CN105170119A - Preparation method of typha gypsum powder composite material for enriching iridium ions in tailing wastewater - Google Patents
Preparation method of typha gypsum powder composite material for enriching iridium ions in tailing wastewater Download PDFInfo
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- CN105170119A CN105170119A CN201510633726.3A CN201510633726A CN105170119A CN 105170119 A CN105170119 A CN 105170119A CN 201510633726 A CN201510633726 A CN 201510633726A CN 105170119 A CN105170119 A CN 105170119A
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- cattail
- typha
- gypsum powder
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- iridium
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Abstract
The invention belongs to the field of composite materials and relates to a preparation method of a typha gypsum powder composite material for enriching iridium ions in tailing wastewater. According to the preparation method, modified gypsum powder is composited to porous channels of ammoniated typha, and a specific process comprises steps of typha cleaning, ammoniation, gypsum powder modification, composite material preparation and the like. The prepared typha gypsum powder composite material has the advantages as follows: (1), the gypsum powder is fixed to typha by the aid of polyvinyl acetate, so that the characteristics of low density and large specific surface area of the typha can be played, and the advantage that the gypsum powder has high enrichment capacity on the iridium ions of rare earth can be utilized; (2), compared with the gypsum powder, the composite material solves the problems of caking of the gypsum powder and reduction of iridium ion enrichment capacity, and can further solve the problem of secondary pollution caused by the fact that the gypsum powder for enriching the iridium ions is difficult to recover; (3), compared with the typha, the composite material increases the iridium ion saturation enrichment quantity greatly and can avoid overflow pollution of organic carbon of the typha in a water treatment process. The iridium ion enrichment quantity of the prepared composite material is increased to 142.8 mg/g, and the composite material can be applied to iridium-containing wastewater treatment of tailings and has a broad market prospect.
Description
Technical field
The invention belongs to technical field of composite materials, be specifically related to the preparation method of the cattail land plaster composite of iridium ion in a kind of enrichment mine tailing wastewater.
Background technology
Rare earth has the title of industry " gold ", and have the physical characteristics such as excellent photoelectromagnetic due to it, new material that can be different, various in style with other materials component property, its most significant function is exactly the quality and performance increasing substantially other products.Such as increase substantially the tactical qualities for the manufacture of the steel of tank, aircraft, guided missile, aluminium alloy, magnesium alloy, titanium alloy.And rare earth is many high-tech lubricants such as electronics, laser, nuclear industry, superconduction equally.With the molecular sieve catalyst that rare earth is made, there is active high, selective good, advantage that preventing from heavy metal poisoning capability is strong, thus instead of alumina silicate catalyst for petroleum catalytic cracking process; In production of synthetic ammonia, be co-catalyst with a small amount of nitric acid rare earth, it processes larger than nickel-alumina catalyst 1.5 times of tolerance; In synthesis butadiene rubber and isoprene rubber process, adopt naphthenic acid rare earth-triisobutyl aluminium profiles catalyst, the properties of product obtained are excellent, have equipment kiss-coating few, and running is stable, the advantages such as postprocessing working procedures is short; Composite rare-earth oxide can also be used as catalyst for purifying internal combustion engine tail gas, and cerium naphthenate also can be used as paint drier etc.
The application of rare earth luminescent material can bring the good and long-life effect of environmental protection and energy saving, color color developing to light source, the update of the display field product that is conducive to promoting throwing light on.At present, the trend that China's rare earth luminescent material industry is researched and developed immediately following international rare earth luminescent material and applied, and establish good market interaction mechanism between downstream industry, become basic material indispensable in energy-saving illumination and Electronic Development of Information Industry process.Except above-mentioned field, rare earth luminescent material is also widely used in Promoting plant growth, ultraviolet disinfection, health care, noctilucence display and the special source such as full spectrum light source of simulating nature light and the production of equipment, and application is constantly expanded.Iridium fluor-complex itself has charge transport ability, and organic EL Material " iridium fluor-complex ", can not be luminous under the environment of the oxygen concentration identical with air about 20% under the irradiation of special light, concentration lower than 10% time then can be luminous.
Creativeness of the present invention is: (1) cattail land plaster composite is a kind of advanced composite material (ACM), huge as rare-earth enrichment material function potentiality to be exploited; (2) be fixed in ammonification cattail by modified landplaster with polyvinyl acetate, the preparation technology preparing cattail land plaster composite has no bibliographical information; (3) compared with land plaster, or cattail adsorption and enrichment material is compared, and the performance such as physical aspect, the structure of matter, rare-earth enrichment amount, recycling utilization of composite all possesses outstanding substantive distinguishing features and progress significantly.
Summary of the invention
The invention belongs to field of compound material, relate to the preparation method of the cattail land plaster composite of iridium ion in a kind of enrichment mine tailing wastewater.Modified landplaster is compound in the duct of ammonification cattail by the preparation method that the present invention proposes, and concrete technology comprises that cattail is cleaned, prepared by ammonification, land plaster modification and composite.Cattail land plaster composite prepared by the present invention has the following advantages: land plaster is fixed in cattail with polyvinyl acetate by (1), the characteristic that cattail density is light, specific area is large can be played, the advantage that land plaster is strong to rare earth iridium ion accumulation ability can be make use of again; (2) compared with gypsum powder, the problem that composite avoids land plaster reunion caking, iridium ion enrichment power reduces, can avoid again the land plaster of enrichment iridium ion to be difficult to reclaim, cause the problem of secondary pollution; (3) compared with cattail, composite significantly improves the saturated enriching quantity of iridium ion, and the spilling of cattail organic carbon in water treatment procedure can be avoided again to pollute.The enriching quantity of iridium ion is promoted to 142.8mg/g by composite, and namely every gram of composite can enrichment 142.8mg iridium ion.Iridium ion enrichment material prepared by the present invention can be used for mine tailing containing iridium wastewater treatment, wide market.
The preparation method of the cattail land plaster composite that the present invention proposes, is characterized in that:
1) clean cattail: by cattail rinsing, oven dry;
2) cattail ammonification: the cattail after clean is placed in ammoniated solution, places 3 hours in 60 DEG C, rinsing, oven dry; Wherein the formula of ammoniated solution is solvent is deionized water, and in solution, various solute concentration is respectively: dibastic sodium phosphate concentration 3 ~ 6g/L, ammonium bicarbonate concentration 3 ~ 6g/L, 1,3-propane diamine concentration 3 ~ 6g/L, ammonia concn 1 ~ 3g/L;
3) land plaster modification: land plaster is placed in cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filters, and in 100 DEG C of dryings 3 ~ 12 hours, cooling, spent deionized water, dry, obtained the land plaster of modification; Wherein material/the liquor ratio of land plaster and cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed solution is 1/5 ~ 1/20g/mL; In wherein cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, the mass concentration of cetyl benzenesulfonic acid is 20 ~ 30%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.1 ~ 0.3%;
4) composite preparation: polyvinyl acetate is dissolved in oxolane, adds ammonification cattail and modified landplaster successively, stir 1 ~ 4 hour, be placed in drying box, in 40 ~ 60 DEG C of dryings 12 hours, obtain cattail land plaster composite; Wherein the weight ratio of various material is: ammonification cattail/modified landplaster/polyvinyl acetate/oxolane=2/1/2/5.
Be placed in containing iridium mine tailing wastewater by cattail land plaster composite, regulate solution ph to be 5 ~ 6, in 25 DEG C of enrichments 4 hours, in waste water, the concentration of iridium ion was 50 ~ 500mg/L, and enrichment is complete, filtered, and detected the iridium ion amount of enrichment in composite.
The composite of above-mentioned enrichment iridium ion is placed in the ammoniacal liquor tetraacethyl disodium aqueous solution 1 hour that concentration is 0.2M, filters, clean, dry, complete solution process of enriching, obtain the cattail land plaster composite of regeneration; Again above-mentioned regenerated composite material is placed in containing iridium mine tailing wastewater, carries out iridium ion enrichment.Multiple circulation like this, until the iridium ion enriching quantity of composite is less than 80% of first enriching quantity.
Detailed description of the invention
The invention is further illustrated by the following examples
embodiment 1
Cattail is gathered in, cleans with running water, dry.
Be dissolved in deionized water by dibastic sodium phosphate, carbonic hydroammonium, 1,3-propane diamine, ammoniacal liquor, dibastic sodium phosphate concentration is 5g/L, and ammonium bicarbonate concentration is 4g/L, 1,3-propane diamine concentration is 4g/L, and ammonia concn is 3g/L, obtains ammoniated solution.
The cattail that 10g cleans is placed in 500mL ammoniated solution, and place 3 hours in 60 DEG C, rinsing, oven dry, obtain the cattail of ammonification.
Be dissolved in deionized water by cetyl benzenesulfonic acid, tetramethyl ammonium hydrogen sulfate, the mass concentration of cetyl benzenesulfonic acid is 28%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.3%, obtains cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution.
100g land plaster is placed in 1500mL cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filter, in 100 DEG C of dryings 5 hours, cooling, spent deionized water, dry, obtained the land plaster of modification.
10g polyvinyl acetate is dissolved in 25g oxolane, adds 10g ammonification cattail and 5g modified landplaster successively, stir 2 hours, be placed in drying box, in 40 DEG C of dryings 12 hours, obtain cattail land plaster composite.
20g cattail land plaster composite is placed in 50L containing iridium mine tailing wastewater, regulates solution ph to be 5 ~ 6, in 25 DEG C of enrichments 4 hours, in waste water, the concentration of iridium ion is 160mg/L, enrichment is complete, filters, and the iridium ion amount detecting composite enrichment is 142.8mg/g.
The composite of above-mentioned enrichment iridium ion is placed in the ammoniacal liquor tetraacethyl disodium aqueous solution 1 hour that concentration is 0.2M, filters, clean, dry, complete solution process of enriching, obtain the cattail land plaster composite of regeneration; Again above-mentioned regenerated composite material is placed in containing iridium mine tailing wastewater, carries out iridium ion enrichment.6 circulations like this, the iridium ion enriching quantity of composite is less than 80% of first enriching quantity.
embodiment 2
Cattail is gathered in, cleans with running water, dry.
Be dissolved in deionized water by dibastic sodium phosphate, carbonic hydroammonium, 1,3-propane diamine, ammoniacal liquor, dibastic sodium phosphate concentration is 6g/L, and ammonium bicarbonate concentration is 6g/L, 1,3-propane diamine concentration is 3g/L, and ammonia concn is 3g/L, obtains ammoniated solution.
The cattail that 50g cleans is placed in 500mL ammoniated solution, and place 3 hours in 60 DEG C, rinsing, oven dry, obtain the cattail of ammonification.
Be dissolved in deionized water by cetyl benzenesulfonic acid, tetramethyl ammonium hydrogen sulfate, the mass concentration of cetyl benzenesulfonic acid is 30%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.1%, obtains cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution.
100g land plaster is placed in 2000mL cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filter, in 100 DEG C of dryings 12 hours, cooling, spent deionized water, dry, obtained the land plaster of modification.
200g polyvinyl acetate is dissolved in 500g oxolane, adds 200g ammonification cattail and 100g modified landplaster successively, stir 4 hours, be placed in drying box, in 40 DEG C of dryings 12 hours, obtain cattail land plaster composite.
10g cattail land plaster composite is placed in 100L containing iridium mine tailing wastewater, regulates solution ph to be 5 ~ 6, in 25 DEG C of enrichments 4 hours, in waste water, the concentration of iridium ion is 50mg/L, enrichment is complete, filters, and the iridium ion amount detecting composite enrichment is 133.1mg/g.
The composite of above-mentioned enrichment iridium ion is placed in the ammoniacal liquor tetraacethyl disodium aqueous solution 1 hour that concentration is 0.2M, filters, clean, dry, complete solution process of enriching, obtain the cattail land plaster composite of regeneration; Again above-mentioned regenerated composite material is placed in containing iridium mine tailing wastewater, carries out iridium ion enrichment.6 circulations like this, the iridium ion enriching quantity of composite is less than 80% of first enriching quantity.
embodiment 3
Cattail is gathered in, cleans with running water, dry.
Be dissolved in deionized water by dibastic sodium phosphate, carbonic hydroammonium, 1,3-propane diamine, ammoniacal liquor, dibastic sodium phosphate concentration is 4g/L, and ammonium bicarbonate concentration is 5g/L, 1,3-propane diamine concentration is 5g/L, and ammonia concn is 2g/L, obtains ammoniated solution.
The cattail that 100g cleans is placed in 500mL ammoniated solution, and place 3 hours in 60 DEG C, rinsing, oven dry, obtain the cattail of ammonification.
Be dissolved in deionized water by cetyl benzenesulfonic acid, tetramethyl ammonium hydrogen sulfate, the mass concentration of cetyl benzenesulfonic acid is 25%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.2%, obtains cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution.
100g land plaster is placed in 1000mL cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filter, in 100 DEG C of dryings 4 hours, cooling, spent deionized water, dry, obtained the land plaster of modification.
100g polyvinyl acetate is dissolved in 250g oxolane, adds 100g ammonification cattail and 50g modified landplaster successively, stir 3 hours, be placed in drying box, in 50 DEG C of dryings 12 hours, obtain cattail land plaster composite.
20g cattail land plaster composite is placed in 10L containing iridium mine tailing wastewater, regulates solution ph to be 5 ~ 6, in 25 DEG C of enrichments 4 hours, in waste water, the concentration of iridium ion is 500mg/L, enrichment is complete, filters, and the iridium ion amount detecting composite enrichment is 109.1mg/g.
The composite of above-mentioned enrichment iridium ion is placed in the ammoniacal liquor tetraacethyl disodium aqueous solution 1 hour that concentration is 0.2M, filters, clean, dry, complete solution process of enriching, obtain the cattail land plaster composite of regeneration; Again above-mentioned regenerated composite material is placed in containing iridium mine tailing wastewater, carries out iridium ion enrichment.6 circulations like this, the iridium ion enriching quantity of composite is less than 80% of first enriching quantity.
embodiment 4
Cattail is gathered in, cleans with running water, dry.
Be dissolved in deionized water by dibastic sodium phosphate, carbonic hydroammonium, 1,3-propane diamine, ammoniacal liquor, dibastic sodium phosphate concentration is 3g/L, and ammonium bicarbonate concentration is 3g/L, 1,3-propane diamine concentration is 6g/L, and ammonia concn is 1g/L, obtains ammoniated solution.
The cattail that 50g cleans is placed in 500mL ammoniated solution, and place 3 hours in 60 DEG C, rinsing, oven dry, obtain the cattail of ammonification.
Be dissolved in deionized water by cetyl benzenesulfonic acid, tetramethyl ammonium hydrogen sulfate, the mass concentration of cetyl benzenesulfonic acid is 20%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.3%, obtains cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution.
100g land plaster is placed in 500mL cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filter, in 100 DEG C of dryings 3 hours, cooling, spent deionized water, dry, obtained the land plaster of modification.
20g polyvinyl acetate is dissolved in 50g oxolane, adds 20g ammonification cattail and 10g modified landplaster successively, stir 1 hour, be placed in drying box, in 60 DEG C of dryings 12 hours, obtain cattail land plaster composite.
100g cattail land plaster composite is placed in 100L containing iridium mine tailing wastewater, regulates solution ph to be 5 ~ 6, in 25 DEG C of enrichments 4 hours, in waste water, the concentration of iridium ion is 50mg/L, enrichment is complete, filters, and the iridium ion amount detecting composite enrichment is 40.1mg/g.
The composite of above-mentioned enrichment iridium ion is placed in the ammoniacal liquor tetraacethyl disodium aqueous solution 1 hour that concentration is 0.2M, filters, clean, dry, complete solution process of enriching, obtain the cattail land plaster composite of regeneration; Again above-mentioned regenerated composite material is placed in containing iridium mine tailing wastewater, carries out iridium ion enrichment.6 circulations like this, the iridium ion enriching quantity of composite is less than 80% of first enriching quantity.
Claims (1)
1. the preparation method of the cattail land plaster composite of iridium ion in enrichment mine tailing wastewater, is characterized in that:
1) clean cattail: by cattail rinsing, oven dry;
2) cattail ammonification: the cattail after clean is placed in ammoniated solution, places 3 hours in 60 DEG C, rinsing, oven dry; Wherein the formula of ammoniated solution is solvent is deionized water, and in solution, various solute concentration is respectively: dibastic sodium phosphate concentration 3 ~ 6g/L, ammonium bicarbonate concentration 3 ~ 6g/L, 1,3-propane diamine concentration 3 ~ 6g/L, ammonia concn 1 ~ 3g/L;
3) land plaster modification: land plaster is placed in cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, stirs 1 hour, filters, and in 100 DEG C of dryings 3 ~ 12 hours, cooling, spent deionized water, dry, obtained the land plaster of modification; Wherein material/the liquor ratio of land plaster and cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed solution is 1/5 ~ 1/20g/mL; In wherein cetyl benzenesulfonic acid/tetramethyl ammonium hydrogen sulfate mixed aqueous solution, the mass concentration of cetyl benzenesulfonic acid is 20 ~ 30%, and the mass concentration of tetramethyl ammonium hydrogen sulfate is 0.1 ~ 0.3%;
4) composite preparation: be dissolved in by polyvinyl acetate in oxolane, add ammonification cattail and modified landplaster successively, stir 1 ~ 4 hour, mixture is placed in drying box, in 40 ~ 60 DEG C of dryings 12 hours, obtains cattail land plaster composite; Wherein the weight ratio of various material is: ammonification cattail/modified landplaster/polyvinyl acetate/oxolane=2/1/2/5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453705A (en) * | 2020-05-29 | 2020-07-28 | 盛隆资源再生（无锡）有限公司 | Method for treating high-COD waste sulfuric acid by using modified gypsum |
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| EP2410104A2 (en) * | 2010-07-20 | 2012-01-25 | Ghj Beteiligungs Gmbh | Structural board |
| CN102989425A (en) * | 2012-12-04 | 2013-03-27 | 复旦大学 | Preparation method and application of water treatment material based on typha orientalis presl |
| CN103320620A (en) * | 2013-07-01 | 2013-09-25 | 金川集团股份有限公司 | Method for efficiently enriching gold and platinum group metals from complex low-grade rhodium iridium residues |
| CN104383882A (en) * | 2014-11-06 | 2015-03-04 | 昆明理工大学 | Method for preparing heavy metal chromium adsorbent and application thereof |
| CN104437389A (en) * | 2014-11-27 | 2015-03-25 | 昆明理工大学 | Preparation method and application of adsorbent for treating lead-containing waste water |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2410104A2 (en) * | 2010-07-20 | 2012-01-25 | Ghj Beteiligungs Gmbh | Structural board |
| CN102989425A (en) * | 2012-12-04 | 2013-03-27 | 复旦大学 | Preparation method and application of water treatment material based on typha orientalis presl |
| CN103320620A (en) * | 2013-07-01 | 2013-09-25 | 金川集团股份有限公司 | Method for efficiently enriching gold and platinum group metals from complex low-grade rhodium iridium residues |
| CN104383882A (en) * | 2014-11-06 | 2015-03-04 | 昆明理工大学 | Method for preparing heavy metal chromium adsorbent and application thereof |
| CN104437389A (en) * | 2014-11-27 | 2015-03-25 | 昆明理工大学 | Preparation method and application of adsorbent for treating lead-containing waste water |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111453705A (en) * | 2020-05-29 | 2020-07-28 | 盛隆资源再生（无锡）有限公司 | Method for treating high-COD waste sulfuric acid by using modified gypsum |
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