CN106215902A - Feature board for adsorption of aniline and preparation method thereof - Google Patents

Feature board for adsorption of aniline and preparation method thereof Download PDF

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Publication number
CN106215902A
CN106215902A CN201610849670.XA CN201610849670A CN106215902A CN 106215902 A CN106215902 A CN 106215902A CN 201610849670 A CN201610849670 A CN 201610849670A CN 106215902 A CN106215902 A CN 106215902A
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mixed liquor
under
stir
conditions
mixed
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不公告发明人
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Beijing Yi Yi Environmental Protection Equipment Technology Co Ltd
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Beijing Yi Yi Environmental Protection Equipment Technology Co Ltd
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Priority to CN201610849670.XA priority Critical patent/CN106215902A/en
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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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • 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
    • B01J20/04Solid 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
    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28033Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • 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 invention discloses the feature board and preparation method thereof for adsorption of aniline.1,4 butanediols, 4 acetamido 3 nitrobenzoic acids, N, N dimethylformamide, polrvinyl chloride, N cyclohexyl 2 benzothiazole sulfenamide are made mixed liquid B;By polystyrene, N, N dimethylformamide, K2HPO4Make mixed liquor D;By benzoyl peroxide, chloroform, N methylformamide, NaNO3, calcium chloride make mixed liquor F;Mixed liquid B, mixed liquor D, mixed liquor F, methyl isobutyrate, Polyethylene Glycol, chloroform are made mixed liquor H;Distilled water is spurted into equipped with the container of liquid nitrogen making ice hockey granule, in the ice hockey granule that particle diameter is 50~100 μm is placed in mould cavity and be compacted;Then mixed liquor H is poured in mould and in liquid nitrogen freeze settled 6 hours, after chloroform and ice hockey granule are removed in vacuum lyophilization, obtains the feature board for adsorption of aniline.

Description

Feature board for adsorption of aniline and preparation method thereof
Technical field
The invention belongs to the processing technology field of organic industrial sewage, particularly to a kind of feature board for adsorption of aniline And preparation method thereof.
Background technology
Absorption method is that adsorbent is mixed mutually with pending waste water, and one or more pollutant in waste water are adsorbed, some Pollutant are reclaimed or are removed, so that the method that waste water is purified, high concentrated organic wastewater is had preferably by the method Treatment effect, occupies important function in organic industrial sewage treatment technology.In absorption method, the adsorbent of excellent performance is general Feature: have good pore structure, excellent surface chemistry;High adsorption capacity to adsorbate;Easily resolve, reusing By force;Mechanical strength is good.Being adsorbed with the most frequently used adsorbing material of organic pollutants at present can be divided into physisorption material, chemistry to inhale Enclosure material and biological adsorption material.Wherein, the active charcoal of physisorption material, molecular sieve, zeolite, active hargil and clay minerals Etc. having the solid of high-specific surface area, there is the advantage that eliminating efficiency is high, enrichment function is strong, but there is also poor stability, easily It is desorbed, easily by deficiencies such as variations in temperature are affected.Chemisorbed material mainly includes silica gel, synthetic fibers, resin, utilizes bioid Learn and the molecularly imprinted polymer etc. of Polymer Synthesizing.Conventional biological adsorption material has broad leaved plant, fungus, soil and water In microorganism etc..
The organic industrial sewage using absorption method to process containing aniline is a kind of up-and-coming technology for treating industrial waste water, Exploitation is needed to have the adsorbent of excellent absorption property to aniline if this technology carries out popularization and application.But, the most scarce Few adsorbing material processed for the organic industrial sewage containing aniline.
Summary of the invention
It is an object of the invention to provide a kind of feature board for adsorption of aniline and preparation method thereof.Its concrete steps are such as Under:
(1) by 150 grams of BDOs and 350 grams of 4-acetamido-3-nitrobenzoic acid mix homogeneously, it is placed in 250mL In tool plug narrow mouth bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, obtain Mixed liquor A;
(2) 11.11 grams of polrvinyl chloride and 1.5 grams of N cyclohexyl 2 benzothiazole sulfenamides are joined mixed liquor A In, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 11.66g polystyrene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-dimethyl methyls Amide, stirs 1h under the conditions of 1000r/min, obtains mixed liquor C;
(4) it is the K of 0.85mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C, under the conditions of 1000r/min Stir 5 minutes, obtain mixed liquor D;
(5) 16.37g benzoyl peroxide is placed in 250mL tool plug narrow mouth bottle, adds 250mL chloroform, Stir 1h under the conditions of 1000r/min, be divided into equivalent 5 parts after shaking up, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3, mixed liquor E4, mixed liquor E5;
(6) 24.52g N-METHYLFORMAMIDE is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, To mixed liquor F1;
(7) it is the NaNO of 0.40mol/L by 5mL mixed liquor F1 and 15mL concentration3Join in mixed liquor E2, at 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor F2;
(8) 5mL mixed liquor F2 and the calcium chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E3, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F3;
(9) it is the NaNO of 0.30mol/L by 5mL mixed liquor F3 and 15mL concentration3Join in mixed liquor E4, at 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor F4;
(10) 5mL mixed liquor F4 and the calcium chloride that 15mL concentration is 0.35mol/L are joined in mixed liquor E5, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F;
(11) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 4.5% Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3;
(12) 40mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(13) 28mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(14) 32mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(15) 54mL mixed liquor H1 is added drop-wise in 40mL mixed liquor H2 under 1000r/min stirring condition, is mixed Liquid H4;
(16) 47mL mixed liquor H4 is added drop-wise in 35mL mixed liquor H3 under 1000r/min stirring condition, is mixed Liquid H;
(17) distilled water is spurted into equipped with quick freezing making ice hockey granule in the container of liquid nitrogen, select with after sieved through sieve Take the ice hockey granule that grain size scope is 50~100 μm, in ice hockey granule screening obtained is placed in mould cavity and be compacted; Then mixed liquor H is poured in mould, and together puts in liquid nitrogen freeze settled 6 hours, obtain solid-state after taking out the demoulding and mix Compound;The feature board for adsorption of aniline is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization.
The invention has the beneficial effects as follows, the feature board for adsorption of aniline the prepared benzene to containing in organic industrial sewage Amine has the advantages such as high adsorption capacity, adsorption capacity is high, adsorption rate is fast.
Detailed description of the invention
The present invention provides a kind of feature board for adsorption of aniline and preparation method thereof, illustrates with an embodiment below The present invention.
Embodiment 1.
(1) by 150 grams of BDOs and 350 grams of 4-acetamido-3-nitrobenzoic acid mix homogeneously, it is placed in 250mL In tool plug narrow mouth bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, obtain Mixed liquor A;
(2) 11.11 grams of polrvinyl chloride and 1.5 grams of N cyclohexyl 2 benzothiazole sulfenamides are joined mixed liquor A In, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 11.66g polystyrene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-dimethyl methyls Amide, stirs 1h under the conditions of 1000r/min, obtains mixed liquor C;
(4) it is the K of 0.85mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C, under the conditions of 1000r/min Stir 5 minutes, obtain mixed liquor D;
(5) 16.37g benzoyl peroxide is placed in 250mL tool plug narrow mouth bottle, adds 250mL chloroform, Stir 1h under the conditions of 1000r/min, be divided into equivalent 5 parts after shaking up, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3, mixed liquor E4, mixed liquor E5;
(6) 24.52g N-METHYLFORMAMIDE is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, To mixed liquor F1;
(7) it is the NaNO of 0.40mol/L by 5mL mixed liquor F1 and 15mL concentration3Join in mixed liquor E2, at 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor F2;
(8) 5mL mixed liquor F2 and the calcium chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E3, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F3;
(9) it is the NaNO of 0.30mol/L by 5mL mixed liquor F3 and 15mL concentration3Join in mixed liquor E4, at 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor F4;
(10) 5mL mixed liquor F4 and the calcium chloride that 15mL concentration is 0.35mol/L are joined in mixed liquor E5, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F;
(11) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 4.5% Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3;
(12) 40mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(13) 28mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(14) 32mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(15) 54mL mixed liquor H1 is added drop-wise in 40mL mixed liquor H2 under 1000r/min stirring condition, is mixed Liquid H4;
(16) 47mL mixed liquor H4 is added drop-wise in 35mL mixed liquor H3 under 1000r/min stirring condition, is mixed Liquid H;
(17) distilled water is spurted into equipped with quick freezing making ice hockey granule in the container of liquid nitrogen, select with after sieved through sieve Take the ice hockey granule that grain size scope is 50~100 μm, in ice hockey granule screening obtained is placed in mould cavity and be compacted; Then mixed liquor H is poured in mould, and together puts in liquid nitrogen freeze settled 6 hours, obtain solid-state after taking out the demoulding and mix Compound;The feature board for adsorption of aniline is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization.
The feature board for adsorption of aniline that use the inventive method prepare is presented herein below the organic industry containing aniline is given up Water has carried out adsorption test, further illustrates the present invention.
Organic industrial sewage containing aniline is carried out by the feature board for adsorption of aniline using the inventive method to prepare Adsorption test, result shows that the aniline of organic industrial sewage can effectively be adsorbed by this feature board: work as organic industry When the initial concentration of Aniline is 39.8mg/L, in 500mL organic industrial sewage, add 15g feature board, through 15 points After clock, the concentration of aniline is reduced to 0.1mg/L.

Claims (1)

1. feature board for adsorption of aniline and preparation method thereof, it is characterised in that specifically comprising the following steps that of the method
(1) by 150 grams of BDOs and 350 grams of 4-acetamido-3-nitrobenzoic acid mix homogeneously, it is placed in 250mL tool plug In narrow mouth bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, mixed Liquid A;
(2) 11.11 grams of polrvinyl chloride and 1.5 grams of N cyclohexyl 2 benzothiazole sulfenamides are joined in mixed liquor A, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 11.66g polystyrene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of DMFs, Under the conditions of 1000r/min, stir 1h, obtain mixed liquor C;
(4) it is the K of 0.85mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C, stirs 5 under the conditions of 1000r/min Minute, obtain mixed liquor D;
(5) 16.37g benzoyl peroxide is placed in 250mL tool plug narrow mouth bottle, adds 250mL chloroform, at 1000r/ Stir 1h under the conditions of min, after shaking up, be divided into equivalent 5 parts, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3, mixed liquor E4, mix Close liquid E5;
(6) 24.52g N-METHYLFORMAMIDE is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, mixed Close liquid F1;
(7) it is the NaNO of 0.40mol/L by 5mL mixed liquor F1 and 15mL concentration3Join in mixed liquor E2, at 1000r/min bar Stir 5 minutes under part, obtain mixed liquor F2;
(8) 5mL mixed liquor F2 and the calcium chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E3, at 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor F3;
(9) it is the NaNO of 0.30mol/L by 5mL mixed liquor F3 and 15mL concentration3Join in mixed liquor E4, at 1000r/min bar Stir 5 minutes under part, obtain mixed liquor F4;
(10) 5mL mixed liquor F4 and the calcium chloride that 15mL concentration is 0.35mol/L are joined in mixed liquor E5, at 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor F;
(11) 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 4.5% are sufficiently mixed, shake It is divided into equivalent 3 parts after even, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3;
(12) 40mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(13) 28mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(14) 32mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(15) 54mL mixed liquor H1 is added drop-wise in 40mL mixed liquor H2 under 1000r/min stirring condition, obtains mixed liquor H4;
(16) 47mL mixed liquor H4 is added drop-wise in 35mL mixed liquor H3 under 1000r/min stirring condition, obtains mixed liquor H;
(17) distilled water is spurted into equipped with quick freezing making ice hockey granule in the container of liquid nitrogen, choose grain with after sieved through sieve Footpath size range is the ice hockey granule of 50~100 μm, in ice hockey granule screening obtained is placed in mould cavity and be compacted;Then Mixed liquor H is poured in mould, and together puts in liquid nitrogen freeze settled 6 hours, after taking out the demoulding, obtain solid mixt; The feature board for adsorption of aniline is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization.
CN201610849670.XA 2016-09-24 2016-09-24 Feature board for adsorption of aniline and preparation method thereof Pending CN106215902A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120028796A1 (en) * 2010-07-29 2012-02-02 Sony Corporation Nicotine adsorbent, quinoline adsorbent, benzopyrene adsorbent, toluidine adsorbent, and carcinogen adsorbent
CN103464102A (en) * 2013-09-23 2013-12-25 北京师范大学 Porous composite adsorbing agent for removing stream substrate sludge contamination and preparation process of agent
CN103613208A (en) * 2013-12-12 2014-03-05 北京师范大学 Adsorption plate with high-efficient adsorption and enhanced biodegradation of petroleum hydrocarbon pollutants and preparation method thereof
CN103623793A (en) * 2013-12-12 2014-03-12 北京师范大学 Porous adsorption plate with multiple functions for petroleum hydrocarbon polluted water bodies and preparation method thereof
CN103623790A (en) * 2013-12-12 2014-03-12 北京师范大学 High-polymer functional material for adsorbing and treating organic chemical industry wastewater and preparation method thereof
CN103965835A (en) * 2014-05-13 2014-08-06 西南石油大学 Ultra-light magnetic oil absorption material and preparation method thereof
CN105632575A (en) * 2016-01-29 2016-06-01 北京师范大学 Hydroxyl-based modified magnetic material with radionuclide adsorption function and preparation method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120028796A1 (en) * 2010-07-29 2012-02-02 Sony Corporation Nicotine adsorbent, quinoline adsorbent, benzopyrene adsorbent, toluidine adsorbent, and carcinogen adsorbent
CN103464102A (en) * 2013-09-23 2013-12-25 北京师范大学 Porous composite adsorbing agent for removing stream substrate sludge contamination and preparation process of agent
CN103613208A (en) * 2013-12-12 2014-03-05 北京师范大学 Adsorption plate with high-efficient adsorption and enhanced biodegradation of petroleum hydrocarbon pollutants and preparation method thereof
CN103623793A (en) * 2013-12-12 2014-03-12 北京师范大学 Porous adsorption plate with multiple functions for petroleum hydrocarbon polluted water bodies and preparation method thereof
CN103623790A (en) * 2013-12-12 2014-03-12 北京师范大学 High-polymer functional material for adsorbing and treating organic chemical industry wastewater and preparation method thereof
CN103965835A (en) * 2014-05-13 2014-08-06 西南石油大学 Ultra-light magnetic oil absorption material and preparation method thereof
CN105632575A (en) * 2016-01-29 2016-06-01 北京师范大学 Hydroxyl-based modified magnetic material with radionuclide adsorption function and preparation method

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Application publication date: 20161214