CN105367737A - Preparation method of multiwalled carbon nanotube modified reticulated polyurethane microbial carrier - Google Patents
Preparation method of multiwalled carbon nanotube modified reticulated polyurethane microbial carrier Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
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- C08G18/4804—Two or more polyethers of different physical or chemical nature
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/02—Enzymes or microbial cells immobilised on or in an organic carrier
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- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- C08G2270/00—Compositions for creating interpenetrating networks
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Abstract
The invention belongs to the technical of microbial carrier preparation method, and relates to a preparation method of a multiwalled carbon nanotube modified reticulated polyurethane microbial carrier. The preparation method comprises following steps: vinyl polyether polyol, polyether polyol, polyester polyol, H2O, silicone oil, a stannum catalyst, an amine catalyst, and an olefin monomer are delivered into a reaction kettle for uniform mixing, multiwalled carbon nanotube is added for uniform stirring, and an obtained mixture is subjected to thermal insulation treatment so as to obtain a component 1; an isocyanate, and a free radical polymerization initiator are delivered into a reaction kettle for uniform stirring so as to obtain a component 2; the component 1 and the component 2 are mixed, and stirred to be uniform, and an obtained mixed material is subjected to foaming so as to obtain polyurethane flexible foam; polyurethane flexible foam is subjected to reticulating treatment via alkaline liquor immersion or explosion method so as to obtain the multiwalled carbon nanotube modified reticulated polyurethane microbial carrier with an interpenetrating network structure. Hydrolysis resistance and biodegradation resistance of the multiwalled carbon nanotube modified reticulated polyurethane microbial carrier are improved via introducing olefin polymers into the interpenetrating network structure of the multiwalled carbon nanotube modified reticulated polyurethane microbial carrier, and compatibility of polyurethane with the olefin polymers is improved.
Description
Technical field
The invention belongs to microbe carrier preparation method technical field, specifically, relate to a kind of preparation method with the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification of inierpeneirating network structure.
Background technology
Along with the fast development of China's industrial or agricultural and the continuous quickening of urbanization process, city domestic sewage is treated as and realizes China's sustainable development of socio-economy, build the problem that ecological harmonious home primarily solves.Be that the biological treatment of sewage technology of representative has been widely used in the process of city and industrial sewage with active sludge.But traditional active sludge technology need further raising in reduction sewage effluents total nitrogen ability, and a large amount of excess sludges produced also become secondary pollution source simultaneously.MBBR (MBBR) technique, has used the ultimate principle of biomembrance process sewage disposal, takes full advantage of again the advantage of activated sludge process, respond well in reduction sewage effluents total nitrogen and excess sludge reduction.
By introducing microbe carrier, a large amount of attachment sites can be provided for sewage disposal microorganism, aerobic environment is provided to improve the nitration reaction speed of nitrobacteria at carrier surface, there is provided anaerobic environment to improve the anti-nitration reaction speed of denitrifying bacterium in carrier inside, the final ability improving process total nitrogen; Meanwhile, microbe carrier can also promote the decomposition in situ of excess sludge, realizes residual sludge reduction.
At present, macromolecular material is most widely used bio-carrier, mainly comprises polyolefins and polyurethanes.In the middle of practical application, simple polymer biological carrier filler wetting ability and biological adhesiveness poor, cause microorganism colonization speed comparatively slow, reduce sewage treating efficiency, and hydrolysis and microbic resolvability poor, work-ing life is short, and use cost is relatively high.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art existence, seek the preparation method with the reticulated polyurethane microbe carrier of inierpeneirating network structure designing a kind of multi-walled carbon nano-tubes modification, improve the hydrolysis of carrier and resistance to biological degradability, increase the biomass of urethane bio-carrier absorption, improve biological sewage treatment ability.
To achieve these goals, the technical solution used in the present invention is: a kind of preparation method of reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification, comprises the following steps:
Step 1: by vinyl polyether polyvalent alcohol 5 ~ 15 parts, polyether glycol 50 ~ 120 parts, polyester polyol 0 ~ 30 part, H
2o5 ~ 8 part, silicone oil 1 ~ 3 part, tin class catalyzer 0.05 ~ 0.2 part, amines catalyst 0.1 ~ 0.8 part, olefinic monomer 5 ~ 50 parts add in reactor, stir; Add 0.1 ~ 1 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 35 ~ 45 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by isocyanic ester 120 ~ 140 parts, radical polymerization initiator 0.01 ~ 0.15 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Preferably, described vinyl polyether polyvalent alcohol is vinyl polyoxypropylene polyol or vinyl polyethylene oxide polyol;
Preferably, described polyether glycol is ethylene glycol polyether glycol, ethylene glycol tetrahydrofuran polyether polyvalent alcohol or propylene oxide polyether glycol;
Preferably, described polyester polyol is adipate polyester polyvalent alcohol or aromatic polyester polyol;
Preferably, described tin class catalyzer is stannous octoate or dibutyl tin dilaurate, amines catalyst is the one in triethylene diamine, trolamine, triethylamine or N-ethylmorpholine, tin class and amines catalyst are used for catalyse isocyanate and polyether glycol, polyester polyol react, and regulates polyurethane foam reactive behavior.
Preferably, described radical polymerization initiator is the one in benzoyl peroxide (BPO), Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), for causing the Raolical polymerizable of olefinic monomer and vinyl polyether polyvalent alcohol.
Preferably, described olefinic monomer is vinylbenzene or divinylbenzene, and vinyl monomer from coalescence and vinyl polyether polyol reaction, generates inierpeneirating network structure in urethane inside under radical polymerization initiator effect.
Preferably, described isocyanic ester is diphenylmethanediisocyanate MDI.
Vinyl polyether polyvalent alcohol contains carbon-carbon double bond and hydroxyl Liang Zhong functional group, can respectively with double bond containing olefinic monomer and isocyanate reaction, in polyurethane system, introduce inierpeneirating network structure.Polyether glycol provides great amount of hydroxy group, generates urethane with isocyanate reaction.
Step 3: component 1 and component 2 are mixed, pours in mould the 12 ~ 24h that foams into, foams, obtain flexible PU foam under room temperature after stirring;
Step 4: flexible PU foam step 3 prepared carries out networking process by dipping by lye or explosion method, cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
Preferably, described dipping by lye method is immersed in alkali lye by flexible PU foam, immersion treatment 12 ~ 24h, and alkali lye consists of: massfraction be 40% the NaOH aqueous solution, Virahol, propylene glycol by volume 4:1 ~ 3:1 be made into mixing solutions; Then distilled water wash is used 2 ~ 3 times.
Preferably, described explosion method is that the flexible PU foam of preparation is put into treatment reactor, first vacuumizes, after pour the explosion gas of certain pressure, igniting blasting after diffusion for some time, obtains the flexible PU foam of networking process.
The reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification is used for the biochemical treatment of city domestic sewage.
Beneficial effect of the present invention is:
(1) introduce olefin polymer by inierpeneirating network structure in reticulated polyurethane carrier inside, the hydrolysis of carrier and resistance to biological degradability can be strengthened, improve work-ing life; The consistency of polyurethane component and olefin polymer components can be strengthened, and retain the characteristic of each component; The raw materials for production cost of carrier filler can be reduced;
(2) the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification has high-ratio surface sum biological adhesiveness energy, is beneficial to attachment and the growth of microorganism, shortens the biofilm time; There is excellent absorption property, the biomass of urethane bio-carrier absorption can be increased, improve biological sewage treatment ability; There is nano tubular structure, be conducive to the mass transfer of Polyurethane carrier internal gas and other materials, improve sewage treating efficiency;
(3) adopt MDI as the isocyanic ester of synthetic vectors filler, security is high, and bioaffinity is good.
(4) bio-carrier that prepared by present method has porousness and wetting ability, for sewage disposal microorganism provides a large amount of attachment site and good aerobic, anoxybiosis environment, microorganism colonization speed is fast, biomass is large, at filling surface for nitrobacteria provides aerobic environment to improve nitration reaction speed, provide anaerobic environment to improve anti-nitration reaction speed in filler inside for denitrifying bacterium, biological treatment effect and stability can be significantly improved, reduce total nitrogen, realize residual sludge reduction.
Embodiment
Below by specific embodiment, the invention will be further described:
Embodiment 1
The preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification of the present embodiment, comprises the following steps:
Step 1: by vinyl polyoxypropylene polyol 10 parts, ethylene glycol polyether glycol 80 parts, H
2o5 part, silicone oil 1 part, sub-0.1 part, the tin of tin class octoate catalyst, amines catalyst triethylene diamine 0.3 part, olefinic monomer vinylbenzene 20 parts add in reactor, stir; Add 0.2 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 40 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by diphenylmethanediisocyanate (MDI) 125 parts, radical polymerization initiator benzoyl peroxide (BPO) 0.08 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Step 3: component 1 and component 2 are mixed, pours in mould the 12 ~ 24h that foams into, foams, obtain flexible PU foam under room temperature after stirring;
Step 4: flexible PU foam step 3 prepared carries out networking process by dipping by lye method, flexible PU foam is immersed in alkali lye, immersion treatment 12h, alkali lye consists of: massfraction be 40% the NaOH aqueous solution, Virahol, propylene glycol by volume 4:1:1 be made into mixing solutions; Then distilled water wash is used 2 times; Cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
Embodiment 2
The preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification of the present embodiment, comprises the following steps:
Step 1: by vinyl polyethylene oxide polyol 15 parts, ethylene glycol tetrahydrofuran polyether polyvalent alcohol 100 parts, adipate polyester polyvalent alcohol 1 part, H
2o6 part, silicone oil 2 parts, sub-0.15 part, the tin of tin class octoate catalyst, amines catalyst triethylene diamine 0.5 part, olefinic monomer vinylbenzene 15 parts add in reactor, stir; Add 0.5 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 40 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by diphenylmethanediisocyanate (MDI) 130 parts, radical polymerization initiator Diisopropyl azodicarboxylate 0.06 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Step 3: component 1 and component 2 are mixed, pours in mould the 24h that foams after stirring into, foam under room temperature, obtain flexible PU foam;
Step 4: flexible PU foam step 3 prepared carries out networking process by explosion method, the flexible PU foam of preparation is put into treatment reactor, first vacuumizes, after pour the explosion gas of certain pressure, igniting blasting after diffusion for some time, obtains the flexible PU foam of networking process; Cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
Embodiment 3
The preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification of the present embodiment, comprises the following steps:
Step 1: by vinyl polyethylene oxide polyol 5 parts, polyether glycol 70 parts, aromatic polyester polyol 15 parts, H
2o8 part, silicone oil 2 parts, tin class catalyzer dibutyl tin dilaurate 0.05 part, amines catalyst triethylamine 0.8 part, olefinic monomer divinylbenzene 5 parts add in reactor, stir; Add 0.1 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 35 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by diphenylmethanediisocyanate (MDI) 120 parts, radical polymerization initiator benzoyl peroxide (BPO) 0.01 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Step 3: component 1 and component 2 are mixed, pours in mould the 12 ~ 24h that foams into, foams, obtain flexible PU foam under room temperature after stirring;
Step 4: flexible PU foam step 3 prepared carries out networking process by dipping by lye method, flexible PU foam is immersed in alkali lye, immersion treatment 18h, alkali lye consists of: massfraction be 40% the NaOH aqueous solution, Virahol, propylene glycol by volume 4:3:1 be made into mixing solutions; Then distilled water wash is used 3 times; Cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
Embodiment 4
The preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification of the present embodiment, comprises the following steps:
Step 1: by vinyl polyether polyvalent alcohol 12 parts, propylene oxide polyether glycol 120 parts, aromatic polyester polyol 30 parts, H
2o7 part, silicone oil 3 parts, tin class catalyzer dibutyl tin dilaurate 0.2 part, amines catalyst trolamine 0.1 part, olefinic monomer divinylbenzene 50 parts add in reactor, stir; Add 1 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 45 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by diphenylmethanediisocyanate (MDI) 140 parts, radical polymerization initiator 2,2'-Azobis(2,4-dimethylvaleronitrile) 0.15 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Step 3: component 1 and component 2 are mixed, pours in mould the 20h that foams after stirring into, foam under room temperature, obtain flexible PU foam;
Step 4: flexible PU foam step 3 prepared carries out networking process by explosion method, the flexible PU foam of preparation is put into treatment reactor, first vacuumizes, after pour the explosion gas of certain pressure, igniting blasting after diffusion for some time, obtains the flexible PU foam of networking process; Cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
Claims (6)
1. a preparation method for the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification, is characterized in that, comprise the following steps:
Step 1: vinyl polyether polyvalent alcohol 5 ~ 15 parts, polyether glycol 50 ~ 120 parts, polyester polyol 0 ~ 30 part, H2O5 ~ 8 part, silicone oil 1 ~ 3 part, tin class catalyzer 0.05 ~ 0.2 part, amines catalyst 0.1 ~ 0.8 part, olefinic monomer 5 ~ 50 parts are added in reactor, stirs; Add 0.1 ~ 1 part of multi-walled carbon nano-tubes (MWCNTS), stir, and insulation is to 35 ~ 45 DEG C, as component 1; Above-mentioned number is mass parts;
Step 2: by isocyanic ester 120 ~ 140 parts, radical polymerization initiator 0.01 ~ 0.15 part, add reactor, stir, as component 2; Above-mentioned number is mass parts;
Step 3: component 1 and component 2 are mixed, pours in mould the 12 ~ 24h that foams into, foams, obtain flexible PU foam under room temperature after stirring;
Step 4: flexible PU foam step 3 prepared carries out networking process by dipping by lye or explosion method, cutting obtains the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification.
2. the preparation method of the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification according to claim 1, it is characterized in that, described tin class catalyzer is stannous octoate or dibutyl tin dilaurate, and amines catalyst is the one in triethylene diamine, trolamine, triethylamine or N-ethylmorpholine.
3. the preparation method of the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification according to claim 1, is characterized in that, described radical polymerization initiator is the one in benzoyl peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
4. the preparation method of the reticulated polyurethane microbe carrier of multi-walled carbon nano-tubes modification according to claim 1, is characterized in that, described olefinic monomer is vinylbenzene or divinylbenzene, and described isocyanic ester is diphenylmethanediisocyanate.
5. the preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification according to any one of claim 1-4, it is characterized in that, described dipping by lye method is immersed in alkali lye by flexible PU foam, immersion treatment 12 ~ 24h, alkali lye consists of: massfraction be 40% the NaOH aqueous solution, Virahol, propylene glycol by volume 4:1 ~ 3:1 be made into mixing solutions; Then distilled water wash is used 2 ~ 3 times.
6. the preparation method of the reticulated polyurethane microbe carrier of the multi-walled carbon nano-tubes modification according to any one of claim 1-4, it is characterized in that, described explosion method is that the flexible PU foam of preparation is put into treatment reactor, first vacuumize, after pour the explosion gas of certain pressure, igniting blasting after diffusion for some time, obtains the flexible PU foam of networking process.
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Cited By (3)
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| CN108178840A (en) * | 2017-12-28 | 2018-06-19 | 南京理工大学 | The preparation method and applications of intelligent temperature control metal-organic nanotube sponge material |
| CN112390378A (en) * | 2020-11-13 | 2021-02-23 | 浙江工商大学 | Biological filler with denitrification function, preparation method and application thereof |
| CN115897245A (en) * | 2022-12-28 | 2023-04-04 | 海泰纺织（苏州）有限公司 | Preparation method of fabric antistatic finishing agent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108178840A (en) * | 2017-12-28 | 2018-06-19 | 南京理工大学 | The preparation method and applications of intelligent temperature control metal-organic nanotube sponge material |
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| CN112390378A (en) * | 2020-11-13 | 2021-02-23 | 浙江工商大学 | Biological filler with denitrification function, preparation method and application thereof |
| CN112390378B (en) * | 2020-11-13 | 2022-08-09 | 浙江工商大学 | Biological filler with denitrification function, preparation method and application thereof |
| CN115897245A (en) * | 2022-12-28 | 2023-04-04 | 海泰纺织（苏州）有限公司 | Preparation method of fabric antistatic finishing agent |
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| CN105367737B (en) | 2018-07-06 |
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