature of 160 ℃ for reaction for 20 hours. Washing the reacted product with water, weighing 10ml of tetraethylenepentamine solution and 30ml of copper sulfate solution with the concentration of 1g/L, mixing, pouring into a reaction kettle containing the product, and sealing. And (3) putting the reaction kettle into an oven at 160 ℃ for reaction for 10 h. The obtained sample is continuously soaked and washed by 0.01mol/L sodium hydroxide solution and 0.01mol/L hydrochloric acid until no copper ions can be detected in the washing solution. And finally, washing the sample with deionized water, and drying at the low temperature of 60 ℃ for 20h to obtain the glucose-based carbon microsphere imprinted material. The preparation process is repeated, the difference is that no copper sulfate solution is added during the secondary hydrothermal process, and the finally obtained product is the non-imprinted glucose-based carbon microsphere material.
0.05g of glucose-based carbon microsphere imprinted material and non-imprinted glucose-based carbon microsphere material are respectively added into 50ml of Cu (II) solution with the initial concentration of 100mg/L, the mixture is filtered and separated after being shaken for 24 hours, supernatant is taken, the residual Cu (II) concentration of the solution is measured by adopting a copper ion electrode method, the removal rate of the imprinted material is 99 percent and the removal rate of the non-imprinted material is only 42 percent.
Example 2
0.02mol/L glucose and 0.01mol/L aluminum chloride were weighed into a small beaker containing about 40ml deionized water. Stirring with glass rod, dissolving, and sealing in steel reactor with PTFE lining. And (3) putting the reaction kettle into an oven at 180 ℃ for reaction for 16 h. Washing the reacted product with water, weighing 12ml of tetraethylenepentamine solution and 30ml of copper sulfate solution with the concentration of 1g/L, mixing, pouring into a reaction kettle containing the product, and sealing. And (3) putting the reaction kettle into an oven at 180 ℃ for reaction for 8 hours. The obtained sample is continuously soaked and washed by 0.01mol/L sodium hydroxide solution and 0.01mol/L hydrochloric acid until no copper ions can be detected in the washing solution. And finally, washing the sample with deionized water, and drying at the low temperature of 50 ℃ for 24h to obtain the glucose-based carbon microsphere imprinted material.
Adding 0.05g of glucose-based carbon microsphere imprinted material into 50ml of Cu (II) solution with the initial concentration of 150mg/L, shaking for 24 hours, filtering and separating, taking supernate, measuring the residual Cu (II) concentration of the solution by adopting a copper ion electrode method, and calculating to obtain the removal rate of the imprinted material, wherein the removal rate of the imprinted material is 99%.
Example 3
0.02mol/L glucose and aluminum chloride with certain concentration are weighed and added into a small beaker containing about 40ml deionized water, and the concentrations of the aluminum chloride are 0 mol/L, 0.005 mol/L, 0.01mol/L, 0.02mol/L and 0.03mol/L respectively. Stirring with glass rod, dissolving, and sealing in steel reactor with PTFE lining. The reaction kettle is put into an oven with the temperature of 160 ℃ for reaction for 20 hours. Washing the reacted product with water, weighing 10ml of tetraethylenepentamine solution and 30ml of copper sulfate solution with the concentration of 1g/L, mixing, pouring into a reaction kettle containing the product, and sealing. And (3) putting the reaction kettle into an oven at 160 ℃ for reaction for 10 h. The obtained sample is continuously soaked and washed by 0.01mol/L sodium hydroxide solution and 0.01mol/L hydrochloric acid until no copper ions can be detected in the washing solution. And finally, washing the sample with deionized water, and drying at the low temperature of 50 ℃ for 24h to obtain the glucose-based carbon microsphere imprinted material.
Respectively weighing 0.05g of AlCl3When the addition amount of the glucose-based carbon microsphere imprinting material is different, the glucose-based carbon microsphere imprinting material is added into 50ml of Cu (II) solution with the initial concentration of 200mg/L, the mixture is shaken for 24 hours and then filtered and separated, the supernatant is taken to measure the residual Cu (II) concentration of the solution by adopting a copper ion electrode method, and the result is shown in figure 2, which shows that AlCl3The optimum addition concentration of (2) is 0.01 mol/L.
Example 4
A series of 0.05g of glucose-based carbon microsphere imprinted material of example 1 was added to 50ml of Cu (II) solution with an initial concentration of 100mg/L, the mixture was shaken for different periods of time, centrifuged, filtered, and the supernatant was collected to measure the residual Cu (II) concentration of the solution by a copper ion electrode method, and the removal rate was calculated, as shown in FIG. 3.
Claims (1)
1. A preparation method of a glucose-based carbon microsphere imprinted material is characterized by comprising the following steps of carrying out hydrothermal reaction on a mixed solution of glucose and aluminum trichloride for a certain time to obtain a carbon microsphere, mixing the carbon microsphere with a tetraethylenepentamine solution and a copper sulfate solution, then continuing carrying out the hydrothermal reaction, washing template ions of the obtained carbon microsphere material with a sodium hydroxide solution and a hydrochloric acid solution, and drying at a low temperature to obtain a Cu (II) carbon microsphere imprinted material;
the mass ratio of the glucose to the aluminum trichloride is 1: 2-3: 1, the temperature of the hydrothermal reaction of the glucose and the aluminum trichloride is 160-180 ℃, and the reaction time is 20-22 h;
the volume percentage of the tetraethylenepentamine is 12.5-25% (V/V);
the ratio of the carbon microspheres to the tetraethylenepentamine is 50:1g/L-200: 1g/L, the volume ratio of the tetraethylenepentamine to the copper sulfate solution is 1:2-1:3, and the hydrothermal reaction time is 8-10 h;
the concentration of the copper sulfate solution is 1.0 g/L;
the drying temperature is 45-60 ℃, and the drying time is 20-30 h.
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| CN103623779A (en) * | 2013-12-06 | 2014-03-12 | 河北工业大学 | Hydrophilic functional carbon sphere and application thereof for removing heavy metal ions in waste water |
| CN104587969A (en) * | 2015-02-03 | 2015-05-06 | 吉林大学 | Preparation method of carbon-base adsorbing material capable of selectively adsorbing copper ions |
| CN105582888A (en) * | 2016-01-21 | 2016-05-18 | 西南科技大学 | Method for preparing carbon microsphere adsorbent under catalysis of metal salt with low-temperature hydrothermal method |
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| CN103623779A (en) * | 2013-12-06 | 2014-03-12 | 河北工业大学 | Hydrophilic functional carbon sphere and application thereof for removing heavy metal ions in waste water |
| CN104587969A (en) * | 2015-02-03 | 2015-05-06 | 吉林大学 | Preparation method of carbon-base adsorbing material capable of selectively adsorbing copper ions |
| CN105582888A (en) * | 2016-01-21 | 2016-05-18 | 西南科技大学 | Method for preparing carbon microsphere adsorbent under catalysis of metal salt with low-temperature hydrothermal method |
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