CN108160049B - Modified corn husk adsorbent for adsorbing gold ions and preparation method and application thereof - Google Patents
Modified corn husk adsorbent for adsorbing gold ions and preparation method and application thereof Download PDFInfo
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
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Abstract
The invention relates to a modified corn husk adsorbent for adsorbing gold ions, a preparation method and application thereof, and belongs to the technical field of adsorbent preparation. Drying and crushing corn husks, adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 10-24 hours at the temperature of 80-100 ℃ under the stirring condition, washing a reaction product to be neutral by using water, drying and grinding the reaction product to obtain a product CCB; adding the product CCB and chloroacetyl chloride into N, N-dimethylformamide, reacting for 10-24 h at the temperature of 90-110 ℃ under the stirring condition, then sequentially washing with the N, N-dimethylformamide and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain the product CC-CCB; adding the product CC-CCB, potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 10-24 h AT the temperature of 80-100 ℃ under the stirring condition, then washing with tetrahydrofuran and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain the modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB. The modified corn husk adsorbent can be used for adsorbing gold ions.
Description
Technical Field
The invention relates to a modified corn husk adsorbent for adsorbing gold ions, a preparation method and application thereof, and belongs to the technical field of adsorbent preparation.
Background
Corn husks are agricultural and forestry wastes, and are usually destroyed by burning in the harvest season, so that the resources are seriously wasted, and meanwhile, the environment is greatly polluted. Gold is a precious metal used for catalysts, alloys, electroplating and various contact materials, has unique physical and chemical properties, is widely applied to a plurality of fields such as microelectronic technology, chemical industry, aviation manufacturing, metallurgical industry and the like, and plays a key and core role in advanced science and modern industry such as petrochemical industry, environmental science, electrical engineering, national defense and the like. Gold in nature is generally of low grade and associated with other elements. With the increasing emphasis on environmental protection and the decreasing of gold resources, the demand of metallic gold is rapidly increasing. In the face of sustainable utilization of resources and the price of metal gold is increased, and the great economic benefit and social benefit are achieved by separating and recovering gold from various gold-containing wastes and waste liquids. Adsorption separation enrichment methods are gradually gaining attention due to the characteristics of simple operation, good selectivity and the like. The adsorbents which are widely applied at present comprise modified nano silicon dioxide, activated carbon, chelating resin and the like.
At present, no adsorbent adopting corn husks as gold ions exists.
Disclosure of Invention
The invention provides a modified corn husk adsorbent for adsorbing gold ions and a preparation method and application thereof, aiming at the problems of the existing gold ion adsorbent technology, and the chemical structural formula of the modified corn husk adsorbent for adsorbing gold ions is shown in the specification
Wherein B is
The invention also aims to provide a preparation method of the modified corn husk adsorbent for adsorbing gold ions, which comprises the following specific steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 10-24 hours at the temperature of 80-100 ℃ under the stirring condition, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB;
(2) adding the CCB and chloroacetyl chloride obtained in the step (1) into N, N-dimethylformamide, reacting for 10-24 h at the temperature of 90-110 ℃ under the stirring condition, then washing with the N, N-dimethylformamide and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a CC-CCB product; the specific synthetic route is as follows:
(3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 10-24 h AT the temperature of 80-100 ℃ under the stirring condition, then washing with tetrahydrofuran and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB; the specific synthetic route is as follows:
the liquid-solid ratio mL of the concentrated sulfuric acid to the corn husks in the step (1) is (5-10) to 1;
the concentrated sulfuric acid in the step (1) is a commercially available concentrated sulfuric acid;
in the step (2), the liquid-solid ratio mL of N, N-dimethylformamide to the product CCB is (8-15) to 1, and the volume ratio of chloroacetyl chloride to N, N-dimethylformamide is (8-15) to 1;
in the step (3), the mass ratio of the 2-aminothiazole to the potassium carbonate is (0.8-1.2) to 1, the liquid-solid ratio mL of the tetrahydrofuran to the 2-aminothiazole is (30-40) to 1, and the liquid-solid ratio mL of the tetrahydrofuran to the product CC-CCB is (15-25) to 1;
the modified corn husk adsorbent for adsorbing gold ions is applied as a gold ion adsorbent.
The invention has the beneficial effects that:
(1) the modified corn husk adsorbent for adsorbing gold ions has high adsorption rate on gold ions;
(2) the raw materials of the method are cheap and easy to synthesize;
(3) the modified corn husk adsorbent is nontoxic and harmless, has stable performance, is easy to separate and can be repeatedly used, does not cause secondary pollution to the environment, and simultaneously realizes comprehensive utilization of resources;
(4) the modified corn husk adsorbent has good application and economic value.
Drawings
FIG. 1 is an infrared spectrum of CCB, CC-CCB and AT-CCB of example 1;
in the figure: a is product CCB, b is product CC-CCB, and c is product AT-CCB.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of a modified corn husk adsorbent for adsorbing gold ions comprises the following specific steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 15 hours at the temperature of 90 ℃ under the stirring condition, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB; wherein the liquid-solid ratio mL/g of concentrated sulfuric acid to corn husks is 5: 1;
(2) adding the product CCB obtained in the step (1) and chloroacetyl chloride into N, N-dimethylformamide, reacting for 24 hours at the temperature of 100 ℃ under the stirring condition, then sequentially washing with the N, N-dimethylformamide and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a product CC-CCB; wherein the liquid-solid ratio mL/g of the N, N-dimethylformamide to the product CCB is 8:1, and the volume ratio of the chloroacetyl chloride to the N, N-dimethylformamide is 8: 1; the specific synthetic route is as follows:
(3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 24 hours AT the temperature of 90 ℃ under the condition of stirring, then sequentially washing with tetrahydrofuran and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB; wherein the mass ratio of the 2-aminothiazole to the potassium carbonate is 0.8:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the 2-aminothiazole is 30:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the product CC-CCB is 15:1, and the specific synthetic route is as follows:
the infrared spectra of the product CCB, the product CC-CCB and the product AT-CCB of this example are shown in FIG. 1 (a is the product CCB, b is the product CC-CCB, and c is the product AT-CCB), 1636, 2924 and 3425cm in FIG. 1-1Respectively judging the positions of the peaks as C, C-H and O-H; in the chloroacetyl chloride-modified product CC-CCB at 794cm-1A new peak appears, and the peak is a stretching vibration peak of C-Cl; AT 2-aminothiazole-modified AT-CCB, AT 2360 and 874cm-1Peaks appearing in (A) belong to S-H and-NH2Of (2) at the same time, 1030 and 669cm-1Characteristic peaks belonging to C-S; in addition, 3425,1636 and 1384cm-1The weakening of the intensity of the characteristic peak also indicates that the 2-aminothiazole is successfully grafted on the product CCB;
and (3) testing the performance of adsorbing gold ions:
10mg of AT-CCB adsorbent is put into a gold ion solution with the initial concentration of 400mg/L for shaking adsorption for 7h, the adsorbent is centrifugally separated, the concentration of the residual gold ions in the filtrate is determined to be 14.88mg/L by ICP-OES, and the adsorption rate is 96.28%. The adsorbent having adsorbed gold ions was washed in EDTA (10 wt%) at pH 10 for 4h with stirring, then 3 times with distilled water, and finally the adsorbent was dried under vacuum at 70 ℃ for 8 h. Adding 10mg of the adsorbent into a gold ion solution with the initial concentration of 400mg/L, performing vibration adsorption for 7 hours, performing centrifugal separation on the adsorbent, and measuring the concentration of the residual gold ions in the filtrate to be 17.12mg/L by using ICP-OES, wherein the adsorption rate is 95.72%; the modified corn husk adsorbent AT-CCB of the example is used for adsorbing gold ions and can be recycled.
Example 2: a preparation method of a modified corn husk adsorbent for adsorbing gold ions comprises the following specific steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 24 hours at the temperature of 80 ℃ under the condition of stirring, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB; wherein the liquid-solid ratio mL/g of concentrated sulfuric acid to corn husks is 8: 1;
(2) adding the product CCB obtained in the step (1) and chloroacetyl chloride into N, N-dimethylformamide, reacting for 10 hours at the temperature of 110 ℃ under the stirring condition, then sequentially washing with the N, N-dimethylformamide and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a product CC-CCB; wherein the liquid-solid ratio mL/g of the N, N-dimethylformamide to the product CCB is 11:1, and the volume ratio of the chloroacetyl chloride to the N, N-dimethylformamide is 11: 1; the specific synthetic route is as follows:
(3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 10 hours AT the temperature of 100 ℃ under the condition of stirring, then sequentially washing with tetrahydrofuran and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB; wherein the mass ratio of the 2-aminothiazole to the potassium carbonate is 1:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the 2-aminothiazole is 35:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the product CC-CCB is 20:1, and the specific synthetic route is as follows:
and (3) testing the performance of adsorbing gold ions:
10mg of AT-CCB adsorbent is put into a gold ion solution with the initial concentration of 400mg/L for oscillation adsorption for 7h, the adsorbent is centrifugally separated, the concentration of the residual gold ions in the filtrate is measured to be 11.05mg/L by ICP-OES, and the adsorption rate is 97.24%; stirring and washing the adsorbent adsorbing gold ions in EDTA (10 wt%) with pH of 10 for 4h, then washing with distilled water for 3 times, and finally vacuum-drying the adsorbent at 70 ℃ for 8 h; adding 10mg of the adsorbent into a gold ion solution with the initial concentration of 400mg/L, oscillating and adsorbing for 7h, centrifuging and separating the adsorbent, and measuring the concentration of the residual gold ions in the filtrate to be 15.28mg/L by using ICP-OES, wherein the adsorption rate is 96.18%; the modified corn husk adsorbent AT-CCB of the example is used for adsorbing gold ions and can be recycled.
Example 3: a preparation method of a modified corn husk adsorbent for adsorbing gold ions comprises the following specific steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 10 hours at the temperature of 100 ℃ under the condition of stirring, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB; wherein the liquid-solid ratio mL/g of concentrated sulfuric acid to corn husks is 10: 1;
(2) adding the product CCB obtained in the step (1) and chloroacetyl chloride into N, N-dimethylformamide, reacting for 16h at the temperature of 90 ℃ under the stirring condition, then sequentially washing with the N, N-dimethylformamide and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a product CC-CCB; wherein the liquid-solid ratio mL/g of the N, N-dimethylformamide to the product CCB is 15:1, and the volume ratio of the chloroacetyl chloride to the N, N-dimethylformamide is 15: 1; the specific synthetic route is as follows:
(3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 15 hours AT the temperature of 80 ℃ under the condition of stirring, then sequentially washing with tetrahydrofuran and distilled water, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB; wherein the mass ratio of the 2-aminothiazole to the potassium carbonate is 1.2:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the 2-aminothiazole is 40:1, the liquid-solid ratio mL: g of the tetrahydrofuran to the product CC-CCB is 25:1, and the specific synthetic route is as follows:
and (3) testing the performance of adsorbing gold ions:
10mg of AT-CCB adsorbent is put into a gold ion solution with the initial concentration of 400mg/L for shaking adsorption for 7h, the adsorbent is centrifugally separated, the concentration of the residual gold ions in the filtrate is measured by ICP-OES to be 8.26mg/L, and the adsorption rate is 97.94%. The adsorbent having adsorbed gold ions was washed in EDTA (10 wt%) at pH 10 for 4h with stirring, then 3 times with distilled water, and finally the adsorbent was dried under vacuum at 70 ℃ for 8 h. Adding 10mg of the adsorbent into a gold ion solution with the initial concentration of 400mg/L, performing vibration adsorption for 7 hours, performing centrifugal separation on the adsorbent, and measuring the concentration of the residual gold ions in the filtrate to be 12.68mg/L by using ICP-OES, wherein the adsorption rate is 96.83%; the modified corn husk adsorbent AT-CCB of the example is used for adsorbing gold ions and can be recycled.
Claims (6)
1. A modified corn husk adsorbent for adsorbing gold ions, which is characterized in that: has a chemical structural formula of
Wherein B is
；
The preparation method of the modified corn husk adsorbent comprises the following specific steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 10-24 hours at the temperature of 80-100 ℃ under the stirring condition, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB;
(2) adding the CCB and chloroacetyl chloride obtained in the step (1) into N, N-dimethylformamide, reacting for 10-24 h at the temperature of 90-110 ℃ under the stirring condition, then washing with the N, N-dimethylformamide and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a CC-CCB product;
(3) and (3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 10-24 h AT the temperature of 80-100 ℃ under the stirring condition, then washing with tetrahydrofuran and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain the modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB.
2. The preparation method of the modified corn husk adsorbent for adsorbing gold ions as claimed in claim 1, characterized by comprising the following steps:
(1) drying and crushing corn husks, then adding the crushed corn husks into concentrated sulfuric acid, reacting and carbonizing for 10-24 hours at the temperature of 80-100 ℃ under the stirring condition, washing a reaction product to be neutral by using water, drying and grinding the reaction product into powder to obtain a product CCB;
(2) adding the CCB and chloroacetyl chloride obtained in the step (1) into N, N-dimethylformamide, reacting for 10-24 h at the temperature of 90-110 ℃ under the stirring condition, then washing with the N, N-dimethylformamide and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a CC-CCB product; the specific synthetic route is as follows:
(3) adding the product CC-CCB obtained in the step (2), potassium carbonate and 2-aminothiazole into a tetrahydrofuran solution, reacting for 10-24 h AT the temperature of 80-100 ℃ under the stirring condition, then washing with tetrahydrofuran and distilled water in sequence, carrying out solid-liquid separation, and drying the solid in vacuum to obtain a modified corn husk adsorbent for adsorbing gold ions, wherein the label is AT-CCB; the specific synthetic route is as follows:
3. the method for preparing the modified corn husk adsorbent for adsorbing gold ions according to claim 2, wherein: in the step (1), the liquid-solid ratio mL of the concentrated sulfuric acid to the corn husks is (5-10) to 1.
4. The method for preparing the modified corn husk adsorbent for adsorbing gold ions according to claim 2, wherein: in the step (2), the liquid-solid ratio mL of the N, N-dimethylformamide to the product CCB is (8-15) to 1, and the volume ratio of the chloroacetyl chloride to the N, N-dimethylformamide is (8-15) to 1.
5. The method for preparing the modified corn husk adsorbent for adsorbing gold ions according to claim 2, wherein: in the step (3), the mass ratio of the 2-aminothiazole to the potassium carbonate is (0.8-1.2): 1, the liquid-solid ratio mL of the tetrahydrofuran to the 2-aminothiazole is (30-40): 1, and the liquid-solid ratio mL of the tetrahydrofuran to the product CC-CCB is (15-25): 1.
6. Use of the modified corn husk adsorbent for adsorbing gold ions according to claim 1 as gold ion adsorbent.
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| CN110841598A (en) * | 2019-11-15 | 2020-02-28 | 昆明理工大学 | Preparation method and application of synthetic metal organic framework adsorbent |
| CN110813248B (en) * | 2019-11-17 | 2023-01-17 | 中山大学 | O-dihydroxybenzaldehyde modified shaddock peel adsorbent and preparation method and application thereof |
| CN110975836B (en) * | 2019-12-23 | 2023-01-17 | 中山大学 | Pomelo peel adsorbent modified by 3-amino-5-mercapto-1, 2, 4-triazole and preparation method and application thereof |
| CN111001392A (en) * | 2019-12-30 | 2020-04-14 | 中山大学 | Preparation method and application of modified zirconium-based metal organic framework adsorbent for gold ion adsorption |
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