CN106362710A - Functional board for adsorbing chloroalkene and preparation method of functional board - Google Patents
Functional board for adsorbing chloroalkene and preparation method of functional board Download PDFInfo
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- CN106362710A CN106362710A CN201610849713.4A CN201610849713A CN106362710A CN 106362710 A CN106362710 A CN 106362710A CN 201610849713 A CN201610849713 A CN 201610849713A CN 106362710 A CN106362710 A CN 106362710A
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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
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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- Chemical Kinetics & Catalysis (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a functional board for adsorbing chloroalkene and a preparation method of the functional board. The preparation method comprises the following steps: preparing butyric acid, trichloracetic aldehyde, N,N-dimethylformamide, N-cyclohexyl-2-benzothiazolesulfenamide into a mixed solution B; preparing nylon 66, N,N-dimethylformamide, (NH4)2HPO4 and 1,3-benzodioxole-4-formaldehyde into a mixed solution D; preparing bis-4-chlorobenzoyl peroxide, chloroform, 2-hydroxyisobutyramide, NH4NO3 and sodium chloride into a mixed solution F; preparing the mixed solution B, the mixed solution D, the mixed liquid F, methyl isobutyrate, polyethylene glycol and chloroform into a mixed solution H; spraying distilled water into a container filled with liquid nitrogen to form ice ball particles; storing the ice ball particles with the particle sizes of 50 to 100mu m in a die cavity and compacting; then pouring the mixed liquid H into a die and freezing and shaping in the liquid nitrogen for 6 hours; performing vacuum freeze drying to remove the chloroform and the ice ball particles, thus obtaining the functional board for adsorbing the chloroalkene.
Description
Technical field
The invention belongs to the processing technology field of organic industrial sewage, particularly to a kind of work(for adsorbing chloroalkene
Energy plate and preparation method thereof.
Background technology
Absorption method is that adsorbent is mixed with pending waste water phase, and one or more of waste water pollutant are adsorbed, some
Pollutant are reclaimed or are removed, so that the method that waste water is purified, the method has preferably to high concentrated organic wastewater
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 parse, reusing
By force；Mechanical strength is good etc..The most frequently used adsorbing material of absorption organic pollution can be divided into physisorption material at present, and chemistry is inhaled
Enclosure material and biological adsorption material.Wherein, the active charcoal of physisorption material, molecular sieve, zeolite, active hargil and clay minerals
Etc. the solid with high-specific surface area, have the advantages that eliminating efficiency height, enrichment function are strong, but it is poor, easily to there is also stability
Desorption, easily the deficiency such as affected by temperature change.Chemisorbed material mainly includes silica gel, synthetic fibers, resin, utilizes bioid
Molecularly imprinted polymer of and Polymer Synthesizing etc..Conventional biological adsorption material has broad leaved plant, funguses, soil and water
In microorganism etc..
Processing the organic industrial sewage containing chloroalkene with absorption method is a kind of up-and-coming Industrial Wastewater Treatment
Technology, needs exploitation to have the adsorbent of excellent absorption property to chloroalkene if this technology is carried out popularization and application.But,
Also lack the adsorbing material processing for the organic industrial sewage containing chloroalkene at present.
Content of the invention
It is an object of the invention to provide a kind of for adsorbing feature board of chloroalkene and preparation method thereof.Its concrete steps
As follows:
(1) by 176.78 grams of butanoic acid and 429.34 grams of Chloral mix homogeneously, it is placed in 250ml tool plug narrow mouth bottle
In, add 250 milliliters of n, n- dimethylformamide, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor a；
(2) poly- for 11.37g isobutyl and 10.21 grams of n- cyclohexyl -2-[4-morpholinodithio sulfenamides are added in mixed liquor a,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor b；
(3) 14.67g polyhexamethylene adipamide 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 5 parts of equivalent after shaking up, and obtains mixed liquor c1, mixed liquor c2, mixes
Close liquid c3, mixed liquor c4, mixed liquor c5；
(4) (the nh for 0.74mol/l by 10ml concentration4)2hpo4Solution is added in mixed liquor c1, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d1；
(5) 5ml mixed liquor d1 and 8.6 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c2, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d2；
(6) 5ml mixed liquor d2 and 8.3 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c3, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d3；
(7) 5ml mixed liquor d3 and 8.0 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c4, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d4；
(8) 5ml mixed liquor d4 and 7.7 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c5, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d；
(9) 16.34g peroxidating two -4- chlorobenzoyl is placed in 250ml tool plug narrow mouth bottle, adds 250ml chlorine
Imitative, stir 1h under the conditions of 1000r/min, after shaking up, be divided into 5 parts of equivalent, obtain mixed liquor e1, mixed liquor e2, mixed liquor e3,
Mixed liquor e4, mixed liquor e5；
(10) 21.26 grams of 2- hydroxy-isobutyric amide are entered in mixed liquor e1, stir 5 minutes under the conditions of 1000r/min,
Obtain mixed liquor f1；
(11) nh for 0.40mol/l by 5ml mixed liquor f1 and 15ml concentration4no3It is added in mixed liquor e2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f2；
(12) by 5ml mixed liquor f2 and 15ml concentration, the sodium chloride for 0.55mol/l is added in mixed liquor e3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f3；
(13) nh for 0.30mol/l by 5ml mixed liquor f3 and 15ml concentration4no3It is added in mixed liquor e4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f4；
(14) by 5ml mixed liquor f4 and 15ml concentration, the sodium chloride for 0.35mol/l is added in mixed liquor e5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f；
(15) will be fully mixed to 140ml methyl isobutyrate and Polyethylene Glycol chloroformic solution that 160ml mass fraction is 7.4%
Close, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor g1, mixed liquor g2, mixed liquor g3；
(16) 38ml mixed liquor b is added drop-wise in mixed liquor g1 under 1000r/min stirring condition, obtains mixed liquor h1；
(17) 22ml mixed liquor d is added drop-wise in mixed liquor g2 under 1000r/min stirring condition, obtains mixed liquor h2；
(18) 43ml mixed liquor f is added drop-wise in mixed liquor g3 under 1000r/min stirring condition, obtains mixed liquor h3；
(19) 34ml mixed liquor h1 is added drop-wise in 66ml mixed liquor h2 under 1000r/min stirring condition, is mixed
Liquid h4；
(20) 42ml mixed liquor h4 is added drop-wise in 58ml mixed liquor h3 under 1000r/min stirring condition, is mixed
Liquid h；
(21) distilled water is spurted into and make ice hockey granule equipped with quick freezing in the container of liquid nitrogen, with selecting after sieved through sieve
Take the ice hockey granule that grain size scope is 50～100 μm, the ice hockey granule that screening is obtained is placed in mould cavity and is compacted；
Then mixed liquor h is poured in mould, and together puts into freeze settled 6 hours in liquid nitrogen, obtain solid-state after taking out the demoulding and mix
Compound；This solid mixt vacuum lyophilization is removed the function of obtaining after chloroform and ice hockey granule for adsorbing chloroalkene
Plate.
The invention has the beneficial effects as follows, the prepared feature board for adsorbing chloroalkene contains in organic industrial sewage
Chloroalkene have the advantages that high adsorption capacity, adsorption capacity be high, adsorption rate is fast.
Specific embodiment
The present invention provide a kind of for adsorbing feature board of chloroalkene and preparation method thereof, below with an embodiment come
The present invention is described.
Embodiment 1.
(1) by 176.78 grams of butanoic acid and 429.34 grams of Chloral mix homogeneously, it is placed in 250ml tool plug narrow mouth bottle
In, add 250 milliliters of n, n- dimethylformamide, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor a；
(2) poly- for 11.37g isobutyl and 10.21 grams of n- cyclohexyl -2-[4-morpholinodithio sulfenamides are added in mixed liquor a,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor b；
(3) 14.67g polyhexamethylene adipamide 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 5 parts of equivalent after shaking up, and obtains mixed liquor c1, mixed liquor c2, mixes
Close liquid c3, mixed liquor c4, mixed liquor c5；
(4) (the nh for 0.74mol/l by 10ml concentration4)2hpo4Solution is added in mixed liquor c1, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d1；
(5) 5ml mixed liquor d1 and 8.6 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c2, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d2；
(6) 5ml mixed liquor d2 and 8.3 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c3, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d3；
(7) 5ml mixed liquor d3 and 8.0 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c4, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d4；
(8) 5ml mixed liquor d4 and 7.7 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c5, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor d；
(9) 16.34g peroxidating two -4- chlorobenzoyl is placed in 250ml tool plug narrow mouth bottle, adds 250ml chlorine
Imitative, stir 1h under the conditions of 1000r/min, after shaking up, be divided into 5 parts of equivalent, obtain mixed liquor e1, mixed liquor e2, mixed liquor e3,
Mixed liquor e4, mixed liquor e5；
(10) 21.26 grams of 2- hydroxy-isobutyric amide are entered in mixed liquor e1, stir 5 minutes under the conditions of 1000r/min,
Obtain mixed liquor f1；
(11) nh for 0.40mol/l by 5ml mixed liquor f1 and 15ml concentration4no3It is added in mixed liquor e2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f2；
(12) by 5ml mixed liquor f2 and 15ml concentration, the sodium chloride for 0.55mol/l is added in mixed liquor e3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f3；
(13) nh for 0.30mol/l by 5ml mixed liquor f3 and 15ml concentration4no3It is added in mixed liquor e4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f4；
(14) by 5ml mixed liquor f4 and 15ml concentration, the sodium chloride for 0.35mol/l is added in mixed liquor e5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor f；
(15) will be fully mixed to 140ml methyl isobutyrate and Polyethylene Glycol chloroformic solution that 160ml mass fraction is 7.4%
Close, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor g1, mixed liquor g2, mixed liquor g3；
(16) 38ml mixed liquor b is added drop-wise in mixed liquor g1 under 1000r/min stirring condition, obtains mixed liquor h1；
(17) 22ml mixed liquor d is added drop-wise in mixed liquor g2 under 1000r/min stirring condition, obtains mixed liquor h2；
(18) 43ml mixed liquor f is added drop-wise in mixed liquor g3 under 1000r/min stirring condition, obtains mixed liquor h3；
(19) 34ml mixed liquor h1 is added drop-wise in 66ml mixed liquor h2 under 1000r/min stirring condition, is mixed
Liquid h4；
(20) 42ml mixed liquor h4 is added drop-wise in 58ml mixed liquor h3 under 1000r/min stirring condition, is mixed
Liquid h；
(21) distilled water is spurted into and make ice hockey granule equipped with quick freezing in the container of liquid nitrogen, with selecting after sieved through sieve
Take the ice hockey granule that grain size scope is 50～100 μm, the ice hockey granule that screening is obtained is placed in mould cavity and is compacted；
Then mixed liquor h is poured in mould, and together puts into freeze settled 6 hours in liquid nitrogen, obtain solid-state after taking out the demoulding and mix
Compound；This solid mixt vacuum lyophilization is removed the function of obtaining after chloroform and ice hockey granule for adsorbing chloroalkene
Plate.
Feature board for adsorb chloroalkene with the inventive method be obtained is presented herein below to be had to containing chloroalkene
Machine industrial wastewater has carried out adsorption test, further illustrates the present invention.
The feature board for adsorbing chloroalkene being obtained with the inventive method is to the organic industry containing chloroalkene
Waste water has carried out adsorption test, and result shows that this feature board effectively can be inhaled to the chloroalkene of organic industrial sewage
Attached: when the initial concentration of chloroalkene in organic industrial sewage is 37.4mg/l, to add in 500ml organic industrial sewage
15g feature board, after 15 minutes, the concentration of chloroalkene is reduced to 0.1mg/l.
Claims (1)
1. a kind of for adsorb feature board of chloroalkene and preparation method thereof it is characterised in that the concrete steps of the method such as
Under:
(1) by 176.78 grams of butanoic acid and 429.34 grams of Chloral mix homogeneously, it is placed in 250ml tool plug narrow mouth bottle, plus
Enter 250 milliliters of n, n- dimethylformamide, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor a；
(2) poly- for 11.37g isobutyl and 10.21 grams of n- cyclohexyl -2-[4-morpholinodithio sulfenamides are added in mixed liquor a,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor b；
(3) 14.67g polyhexamethylene adipamide 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 5 parts of equivalent, obtains mixed liquor c1, mixed liquor c2, mixed liquor after shaking up
C3, mixed liquor c4, mixed liquor c5；
(4) (the nh for 0.74mol/l by 10ml concentration4)2hpo4Solution is added in mixed liquor c1, under the conditions of 1000r/min
Stirring 5 minutes, obtains mixed liquor d1；
(5) 5ml mixed liquor d1 and 8.6 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c2, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d2；
(6) 5ml mixed liquor d2 and 8.3 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c3, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d3；
(7) 5ml mixed liquor d3 and 8.0 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c4, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d4；
(8) 5ml mixed liquor d4 and 7.7 grams of 1,3- benzo dioxy -4- formaldehyde are added in mixed liquor c5, in 1000r/min bar
Stir 5 minutes under part, obtain mixed liquor d；
(9) 16.34g peroxidating two -4- chlorobenzoyl is placed in 250ml tool plug narrow mouth bottle, adds 250ml chloroform,
Stir 1h under the conditions of 1000r/min, be divided into 5 parts of equivalent after shaking up, obtain mixed liquor e1, mixed liquor e2, mixed liquor e3, mixed liquor
E4, mixed liquor e5；
(10) 21.26 grams of 2- hydroxy-isobutyric amide are entered in mixed liquor e1, stir 5 minutes under the conditions of 1000r/min, obtain
Mixed liquor f1；
(11) nh for 0.40mol/l by 5ml mixed liquor f1 and 15ml concentration4no3It is added in mixed liquor e2, in 1000r/min
Under the conditions of stir 5 minutes, obtain mixed liquor f2；
(12) by 5ml mixed liquor f2 and 15ml concentration, the sodium chloride for 0.55mol/l is added in mixed liquor e3, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor f3；
(13) nh for 0.30mol/l by 5ml mixed liquor f3 and 15ml concentration4no3It is added in mixed liquor e4, in 1000r/min
Under the conditions of stir 5 minutes, obtain mixed liquor f4；
(14) by 5ml mixed liquor f4 and 15ml concentration, the sodium chloride for 0.35mol/l is added in mixed liquor e5, in 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor f；
(15) 140ml methyl isobutyrate and Polyethylene Glycol chloroformic solution that 160ml mass fraction is 7.4% are sufficiently mixed, shake
It is divided into 3 parts of equivalent after even, obtain mixed liquor g1, mixed liquor g2, mixed liquor g3；
(16) 38ml mixed liquor b is added drop-wise in mixed liquor g1 under 1000r/min stirring condition, obtains mixed liquor h1；
(17) 22ml mixed liquor d is added drop-wise in mixed liquor g2 under 1000r/min stirring condition, obtains mixed liquor h2；
(18) 43ml mixed liquor f is added drop-wise in mixed liquor g3 under 1000r/min stirring condition, obtains mixed liquor h3；
(19) 34ml mixed liquor h1 is added drop-wise in 66ml mixed liquor h2 under 1000r/min stirring condition, obtains mixed liquor h4；
(20) 42ml mixed liquor h4 is added drop-wise in 58ml mixed liquor h3 under 1000r/min stirring condition, obtains mixed liquor h；
(21) distilled water is spurted into and make ice hockey granule equipped with quick freezing in the container of liquid nitrogen, with choosing grain after sieved through sieve
Footpath size range is 50～100 μm of ice hockey granule, and the ice hockey granule that screening is obtained is placed in mould cavity and is compacted；Then
Mixed liquor h is poured in mould, and together puts into freeze settled 6 hours in liquid nitrogen, after taking out the demoulding, obtain solid mixt；
This solid mixt vacuum lyophilization is removed the feature board obtaining after chloroform and ice hockey granule for adsorbing chloroalkene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610849713.4A CN106362710A (en) | 2016-09-24 | 2016-09-24 | Functional board for adsorbing chloroalkene and preparation method of functional board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610849713.4A CN106362710A (en) | 2016-09-24 | 2016-09-24 | Functional board for adsorbing chloroalkene and preparation method of functional board |
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| CN106362710A true CN106362710A (en) | 2017-02-01 |
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| CN201610849713.4A Pending CN106362710A (en) | 2016-09-24 | 2016-09-24 | Functional board for adsorbing chloroalkene and preparation method of functional board |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539225A (en) * | 2013-10-30 | 2014-01-29 | 北京师范大学 | Internal-circulating fluidized bed electro-catalytic reactor for treating chemical organic wastewater and operation conditions of reactor |
| 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 |
| CN103965835A (en) * | 2014-05-13 | 2014-08-06 | 西南石油大学 | Ultra-light magnetic oil absorption material and preparation method thereof |
-
2016
- 2016-09-24 CN CN201610849713.4A patent/CN106362710A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539225A (en) * | 2013-10-30 | 2014-01-29 | 北京师范大学 | Internal-circulating fluidized bed electro-catalytic reactor for treating chemical organic wastewater and operation conditions of reactor |
| 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 |
| CN103965835A (en) * | 2014-05-13 | 2014-08-06 | 西南石油大学 | Ultra-light magnetic oil absorption material and preparation method thereof |
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Application publication date: 20170201 |