CN106215903A - For feature board adsorbing phthalic acid ester and preparation method thereof - Google Patents
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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
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
- B01J20/28—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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
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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
- C02F1/281—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
- 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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- 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
- C02F2101/34—Organic compounds containing oxygen
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Abstract
The invention discloses for feature board adsorbing phthalic acid ester and preparation method thereof.1,3-propanedicarboxylic acid, methylprednisolone second propionic ester, N, N dimethylformamide, Merlon, zinc isopropyl xanthate are made mixed liquid B；By polypropylene, N, N dimethylformamide, 4 acetamido 3 nitrobenzoic acids make mixed liquor D；By peroxide acid tert-amyl acetate, chloroform, N methyl caprolactam, Ca (NO3)2, 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 adsorbing phthalic acid ester.
Description
Technical field
The invention belongs to the processing technology field of organic industrial sewage, be used for adsorbing phthalic acid ester particularly to one
Feature board 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 phthalic acid ester is a kind of up-and-coming industrial wastewater
Treatment technology, needs exploitation to have the absorption of excellent absorption property to phthalic acid ester if this technology carries out popularization and application
Agent.But, the most also lack the adsorbing material processed for the organic industrial sewage containing phthalic acid ester.
Summary of the invention
It is an object of the invention to provide a kind of for feature board adsorbing phthalic acid ester and preparation method thereof.It is concrete
Step is as follows:
(1) by 169.39g 1,3-propanedicarboxylic acid and 384.57g methylprednisolone second propionic ester mix homogeneously, it is placed in 250mL tool plug
In narrow mouth bottle, add 500 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, divide after shaking up
Become equivalent 5 parts, obtain mixed liquor A 1, mixed liquor A 2, mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(2) 12.24g Merlon is joined in mixed liquor A 1, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid B1；
(3) 5mL mixed liquid B 1 and 10.6g zinc isopropyl xanthate is joined in mixed liquor A 2, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 2；
(4) 5mL mixed liquid B 2 and 10.2g zinc isopropyl xanthate is joined in mixed liquor A 3, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 3；
(5) 5mL mixed liquid B 3 and 9.8g zinc isopropyl xanthate is joined in mixed liquor A 4, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 4；
(6) 5mL mixed liquid B 4 and 9.4g zinc isopropyl xanthate is joined in mixed liquor A 5, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B；
(7) 11.17g polypropylene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-dimethyl formyls
Amine, under the conditions of 1000r/min stir 1h, be divided into equivalent 5 parts after shaking up, obtain mixed liquor C1, mixed liquor C2, mixed liquor C3,
Mixed liquor C4, mixed liquor C5；
(8) 10.8 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C1, under the conditions of 1000r/min
Stir 5 minutes, obtain mixed liquor D1；
(9) 5mL mixed liquor D1 and 10.1 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D2；
(10) 5mL mixed liquor D2 and 9.4 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D3；
(11) 5mL mixed liquor D3 and 8.7 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D4；
(12) 5mL mixed liquor D4 and 8.0 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D；
(13) 17.66g peroxide acid tert-amyl acetate is placed in 250mL tool plug narrow mouth bottle, adds 250mL chlorine
Imitative, under the conditions of 1000r/min, stir 1h, after shaking up, be divided into equivalent 5 parts, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3,
Mixed liquor E4, mixed liquor E5；
(14) 22.26 grams of N-methyl caprolactam are entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min,
Obtain mixed liquor F1；
(15) 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；
(16) 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；
(17) 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；
(18) 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；
(19) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 7.4%
Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3；
(20) 24mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1；
(21) 21mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2；
(22) 29mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3；
(23) 41mL mixed liquor H1 is added drop-wise in 59mL mixed liquor H2 under 1000r/min stirring condition, is mixed
Liquid H4；
(24) 32mL mixed liquor H4 is added drop-wise in 68mL mixed liquor H3 under 1000r/min stirring condition, is mixed
Liquid H；
(25) 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；Obtain for adsorbing phthalic acid ester after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization
Feature board.
The invention has the beneficial effects as follows, prepare for adsorbing the feature board of phthalic acid ester in organic industrial sewage
The phthalic acid ester contained 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 for feature board adsorbing phthalic acid ester and preparation method thereof, below with an enforcement
Example illustrates the present invention.
Embodiment 1.
(1) by 169.39g 1,3-propanedicarboxylic acid and 384.57g methylprednisolone second propionic ester mix homogeneously, it is placed in 250mL tool plug
In narrow mouth bottle, add 500 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, divide after shaking up
Become equivalent 5 parts, obtain mixed liquor A 1, mixed liquor A 2, mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(2) 12.24g Merlon is joined in mixed liquor A 1, stir 5 minutes under the conditions of 1000r/min, mixed
Close liquid B1；
(3) 5mL mixed liquid B 1 and 10.6g zinc isopropyl xanthate is joined in mixed liquor A 2, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 2；
(4) 5mL mixed liquid B 2 and 10.2g zinc isopropyl xanthate is joined in mixed liquor A 3, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 3；
(5) 5mL mixed liquid B 3 and 9.8g zinc isopropyl xanthate is joined in mixed liquor A 4, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B 4；
(6) 5mL mixed liquid B 4 and 9.4g zinc isopropyl xanthate is joined in mixed liquor A 5, in 1000r/min condition
Lower stirring 5 minutes, obtains mixed liquid B；
(7) 11.17g polypropylene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of N, N-dimethyl formyls
Amine, under the conditions of 1000r/min stir 1h, be divided into equivalent 5 parts after shaking up, obtain mixed liquor C1, mixed liquor C2, mixed liquor C3,
Mixed liquor C4, mixed liquor C5；
(8) 10.8 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C1, under the conditions of 1000r/min
Stir 5 minutes, obtain mixed liquor D1；
(9) 5mL mixed liquor D1 and 10.1 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C2,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D2；
(10) 5mL mixed liquor D2 and 9.4 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C3,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D3；
(11) 5mL mixed liquor D3 and 8.7 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C4,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D4；
(12) 5mL mixed liquor D4 and 8.0 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C5,
Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor D；
(13) 17.66g peroxide acid tert-amyl acetate is placed in 250mL tool plug narrow mouth bottle, adds 250mL chlorine
Imitative, under the conditions of 1000r/min, stir 1h, after shaking up, be divided into equivalent 5 parts, obtain mixed liquor E1, mixed liquor E2, mixed liquor E3,
Mixed liquor E4, mixed liquor E5；
(14) 22.26 grams of N-methyl caprolactam are entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min,
Obtain mixed liquor F1；
(15) 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；
(16) 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；
(17) 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；
(18) 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；
(19) by the most mixed to 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 7.4%
Close, be divided into equivalent 3 parts after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3；
(20) 24mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1；
(21) 21mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2；
(22) 29mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3；
(23) 41mL mixed liquor H1 is added drop-wise in 59mL mixed liquor H2 under 1000r/min stirring condition, is mixed
Liquid H4；
(24) 32mL mixed liquor H4 is added drop-wise in 68mL mixed liquor H3 under 1000r/min stirring condition, is mixed
Liquid H；
(25) 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；Obtain for adsorbing phthalic acid ester after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization
Feature board.
The feature board for adsorb phthalic acid ester that use the inventive method prepare is presented herein below to containing O-phthalic
The organic industrial sewage of acid esters has carried out adsorption test, further illustrates the present invention.
What utilization the inventive method prepared is used for adsorbing the feature board of phthalic acid ester to containing phthalic acid ester
Organic industrial sewage has carried out adsorption test, and result shows that the phthalic acid ester of organic industrial sewage can be entered by this feature board
The effective absorption of row: when the initial concentration of phthalic acid ester is 34.7mg/L in organic industrial sewage, to the organic work of 500mL
Adding 15g feature board in industry waste water, after 15 minutes, the concentration of phthalic acid ester is reduced to 0.1mg/L.
Claims (1)
1. one kind is used for feature board adsorbing phthalic acid ester and preparation method thereof, it is characterised in that the concrete step of the method
Rapid as follows:
(1) by 169.39g 1,3-propanedicarboxylic acid and 384.57g methylprednisolone second propionic ester mix homogeneously, it is placed in 250mL tool and fills in thin mouth
In reagent bottle, add 500 milliliters of DMFs, stir 5 minutes under the conditions of 1000r/min, be divided into after shaking up
Measure 5 parts, obtain mixed liquor A 1, mixed liquor A 2, mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(2) 12.24g Merlon is joined in mixed liquor A 1, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor
B1；
(3) 5mL mixed liquid B 1 and 10.6g zinc isopropyl xanthate is joined in mixed liquor A 2, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquid B 2；
(4) 5mL mixed liquid B 2 and 10.2g zinc isopropyl xanthate is joined in mixed liquor A 3, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquid B 3；
(5) 5mL mixed liquid B 3 and 9.8g zinc isopropyl xanthate is joined in mixed liquor A 4, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquid B 4；
(6) 5mL mixed liquid B 4 and 9.4g zinc isopropyl xanthate is joined in mixed liquor A 5, stir under the conditions of 1000r/min
Mix 5 minutes, obtain mixed liquid B；
(7) 11.17g polypropylene is placed in 250mL tool plug narrow mouth bottle, adds 250 milliliters of DMFs,
Stir 1h under the conditions of 1000r/min, be divided into equivalent 5 parts after shaking up, obtain mixed liquor C1, mixed liquor C2, mixed liquor C3, mixed liquor
C4, mixed liquor C5；
(8) 10.8 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C1, under the conditions of 1000r/min, stir 5
Minute, obtain mixed liquor D1；
(9) 5mL mixed liquor D1 and 10.1 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C2, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor D2；
(10) 5mL mixed liquor D2 and 9.4 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C3, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor D3；
(11) 5mL mixed liquor D3 and 8.7 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C4, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor D4；
(12) 5mL mixed liquor D4 and 8.0 grams of 4-acetamido-3-nitrobenzoic acids are joined in mixed liquor C5, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor D；
(13) 17.66g peroxide acid tert-amyl acetate 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；
(14) 22.26 grams of N-methyl caprolactam are entered in mixed liquor E1, stir 5 minutes under the conditions of 1000r/min, obtain
Mixed liquor F1；
(15) 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；
(16) 5mL mixed liquor F2 and the calcium chloride that 15mL concentration is 0.55mol/L are joined in mixed liquor E3, at 1000r/
Stir 5 minutes under the conditions of min, obtain mixed liquor F3；
(17) 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；
(18) 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；
(19) 140mL methyl isobutyrate and the Polyethylene Glycol chloroformic solution that 160mL mass fraction is 7.4% are sufficiently mixed, shake
It is divided into equivalent 3 parts after even, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3；
(20) 24mL mixed liquid B is added drop-wise in mixed liquor G1 under 1000r/min stirring condition, obtains mixed liquor H1；
(21) 21mL mixed liquor D is added drop-wise in mixed liquor G2 under 1000r/min stirring condition, obtains mixed liquor H2；
(22) 29mL mixed liquor F is added drop-wise in mixed liquor G3 under 1000r/min stirring condition, obtains mixed liquor H3；
(23) 41mL mixed liquor H1 is added drop-wise in 59mL mixed liquor H2 under 1000r/min stirring condition, obtains mixed liquor H4；
(24) 32mL mixed liquor H4 is added drop-wise in 68mL mixed liquor H3 under 1000r/min stirring condition, obtains mixed liquor H；
(25) 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 function for adsorbing phthalic acid ester is obtained after chloroform and ice hockey granule are removed in this solid mixt vacuum lyophilization
Plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610849702.6A CN106215903A (en) | 2016-09-24 | 2016-09-24 | For feature board adsorbing phthalic acid ester and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610849702.6A CN106215903A (en) | 2016-09-24 | 2016-09-24 | For feature board adsorbing phthalic acid ester and preparation method thereof |
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Application publication date: 20161214 |