CN105170118B - The preparation method of the titanium white powder composite material of Acid Orange II in a kind of removal dyeing waste water - Google Patents
The preparation method of the titanium white powder composite material of Acid Orange II in a kind of removal dyeing waste water Download PDFInfo
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Abstract
The invention belongs to technical field of water treatment, is related to a kind of preparation method for removing the titanium white powder composite material of Acid Orange II in dyeing waste water.Preparation method proposed by the present invention is combined to modified titanium, modified kaolin in the duct of ammonification shuck, and concrete technology includes clean shuck, ammonification, titanium dioxide modification, Modification of kaolin and composite preparation etc..Composite prepared by the present invention has advantages below：（1）Titanium dioxide and kaolin are fixed in shuck with epoxy resin, the characteristic that shuck density is light, specific surface area is big can be played, the advantages of and can utilizes titanium dioxide and kaolin strong to Acid Orange II adsorption capacity；（2）Compared with titanium dioxide and kaolin powder, composite avoids titanium dioxide and kaolin powder and reunited caking, Acid Orange II absorption affinity the problem of reducing, and and can avoids adsorbing the titanium dioxide of Acid Orange II dyestuff and kaolin from being difficult to reclaim, the problem of triggering secondary pollution；（3）Compared with shuck, the saturated extent of adsorption of Acid Orange II dyestuff is greatly improved in composite.Composite can be used for treatment of dyeing wastewater, wide market.
Description
Technical field
The invention belongs to material for water treatment technical field, and in particular to a kind of titanium white for removing Acid Orange II in dyeing waste water
The preparation method of powder composite material.
Background technology
Dyestuff is one of chemicals class the closest with human lives' relation, and its product attribute determines that this is one
The industry of power is most directly driven to innovate.The also clear proof this point of the dyestuff development history of more than 160 years.The mankind were to color before this
Pursue, expedited the emergence of synthetic dyestuffs industry；And with the birth of novel textile material, scientist develops point for being suitable for terylene again
Dissipate dyestuff and the dyeing and printing process different for the dye of positive ion ... of acrylic fibers, different application fields, the consumption to grow with each passing hour
Demand, various new demands are proposed to dyestuff, and dye industry is exactly to be sent out constantly by products innovation, technological innovation
Exhibition grows what is got up.It can be said that modern dye industry day is born with and possesses the original gene of innovation.At present, Chinese dye industry turns
The maximum difficulty that type upgrading faces is how to effect a radical cure " three wastes " pollution, particularly high-salt wastewater and spent acid, and to remove pollution
The most strong means of chronic illness are exactly to research and develop new process for cleanly preparing.With catalytic hydrogenating reduction replace iron powder reducing technique, with
The development and application of the innovative technologies such as continuous production substitution batch production, eliminates the generation of " three wastes ", together from root
When clean manufacture integration technology original " three wastes " is become resource, both reduce pollutant emission, improve again production effect
Rate and resource, energy utilization rate.And only possess the enterprise of such innovative technology and ability, just can be in the king of dye industry
The survival and development in state.
Acid Orange II, golden yellow powder, it is in feux rouges yellow to be dissolved in water, and it is in orange to be dissolved in ethanol, is pinkish red in the concentrated sulfuric acid
Color, brown color precipitation is generated after being diluted.Its aqueous solution adds hydrochloric acid generation brown color precipitation, and hydrogenation sodium oxide molybdena is in dark-brown.
It is mainly used in silk, the dyeing of woollen fabrics, it can also be used to leather, the dyeing of paper.Polyamide fibre can be contaminated in formic acid bath.The product can
The direct printing on hair, doskin synthetic fibre, it is also possible to make index agent and biology colours.
Titanium dioxide scientific name is titanium dioxide (titanium dioxide), molecular formula TiO2, is a kind of polycrystalline compounds,
Its particle is in regularly arranged, has grid system.As the increasing brand of the continuous development of titanium dioxide industry is recognized by the mankind
Know,《2013-2017 China titanium dioxide industry production and marketing demand and investment forecasting analysis report》Data show that China's titanium dioxide is total
Production capacity accounts for the 30% of the world, is titanium white production state the biggest in the world, and national titanium dioxide aggregated capacity in 2011 is about 2,600,000 tons.
The creativeness of the present invention is：(1) shuck/epoxy resin/polyvinyl alcohol/titanium dioxide/kaolin composite material
It is a kind of new material for water treatment, is had a high potential as environment-friendly materials functional development；(2) with epoxy resin by modified titanium and
Modified kaolin is fixed in ammonification shuck, and the preparation technology for preparing shuck biomass composite has no document report；
(3) compound polyvinyl alcohol can improve the adaptability of composite absorption dyestuff；(4) with titanium dioxide, kaolin powder phase
Than or shuck compares, and the performance such as the physical form of composite, constituent structure, water treatment efficiency is provided with the reality of protrusion
Matter feature and significant progress.
The content of the invention
The invention belongs to technical field of water treatment, is related to a kind of titanium dioxide composite wood for removing Acid Orange II in dyeing waste water
The preparation method of material.Preparation method proposed by the present invention is that modified titanium, modified kaolin are combined into ammonification shuck
In duct, concrete technology includes clean shuck, ammonification, titanium dioxide modification, Modification of kaolin and composite preparation etc..This
Composite prepared by invention has advantages below：(1) titanium dioxide and kaolin are fixed in shuck with epoxy resin, both
The characteristic that shuck density is light, specific surface area is big can be played, and can is using titanium dioxide and kaolin to Acid Orange II adsorption capacity
The advantages of strong；(2) compared with titanium dioxide and kaolin powder, composite avoids titanium dioxide and kaolin powder reunion knot
The problem of block, Acid Orange II absorption affinity reduce, and can avoid adsorbing the titanium dioxide of Acid Orange II dyestuff and kaolin from being difficult to reclaim,
The problem of triggering secondary pollution；(3) compared with shuck, the saturation that Acid Orange II dyestuff is greatly improved in composite is inhaled
Attached amount.Composite can be used for treatment of dyeing wastewater, wide market.
The preparation method of the titanium white powder composite material of Acid Orange II, its feature exist in removal dyeing waste water proposed by the present invention
In：
1) shuck is cleaned：Shuck is rinsed, dried；Wherein shuck is chestnut shell, walnut shell, gingko shell, melon seeds
One kind of shell；
2) shuck ammonification：Shuck after cleaning is placed in ammoniated solution, placed 2 hours in 40~60 DEG C, rinsing,
Drying；The formula of wherein ammoniated solution is that solvent is deionized water, and various solute concentrations are respectively in solution：Urea concentration 5~
10g/L, ethylenediamine 5~10g/L of concentration, acetic acid 5~10g/L of ammonium concentration, 5~10g/L of carbonic acid ammonium concentration；
3) titanium dioxide is modified：Titanium dioxide is placed in oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in
90 DEG C of dryings 9 hours, cooling, are washed with deionized, and dry, obtain modified titanium dioxide；Its mesoxalic acid/potassium permanganate mixing water
The mass concentration of solution mesoxalic acid is 10~30%, and the mass concentration of potassium permanganate is 0.1~0.3%；
4) Modification of kaolin：Kaolin is placed in sodium tartrate/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering,
Dry 6 hours, cooling, be washed with deionized in 120 DEG C, dry, obtain modified kaolin；Wherein sodium tartrate/hydrogen peroxide
The mass concentration of mixed aqueous solution mesotartaric acid sodium is 5~10%, and the mass concentration of hydrogen peroxide is 1~3%；
5) prepared by composite：In the aqueous acetone solution that mass concentration is 50%, epoxy resin, polyethylene are sequentially added
Alcohol, ammonification shuck, modified titanium, modified kaolin, stir 3 hours, mixture is placed in drying box, and 6 are dried in 100 DEG C
Hour, obtain titanium white powder composite material；The weight ratio of wherein various materials is aqueous acetone solution/epoxy resin/polyvinyl alcohol/ammonification
Shuck/modified titanium/modified kaolin=4/1/1/1/1/1.
Above-mentioned titanium white powder composite material is placed in the dyeing waste water containing Acid Orange II, regulation solution ph is 5~6, in
25 DEG C adsorb 4 hours, and the concentration of Acid Orange II is 10~100mg/L in waste water, and absorption finishes, filtering；By detecting in solution
The Acid Orange II amount of residual, draw the Acid Orange II adsorbance of shuck biomass composite.
Embodiment
The invention is further illustrated by the following examples
Embodiment 1
Melon seed cases are cleaned with running water, dried.
Urea, ethylenediamine, ammonium acetate, ammonium carbonate are dissolved in deionized water, urea concentration 5g/L, ethylenediamine concentration is
10g/L, acetic acid ammonium concentration are 5g/L, and carbonic acid ammonium concentration is 10g/L, obtains ammoniated solution.
The 50g melon seed cases cleaned are placed in 500mL ammoniated solutions, placed 2 hours in 50 DEG C, rinsing, drying, obtain ammonification
Melon seed cases.
Oxalic acid, potassium permanganate are dissolved in deionized water, the mass concentration of oxalic acid is 20%, the mass concentration of potassium permanganate
For 0.2%, oxalic acid/potassium permanganate mixed aqueous solution is obtained.
100g titanium dioxides are placed in 500mL oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in 90 DEG C
Dry 9 hours, cooling, be washed with deionized, dry, obtain modified titanium dioxide.
Sodium tartrate, hydrogen peroxide are dissolved in deionized water, the mass concentration of sodium tartrate is 8%, the quality of hydrogen peroxide
Concentration is 2%, obtains sodium tartrate/hydrogen peroxide mixed aqueous solution.
100g kaolin is placed in 500mL sodium tartrates/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering, in 120
DEG C dry 6 hours, cooling, be washed with deionized, dry, obtain modified kaolin.
In the aqueous acetone solution that 40g mass concentrations are 50%, 10g epoxy resin, 10g polyvinyl alcohol, 10g ammonia are sequentially added
Change melon seed cases, 10g modified titaniums, 10g modified kaolins, stir 3 hours, mixture is placed in drying box, in 100 DEG C of dryings
6 hours, obtain titanium white powder composite material.
Above-mentioned 10g titanium whites powder composite material is placed in the dyeing waste water containing Acid Orange II, regulation solution ph is 5~6,
Adsorbed 4 hours in 25 DEG C, the concentration of Acid Orange II is 50mg/L in waste water, and absorption finishes, filtering；Remained by detecting in solution
Acid Orange II amount, the Acid Orange II adsorbance for drawing shuck biomass composite is 101mg/g.
Embodiment 2
Gingko shell is cleaned with running water, dried.
Urea, ethylenediamine, ammonium acetate, ammonium carbonate are dissolved in deionized water, urea concentration 6g/L, ethylenediamine concentration is
7g/L, acetic acid ammonium concentration are 8g/L, and carbonic acid ammonium concentration is 9g/L, obtains ammoniated solution.
The 50g gingko shells cleaned are placed in 500mL ammoniated solutions, placed 2 hours in 45 DEG C, rinsing, drying, obtain ammonification
Gingko shell.
Oxalic acid, potassium permanganate are dissolved in deionized water, the mass concentration of oxalic acid is 25%, the mass concentration of potassium permanganate
For 0.3%, oxalic acid/potassium permanganate mixed aqueous solution is obtained.
100g titanium dioxides are placed in 500mL oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in 90 DEG C
Dry 9 hours, cooling, be washed with deionized, dry, obtain modified titanium dioxide.
Sodium tartrate, hydrogen peroxide are dissolved in deionized water, the mass concentration of sodium tartrate is 6%, the quality of hydrogen peroxide
Concentration is 1%, obtains sodium tartrate/hydrogen peroxide mixed aqueous solution.
100g kaolin is placed in 500mL sodium tartrates/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering, in 120
DEG C dry 6 hours, cooling, be washed with deionized, dry, obtain modified kaolin.
In the aqueous acetone solution that 40g mass concentrations are 50%, 10g epoxy resin, 10g polyvinyl alcohol, 10g ammonia are sequentially added
Change gingko shell, 10g modified titaniums, 10g modified kaolins, stir 3 hours, mixture is placed in drying box, in 100 DEG C of dryings
6 hours, obtain titanium white powder composite material.
Above-mentioned 10g titanium whites powder composite material is placed in the dyeing waste water containing Acid Orange II, regulation solution ph is 5~6,
Adsorbed 4 hours in 25 DEG C, the concentration of Acid Orange II is 80mg/L in waste water, and absorption finishes, filtering；Remained by detecting in solution
Acid Orange II amount, the Acid Orange II adsorbance for drawing shuck biomass composite is 81mg/g.
Embodiment 3
Walnut shell is cleaned with running water, dried.
Urea, ethylenediamine, ammonium acetate, ammonium carbonate are dissolved in deionized water, urea concentration 5g/L, ethylenediamine concentration is
5g/L, acetic acid ammonium concentration are 5g/L, and carbonic acid ammonium concentration is 5g/L, obtains ammoniated solution.
The 50g walnut shells cleaned are placed in 500mL ammoniated solutions, placed 2 hours in 40 DEG C, rinsing, drying, obtain ammonification
Walnut shell.
Oxalic acid, potassium permanganate are dissolved in deionized water, the mass concentration of oxalic acid is 10%, the mass concentration of potassium permanganate
For 0.1%, oxalic acid/potassium permanganate mixed aqueous solution is obtained.
100g titanium dioxides are placed in 500mL oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in 90 DEG C
Dry 9 hours, cooling, be washed with deionized, dry, obtain modified titanium dioxide.
Sodium tartrate, hydrogen peroxide are dissolved in deionized water, the mass concentration of sodium tartrate is 5%, the quality of hydrogen peroxide
Concentration is 1%, obtains sodium tartrate/hydrogen peroxide mixed aqueous solution.
100g kaolin is placed in 500mL sodium tartrates/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering, in 120
DEG C dry 6 hours, cooling, be washed with deionized, dry, obtain modified kaolin.
In the aqueous acetone solution that 40g mass concentrations are 50%, 10g epoxy resin, 10g polyvinyl alcohol, 10g ammonia are sequentially added
Change walnut shell, 10g modified titaniums, 10g modified kaolins, stir 3 hours, mixture is placed in drying box, in 100 DEG C of dryings
6 hours, obtain titanium white powder composite material.
Above-mentioned 10g titanium whites powder composite material is placed in the dyeing waste water containing Acid Orange II, regulation solution ph is 5~6,
Adsorbed 4 hours in 25 DEG C, the concentration of Acid Orange II is 10mg/L in waste water, and absorption finishes, filtering；Remained by detecting in solution
Acid Orange II amount, the Acid Orange II adsorbance for drawing shuck biomass composite is 97mg/g.
Embodiment 4
Chestnut shell is cleaned with running water, dried.
Urea, ethylenediamine, ammonium acetate, ammonium carbonate are dissolved in deionized water, urea concentration 10g/L, ethylenediamine concentration
For 10g/L, acetic acid ammonium concentration is 10g/L, and carbonic acid ammonium concentration is 10g/L, obtains ammoniated solution.
The 50g chestnut shells cleaned are placed in 500mL ammoniated solutions, placed 2 hours in 60 DEG C, rinsing, drying, obtain ammonification
Chestnut shell.
Oxalic acid, potassium permanganate are dissolved in deionized water, the mass concentration of oxalic acid is 30%, the mass concentration of potassium permanganate
For 0.3%, oxalic acid/potassium permanganate mixed aqueous solution is obtained.
100g titanium dioxides are placed in 500mL oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in 90 DEG C
Dry 9 hours, cooling, be washed with deionized, dry, obtain modified titanium dioxide.
Sodium tartrate, hydrogen peroxide are dissolved in deionized water, the mass concentration of sodium tartrate is 10%, the quality of hydrogen peroxide
Concentration is 3%, obtains sodium tartrate/hydrogen peroxide mixed aqueous solution.
100g kaolin is placed in 500mL sodium tartrates/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering, in 120
DEG C dry 6 hours, cooling, be washed with deionized, dry, obtain modified kaolin.
In the aqueous acetone solution that 40g mass concentrations are 50%, 10g epoxy resin, 10g polyvinyl alcohol, 10g ammonia are sequentially added
Change chestnut shell, 10g modified titaniums, 10g modified kaolins, stir 3 hours, mixture is placed in drying box, in 100 DEG C of dryings
6 hours, obtain titanium white powder composite material.
Above-mentioned 10g titanium whites powder composite material is placed in the dyeing waste water containing Acid Orange II, regulation solution ph is 5~6,
Adsorbed 4 hours in 25 DEG C, the concentration of Acid Orange II is 100mg/L in waste water, and absorption finishes, filtering；It is residual in solution by detecting
The Acid Orange II amount stayed, the Acid Orange II adsorbance for drawing shuck biomass composite are 111mg/g.
Claims (1)
- A kind of 1. preparation method for removing the titanium white powder composite material of Acid Orange II in dyeing waste water, it is characterised in that：1）Clean shuck：Shuck is rinsed, dried；Wherein shuck be chestnut shell, walnut shell, gingko shell, melon seed cases it It is a kind of；2）Shuck ammonification：Shuck after cleaning is placed in ammoniated solution, placed 2 hours in 40 ~ 60 DEG C, rinsing, drying； The formula of wherein ammoniated solution is that solvent is deionized water, and various solute concentrations are respectively in solution：5 ~ 10g/L of urea concentration, Ethylenediamine 5 ~ 10g/L of concentration, acetic acid 5 ~ 10g/L of ammonium concentration, 5 ~ 10g/L of carbonic acid ammonium concentration；3）Titanium dioxide is modified：Titanium dioxide is placed in oxalic acid/potassium permanganate mixed aqueous solution, stirred 3 hours, filtering, in 90 DEG C Dry 9 hours, cooling, be washed with deionized, dry, obtain modified titanium dioxide；Its mesoxalic acid/potassium permanganate mixed aqueous solution The mass concentration of mesoxalic acid is 10 ~ 30%, and the mass concentration of potassium permanganate is 0.1 ~ 0.3%；4）Modification of kaolin：Kaolin is placed in sodium tartrate/hydrogen peroxide mixed aqueous solution, stirred 6 hours, filtering, in 120 DEG C dry 6 hours, cooling, be washed with deionized, dry, obtain modified kaolin；Wherein sodium tartrate/hydrogen peroxide mixing water The mass concentration of solution mesotartaric acid sodium is 5 ~ 10%, and the mass concentration of hydrogen peroxide is 1 ~ 3%；5）It is prepared by composite：In the aqueous acetone solution that mass concentration is 50%, epoxy resin, polyvinyl alcohol, ammonia are sequentially added To change shuck, modified titanium, modified kaolin, stir 3 hours, mixture is placed in drying box, is dried 6 hours in 100 DEG C, Obtain titanium white powder composite material；The weight ratio of wherein various materials is aqueous acetone solution/epoxy resin/polyvinyl alcohol/ammonification nut Shell/modified titanium/modified kaolin=4/1/1/1/1/1.
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Citations (4)
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|---|---|---|---|---|
| CN1063239A (en) * | 1990-10-30 | 1992-08-05 | 法国石油公司 | The preparation method of the solid capture agent of mercury |
| CN101959973A (en) * | 2007-10-16 | 2011-01-26 | Nxp股份有限公司 | Comprise the particle and the application thereof of nuclear and shell |
| CN103433000A (en) * | 2013-08-21 | 2013-12-11 | 太仓碧奇新材料研发有限公司 | Preparation method for zinc ion adsorption material |
| CN103585999A (en) * | 2013-10-17 | 2014-02-19 | 青岛昊源环境工程技术有限公司 | Composite biological adsorption material for water purification |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120067828A1 (en) * | 2009-02-16 | 2012-03-22 | CRC Care Pty., Ltd. | Photocatalyst and method for production |
-
2015
- 2015-09-30 CN CN201510633295.0A patent/CN105170118B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063239A (en) * | 1990-10-30 | 1992-08-05 | 法国石油公司 | The preparation method of the solid capture agent of mercury |
| CN101959973A (en) * | 2007-10-16 | 2011-01-26 | Nxp股份有限公司 | Comprise the particle and the application thereof of nuclear and shell |
| CN103433000A (en) * | 2013-08-21 | 2013-12-11 | 太仓碧奇新材料研发有限公司 | Preparation method for zinc ion adsorption material |
| CN103585999A (en) * | 2013-10-17 | 2014-02-19 | 青岛昊源环境工程技术有限公司 | Composite biological adsorption material for water purification |
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