CN106311180A - Functional plate for pyrrole adsorption and preparation method thereof - Google Patents
Functional plate for pyrrole adsorption and preparation method thereof Download PDFInfo
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- CN106311180A CN106311180A CN201610849696.4A CN201610849696A CN106311180A CN 106311180 A CN106311180 A CN 106311180A CN 201610849696 A CN201610849696 A CN 201610849696A CN 106311180 A CN106311180 A CN 106311180A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 title abstract description 11
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 title abstract description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 16
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- BHIWKHZACMWKOJ-UHFFFAOYSA-N methyl isobutyrate Chemical compound COC(=O)C(C)C BHIWKHZACMWKOJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 229920000305 Nylon 6,10 Polymers 0.000 claims abstract description 4
- 239000005062 Polybutadiene Substances 0.000 claims abstract description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 229960003750 ethyl chloride Drugs 0.000 claims abstract description 4
- 238000007710 freezing Methods 0.000 claims abstract description 4
- 230000008014 freezing Effects 0.000 claims abstract description 4
- WDAXFOBOLVPGLV-UHFFFAOYSA-N isobutyric acid ethyl ester Natural products CCOC(=O)C(C)C WDAXFOBOLVPGLV-UHFFFAOYSA-N 0.000 claims abstract description 4
- WRIRWRKPLXCTFD-UHFFFAOYSA-N malonamide Chemical compound NC(=O)CC(N)=O WRIRWRKPLXCTFD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920002857 polybutadiene Polymers 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- -1 polyhexamethylene sebacamide Polymers 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 66
- 150000003233 pyrroles Chemical class 0.000 claims description 19
- 239000008187 granular material Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 abstract 8
- 239000002245 particle Substances 0.000 abstract 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 abstract 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 abstract 1
- NVTRPRFAWJGJAJ-UHFFFAOYSA-L EDTA monocalcium salt Chemical compound [Ca+2].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O NVTRPRFAWJGJAJ-UHFFFAOYSA-L 0.000 abstract 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 abstract 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 abstract 1
- 235000019797 dipotassium phosphate Nutrition 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 238000009777 vacuum freeze-drying Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 239000010865 sewage Substances 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000004375 physisorption Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- 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
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- 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
- B01J20/0274—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 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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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
- B01J20/04—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
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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
-
- 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
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- 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
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- 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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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- 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
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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
- C02F2101/38—Organic compounds containing nitrogen
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a functional plate for pyrrole adsorption and a preparation method thereof. Chloroethane, 1,3-benzo dioxo-4-formaldehyde, N,N-dimethylformamide, polybutadiene and ethylenediaminetetraacetic acid dicalcium salt are prepared into a mixed solution B; polyhexamethylene sebacamide, N, N-dimethylformamide, K2HPO4 and methyl formate are prepared into a mixed solution D; bis(2,4-dichlorobenzoyl) peroxide, chloroform, malonamide, Ca(NO3)2 and aluminum chloride are prepared into a mixed solution F; the mixed solution B, the mixed solution D, the mixed solution F, methyl isobutyrate, polyethylene glycol and chloroform are prepared into a mixed solution H; distilled water is sprayed into a container with liquid nitrogen to prepare ice ball particles; ice ball particles with the particle diameter being 50 to 100 mum are put into a mold die cavity and are compactly pressed; then, the mixed solution H is cast into a mold and is subjected to freezing shaping for 6 hours in liquid nitrogen; the functional plate for pyrrole adsorption is obtained after the chloroform and the ice ball particles are removed through vacuum freeze drying.
Description
Technical field
The invention belongs to the processing technology field of organic industrial sewage, particularly to a kind of feature board for adsorbing pyrroles
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 pyrroles 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 pyrroles if this technology carries out popularization and application.But, the most scarce
Few adsorbing material processed for the organic industrial sewage containing pyrroles.
Summary of the invention
It is an object of the invention to provide a kind of for feature board adsorbing pyrroles and preparation method thereof.Its concrete steps are such as
Under:
(1) by 163.68 grams of ethyl chloride and 397.24 gram 1,3-benzo dioxy-4-formaldehyde mix homogeneously, it is placed in 250mL tool
In plug narrow mouth bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid A;
(2) 13.27g polybutadiene and the calcio-disodium edetate solution that 10mL concentration is 0.22mol/L are joined
In mixed liquor A, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 17.63g polyhexamethylene sebacamide is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-bis-
Methylformamide, stirs 1h under the conditions of 1000r/min, is divided into equivalent 5 parts after shaking up, and obtains mixed liquor C1, mixed liquor C2, mixes
Close liquid C3, mixed liquor C4, mixed liquor C5;
(4) it is the K of 0.91mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C1, under the conditions of 1000r/min
Stir 5 minutes, obtain mixed liquor D1;
(5) 5mL mixed liquor D1 and 10.6 grams of methyl formates are joined in mixed liquor C2, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D2;
(6) 5mL mixed liquor D2 and 10.3 grams of methyl formates are joined in mixed liquor C3, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D3;
(7) 5mL mixed liquor D3 and 10.0 grams of methyl formates are joined in mixed liquor C4, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D4;
(8) 5mL mixed liquor D4 and 9.7 grams of methyl formates are joined in mixed liquor C5, stir under the conditions of 1000r/min
5 minutes, obtain mixed liquor D;
(9) by 16.37g peroxidating two-2,4-dichloro-benzoyl is placed in 250mL tool plug narrow mouth bottle, adds 400mL
Chloroform, stirs 1h under the conditions of 1000r/min, is divided into equivalent 8 parts, obtains mixed liquor E1, mixed liquor E2, mixed liquor after shaking up
E3, mixed liquor E4, mixed liquor E5, mixed liquor E6, mixed liquor E7, mixed liquor E8;
(10) 29.47g Malondiamide is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid F1;
(11) by 5mL mixed liquor F1 and Ca (NO that 15mL concentration is 0.40mol/L3)2Join in mixed liquor E2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F2;
(12) 5mL mixed liquor F2 and the aluminum chloride that 15mL concentration is 0.65mol/L are joined in mixed liquor E3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F3;
(13) by 5mL mixed liquor F3 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F4;
(14) 5mL mixed liquor F4 and the aluminum chloride that 15mL concentration is 0.60mol/L are joined in mixed liquor E5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F5;
(15) by 5mL mixed liquor F5 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E6,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F6;
(16) 5mL mixed liquor F6 and the aluminum chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E7,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F7;
(17) 5mL mixed liquor F7 and the aluminum chloride that 15mL concentration is 0.50mol/L are joined in mixed liquor E8,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F;
(18) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 8.3%
Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3;
(19) 26mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(20) 24mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(21) 33mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(22) 47mL mixed liquor H1 is added drop-wise in 53mL mixed liquor H2 under 1000r/min stirring condition, is mixed
Liquid H4;
(23) 41mL mixed liquor H4 is added drop-wise in 59mL mixed liquor H3 under 1000r/min stirring condition, is mixed
Liquid H;
(24) 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 adsorbing pyrroles 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 adsorbing pyrroles the prepared pyrrole to containing in organic industrial sewage
Cough up and there is 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 for feature board adsorbing pyrroles and preparation method thereof, illustrates with an embodiment below
The present invention.
Embodiment 1.
(1) by 163.68 grams of ethyl chloride and 397.24 gram 1,3-benzo dioxy-4-formaldehyde mix homogeneously, it is placed in 250mL tool
In plug narrow mouth bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid A;
(2) 13.27g polybutadiene and the calcio-disodium edetate solution that 10mL concentration is 0.22mol/L are joined
In mixed liquor A, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 17.63g polyhexamethylene sebacamide is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-bis-
Methylformamide, stirs 1h under the conditions of 1000r/min, is divided into equivalent 5 parts after shaking up, and obtains mixed liquor C1, mixed liquor C2, mixes
Close liquid C3, mixed liquor C4, mixed liquor C5;
(4) it is the K of 0.91mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C1, under the conditions of 1000r/min
Stir 5 minutes, obtain mixed liquor D1;
(5) 5mL mixed liquor D1 and 10.6 grams of methyl formates are joined in mixed liquor C2, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D2;
(6) 5mL mixed liquor D2 and 10.3 grams of methyl formates are joined in mixed liquor C3, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D3;
(7) 5mL mixed liquor D3 and 10.0 grams of methyl formates are joined in mixed liquor C4, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquor D4;
(8) 5mL mixed liquor D4 and 9.7 grams of methyl formates are joined in mixed liquor C5, stir under the conditions of 1000r/min
5 minutes, obtain mixed liquor D;
(9) by 16.37g peroxidating two-2,4-dichloro-benzoyl is placed in 250mL tool plug narrow mouth bottle, adds 400mL
Chloroform, stirs 1h under the conditions of 1000r/min, is divided into equivalent 8 parts, obtains mixed liquor E1, mixed liquor E2, mixed liquor after shaking up
E3, mixed liquor E4, mixed liquor E5, mixed liquor E6, mixed liquor E7, mixed liquor E8;
(10) 29.47g Malondiamide is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid F1;
(11) by 5mL mixed liquor F1 and Ca (NO that 15mL concentration is 0.40mol/L3)2Join in mixed liquor E2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F2;
(12) 5mL mixed liquor F2 and the aluminum chloride that 15mL concentration is 0.65mol/L are joined in mixed liquor E3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F3;
(13) by 5mL mixed liquor F3 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F4;
(14) 5mL mixed liquor F4 and the aluminum chloride that 15mL concentration is 0.60mol/L are joined in mixed liquor E5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F5;
(15) by 5mL mixed liquor F5 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E6,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F6;
(16) 5mL mixed liquor F6 and the aluminum chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E7,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F7;
(17) 5mL mixed liquor F7 and the aluminum chloride that 15mL concentration is 0.50mol/L are joined in mixed liquor E8,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor F;
(18) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 8.3%
Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3;
(19) 26mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(20) 24mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(21) 33mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(22) 47mL mixed liquor H1 is added drop-wise in 53mL mixed liquor H2 under 1000r/min stirring condition, is mixed
Liquid H4;
(23) 41mL mixed liquor H4 is added drop-wise in 59mL mixed liquor H3 under 1000r/min stirring condition, is mixed
Liquid H;
(24) 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 adsorbing pyrroles is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization.
For adsorb the feature board of pyrroles organic industry containing pyrroles being given up of using the inventive method prepare is presented herein below
Water has carried out adsorption test, further illustrates the present invention.
Organic industrial sewage containing pyrroles is carried out by the feature board being used for adsorbing pyrroles using the inventive method to prepare
Adsorption test, result shows that the pyrroles of organic industrial sewage can effectively be adsorbed by this feature board: work as organic industry
When the initial concentration of pyrroles is 27.6mg/L in waste water, in 500mL organic industrial sewage, add 15g feature board, through 15 points
After clock, the concentration of pyrroles is reduced to 0.1mg/L.
Claims (1)
1. one kind is used for feature board adsorbing pyrroles and preparation method thereof, it is characterised in that specifically comprising the following steps that of the method
(1) by 163.68 grams of ethyl chloride and 397.24 gram 1,3-benzo dioxy-4-formaldehyde mix homogeneously, it is placed in 250mL tool plug thin
In opening reagent bottle, add 250 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor
A;
(2) 13.27g polybutadiene and the calcio-disodium edetate solution that 10mL concentration is 0.22mol/L are joined mixing
In liquid A, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquid B;
(3) 17.63g polyhexamethylene sebacamide is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-dimethyl
Methanamide, stirs 1h under the conditions of 1000r/min, is divided into equivalent 5 parts, obtains mixed liquor C1, mixed liquor C2, mixed liquor after shaking up
C3, mixed liquor C4, mixed liquor C5;
(4) it is the K of 0.91mol/L by 10mL concentration2HPO4Solution joins in mixed liquor C1, stirs under the conditions of 1000r/min
5 minutes, obtain mixed liquor D1;
(5) 5mL mixed liquor D1 and 10.6 grams of methyl formates are joined in mixed liquor C2, under the conditions of 1000r/min, stir 5 points
Clock, obtains mixed liquor D2;
(6) 5mL mixed liquor D2 and 10.3 grams of methyl formates are joined in mixed liquor C3, under the conditions of 1000r/min, stir 5 points
Clock, obtains mixed liquor D3;
(7) 5mL mixed liquor D3 and 10.0 grams of methyl formates are joined in mixed liquor C4, under the conditions of 1000r/min, stir 5 points
Clock, obtains mixed liquor D4;
(8) 5mL mixed liquor D4 and 9.7 grams of methyl formates are joined in mixed liquor C5, under the conditions of 1000r/min, stir 5 points
Clock, obtains mixed liquor D;
(9) by 16.37g peroxidating two-2,4-dichloro-benzoyl is placed in 250mL tool plug narrow mouth bottle, adds 400mL chlorine
Imitative, under the conditions of 1000r/min, stir 1h, after shaking up, be divided into equivalent 8 parts, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3,
Mixed liquor E4, mixed liquor E5, mixed liquor E6, mixed liquor E7, mixed liquor E8;
(10) 29.47g Malondiamide is entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor
F1;
(11) by 5mL mixed liquor F1 and Ca (NO that 15mL concentration is 0.40mol/L3)2Join in mixed liquor E2, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F2;
(12) 5mL mixed liquor F2 and the aluminum chloride that 15mL concentration is 0.65mol/L are joined in mixed liquor E3, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F3;
(13) by 5mL mixed liquor F3 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E4, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F4;
(14) 5mL mixed liquor F4 and the aluminum chloride that 15mL concentration is 0.60mol/L are joined in mixed liquor E5, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F5;
(15) by 5mL mixed liquor F5 and Ca (NO that 15mL concentration is 0.30mol/L3)2Join in mixed liquor E6, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F6;
(16) 5mL mixed liquor F6 and the aluminum chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E7, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F7;
(17) 5mL mixed liquor F7 and the aluminum chloride that 15mL concentration is 0.50mol/L are joined in mixed liquor E8, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F;
(18) 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 8.3% are sufficiently mixed, shake
It is divided into equivalent 3 parts after even, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3;
(19) 26mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1;
(20) 24mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2;
(21) 33mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3;
(22) 47mL mixed liquor H1 is added drop-wise in 53mL mixed liquor H2 under 1000r/min stirring condition, obtains mixed liquor H4;
(23) 41mL mixed liquor H4 is added drop-wise in 59mL mixed liquor H3 under 1000r/min stirring condition, obtains mixed liquor H;
(24) 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 adsorbing pyrroles is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization.
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