CN105597704A - Preparation method of silica-gel powder composite material for enrichment of palladium ions in electroplating wastewater - Google Patents
Preparation method of silica-gel powder composite material for enrichment of palladium ions in electroplating wastewater Download PDFInfo
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- CN105597704A CN105597704A CN201510633494.1A CN201510633494A CN105597704A CN 105597704 A CN105597704 A CN 105597704A CN 201510633494 A CN201510633494 A CN 201510633494A CN 105597704 A CN105597704 A CN 105597704A
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Abstract
Belonging to the field of water treatment materials, the invention relates to a preparation method of a silica-gel powder composite material for enrichment of palladium ions in electroplating wastewater. According to the preparation method put forward by the invention, modification silica-gel powder is compounded into the pore channels of ammoniated cotton straws, and the specific process consists of cotton straw cleaning, ammoniation, silica-gel powder modification and composite material preparation, etc. The cotton straw silica-gel powder composite material prepared by the method provided by the invention has the advantages that: (1) polyurethane is employed to fix silica-gel powder into cotton straws, thereby giving play to the characteristics of small density and large specific surface area of cotton straws, and also utilizing the advantage of silica-gel powder's strong enrichment capacity to heavy metal palladium ions; (2) compared with silica-gel powder, the composite material avoids the problems of silica-gel powder agglomeration and palladium ion enrichment capacity reduction, also avoids the problems that palladium ion enriched silica-gel powder is difficult to recover and can cause secondary pollution; and (3) compared with cotton straws, the composite material greatly improves the palladium ion saturation enrichment amount, and also can avoid the overflow pollution of cotton straw organic carbon in a water treatment process. The composite material prepared by the method provided by the invention can increase the enrichment amount of palladium ions to 103.4mg/g, can be used for treatment of palladium-containing wastewater in electroplating factories, and has broad market prospects.
Description
Technical field
The invention belongs to material for water treatment technical field, be specifically related to the silica white of palladium ion in a kind of enrichment electroplating wastewaterThe preparation method of composite.
Background technology
Electroplating (Electroplating) utilizes electrolysis principle on some metal surface, to plate other gold of skimBelong to or the process of alloy, be utilize electrolysis make metal or other material product surface attachment layer of metal film technique fromPrevent burning (as corrosion) and play, improve wearability, electric conductivity, reflective, corrosion resistance (copper sulphate etc.) and promoteGrade attractive in appearance effect. When plating, coated metal or other insoluble materials do anode, and workpiece to be plated does negative electrode, coated metalCation is reduced formation coating at surface of the work to be plated. For getting rid of other cationic interference, and make coating evenly, firmly,Need be with cooking electroplate liquid containing the cationic solution of coated metal, to keep the cationic concentration of coated metal constant. The object of electroplatingBe on base material, to plate the coat of metal, change substrate surface character or size. Plating can strengthen corrosion resistance (the coating gold of metalBelong to the corrosion resistant metals that adopt more), increase hardness, prevent abrasion, improve electric conductivity, slickness, heat resistance and surface aesthetic. PlatingPalladium nickel: improve conductive contact impedance, promote signal transmission, wearability is higher than gold.
Silica white is white single-size, and main component is silica. There is purity high, the feature of safety and sanitation. BeThe colloidal state system with solid property, is made up of the colloidal particle that forms agglutinate structure. Colloidal particle is that hydration status silica gel is (manySilicic acid) condensation polymer, belong to amorphous substance. The gap of the aggregate of colloidal particle forms reagent column chromatography silica gel granule interiorMicro hole structure. Therefore, it is that one has the microcellular structure of enriching, high-specific surface area, high-purity, highly active high-quality enrichment materialMaterial. The Main Feature of reagent silica white--enriched character, depends on the micropore knot forming in raw material silica gel production processStructure and bore area.
Creativeness of the present invention is: (1) cotton stalk/silica white composite is a kind of novel material for water treatment, doesFor environment-friendly materials functional development has a high potential; (2) with polyurethanes, modified silicon rubber powder is fixed in ammonification cotton stalk,The preparation technology who prepares cotton stalk silica white composite has no bibliographical information; (3) compared with silica white, or cottonStalk metal enrichment material is compared, the property such as the physical aspect of composite, the structure of matter, metal enrichment amount, recycling utilizationCan all possess outstanding substantive distinguishing features and significant progressive.
Summary of the invention
The invention belongs to material for water treatment field, relate to the silica white composite of palladium ion in a kind of enrichment electroplating wastewaterPreparation method. The preparation method that the present invention proposes is compound to modified silicon rubber powder in the duct of ammonification cotton stalk, concreteTechnique comprises that cotton stalk is cleaned, prepared by ammonification, silica white modification and composite etc. Cotton stalk silicon prepared by the present inventionRubber powder composite has the following advantages: (1) is fixed to silica white in cotton stalk with polyurethanes, can bring into play cottonThe characteristic that flower densified straw is light, specific area is large, can utilize again silica white to the strong advantage of Metal Palladium ion enrichment ability;(2), compared with silica gel powder, the problem that composite has avoided silica gel powder reuniting caking, palladium ion enrichment power to reduce, again canAvoid the silica white of enriched palladium ion to be difficult to reclaim, cause the problem of secondary pollution; (3) compared with cotton stalk, compositeSignificantly improve the saturated enriching quantity of palladium ion, can avoid again the pollution of overflowing of cotton stalk organic carbon in water treatment procedure.The enriching quantity of palladium ion is promoted to 103.4mg/g by composite, and every gram of composite can enrichment 103.4mg palladium ion.Palladium ion enrichment material prepared by the present invention can be used for Electroplate Factory containing palladium wastewater treatment, and market prospects are wide.
The preparation method of the silica white composite that the present invention proposes, is characterized in that:
1) clean cotton stalk: by cotton stalk rinsing, oven dry;
2) cotton stalk ammonification: the cotton stalk after clean is placed in to ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, bakingDry; Wherein the formula of ammoniated solution is that solvent is deionized water, and in solution, various solute concentrations are respectively: ammonium acetate concentration 3 ~6g/L, ammonia concn 3 ~ 6g/L, 1,3-propane diamine concentration, 3 ~ 6g/L, glycol concentration 1 ~ 3g/L;
3) silica white modification: silica white is placed in to acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in 100DEG C dry 3 ~ 12 hours, cooling, with deionized water washing, dry, obtain the silica white of modification; Wherein silica white and acrylic acid/heightMaterial/the liquor ratio of potassium manganate mixed solution is 1/5 ~ 1/20g/mL; Wherein acrylic acid in acrylic acid/potassium permanganate mixed aqueous solutionMass concentration be 20 ~ 30%, the mass concentration of potassium permanganate is 0.1 ~ 0.3%;
4) composite preparation: polyurethanes is dissolved in butanone, adds successively ammonification cotton stalk and modified silicon rubber powder,Stir 1 ~ 4 hour, be placed in drying box, in 40 ~ 60 DEG C dry 12 hours, obtain silica white composite; Wherein various materialsWeight ratio is: ammonification cotton stalk/modified silicon rubber powder/polyurethanes/butanone=2/1/2/5.
Cotton stalk silica white composite is placed in containing palladium electroplating wastewater, and regulator solution pH value is 5 ~ 6, in 25 DEG C of richnessesCollect 4 hours, in waste water, the concentration of palladium ion is 50 ~ 500mg/L, and enrichment is complete, filters, and detects the palladium of enrichment in material for water treatmentIonic weight.
It is that the disodium ethylene diamine tetra-acetic acid aqueous solution 1 of 0.2M is little that the composite of above-mentioned enriched palladium ion is placed in to concentrationTime, filter, clean, dry, complete desorption technique, obtain the cotton stalk silica white composite of regeneration; Again by above-mentioned regenerationComposite is placed in containing palladium electroplating wastewater, carries out palladium ion enrichment. Multiple circulation like this, until the palladium ion richness of compositeCollection amount is less than 75% of first enriching quantity.
Detailed description of the invention
The invention is further illustrated by the following examples
Embodiment 1
By cotton stalk harvesting, clean with running water, dry.
By ammonium acetate, ammoniacal liquor, 1,3-propane diamine, ethylene glycol are dissolved in deionized water, and ammonium acetate concentration is 4g/L, and ammoniacal liquor is denseDegree is 5g/L, and 1,3-propane diamine concentration is 5g/L, and glycol concentration is 2g/L, obtains ammoniated solution.
Cotton stalk clean 100g is placed in to 500mL ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, oven dry,Obtain the cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, and acrylic acid mass concentration is 25%, the quality of potassium permanganateConcentration is 0.2%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica white is placed in to 1000mL acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in100 DEG C are dried 4 hours, cooling, with deionized water washing, dry, obtain the silica white of modification.
100g polyurethanes is dissolved in 250g butanone, adds successively 100g ammonification cotton stalk and 50g modified siliconRubber powder, stirs 3 hours, is placed in drying box, in 50 DEG C dry 12 hours, obtain silica white composite.
20g cotton stalk silica white composite is placed in to 10L containing palladium electroplating wastewater, and regulator solution pH value is 5 ~ 6, in25 DEG C of enrichments 4 hours, in waste water, the concentration of palladium ion is 500mg/L, enrichment is complete, filters, and detects the palladium of composite enrichmentIonic weight is 103.4mg/g.
It is that the disodium ethylene diamine tetra-acetic acid aqueous solution 1 of 0.2M is little that the composite of above-mentioned enriched palladium ion is placed in to concentrationTime, filter, clean, dry, complete desorption technique, obtain the cotton stalk silica white composite of regeneration; Again by above-mentioned regenerationComposite is placed in containing palladium electroplating wastewater, carries out palladium ion enrichment. 8 circulations like this, the palladium ion enriching quantity of compositeBe less than 75% of first enriching quantity.
Embodiment 2
By cotton stalk harvesting, clean with running water, dry.
By ammonium acetate, ammoniacal liquor, 1,3-propane diamine, ethylene glycol are dissolved in deionized water, and ammonium acetate concentration is 6g/L, and ammoniacal liquor is denseDegree is 6g/L, and 1,3-propane diamine concentration is 3g/L, and glycol concentration is 3g/L, obtains ammoniated solution.
Cotton stalk clean 50g is placed in to 500mL ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, oven dry,The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, and acrylic acid mass concentration is 30%, the quality of potassium permanganateConcentration is 0.1%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica white is placed in to 2000mL acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in100 DEG C are dried 12 hours, cooling, with deionized water washing, dry, obtain the silica white of modification.
200g polyurethanes is dissolved in 500g butanone, adds successively 200g ammonification cotton stalk and 100g modified siliconRubber powder, stirs 4 hours, is placed in drying box, in 40 DEG C dry 12 hours, obtain silica white composite.
10g cotton stalk silica white composite is placed in to 100L containing palladium electroplating wastewater, and regulator solution pH value is 5 ~ 6,In 25 DEG C of enrichments 4 hours, in waste water, the concentration of palladium ion was 50mg/L, and enrichment is complete, filtered, and detected the palladium of composite enrichmentIonic weight is 99.6mg/g.
It is that the disodium ethylene diamine tetra-acetic acid aqueous solution 1 of 0.2M is little that the composite of above-mentioned enriched palladium ion is placed in to concentrationTime, filter, clean, dry, complete desorption technique, obtain the cotton stalk silica white composite of regeneration; Again by above-mentioned regenerationComposite is placed in containing palladium electroplating wastewater, carries out palladium ion enrichment. 12 circulations like this, the palladium ion enriching quantity of compositeBe less than 75% of first enriching quantity.
Embodiment 3
By cotton stalk harvesting, clean with running water, dry.
By ammonium acetate, ammoniacal liquor, 1,3-propane diamine, ethylene glycol are dissolved in deionized water, and ammonium acetate concentration is 5g/L, and ammoniacal liquor is denseDegree is 4g/L, and 1,3-propane diamine concentration is 4g/L, and glycol concentration is 3g/L, obtains ammoniated solution.
Cotton stalk clean 10g is placed in to 500mL ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, oven dry,The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, and acrylic acid mass concentration is 28%, the quality of potassium permanganateConcentration is 0.3%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica white is placed in to 1500mL acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in100 DEG C are dried 5 hours, cooling, with deionized water washing, dry, obtain the silica white of modification.
10g polyurethanes is dissolved in 25g butanone, adds successively 10g ammonification cotton stalk and 5g modified silicon rubber powder,Stir 2 hours, be placed in drying box, in 40 DEG C dry 12 hours, obtain silica white composite.
20g cotton stalk silica white composite is placed in to 50L containing palladium electroplating wastewater, and regulator solution pH value is 5 ~ 6, in25 DEG C of enrichments 4 hours, in waste water, the concentration of palladium ion is 160mg/L, enrichment is complete, filters, and detects the palladium of composite enrichmentIonic weight is 100.1mg/g.
It is that the disodium ethylene diamine tetra-acetic acid aqueous solution 1 of 0.2M is little that the composite of above-mentioned enriched palladium ion is placed in to concentrationTime, filter, clean, dry, complete desorption technique, obtain the cotton stalk silica white composite of regeneration; Again by above-mentioned regenerationComposite is placed in containing palladium electroplating wastewater, carries out palladium ion enrichment. 10 circulations like this, the palladium ion enriching quantity of compositeBe less than 75% of first enriching quantity.
Embodiment 4
By cotton stalk harvesting, clean with running water, dry.
By ammonium acetate, ammoniacal liquor, 1,3-propane diamine, ethylene glycol are dissolved in deionized water, and ammonium acetate concentration is 3g/L, and ammoniacal liquor is denseDegree is 3g/L, and 1,3-propane diamine concentration is 6g/L, and glycol concentration is 1g/L, obtains ammoniated solution.
Cotton stalk clean 50g is placed in to 500mL ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, oven dry,The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, and acrylic acid mass concentration is 20%, the quality of potassium permanganateConcentration is 0.3%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica white is placed in to 500mL acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in 100DEG C dry 3 hours, cooling, with deionized water washing, dry, obtain the silica white of modification.
20g polyurethanes is dissolved in 50g butanone, adds successively 20g ammonification cotton stalk and 10g modified silica-gelPowder, stirs 1 hour, is placed in drying box, in 60 DEG C dry 12 hours, obtain silica white composite.
100g cotton stalk silica white composite is placed in to 100L containing palladium electroplating wastewater, and regulator solution pH value is 5 ~ 6,In 25 DEG C of enrichments 4 hours, in waste water, the concentration of palladium ion was 50mg/L, and enrichment is complete, filtered, and detected the palladium of composite enrichmentIonic weight is 36.1mg/g.
It is that the disodium ethylene diamine tetra-acetic acid aqueous solution 1 of 0.2M is little that the composite of above-mentioned enriched palladium ion is placed in to concentrationTime, filter, clean, dry, complete desorption technique, obtain the cotton stalk silica white composite of regeneration; Again by above-mentioned regenerationComposite is placed in containing palladium electroplating wastewater, carries out palladium ion enrichment. 6 circulations like this, the palladium ion enriching quantity of compositeBe less than 75% of first enriching quantity.
Claims (1)
1. a preparation method for the silica white composite of palladium ion in enrichment electroplating wastewater, is characterized in that:
1) clean cotton stalk: by cotton stalk rinsing, oven dry;
2) cotton stalk ammonification: the cotton stalk after clean is placed in to ammoniated solution, in 60 DEG C of placements 180 minutes, rinsing, bakingDry; Wherein the formula of ammoniated solution is that solvent is deionized water, and in solution, various solute concentrations are respectively: ammonium acetate concentration 3 ~6g/L, ammonia concn 3 ~ 6g/L, 1,3-propane diamine concentration, 3 ~ 6g/L, glycol concentration 1 ~ 3g/L;
3) silica white modification: silica white is placed in to acrylic acid/potassium permanganate mixed aqueous solution, stirs 1 hour, filter, in 100DEG C dry 3 ~ 12 hours, cooling, with deionized water washing, dry, obtain the silica white of modification; Wherein silica white and acrylic acid/heightMaterial/the liquor ratio of potassium manganate mixed solution is 1/5 ~ 1/20g/mL; Wherein acrylic acid in acrylic acid/potassium permanganate mixed aqueous solutionMass concentration be 20 ~ 30%, the mass concentration of potassium permanganate is 0.1 ~ 0.3%;
4) composite preparation: polyurethanes is dissolved in butanone, adds successively ammonification cotton stalk and modified silicon rubber powder,Stir 1 ~ 4 hour, mixture is placed in drying box, in 40 ~ 60 DEG C dry 12 hours, obtain silica white composite; Wherein variousThe weight ratio of material is: ammonification cotton stalk/modified silicon rubber powder/polyurethanes/butanone=2/1/2/5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030116504A1 (en) * | 2001-07-24 | 2003-06-26 | Vempati Rajan K. | Absorbent for arsenic species and method of treating arsenic-contaminated waters |
| CN103551121A (en) * | 2013-11-15 | 2014-02-05 | 南京大学 | Adsorbing material prepared from waste straws and capable of adsorbing trivalent arsenic from water as well as preparation method and application thereof |
| CN104043414A (en) * | 2014-06-26 | 2014-09-17 | 青岛乾祥环保技术有限公司 | Environment-friendly absorbing material for lead-containing industrial waste water |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030116504A1 (en) * | 2001-07-24 | 2003-06-26 | Vempati Rajan K. | Absorbent for arsenic species and method of treating arsenic-contaminated waters |
| CN103551121A (en) * | 2013-11-15 | 2014-02-05 | 南京大学 | Adsorbing material prepared from waste straws and capable of adsorbing trivalent arsenic from water as well as preparation method and application thereof |
| CN104043414A (en) * | 2014-06-26 | 2014-09-17 | 青岛乾祥环保技术有限公司 | Environment-friendly absorbing material for lead-containing industrial waste water |
Non-Patent Citations (1)
| Title |
|---|
| 李国胜: "《建筑结构裂缝及加层加固疑难问题的处理》", 31 March 2006, 中国建筑工业出版社 * |
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