CN104475048A - Preparation method of crosslinking membrane for water processing - Google Patents

Preparation method of crosslinking membrane for water processing Download PDF

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Publication number
CN104475048A
CN104475048A CN201410618090.0A CN201410618090A CN104475048A CN 104475048 A CN104475048 A CN 104475048A CN 201410618090 A CN201410618090 A CN 201410618090A CN 104475048 A CN104475048 A CN 104475048A
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Prior art keywords
furfural
glucan
methyl acrylate
membrane
ether solution
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CN201410618090.0A
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Chinese (zh)
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华玉叶
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Individual
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Priority to CN201410618090.0A priority Critical patent/CN104475048A/en
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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
    • B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
    • B01J20/267—Cross-linked polymers
    • 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
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

A disclosed preparation method of a crosslinking membrane for water processing comprises the following steps: respectively weighing a certain amount of glucan, furfural and methyl acrylate, controlling the mass ratio of glucan, furfural and methyl acrylate to be 5-8:3-7:2-3, respectively dissolving glucan, furfural and methyl acrylate into an ethyl ether solution, then adding an initiator azodiisobutyronitrile and a cross-linking agent formaldehyde solution, continuing to stir, and keeping the temperature of 60-80 DEG C in a drying box for 1-24 h; stirring according to the rotation speed of 1000-3000 r/min for 2-4 min, so as to obtain a membrane casting liquid; employing a tape casting method to coat a glass sheet with the generated membrane casting liquid, performing vacuum drying at 60-80 DEG C, taking out and immersing in an ethyl ether solution for 2-4 h, and finally using ethanol and distilled water to wash for multiple times, and drying to obtain the crosslinking membrane. The preparation method is abundant in raw materials, simple in operation and low in energy consumption. The obtained crosslinking membrane is substantially improved in heavy-metal adsorption capacity, is easy to separate from wastewater, is recyclable and usable after being regenerated, is low in cost and does not easily cause secondary pollution.

Description

A kind of preparation method of the cross linking membrane for water treatment
Technical field
The present invention relates to a kind of preparation method of the cross linking membrane for water treatment.
Background technology
The method of current removal heavy metal ions in wastewater comprises the methods such as chemical precipitation, membrane technology, counter-infiltration and electrochemistry.But most process costs is higher, complicated operation, subsequent treatment difficulty.Wherein absorption method is lower, simple to operate and one of the method be widely adopted of process costs.The manufacture method (with reference to Unexamined Patent 4-132637 publication, Unexamined Patent 4-221630 publication, Unexamined Patent 4-367721 publication) of known several manufacturing chemistry adsorbed monomolecular film, the peel resistance of this chemical adsorption monomolecular film is strong, pore-free, there is nano level thickness, namely transparent high, have and do not affect the gloss of substrate surface and the transparency of base material.But the manufacture method due to existing such chemisorbed film is the active hydrogen generation desalination acid reaction of surfactant by chlorosilane system and substrate surface, forms coating, therefore produce harmful HCl gas when manufacturing film, there is very large problem.Also have alkoxysilane surface activating agent generation dealcoholization to form the trial of molecular film in addition, but exist can not easily film forming problem because reaction speed is slow.Also can consider to use dealcoholysis catalyst, but only add dealcoholysis catalyst, utilize the moisture in air that surfactant self is occurred crosslinked, there is the problem of inactivation.Namely in surface conditioning agent once containing water, then surfactant generation self-crosslinking before react with substrate surface, hinder the reaction in the solid liquid interface of substrate surface, be difficult to formation chemisorbed film.
In order to solve the problem, formed in the method for chemisorbed film at the substrate surface containing active hydrogen, the feature of the manufacture method of known chemisorbed film is, make at least alkoxyl silicone methane series surfactant, not containing the non-water solvent of active hydrogen and the mixed solution containing silanol condensation catalyst and aforementioned substrates surface contact, form the chemisorbed film of the covalent bond combination via siloxane bond on the surface in aforementioned substrates.Silanol condensation catalyst such as has at least one material being selected from carboxylic metallic salt, carboxylate metal's salt, carboxylic metallic salt polymer, carboxylic metallic salt chelate, titanate esters and titanate chelate class.(with reference to Unexamined Patent 8-337654 publication)
Summary of the invention
The object of the invention is to the preparation method proposing a kind of cross linking membrane for water treatment.
For reaching this object, the present invention by the following technical solutions:
A kind of preparation method of the cross linking membrane for water treatment, comprise the following steps: to take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 5-8:3-7:2-3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
This preparation method's abundant raw material, simple to operate, energy consumption is low.The adsorption capacity of gained cross linking membrane heavy metal improves greatly, and be easy to be separated from waste water, can be recycled after regeneration, cost is low, not easily causes secondary pollution.
Body embodiment
Embodiment 1
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:7:3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 2
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:7:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 3
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:6:3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 4
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:6:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 5
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:5:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 6
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:4:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 7
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:4:3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 8
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 7:3:3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 9
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 6:3:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 10
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 5:4:3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 11
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 5-8:3-7:2-3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 12
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 5:4:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 13
Take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 6:7:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
Embodiment 14
A certain amount of glucan, furfural and methyl acrylate will be taken respectively, the mass ratio of glucan, furfural and methyl acrylate is 5:3:2, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.

Claims (1)

1. the preparation method for the cross linking membrane of water treatment, it is characterized in that, comprise the following steps: to take a certain amount of glucan, furfural and methyl acrylate respectively, the mass ratio of glucan, furfural and methyl acrylate is 5-8:3-7:2-3, respectively glucan, furfural and methyl acrylate are dissolved in diethyl ether solution, add initator azodiisobutyronitrile and crosslinking agent formalin subsequently, continue to stir, in drying box, be incubated 1-24 hour at 60 ~ 80 DEG C; Be that 1000-3000r/min stirred after 2-4 minute by rotating speed, obtain casting solution; Stream method is prolonged in employing, is applied on the glass sheet by the casting solution generated, and after 60-80 DEG C of vacuum drying, taking-up diethyl ether solution soaks 2-4 hour, and finally repeatedly wash with ethanol and distilled water, drying obtains cross linking membrane.
CN201410618090.0A 2014-11-05 2014-11-05 Preparation method of crosslinking membrane for water processing Pending CN104475048A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105440299A (en) * 2015-08-11 2016-03-30 无锡桥阳机械制造有限公司 Preparation method for hydrophilic modified film

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04132637A (en) * 1990-09-26 1992-05-06 Matsushita Electric Ind Co Ltd Glass and production thereof
EP0511548A2 (en) * 1991-04-30 1992-11-04 Matsushita Electric Industrial Co., Ltd. Chemically adsorbed film and method of manufacturing the same
EP0748658A2 (en) * 1995-06-14 1996-12-18 Matsushita Electric Industrial Co., Ltd A method for manufacturing a chemically adsorbed film and a chemical adsorbent solution for the method
CN102430395A (en) * 2011-10-10 2012-05-02 沈阳理工大学 Method for preparing chitosan cross-linking vanillin absorbing membrane
CN102430391A (en) * 2011-09-11 2012-05-02 大连理工大学 Preparation method of metal ion imprinted chitosan crosslinked membrane adsorbent and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04132637A (en) * 1990-09-26 1992-05-06 Matsushita Electric Ind Co Ltd Glass and production thereof
EP0511548A2 (en) * 1991-04-30 1992-11-04 Matsushita Electric Industrial Co., Ltd. Chemically adsorbed film and method of manufacturing the same
EP0748658A2 (en) * 1995-06-14 1996-12-18 Matsushita Electric Industrial Co., Ltd A method for manufacturing a chemically adsorbed film and a chemical adsorbent solution for the method
CN102430391A (en) * 2011-09-11 2012-05-02 大连理工大学 Preparation method of metal ion imprinted chitosan crosslinked membrane adsorbent and application thereof
CN102430395A (en) * 2011-10-10 2012-05-02 沈阳理工大学 Method for preparing chitosan cross-linking vanillin absorbing membrane

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105440299A (en) * 2015-08-11 2016-03-30 无锡桥阳机械制造有限公司 Preparation method for hydrophilic modified film

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