CN108993457A - A method of adsorbent is prepared by raw material of flyash - Google Patents

A method of adsorbent is prepared by raw material of flyash Download PDF

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Publication number
CN108993457A
CN108993457A CN201810845430.1A CN201810845430A CN108993457A CN 108993457 A CN108993457 A CN 108993457A CN 201810845430 A CN201810845430 A CN 201810845430A CN 108993457 A CN108993457 A CN 108993457A
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flyash
reaction
adsorbent
product
mixed
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CN108993457B (en
Inventor
刘东基
赵风清
郝亚菲
李超
***
田晓华
李领肖
陈雄木
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen

Abstract

The present invention provides a kind of method for preparing adsorbent as raw material using flyash, specific steps are as follows: (1) by flyash grinding, sieving, washing;(2) NaOH solution is mixed with flyash by the weight ratio of 7 ~ 15:1, after displaying, under microwave condition in 70 ~ 90 DEG C of 0.5 ~ 1h of reaction;(3) it filters, liquid phase pH is adjusted to 6 or so and obtains flocculent deposit, reacted, filtered in 70 ~ 90 DEG C using microwave again, drying filtrate obtains first product;(4) the CTAB solution of first product and 2g/L is mixed and modified, separation is drying to obtain adsorbent.This method manufacturing cost is low, and product has superior adsorption effect, and high-qualityization for realizing flyash utilizes.The present invention prepares adsorbent with the modified method mutually cooperateed with of CTAB by hydro-thermal-microwave, reduces energy consumption compared to traditional alkali fusion;Compared to traditional hydro-thermal method, generated time has been saved, has improved production efficiency.

Description

A method of adsorbent is prepared by raw material of flyash
Technical field
The invention belongs to field of solid waste comprehensive utilization, and in particular to a kind of to prepare high-performance by raw material of flyash The method of adsorbent.
Background technique
In recent years, the discharge of industrial production and sanitary wastewater exhaust gas is also growing day by day, seriously threaten people's lives and Health.Therefore, the purifying problem for solving waste water and gas is the task of top priority.
Adsorbent be one kind can from gas or liquid by therein a certain or several substances be adsorbed on its surface from And reach the material of separating effect, it can be used for the purification of waste water, exhaust gas.Currently, common adsorbent is zeolite, molecular sieve and each Kind active carbon etc..
Flyash is solid waste caused by the fire coal of thermal power plant, main component SiO2、Al2O3Deng the two Content often accounts for 60% or more, either zeolite or molecular sieve, and main component is SiO2And Al2O3.Therefore, powder is utilized Coal ash prepares the attention that zeolites adsorbent causes academia.
Some scholars, at zeolite or molecular sieve, are used to handle waste water or exhaust gas as adsorbent, still using coal ash for manufacturing Synthesis condition is relatively harsh, and energy consumption is larger.Therefore, inventor is by coal ash for manufacturing at a kind of absorption that synthesis condition is relatively mild Agent further reduces the energy consumption in synthesis process to handle waste water, has saved the energy, the absorption of the adsorbent of preparation Property is excellent.
Summary of the invention
The present invention provides a kind of using coal ash for manufacturing for the method for adsorbent, passes through hydro-thermal-microwave cooperating heating side Method contains a large amount of holes using coal ash for manufacturing for a kind of adsorbent for Si-O tetrahedron or Al-O tetrahedron framework, this structure And duct, there is biggish specific surface area and excellent absorption property.This product can be used for the net of more demanding waste water and gas Change.
A method of with coal ash for manufacturing for high-performance adsorbent, specific steps are as follows:
(1) by flyash grinding by 200 meshes, washing removes the impurity in flyash;The purpose of grinding is to destroy flyash The vitreous structure on surface improves its reactivity;
(2) NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 7 ~ 15:1, after displaying 1h at room temperature, will be mixed Object is under microwave condition in 70 ~ 90 DEG C of 0.5 ~ 1h of reaction;
(3) it filters after reaction, liquid phase pH is adjusted to 6 or so with the HCl solution of 2mol/L, flocculent deposit can be obtained, then It is secondary to utilize microwave in 70 ~ 90 DEG C of reaction 1.5h;It filters after reaction, drying filtrate obtains first product;
(4) by the CTAB(cetyl trimethylammonium bromide of first product and 2g/L) solution mixes, and concussion is modified, and is then centrifuged for point From obtained solid phase is drying to obtain adsorbent.
Beneficial effects of the present invention: the present invention is low as raw material adsorbent cost using flyash, and properties of product are excellent, realize High-qualityization of flyash utilizes.The present invention prepares adsorbent with the modified method mutually cooperateed with of CTAB by hydro-thermal-microwave, compared to Traditional alkali fusion reduces energy consumption;Compared to traditional hydro-thermal method, generated time has been saved, has improved production efficiency, has been obtained Adsorbent has superior adsorption effect.
Specific embodiment
Embodiment one
200 meshes will be crossed after flyash in the ball mill grinding 0.5h, washing removes the impurity in flyash.
The NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 7:1, after displaying 1h at room temperature;By mixture It moves into microwave reactor in 90 DEG C of reaction 0.5h.It filters, is adjusted to liquid phase pH after reaction with the HCl solution of 2mol/L 6 or so, flocculent deposit is obtained, moves into microwave reactor again, 1.5h is reacted at 80 DEG C, is filtered after reaction, is dried Filtrate obtains first product.
By the CTAB(cetyl trimethylammonium bromide of first product and 2g/L) solution mixes, shakes on earthquake shaking table 15min is modified.Be centrifuged 10min at 3500r, obtained solid phase be placed in baking oven, at 110 DEG C dry 6h to get To final modified adsorbent product.Sample is 247mg/g for the adsorptive value of methyl orange.
Embodiment two
200 meshes will be crossed after flyash in the ball mill grinding 0.5h, washing removes the impurity in flyash.
The NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 10:1, after displaying 1h at room temperature;It will mixing Object moves into microwave reactor in 70 DEG C of reaction 1.5h.It filters, is adjusted liquid phase pH after reaction with the HCl solution of 2mol/L To 6 or so, flocculent deposit is obtained, moves into microwave reactor again, 0.75h is reacted at 70 DEG C, is filtered after reaction, is dried Dry filtrate obtains first product.
By the CTAB(cetyl trimethylammonium bromide of first product and 2g/L) solution mixes, shakes on earthquake shaking table 15min is modified.Be centrifuged 10min at 3500r, obtained solid phase be placed in baking oven, at 110 DEG C dry 6h to get To final modified adsorbent product.Sample is 210mg/g for the adsorptive value of methyl orange.
Embodiment three
200 meshes will be crossed after flyash in the ball mill grinding 0.5h, washing removes the impurity in flyash.
The NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 15:1, after displaying 1h at room temperature;It will mixing Object moves into microwave reactor in 80 DEG C of reaction 1h.It filters, is adjusted to liquid phase pH after reaction with the HCl solution of 2mol/L 6 or so, flocculent deposit is obtained, moves into microwave reactor again, 1.5h is reacted at 90 DEG C, is filtered after reaction, is dried Filtrate obtains first product.
By the CTAB(cetyl trimethylammonium bromide of first product and 2g/L) solution mixes, shakes on earthquake shaking table 15min is modified.Be centrifuged 10min at 3500r, obtained solid phase be placed in baking oven, at 110 DEG C dry 6h to get To final modified adsorbent product.Sample is 267mg/g for the adsorptive value of methyl orange.
Comparative example one
In the preparation of fly ash-based adsorbent " and its to the Study on adsorption properties of fuel " article, author carries out alkali to flyash The modified absorption for being used for methyl orange, being converted, it is 14.865mg/g for the adsorptive value of methyl orange.
Comparative example two
In " application study flyash modified and its to Methyl Orange in Wastewater " article, author carries out acid modification to flyash and is used for The absorption of methyl orange, being converted, it is 21.09mg/g for the adsorptive value of methyl orange.
Comparative example three (modified without CTAB)
200 meshes will be crossed after flyash in the ball mill grinding 0.5h, washing removes the impurity in flyash.
The NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 7:1, after displaying 1h at room temperature;By mixture It moves into microwave reactor in 90 DEG C of reaction 0.5h.It filters, is adjusted to liquid phase pH after reaction with the HCl solution of 2mol/L 6 or so, flocculent deposit is obtained, moves into microwave reactor again, 1.5h is reacted at 80 DEG C, is filtered after reaction, is dried Filtrate obtains first product.First product is 7mg/g for the adsorptive value of methyl orange.

Claims (2)

1. it is a kind of with coal ash for manufacturing for the method for high-performance adsorbent, specific steps are as follows:
(1) by flyash grinding by 200 meshes, washing removes the impurity in flyash;The purpose of grinding is to destroy flyash The vitreous structure on surface improves its reactivity;
(2) NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 7 ~ 15:1, after displaying 1h at room temperature, will be mixed Object is under microwave condition in 70 ~ 90 DEG C of 0.5 ~ 1h of reaction;
(3) it filters after reaction, liquid phase pH is adjusted to 6 or so with the HCl solution of 2mol/L, flocculent deposit can be obtained, then It is secondary to utilize microwave in 70 ~ 90 DEG C of reaction 1.5h;It filters after reaction, drying filtrate obtains first product;
(4) first product being mixed with the cetyl trimethylammonium bromide solution of 2g/L, concussion is modified, it is then centrifuged for separating, To solid phase be drying to obtain adsorbent.
2. it is according to claim 1 it is a kind of with coal ash for manufacturing for the method for high-performance adsorbent, it is characterised in that: its optimize Step is
(1) by flyash grinding by 200 meshes, washing removes the impurity in flyash;The purpose of grinding is to destroy flyash The vitreous structure on surface improves its reactivity;
(2) NaOH solution of 2mol/L is mixed with flyash by the weight ratio of 15:1, after displaying 1h at room temperature, by mixture Under microwave condition in 80 DEG C of reaction 1h;
(3) it filters after reaction, liquid phase pH is adjusted to 6 or so with the HCl solution of 2mol/L, flocculent deposit can be obtained, then It is secondary to utilize microwave in 90 DEG C of reaction 1.5h;It filters after reaction, drying filtrate obtains first product;
(4) first product being mixed with the cetyl trimethylammonium bromide solution of 2g/L, concussion is modified, it is then centrifuged for separating, To solid phase be drying to obtain adsorbent.
CN201810845430.1A 2018-07-27 2018-07-27 Method for preparing adsorbent by taking fly ash as raw material Active CN108993457B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN110773114A (en) * 2019-10-23 2020-02-11 华北电力大学(保定) Preparation method of modified fly ash adsorbent for VOCs (volatile organic chemicals)
CN111186844A (en) * 2020-01-17 2020-05-22 河北科技大学 Preparation method of fly ash based zeolite molecular sieve for adsorbing VOCs (volatile organic compounds)
CN114471449A (en) * 2020-10-23 2022-05-13 中国石油化工股份有限公司 Adsorbing material, preparation method thereof and application of adsorbing material in treatment of printing and dyeing wastewater
CN115703637A (en) * 2021-08-10 2023-02-17 中国石油化工股份有限公司 Porous silicon oxide and preparation method and application thereof
CN115722193A (en) * 2022-12-01 2023-03-03 吉林大学 Modification of low-concentration ammonia nitrogen in water preparation method and application of adsorbing material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110773114A (en) * 2019-10-23 2020-02-11 华北电力大学(保定) Preparation method of modified fly ash adsorbent for VOCs (volatile organic chemicals)
CN111186844A (en) * 2020-01-17 2020-05-22 河北科技大学 Preparation method of fly ash based zeolite molecular sieve for adsorbing VOCs (volatile organic compounds)
CN114471449A (en) * 2020-10-23 2022-05-13 中国石油化工股份有限公司 Adsorbing material, preparation method thereof and application of adsorbing material in treatment of printing and dyeing wastewater
CN114471449B (en) * 2020-10-23 2023-07-14 中国石油化工股份有限公司 Adsorption material, preparation method thereof and application thereof in treatment of printing and dyeing wastewater
CN115703637A (en) * 2021-08-10 2023-02-17 中国石油化工股份有限公司 Porous silicon oxide and preparation method and application thereof
CN115722193A (en) * 2022-12-01 2023-03-03 吉林大学 Modification of low-concentration ammonia nitrogen in water preparation method and application of adsorbing material
CN115722193B (en) * 2022-12-01 2024-04-12 吉林大学 Preparation method and application of ammonia nitrogen modified adsorption material with low concentration in water

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