CN105597704B - The preparation method of the silica gel powder composite material of palladium ion in a kind of enrichment electroplating wastewater - Google Patents
The preparation method of the silica gel powder composite material of palladium ion in a kind of enrichment electroplating wastewater Download PDFInfo
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- CN105597704B CN105597704B CN201510633494.1A CN201510633494A CN105597704B CN 105597704 B CN105597704 B CN 105597704B CN 201510633494 A CN201510633494 A CN 201510633494A CN 105597704 B CN105597704 B CN 105597704B
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Abstract
The invention belongs to technical field of water treatment, is related to a kind of preparation method for being enriched with the silica gel powder composite material of palladium ion in electroplating wastewater.Preparation method proposed by the present invention is combined to modified silicon rubber powder in the duct of ammonification cotton stalk, and concrete technology includes clean cotton stalk, ammonification, silica white modification and composite preparation etc..Cotton stalk silica gel powder composite material prepared by the present invention has advantages below：（1）Silica white is fixed in cotton stalk with polyurethanes, the characteristic that cotton stalk density is light, specific surface area is big can be played, the advantages of and can make use of silica white heavy metal palladium ion accumulation ability strong；（2）With silica white body phase ratio, composite avoid silica gel powder reuniting caking, palladium ion enrichment power reduce the problem of, and can avoid be enriched with palladium ion silica white be difficult to reclaim, trigger secondary pollution the problem of；（3）Compared with cotton stalk, palladium ion saturation enriching quantity is greatly improved in composite, and and can avoids the spilling of cotton stalk organic carbon in water treatment procedure from polluting.The enriching quantity of palladium ion is promoted to 103.4mg/g by composite prepared by the present invention, available for Electroplate Factory's wastewater treatment containing palladium, wide market.
Description
Technical field
The invention belongs to material for water treatment technical field, and in particular to a kind of silica white for being enriched with palladium ion in electroplating wastewater
The preparation method of composite.
Background technology
It is exactly to plate the other gold of a thin layer on some metal surfaces using electrolysis principle to electroplate (Electroplating)
Category or alloy process, be using electrolysis make metal or other materials product surface attachment layer of metal film technique from
And playing prevents metal from aoxidizing（Such as corrosion）, improve wearability, electric conductivity, reflective, corrosion resistance (copper sulphate etc.）And promote
It is attractive in appearance to wait effect.During plating, coated metal or other insoluble materials do anode, and workpiece to be plated does negative electrode, coated metal
Cation is reduced to form coating in workpiece surface to be plated.To exclude the interference of other cations, and make coating uniformly, firmly,
Electroplate liquid need to be done with the solution of the cation containing coated metal, to keep the concentration of coated metal cation constant.The purpose of plating
It is that the coat of metal is plated on base material, changes substrate surface property or size.Plating can strengthen corrosion resistance (the coating gold of metal
Category is more using corrosion resistant metal), increase hardness, prevent from wearing away, improve electric conductivity, slickness, heat resistance and surface aesthetic.Plating
Palladium nickel：Improve conductive contact impedance, promote signal transmission, wearability is higher than gold.
Silica white is white uniformity particle, and main component is silica.High, the feature of safety and sanitation with purity.It is
Colloid system with solid property, it is made up of the colloidal particle for forming agglutinate structure.Colloidal particle is hydration status silica gel（It is more
Silicic acid）Condensation polymer, belong to amorphous substance.The gap of the aggregate of colloidal particle is formed inside reagent column chromatography silica gel particle
Micro hole structure.Therefore, it is a kind of with abundant microcellular structure, high-specific surface area, high-purity, the high-quality enrichment material of high activity
Material.The Main Feature of reagent silica white -- enriched character, depending on the micropore knot formed in raw material silica gel production process
Structure and bore area.
The creativeness of the present invention is：（1）Cotton stalk/silica gel powder composite material is a kind of new material for water treatment, is made
Had a high potential for environment-friendly materials functional development；（2）Modified silicon rubber powder is fixed in ammonification cotton stalk with polyurethanes,
The preparation technology for preparing cotton stalk silica gel powder composite material has no document report；（3）Compared with silica white, or cotton
Stalk metal enrichment material is compared, the property such as the physical aspect of composite, the structure of matter, metal enrichment amount, recycling utilization
Prominent substantive distinguishing features and significant progress can be provided with.
The content of the invention
The invention belongs to technical field of water treatment, is related to a kind of silica gel powder composite material for being enriched with palladium ion in electroplating wastewater
Preparation method.Preparation method proposed by the present invention is combined to modified silicon rubber powder in the duct of ammonification cotton stalk, specifically
Technique includes clean cotton stalk, ammonification, silica white modification and composite preparation etc..Cotton stalk silicon prepared by the present invention
Rubber powder composite has advantages below：（1）Silica white is fixed in cotton stalk with polyurethanes, cotton can be played
Flower densified straw is light, specific surface area is big characteristic, the advantages of and can make use of silica white strong to Metal Palladium ion enrichment ability；
（2）With silica white body phase ratio, composite avoids silica gel powder reuniting caking, palladium ion is enriched with the problem of power reduces, and can
Avoid be enriched with palladium ion silica white be difficult to reclaim, trigger secondary pollution the problem of；（3）Compared with cotton stalk, composite
Palladium ion saturation enriching quantity is greatly improved, and can avoids the spilling of cotton stalk organic carbon in water treatment procedure from polluting.
The enriching quantity of palladium ion is promoted to 103.4 mg/g by composite, i.e. every gram of composite can be enriched with 103.4 mg palladium ions.
Palladium ion enrichment material prepared by the present invention can be used for Electroplate Factory's wastewater treatment containing palladium, wide market.
The preparation method of silica gel powder composite material proposed by the present invention, it is characterised in that：
1）Clean cotton stalk：Cotton stalk is rinsed, dried；
2）Cotton stalk ammonification：Cotton stalk after cleaning is placed in ammoniated solution, placed 180 minutes in 60 DEG C, drift
Wash, dry；The formula of wherein ammoniated solution is that solvent is deionized water, and various solute concentrations are respectively in solution：Ammonium acetate is dense
Spend 3 ~ 6g/L, ammonia concn 3 ~ 6g/L, 1,3- propane diamine 3 ~ 6g/L of concentration, 1 ~ 3g/L of glycol concentration；
3）Silica white is modified：Silica white is placed in acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering,
Dry 3 ~ 12 hours, cooling, be washed with deionized in 100 DEG C, dry, obtain modified silica white；Wherein silica white and propylene
Material/liquor ratio of acid/potassium permanganate mixed solution is 1/5 ~ 1/20 g/ mL；Wherein in acrylic acid/potassium permanganate mixed aqueous solution
The mass concentration of acrylic acid is 20 ~ 30%, and the mass concentration of potassium permanganate is 0.1 ~ 0.3%；
4）It is prepared by composite：Polyurethanes is dissolved in butanone, sequentially adds ammonification cotton stalk and modified silicon
Rubber powder, stir 1 ~ 4 hour, be placed in drying box, dried 12 hours in 40 ~ 60 DEG C, obtain silica gel powder composite material；Wherein various things
The weight ratio of material is：Ammonification cotton stalk/modified silicon rubber powder/polyurethanes/butanone=2/1/2/5.
Cotton stalk silica gel powder composite material is placed in electroplating wastewater containing palladium, regulation solution ph is 5 ~ 6, in 25 DEG C of richnesses
Collection 4 hours, the concentration of palladium ion is 50 ~ 500mg/L in waste water, and enrichment finishes, and filtering, detects the palladium being enriched with material for water treatment
Ionic weight.
It is small in 0.2M disodium ethylene diamine tetra-acetic acid aqueous solution 1 that the composite of above-mentioned enrichment palladium ion is placed in concentration
When, filter, clean, drying, complete desorption process, obtain the cotton stalk silica gel powder composite material of regeneration；Again by above-mentioned regeneration
Composite is placed in electroplating wastewater containing palladium, carries out palladium ion enrichment.Such multiple circulations, until the palladium ion of composite is rich
Collection amount is less than the 75% of first enriching quantity.
Embodiment
The invention is further illustrated by the following examples
Embodiment 1
By cotton stalk harvesting, cleaned, dried with running water.
Ammonium acetate, ammoniacal liquor, 1,3- propane diamine, ethylene glycol are dissolved in deionized water, acetic acid ammonium concentration is 4g/L, and ammoniacal liquor is dense
It is 5g/L to spend for 5g/L, 1,3- propane diamine concentration, glycol concentration 2g/L, obtains ammoniated solution.
The 100g cotton stalks cleaned are placed in 500mL ammoniated solutions, placed 180 minutes in 60 DEG C, rinsing, drying,
Obtain the cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, the mass concentration of acrylic acid is 25%, the quality of potassium permanganate
Concentration is 0.2%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica whites are placed in 1000mL acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering, in
100 DEG C of dryings 4 hours, cooling, are washed with deionized, and dry, obtain modified silica white.
100g polyurethanes is dissolved in 250g butanone, sequentially adds 100g ammonifications cotton stalk and 50g modified silicons
Rubber powder, stir 3 hours, be placed in drying box, dried 12 hours in 50 DEG C, obtain silica gel powder composite material.
20g cotton stalk silica gel powder composite materials are placed in 10L electroplating wastewaters containing palladium, regulation solution ph is 5 ~ 6, in
25 DEG C are enriched with 4 hours, and the concentration of palladium ion is 500mg/L in waste water, and enrichment finishes, filtering, the palladium of detection composite enrichment
Ionic weight is 103.4mg/g.
It is small in 0.2M disodium ethylene diamine tetra-acetic acid aqueous solution 1 that the composite of above-mentioned enrichment palladium ion is placed in concentration
When, filter, clean, drying, complete desorption process, obtain the cotton stalk silica gel powder composite material of regeneration；Again by above-mentioned regeneration
Composite is placed in electroplating wastewater containing palladium, carries out palladium ion enrichment.Such 8 circulations, the palladium ion enriching quantity of composite
Less than the 75% of first enriching quantity.
Embodiment 2
By cotton stalk harvesting, cleaned, dried with running water.
Ammonium acetate, ammoniacal liquor, 1,3- propane diamine, ethylene glycol are dissolved in deionized water, acetic acid ammonium concentration is 6g/L, and ammoniacal liquor is dense
It is 3g/L to spend for 6g/L, 1,3- propane diamine concentration, glycol concentration 3g/L, obtains ammoniated solution.
The 50g cotton stalks cleaned are placed in 500mL ammoniated solutions, placed 180 minutes in 60 DEG C, rinsing, drying, are obtained
The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, the mass concentration of acrylic acid is 30%, the quality of potassium permanganate
Concentration is 0.1%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica whites are placed in 2000mL acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering, in
100 DEG C of dryings 12 hours, cooling, are washed with deionized, and dry, obtain modified silica white.
200g polyurethanes is dissolved in 500g butanone, sequentially adds 200g ammonifications cotton stalk and 100g modified silicons
Rubber powder, stir 4 hours, be placed in drying box, dried 12 hours in 40 DEG C, obtain silica gel powder composite material.
10g cotton stalk silica gel powder composite materials are placed in 100L electroplating wastewaters containing palladium, regulation solution ph is 5 ~ 6,
It is enriched with 4 hours in 25 DEG C, the concentration of palladium ion is 50mg/L in waste water, and enrichment finishes, filtering, the palladium of detection composite enrichment
Ionic weight is 99.6mg/g.
It is small in 0.2M disodium ethylene diamine tetra-acetic acid aqueous solution 1 that the composite of above-mentioned enrichment palladium ion is placed in concentration
When, filter, clean, drying, complete desorption process, obtain the cotton stalk silica gel powder composite material of regeneration；Again by above-mentioned regeneration
Composite is placed in electroplating wastewater containing palladium, carries out palladium ion enrichment.Such 12 circulations, the palladium ion enriching quantity of composite
Less than the 75% of first enriching quantity.
Embodiment 3
By cotton stalk harvesting, cleaned, dried with running water.
Ammonium acetate, ammoniacal liquor, 1,3- propane diamine, ethylene glycol are dissolved in deionized water, acetic acid ammonium concentration is 5g/L, and ammoniacal liquor is dense
It is 4g/L to spend for 4g/L, 1,3- propane diamine concentration, glycol concentration 3g/L, obtains ammoniated solution.
The 10g cotton stalks cleaned are placed in 500mL ammoniated solutions, placed 180 minutes in 60 DEG C, rinsing, drying, are obtained
The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, the mass concentration of acrylic acid is 28%, the quality of potassium permanganate
Concentration is 0.3%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica whites are placed in 1500mL acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering, in
100 DEG C of dryings 5 hours, cooling, are washed with deionized, and dry, obtain modified silica white.
10g polyurethanes is dissolved in 25g butanone, sequentially adds 10g ammonifications cotton stalk and 5g modified silicon rubber powders,
Stirring 2 hours, is placed in drying box, is dried 12 hours in 40 DEG C, obtains silica gel powder composite material.
20g cotton stalk silica gel powder composite materials are placed in 50L electroplating wastewaters containing palladium, regulation solution ph is 5 ~ 6, in
25 DEG C are enriched with 4 hours, and the concentration of palladium ion is 160mg/L in waste water, and enrichment finishes, filtering, the palladium of detection composite enrichment
Ionic weight is 100.1mg/g.
It is small in 0.2M disodium ethylene diamine tetra-acetic acid aqueous solution 1 that the composite of above-mentioned enrichment palladium ion is placed in concentration
When, filter, clean, drying, complete desorption process, obtain the cotton stalk silica gel powder composite material of regeneration；Again by above-mentioned regeneration
Composite is placed in electroplating wastewater containing palladium, carries out palladium ion enrichment.Such 10 circulations, the palladium ion enriching quantity of composite
Less than the 75% of first enriching quantity.
Embodiment 4
By cotton stalk harvesting, cleaned, dried with running water.
Ammonium acetate, ammoniacal liquor, 1,3- propane diamine, ethylene glycol are dissolved in deionized water, acetic acid ammonium concentration is 3g/L, and ammoniacal liquor is dense
It is 6g/L to spend for 3g/L, 1,3- propane diamine concentration, glycol concentration 1g/L, obtains ammoniated solution.
The 50g cotton stalks cleaned are placed in 500mL ammoniated solutions, placed 180 minutes in 60 DEG C, rinsing, drying, are obtained
The cotton stalk of ammonification.
Acrylic acid, potassium permanganate are dissolved in deionized water, the mass concentration of acrylic acid is 20%, the quality of potassium permanganate
Concentration is 0.3%, obtains acrylic acid/potassium permanganate mixed aqueous solution.
100g silica whites are placed in 500mL acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering, in 100
DEG C dry 3 hours, cooling, be washed with deionized, dry, obtain modified silica white.
20g polyurethanes is dissolved in 50g butanone, sequentially adds 20g ammonifications cotton stalk and 10g modified silica-gels
Powder, stir 1 hour, be placed in drying box, dried 12 hours in 60 DEG C, obtain silica gel powder composite material.
100g cotton stalk silica gel powder composite materials are placed in 100L electroplating wastewaters containing palladium, regulation solution ph is 5 ~ 6,
It is enriched with 4 hours in 25 DEG C, the concentration of palladium ion is 50mg/L in waste water, and enrichment finishes, filtering, the palladium of detection composite enrichment
Ionic weight is 36.1mg/g.
It is small in 0.2M disodium ethylene diamine tetra-acetic acid aqueous solution 1 that the composite of above-mentioned enrichment palladium ion is placed in concentration
When, filter, clean, drying, complete desorption process, obtain the cotton stalk silica gel powder composite material of regeneration；Again by above-mentioned regeneration
Composite is placed in electroplating wastewater containing palladium, carries out palladium ion enrichment.Such 6 circulations, the palladium ion enriching quantity of composite
Less than the 75% of first enriching quantity.
Claims (1)
- A kind of 1. preparation method for being enriched with the silica gel powder composite material of palladium ion in electroplating wastewater, it is characterised in that：1）Clean cotton stalk：Cotton stalk is rinsed, dried；2）Cotton stalk ammonification：Cotton stalk after cleaning is placed in ammoniated solution, placed 180 minutes in 60 DEG C, rinsing, is dried It is dry；The formula of wherein ammoniated solution is that solvent is deionized water, and various solute concentrations are respectively in solution：Acetic acid ammonium concentration 3 ~ 6g/L, ammonia concn 3 ~ 6g/L, 1,3- propane diamine 3 ~ 6g/L of concentration, 1 ~ 3g/L of glycol concentration；3）Silica white is modified：Silica white is placed in acrylic acid/potassium permanganate mixed aqueous solution, stirred 1 hour, filtering, in 100 DEG C dry 3 ~ 12 hours, cooling, be washed with deionized, dry, obtain modified silica white；Wherein silica white and acrylic acid/height Material/liquor ratio of potassium manganate mixed solution is 1/5 ~ 1/20 g/ mL；Wherein acrylic acid in acrylic acid/potassium permanganate mixed aqueous solution Mass concentration be 20 ~ 30%, the mass concentration of potassium permanganate is 0.1 ~ 0.3%；4）It is prepared by composite：Polyurethanes is dissolved in butanone, sequentially adds ammonification cotton stalk and modified silicon rubber powder, Stirring 1 ~ 4 hour, mixture is placed in drying box, is dried 12 hours in 40 ~ 60 DEG C, is obtained silica gel powder composite material；It is wherein various The 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 |
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