CN106423109A - Cation-modified fly ash adsorbent and preparation method thereof - Google Patents

Cation-modified fly ash adsorbent and preparation method thereof Download PDF

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CN106423109A
CN106423109A CN201610870150.7A CN201610870150A CN106423109A CN 106423109 A CN106423109 A CN 106423109A CN 201610870150 A CN201610870150 A CN 201610870150A CN 106423109 A CN106423109 A CN 106423109A
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solution
flying dust
coupling agent
fly ash
adsorbent
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CN106423109B (en
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张晓东
刘馨
杜辉
陈照军
孙德帅
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Qingdao University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0262—Compounds of O, S, Se, Te
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a cationic polymer modified fly ash adsorbent and a preparation method thereof. The cation-modified fly ash adsorbent is characterized by being prepared from the following steps: in an alcohol solution with the mass concentration of 90%, acetic acid is used for adjusting pH to be 3-4 while an amino silane coupling agent is added dropwise slowly, stirring is continued until the solution is transparent after completion of addition, and an amino silane coupling agent solution with mass fraction of 0.1%-3% is prepared for standby application; the prepared amino silane coupling agent solution is weighed, fly ash is added and stirred at the room temperature for 30-60 minutes, filtering is performed, a filter cake is dried at 50-60 DEG C for 1-3 hours, then reacts for 1-2 hours at the constant temperature of 120 DEG C under the dry condition and is cooled, and amino silane coupling agent modified fly ash is prepared for standby application; the prepared amino silane coupling agent modified fly ash is evenly mixed with an alkaline epoxy group terminated epicholorohydrin-dimethylamine cationic polymer solution, the mixture is then dried at 50-60 DEG C to constant weight, a material is taken out and crushed, and the cationic polymer modified fly ash adsorbent is obtained. Adsorption decolourization experiments show that compared with fly ash, the adsorptive decolorization capacity of the cationic polymer modified fly ash adsorbent is remarkably improved.

Description

A kind of cation-modified flying dust adsorbent and preparation method thereof
Technical field
The present invention relates to a kind of adsorbing material, more particularly to a kind of cation-modified flying dust absorption for dyeing waste water Agent and preparation method thereof.
Background technology
Up to more than 70 ten thousand tons of the annual production of whole world organic dyestuff, wherein about 12% dyestuff is in production and application process In be discharged in the way of colorful wastewater.Due to waste water from dyestuff complicated components, colourity is deep and COD and BOD value is of a relatively high, Directly discharge will necessarily cause severe contamination to environment, therefore needs before discharging to carry out wastewater treatment.Common dyes waste water Processing method mainly includes flocculence, oxidizing process, bioanalysises, absorption method etc., and the sludge quantity that wherein flocculence produces is big and is dehydrated Difficulty, Treatment of Sludge operating cost is high, and easily causes secondary pollution；Oxidizing process energy consumption is larger, and COD clearance is relatively low；Biological Method has certain requirement to conditions such as the pH of waste water from dyestuff, temperature it is difficult to adapt to that waste water quality fluctuation is big, kind of dyes is many, malicious The high feature of property；It is relatively fewer with floor space that absorption method has an obvious equipment investment, and simple to operate and decolorizing effect is excellent Feature.In absorption method, conventional adsorbent is mainly activated carbon and ion exchange resin.Activated carbon is as a kind of excellent Adsorbent is early widely used in water process, remains the best adsorbent of colored dyes waste water so far, yet with price Costliness, is therefore typically only applied to the relatively low dye wastewater treatment of concentration；Ion exchange resin has stronger to dye molecule Absorbability, but lead to cost for wastewater treatment higher because regeneration is difficult, thus also limit it in dye wastewater treatment Application, therefore develop a kind of excellent, the cheap adsorbent of absorption property be always treatment of dyeing wastewater research lead The hot subject in domain.
Flying dust also known as flyash, is the garbage of coal-burning power plant's pulverized coal friring discharge, its main chemical compositions is silicon, aluminum, The oxide of ferrum and a certain amount of calcium, magnesium, oxysulfide, wherein silicon oxide, aluminium oxide, that ferrum oxide gross mass accounts for flying dust is total The 85% of quality.Flying dust is a kind of porous bulk solids aggregation, and porosity is generally 60%-75%, has substantial amounts of micropore Structure and larger specific surface area, and wide material sources, cheap, high adsorption capacity, therefore can be used as in wastewater treatment Adsorbent and flocculant use.But flying dust itself is weaker to the dye adsorption ability in dyeing waste water, its adsorption bleaching ability It is difficult to meet dyeing waste water and performance of the adsorbent is actually needed.
It is cheap and easy to get that the purpose of the present invention is aiming at flying dust, has the characteristics that good adsorption properties, exploitation a kind of to dye Material and dyestuff in dyeing waste water have stronger adsorption bleaching ability and can meet the cation-modified flying dust absorption of fixed bed needs Agent and preparation method thereof.This cation-modified flying dust adsorbent removes and flying dust can be substantially improved to energy dye adsorption in dyeing waste water Outside power, the cationic polymer that existing cation-modified flying dust adsorbent exists can also be overcome to be combined loosely with flying dust, de- During color, cationic polymer is easy to the shortcoming departing from from flying dust, and is significantly lower than strong alkalinity anion in operating cost Exchanger resin.
Content of the invention
A kind of preparation method of cation-modified flying dust adsorbent is it is characterised in that implement as follows：In quality hundred Point concentration is in 90% alcoholic solution, while being slowly added dropwise amino silicane coupling agent, while adjusting pH=3-4 with acetic acid, after dripping off, continues to stir Mix transparent to solution, obtain the amino silicane coupling agent solution for standby that mass fraction is 0.1%-3%；Weigh the amino silicone of above-mentioned preparation Alkane coupling agent solution, adds flying dust, after 30-60 minute is stirred at room temperature, filters, after filter cake is dried 1-3 hour at 50-60 DEG C, then React 1-2 hour, cooling in 120 DEG C of freeze-day with constant temperature, obtain aminosilane coupling agent modifying flying dust standby；Amino silane by preparation After coupling agent modified flying dust is mixed homogeneously with polyepichlorohydrin-dimethylamine cationic polymer solution more dry at 50-60 DEG C Dry take out material to constant weight, pulverize, obtain cation-modified flying dust adsorbent；Alcohol-water solution described above is methanol solution, or Ethanol solution；Silane coupler described above is 3- aminopropane triethoxysilane, or 3- aminopropane trimethoxy silicon Alkane, or 3- aminopropane-methyldiethoxysilane；Flying dust described above, its SiO2、Al2O3And Fe2O3Quality sum is higher than The 80% of flying dust gross mass, porosity is higher than 60%, mesh number >=80 mesh；Polyepichlorohydrin-dimethylamine cation described above Polymer solution, its cationic polymeric molecule end group is epoxide group, and solution ph is more than 9.
Further illustrate the present invention below by instantiation.
Specific embodiment
Embodiment 1
The preparation of polyepichlorohydrin-dimethylamine cationic polymer solution：By document（Yellow new photograph etc., cationic polymer Preparation and application performance, chemical industry and engineering, 2009,26 (2), p114-118）Synthetically prepared Hydrin-diformazan Amine cation polymer solution, wherein monomer epoxychloropropane are 1.5 with the mol ratio of monomer dimethylamine:1, cross-linking agent divinyl Triamine consumption accounts for the 2% of monomer epoxychloropropane and dimethylamine gross mass.Prepared polyepichlorohydrin-dimethylamine cation Polymer solution, solid content is 33.33%, and outward appearance is weak yellow liquid, and viscosity is 300-500mPa s, and pH is 4-5.
Embodiment 2
The preparation of silane coupler modified flying dust：Weigh the ethanol that 190 gram mass concentration are 90%, adjust pH=3-3.5 with acetic acid, It is slowly added dropwise 2 grams of silane coupler 3- aminopropane triethoxysilanes under pH=3-3.5, after dripping off, continue stirring 30-60 and divide Clock is transparent to solution, adds the ethanol that mass concentration is 90%, to 200 grams of total amount, obtains the amino silane that mass fraction is 1% and is coupled Agent solution is standby；100 grams of amino silicane coupling agent solution weighing above-mentioned preparation is put in 250ml beaker, adds 40 grams and flies Ash, after being stirred at room temperature 30 minutes, filters, and filter cake, after 50 DEG C of vacuum drying 2 hours, reacts 1 then at 120 DEG C of normal pressure freeze-day with constant temperature Hour, cooling, obtain silane coupler modified flying dust.
Embodiment 3
The preparation of cation-modified flying dust adsorbent A：Weigh the polyepichlorohydrin-dimethylamine cation of 40g embodiment 1 preparation Polymer solution（Solid content is 33.33%）Mix with 260g water, add 10g sodium hydroxide, after being uniformly mixed.Side again Stirring side adds 190g flying dust, after stirring, puts in vacuum drying oven, in 50 DEG C of drying under reduced pressure, to constant weight, pulverizes, obtains Cation-modified flying dust adsorbent A.
Embodiment 4
The preparation of cation-modified flying dust adsorbent B：With embodiment 3, simply 190g flying dust is changed to silane prepared by embodiment 2 Coupling agent modified flying dust, obtains cation-modified flying dust adsorbent B.
Embodiment 5
Column chromatography adsorption bleaching is tested：Cation-modified with 20g flying dust, 20g cation-modified flying dust adsorbent A and 20g respectively Flying dust adsorbent B is adsorbent, using dry column-packing, prepares the thin layer chromatography post of a diameter of 20mm, at room temperature to simulation dye Material waste water（500 mg/L）Carry out column chromatography, record colourless chromatography liquid and amass, result is as shown in table 1.
Table 1 adsorbent adsorption bleaching characteristic
The as shown by data of table 1, is significantly larger than former flying using the cation-modified flying dust adsorbent A adsorption bleaching characteristic of flying dust preparation Ash, and enter one using the adsorption bleaching characteristic of the cation-modified flying dust adsorbent B of aminosilane coupling agent modifying flying dust preparation Step strengthens.
Certainly, described above is not limitation of the present invention, and the present invention is also not limited to the example above, the art Those of ordinary skill, in the essential scope of the present invention, change, interpolation or the replacement made, all should belong to the guarantor of the present invention Shield scope.

Claims (2)

1. a kind of preparation method of cationic polymer modification flying dust adsorbent is it is characterised in that implement as follows：In matter Amount concentration is in 90% alcohol-water solution, while being slowly added dropwise amino silicane coupling agent, while adjusting pH=3-4 with acetic acid, after being added dropwise to complete, Continuation stirring is transparent to solution, obtains the amino silicane coupling agent solution for standby that mass fraction is 0.1%-3%；Weigh above-mentioned preparation Amino silicane coupling agent solution, adds flying dust, after 30-60 minute is stirred at room temperature, filters, filter cake is dried 1-3 hour at 50-60 DEG C Afterwards, react 1-2 hour, cooling then at 120 DEG C of freeze-day with constant temperature, obtain aminosilane coupling agent modifying flying dust standby；Ammonia by preparation After the coupling agent modified flying dust of base silane is mixed homogeneously with polyepichlorohydrin-dimethylamine cationic polymer solution, in 50-60 DEG C Lower drying, to constant weight, takes out material, pulverizes, obtain cation-modified flying dust adsorbent；Alcohol-water solution described above is that methanol is molten Liquid, or ethanol solution；Silane coupler described above is 3- aminopropane triethoxysilane, or 3- aminopropane trimethoxy Base silane, or 3- aminopropane-methyldiethoxysilane；Flying dust described above, its SiO2、Al2O3And Fe2O3Quality sum Higher than the 80% of flying dust gross mass, porosity is higher than 60%, mesh number >=80 mesh；Polyepichlorohydrin-dimethylamine sun described above Ionomer solution, its cationic polymeric molecule end group is epoxide group, and solution ph is more than 9.
2. a kind of cationic polymer modification flying dust adsorbent is it is characterised in that prepare according to preparation method described in claim 1 And obtain.
CN201610870150.7A 2016-10-04 2016-10-04 A kind of cation-modified flying dust adsorbent and preparation method thereof Expired - Fee Related CN106423109B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108311124A (en) * 2018-03-08 2018-07-24 东华理工大学 A kind of preparation method and application of hyperbranched polyorganosiloxane modified coal ash
CN108927117A (en) * 2018-08-02 2018-12-04 深圳市深港产学研环保工程技术股份有限公司 A kind of preparation method of flyash-sodium alginate composite adsorbing material
CN111636242A (en) * 2020-04-17 2020-09-08 仙鹤股份有限公司 Micro-coating sublimation thermal transfer paper and preparation method thereof
CN113893828A (en) * 2021-11-23 2022-01-07 华东理工大学 Preparation method of porous electropositive fly ash adsorbent

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108311124A (en) * 2018-03-08 2018-07-24 东华理工大学 A kind of preparation method and application of hyperbranched polyorganosiloxane modified coal ash
CN108311124B (en) * 2018-03-08 2021-02-02 东华理工大学 Preparation method and application of hyperbranched polysiloxane modified fly ash
CN108927117A (en) * 2018-08-02 2018-12-04 深圳市深港产学研环保工程技术股份有限公司 A kind of preparation method of flyash-sodium alginate composite adsorbing material
CN111636242A (en) * 2020-04-17 2020-09-08 仙鹤股份有限公司 Micro-coating sublimation thermal transfer paper and preparation method thereof
CN111636242B (en) * 2020-04-17 2022-06-21 仙鹤股份有限公司 Micro-coating sublimation thermal transfer paper and preparation method thereof
CN113893828A (en) * 2021-11-23 2022-01-07 华东理工大学 Preparation method of porous electropositive fly ash adsorbent

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