CN106540652A - Modified flying dust of a kind of quaternary ammonium salt cationic and preparation method thereof - Google Patents
Modified flying dust of a kind of quaternary ammonium salt cationic and preparation method thereof Download PDFInfo
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- CN106540652A CN106540652A CN201610871039.XA CN201610871039A CN106540652A CN 106540652 A CN106540652 A CN 106540652A CN 201610871039 A CN201610871039 A CN 201610871039A CN 106540652 A CN106540652 A CN 106540652A
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- flying dust
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- quaternary ammonium
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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
- B01J20/02—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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- 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
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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
- 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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of modified flying dust adsorbent of quaternary ammonium salt cationic, it is characterised in that be prepared as follows：In the alcoholic solution that mass concentration is 90%, while be slowly added dropwise amino silicane coupling agent, while pH=3 4 is adjusted with acetic acid, after dripping off, continue that stirring is transparent to solution, obtain the amino silicane coupling agent solution for standby that mass fraction is 0.1% 3%；The amino silicane coupling agent solution of above-mentioned preparation is weighed, flying dust is added, after being stirred at room temperature 30 60 minutes, is filtered, filter cake is after 50 60 DEG C of dryings 13 hours, then reacts 12 hours in 120 DEG C of freeze-day with constant temperature, cooling, obtains aminosilane coupling agent modifying flying dust standby；The aminosilane coupling agent modifying flying dust of preparation and cationic reagent are carried out into nitrogen alkylation reaction, the modified flying dust adsorbent of quaternary ammonium salt cationic is prepared.Adsorption bleaching it is demonstrated experimentally that a kind of quaternary ammonium salt cationic of the present invention is modified, compare by the more former flying dust of flying dust, can significantly improve the clearance of dyestuff and organic dyestuff in printing and dyeing industrial waste water.
Description
Technical field
The present invention relates to a kind of cation adsorbing material, more particularly to a kind of to process with printing and dyeing industrial waste water for dyestuff
Modified flying dust adsorbent of quaternary ammonium salt cationic 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.As waste water from dyestuff complicated components, colourity are deep, and COD and BOD values it is of a relatively high,
Directly discharge will necessarily cause severe contamination to environment, therefore need before discharging to carry out wastewater treatment.Common dyes waste water
Processing method mainly includes flocculence, oxidizing process, bioanalysises, absorption method etc., wherein, the sludge quantity that flocculence is produced is big and is dehydrated
Difficulty, Treatment of Sludge operating cost are high, and easily cause secondary pollution；Oxidizing process energy consumption is larger, and COD clearances are relatively low；It is biological
Method has certain requirement to conditions such as the pH of waste water from dyestuff, temperature, it is difficult to adapt to that variation water quality is big, kind of dyes is more, toxicity is high
Waste water from dyestuff；Absorption method has equipment investment relatively fewer with floor space, the characteristics of simple to operate excellent with decolorizing effect.
In absorption method, conventional adsorbent is mainly activated carbon and ion exchange resin.Activated carbon is used as a kind of excellent adsorbent
Early it is widely used in water process, remains the best adsorbent of colored dyes waste water so far, yet with expensive, because
This is typically only applied to the relatively low dye wastewater treatment of concentration；Ion exchange resin has stronger energy of adsorption to dye molecule
Power, but cause cost for wastewater treatment higher as regeneration is difficult, so limit its popularization in dye wastewater treatment should
With, therefore develop a kind of excellent, the cheap adsorbent of absorption property always dyestuff and printing and dyeing industrial waste water process
The hot subject of research field.Flying dust also known as flyash, is the garbage of coal-burning power plant's pulverized coal friring discharge, its primary chemical into
It is divided into silicon, aluminum, the oxide of ferrum and a certain amount of calcium, magnesium, oxysulfide, wherein silicon oxide, aluminium oxide, ferrum oxide gross mass
Account for the 85% of flying dust gross mass.Flying dust is a kind of porous bulk solids aggregation, and porosity is generally 60%-75%, has
Substantial amounts of microcellular structure and larger specific surface area, and wide material sources, cheap, high adsorption capacity, therefore at waste water
Can be used as adsorbent during reason and flocculant is used.But flying dust itself to dyeing waste water in dye adsorption ability it is weaker, its suction
Attached decoloring ability 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, and the characteristics of with good filter-aid performance, exploitation is a kind of to dye
Material and dyestuff in printing and dyeing industrial waste water are with stronger adsorption bleaching ability and can meet the quaternary ammonium salt cationic of fixed bed needs and change
Property flying dust adsorbent and preparation method thereof.
The content of the invention
A kind of quaternary ammonium salt cationic is modified flying dust, it is characterised in that implement as follows：In the alcohol that mass concentration is 90%
In aqueous solution, while being slowly added dropwise amino silicane coupling agent, while adjusting pH=3-4 with acetic acid, after dripping off, continue to stir transparent to solution,
Obtain amino silicane coupling agent solution for standby of the mass fraction for 0.1%-3%；The amino silicane coupling agent solution of above-mentioned preparation is weighed,
Flying dust is added, after 30-60 minutes are stirred at room temperature, is filtered, it is after filter cake is dried 1-3 hours at 50-60 DEG C, dry then at 120 DEG C of constant temperature
Dry reaction 1-2 hours, cooling, obtain aminosilane coupling agent modifying flying dust standby；The aminosilane coupling agent modifying for obtaining is flown
Ash is added in the water of 4-6 times of flying dust quality, with lye pH adjustment=9-11.Stirring is warming up to 40-70 DEG C, controls pH=9-11, protects
Under the conditions of temperature, Deca cation etherifying reagent solution, continues stirring insulation reaction 1-2 hour, adjusts pH=after adding while stirring
6.5-7, filters, washing, less than 80 DEG C of dryings, obtains the modified flying dust of quaternary ammonium salt cationic；Alcohol-water solution described above is methanol
Solution, or ethanol solution；Silane coupler described above is 3- aminopropane triethoxysilanes, or 3- aminopropane front threes
TMOS, or 3- aminopropanes-methyldiethoxysilane；Flying dust described above, its SiO2、Al2O3And Fe2O3Quality contains
Amount more than flying dust gross mass 80%, porosity are 60%-75%, and particle diameter is 1-300 μm；Cation etherifying reagent described above
For 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, or 2,3- epoxypropyltrimethylchloride chloride.
The technical characterstic and excellent results of the present invention：
The modified flying dust of quaternary ammonium salt cationic prepared by the present invention not only can utilize the micro-porous adsorption of its own to decolourize, while may be used also
So that flying dust absorption in prior art using anionic pollutant in its surface cation positive charge adsorbing and removing waste water, can be overcome
The relatively poor defect of decoloration performance.The modified flying dust of quaternary ammonium salt cationic prepared with the present invention, using absorption method to dyestuff with
Printing and dyeing industrial waste water is processed, and compared with strong-base anion-exchange resin, can substantially reduce operating cost.
The present invention is further illustrated below by instantiation.
Specific embodiment
Embodiment 1
The preparation of silane coupler modified flying dust：The ethanol that 190 gram mass concentration are 90% is weighed, and pH=3-3.5 is adjusted with acetic acid,
2 grams of silane coupler 3- aminopropane triethoxysilanes are slowly added dropwise under pH=3-3.5, after dripping off, continue 30-60 point of stirring
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 for weighing above-mentioned preparation is put in 250ml beakers, is added 40 grams and is flown
Ash, after being stirred at room temperature 30 minutes, filters, and filter cake reacts 1 then at 120 DEG C of normal pressure freeze-day with constant temperature after 50 DEG C of vacuum drying 2 hours
Hour, cooling obtains silane coupler modified flying dust.
Embodiment 2
The preparation of the modified flying dust adsorbent A of quaternary ammonium salt cationic：In the four-hole boiling flask of the 250ml equipped with reflux condenser, plus
Enter 80ml deionized waters, the silane coupler modified flying dust for adding 20 grams of embodiments 1 to prepare, with the hydrogen-oxygen that mass concentration is 10%
Changing sodium solution adjusts pH=9.5-10, stirring to be warming up to 50 DEG C, controls pH=9.5-10, under 50 DEG C of heat-retaining conditions, Deca while stirring
18 gram mass percentage concentrations are 50% 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride solution, continue stirring insulation reaction 90 after adding
Minute, pH=6.5-7 to be adjusted, is filtered, washing is dried at 80 DEG C, obtains the modified flying dust adsorbent A of quaternary ammonium salt cationic.
Embodiment 3
Adsorption bleaching characteristic is tested：Respectively with 20g flying dusts, the modified flying dust adsorbent of 20g quaternary ammonium salt cationics as adsorbent, adopt
Dry column-packing, prepares the thin layer chromatography post of a diameter of 20mm, at room temperature to dye wastewater（500 mg/L）Carry out post layer
Analysis, records colourless chromatography liquid product, as a result as shown in table 1.
The comparison of different adsorbent absorbabilitys in 1 column chromatography adsorption experiment of table
1 as shown by data of table, the modified flying dust adsorbent A of quaternary ammonium salt cationic is to the adsorption bleaching ability of organic dyestuff apparently higher than flying
The adsorption bleaching ability of ash.
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, the change made, addition or replace, should all belong to the guarantor of the present invention
Shield scope.
Claims (2)
1. the preparation method of the modified flying dust of a kind of quaternary ammonium salt cationic, it is characterised in that implement as follows：In mass concentration
In for 90% alcohol-water solution, while being slowly added dropwise amino silicane coupling agent, while pH=3-4 is adjusted with acetic acid, after dripping off, continue stirring extremely
Solution is transparent, obtains the amino silicane coupling agent solution for standby that mass fraction is 0.1%-3%；Weigh the amino silane idol of above-mentioned preparation
Connection agent solution, adds flying dust, after 30-60 minutes are stirred at room temperature, filters, after filter cake is dried 1-3 hours at 50-60 DEG C, then at 120
DEG C freeze-day with constant temperature reaction 1-2 hours, cooling obtain aminosilane coupling agent modifying flying dust standby；The amino silane for obtaining is coupled
The modified flying dust of agent is added in the water of 4-6 times of flying dust quality, with lye pH adjustment=9-11, is stirred and is warming up to 40-70 DEG C, controls pH=
9-11, under heat-retaining condition, Deca cation etherifying reagent solution, continues stirring insulation reaction 1-2 hour after adding while stirring,
PH=6.5-7 is adjusted, is filtered, washing, less than 80 DEG C of dryings, obtains the modified flying dust of quaternary ammonium salt cationic；Alcohol-water solution described above is
Methanol solution, or ethanol solution；Silane coupler described above is 3- aminopropane triethoxysilanes, or 3- aminopropanes
Trimethoxy silane, or 3- aminopropanes-methyldiethoxysilane；Flying dust described above, its SiO2、Al2O3And Fe2O3Matter
Amount content more than flying dust gross mass 80%, porosity are 60%-75%, and particle diameter is 1-300 μm；Cation etherificate described above
Reagent is 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, or 2,3- epoxypropyltrimethylchloride chloride.
2. the modified flying dust adsorbent of a kind of quaternary ammonium salt cationic, it is characterised in that prepare according to preparation method described in claim 1
And obtain.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107511140A (en) * | 2017-10-09 | 2017-12-26 | 常州建轩纺织品有限公司 | A kind of preparation method of high dephosphorization amount diatomite adsorbing material |
| CN110655137A (en) * | 2019-08-23 | 2020-01-07 | 中国矿业大学 | Fly ash-based high-salinity organic wastewater purification and biomass catalytic pyrolysis combined treatment process |
| CN113893828A (en) * | 2021-11-23 | 2022-01-07 | 华东理工大学 | Preparation method of porous electropositive fly ash adsorbent |
| CN115717276A (en) * | 2022-11-30 | 2023-02-28 | 芯安健康科技(广东)有限公司 | Far infrared antibacterial anti-mite antiviral multifunctional fiber and mattress protection pad |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110655137B (en) * | 2019-08-23 | 2020-06-23 | 中国矿业大学 | Fly ash-based high-salinity organic wastewater purification and biomass catalytic pyrolysis combined treatment process |
| CN113893828A (en) * | 2021-11-23 | 2022-01-07 | 华东理工大学 | Preparation method of porous electropositive fly ash adsorbent |
| CN115717276A (en) * | 2022-11-30 | 2023-02-28 | 芯安健康科技(广东)有限公司 | Far infrared antibacterial anti-mite antiviral multifunctional fiber and mattress protection pad |
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