CN106423109B - A kind of cation-modified flying dust adsorbent and preparation method thereof - Google Patents

A kind of cation-modified flying dust adsorbent and preparation method thereof Download PDF

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CN106423109B
CN106423109B CN201610870150.7A CN201610870150A CN106423109B CN 106423109 B CN106423109 B CN 106423109B CN 201610870150 A CN201610870150 A CN 201610870150A CN 106423109 B CN106423109 B CN 106423109B
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flying dust
solution
coupling agent
preparation
modified
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CN106423109A (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)
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  • 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 kind of cationic polymers to be modified flying dust adsorbent and preparation method thereof, it is characterised in that is prepared as follows：In the alcoholic solution that mass concentration is 90%, while amino silicane coupling agent is slowly added dropwise, while with acetic acid tune pH=3-4, after being added dropwise to complete, continues that stirring is transparent to solution, obtain the amino silicane coupling agent solution for standby that mass fraction is 0.1%-3%；It weighs the amino silicane coupling agent solution of above-mentioned preparation, flying dust is added, after being stirred at room temperature 30-60 minute, filtering, filter cake cools down at 50-60 DEG C after dry 1-3 hours, then in 120 DEG C of freeze-day with constant temperature reactions 1-2 hours, it is spare to obtain aminosilane coupling agent modifying flying dust；By the aminosilane coupling agent modifying flying dust of preparation with alkalinity end group be epoxy group polyepichlorohydrin-dimethylamine cationic polymer solution after mixing, it is dry at 50-60 DEG C, until constant weight, takes out material, it crushes, obtains cationic polymer and be modified flying dust adsorbent.It is demonstrated experimentally that compared with flying dust, which is modified flying dust adsorbent and is significantly improved to the adsorption bleaching ability of organic dyestuff adsorption bleaching.

Description

A kind of cation-modified flying dust adsorbent and preparation method thereof
Technical field
The present invention relates to a kind of sorbing materials, are adsorbed more particularly to a kind of cation-modified flying dust for dyeing waste water Agent and preparation method thereof.
Background technology
The annual output of whole world organic dyestuff is up to more than 70 ten thousand tons, wherein about 12% dyestuff is in production and application process In be discharged in a manner of colorful wastewater.Due to waste water from dyestuff complicated components, coloration is deep and COD and BOD values are relatively high, Direct emission will necessarily cause seriously to pollute to environment, therefore need to carry out wastewater treatment before discharging.Common dyes waste water Processing method includes mainly flocculence, oxidizing process, bioanalysis, absorption method etc., and the sludge quantity that wherein flocculence generates is big and is dehydrated Difficulty, Treatment of Sludge operating cost is high, and be easy to cause secondary pollution；Oxidizing process energy consumption is larger, and COD removal rates are relatively low；Biology Method has certain requirement to conditions such as pH, the temperature of waste water from dyestuff, it is difficult to adapt to that waste water quality fluctuation is big, dyes is more, malicious The high feature of property；Absorption method has apparent equipment investment and floor space relatively fewer, and easy to operate and decolorizing effect is excellent The characteristics of.In absorption method, common 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, is still the best adsorbent of colored dyes waste water so far, however due to price Costliness, therefore generally it is only applied to the lower dye wastewater treatment of concentration；Ion exchange resin has dye molecule stronger Adsorption capacity, but cause cost for wastewater treatment higher since regeneration is difficult, thus it is also limited in dye wastewater treatment Application, therefore it is always that treatment of dyeing wastewater research is led to develop a kind of adsorbent that absorption property is excellent, cheap The hot subject in domain.
Flying dust is also known as flyash, is the waste of coal-burning power plant pulverized coal friring discharge, main chemical compositions be silicon, aluminium, The oxide of iron and a certain amount of calcium, magnesium, oxysulfide, wherein silica, aluminium oxide, that iron oxide gross mass accounts for about flying dust is total The 85% of quality.Flying dust is a kind of porosity bulk solids aggregation, and porosity is generally 60%-75%, has a large amount of micropore Structure and larger specific surface area, and derive from a wealth of sources, cheap, adsorption capacity is strong, therefore can be used as in wastewater treatment Adsorbent and flocculant use.However flying dust itself is weaker to the Dye Adsorption ability in dyeing waste water, adsorption bleaching ability It is difficult to the actual needs for meeting dyeing waste water to performance of the adsorbent.
The purpose of the present invention is cheap and easy to get aiming at flying dust, has the characteristics that good adsorption properties, exploitation are a kind of to dye Material has stronger adsorption bleaching ability with dyestuff in dyeing waste water and can meet the cation-modified flying dust absorption of fixed bed needs Agent and preparation method thereof.The cation-modified flying dust adsorbent, which removes, can be substantially improved flying dust to Dye Adsorption energy in dyeing waste water Outside power, cationic polymer existing for existing cation-modified flying dust adsorbent can also be overcome to be combined with flying dust loosely, de- The shortcomings that cationic polymer is easy to be detached from from flying dust during color, and strong alkalinity anion is significantly lower than in operating cost Exchanger resin.
Invention content
A kind of preparation method of cation-modified flying dust adsorbent, it is characterised in that implement as follows：In quality hundred Divide in a concentration of 90% alcoholic solution, while amino silicane coupling agent is slowly added dropwise, while with acetic acid tune pH=3-4, after dripping off, continues to stir Mix it is transparent to solution, obtain mass fraction be 0.1%-3% amino silicane coupling agent solution for standby；Weigh the amino silicone of above-mentioned preparation Flying dust is added in alkane coupling agent solution, after being stirred at room temperature 30-60 minute, filters, filter cake at 50-60 DEG C after dry 1-3 hours, then It is reacted 1-2 hours in 120 DEG C of freeze-day with constant temperature, it is spare to obtain aminosilane coupling agent modifying flying dust for cooling；By the amino silane of preparation Coupling agent modified flying dust and polyepichlorohydrin-dimethylamine cationic polymer solution after mixing, then at 50-60 DEG C are done It is dry to take out material to constant weight, it crushes, obtains cation-modified flying dust adsorbent；Alcohol solution described above is methanol solution, or Ethanol solution；Silane coupling agent described above is 3- aminopropanes triethoxysilane or 3- aminopropane trimethoxy silicon Alkane or 3- aminopropanes-methyldiethoxysilane；Flying dust described above, SiO2、Al2O3And Fe2O3Quality sum is higher than The 80% of flying dust gross mass, porosity are higher than 60%, the mesh of mesh number >=80；Polyepichlorohydrin-dimethylamine cation described above Polymer solution, cationic polymeric molecule end group are epoxy group, and solution ph is more than 9.
It is further illustrated the present invention below by specific example.
Specific implementation mode
Embodiment 1
The preparation of polyepichlorohydrin-dimethylamine cationic polymer solution：By document（Yellow new photograph etc., cationic polymerization The preparation and application performance of object, chemical industry and engineering, 2009,26 (2), p114-118）It is synthetically prepared Hydrin- The molar ratio of dimethylamine cation polymer solution, wherein monomer epoxychloropropane and monomer dimethylamine is 1.5:1, crosslinking agent two Ethylene triamine dosage accounts for the 2% of monomer epoxychloropropane and dimethylamine gross mass.Prepared polyepichlorohydrin-dimethylamine sun Ionomer solution, solid content 33.33%, appearance are weak yellow liquid, viscosity 300-500mPas, pH 4-5.
Embodiment 2
The preparation of silane coupler modified flying dust：The ethyl alcohol for weighing 190 gram masses a concentration of 90%, with acetic acid tune pH=3- 3.5,2 grams of silane coupling agent 3- aminopropane triethoxysilanes are slowly added dropwise at pH=3-3.5, after dripping off, continue to stir 30-60 minutes transparent to solution, adds the ethyl alcohol that mass concentration is 90%, until 200 grams of total amount, obtains the amino that mass fraction is 1% Silane coupler solution is spare；100 grams of amino silicane coupling agent solution for weighing above-mentioned preparation is put into 250ml beakers, then is added Enter 40 grams of flying dusts, after being stirred at room temperature 30 minutes, filtering, after filter cake is dried in vacuo 2 hours at 50 DEG C, then at 120 DEG C of normal pressure constant temperature Dry reaction 1 hour, cooling, obtains silane coupler modified flying dust.
Embodiment 3
The preparation of cation-modified flying dust adsorbent A：Weigh the polyepichlorohydrin-dimethylamine sun of the preparation of 40g embodiments 1 Ionomer solution（Solid content is 33.33%）It is mixed with 260g water, 10g sodium hydroxides is added, after being uniformly mixed. 190g flying dusts are added while stirring again, after stirring evenly, is put into vacuum drying chamber, is dried under reduced pressure in 50 DEG C, until constant weight, powder It is broken, obtain cation-modified flying dust adsorbent A.
Embodiment 4
The preparation of cation-modified flying dust adsorbent B：With embodiment 3,190g flying dusts are only changed to embodiment 2 and are prepared Silane coupler modified flying dust obtains cation-modified flying dust adsorbent B.
Embodiment 5
Column chromatography adsorption bleaching is tested：Respectively with 20g flying dusts, the cation-modified flying dust adsorbent As of 20g and 20g cations Modified flying dust adsorbent B is that adsorbent prepares the thin layer chromatography column of a diameter of 20mm, at room temperature to mould using dry column-packing Quasi- waste water from dyestuff（500 mg/L）Column chromatography is carried out, records colourless chromatography liquid product, the results are shown in Table 1.
1 adsorbent adsorption bleaching characteristic of table
Table 1 statistics indicate that, using flying dust prepare cation-modified flying dust adsorbent A adsorption bleaching characteristic be significantly larger than Former flying dust, and use the adsorption bleaching characteristic of the cation-modified flying dust adsorbent B of aminosilane coupling agent modifying flying dust preparation It further enhances.
Certainly, above description 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, the present invention essential scope in, variation, addition or the replacement made, should all belong to the present invention guarantor Protect range.

Claims (2)

1. a kind of cationic polymer is modified the preparation method of flying dust adsorbent, it is characterised in that implement as follows：In matter It measures in a concentration of 90% alcohol solution, while amino silicane coupling agent is slowly added dropwise, while with acetic acid tune pH=3-4, after being added dropwise to complete, Continue stirring it is transparent to solution, obtain mass fraction be 0.1%-3% amino silicane coupling agent solution for standby；Weigh above-mentioned preparation Flying dust is added in amino silicane coupling agent solution, after being stirred at room temperature 30-60 minutes, filters, filter cake is 1-3 hours dry at 50-60 DEG C Afterwards, it is reacted 1-2 hours then at 120 DEG C of freeze-day with constant temperature, it is spare to obtain aminosilane coupling agent modifying flying dust for cooling；By the ammonia of preparation The coupling agent modified flying dust of base silane and polyepichlorohydrin-dimethylamine cationic polymer solution after mixing, in 50-60 DEG C Lower drying crushes until constant weight, takes out material, obtains cation-modified flying dust adsorbent；Alcohol solution described above is that methanol is molten Liquid or ethanol solution；Silane coupling agent described above is 3- aminopropanes triethoxysilane or 3- aminopropane trimethoxies Base silane or 3- aminopropanes-methyldiethoxysilane；Flying dust described above, SiO2、Al2O3And Fe2O3Quality sum Higher than the 80% of flying dust gross mass, porosity is higher than 60%, the mesh of mesh number >=80；Polyepichlorohydrin-dimethylamine sun described above Ionomer solution, cationic polymeric molecule end group are epoxy group, and solution ph is more than 9.
2. a kind of cationic polymer is modified flying dust adsorbent, it is characterised in that prepared according to preparation method described in claim 1 And it obtains.
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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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
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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