CN106478866A - A kind of preparation method of organic porous material - Google Patents
A kind of preparation method of organic porous material Download PDFInfo
- Publication number
- CN106478866A CN106478866A CN201610870507.1A CN201610870507A CN106478866A CN 106478866 A CN106478866 A CN 106478866A CN 201610870507 A CN201610870507 A CN 201610870507A CN 106478866 A CN106478866 A CN 106478866A
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- Prior art keywords
- porous material
- maleic acid
- sodium salt
- surfactant
- organic porous
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
-
- 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
- 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
Abstract
The invention discloses a kind of method that high internal phase ratio emulsions system prepares organic porous material for template, described preparation method is that vinyl monomer, initiator, porogen, cross-linking agent, calcium chloride, polymerisable surfactant are mixed together in water, it is polymerized under certain condition, the organic porous material apparatus,Soxhlet'ses obtaining purify.Uniform pore diameter is had using the organic porous material of the method preparation, physicochemical properties are stable, specific surface area is big property.
Description
Technical field
The present invention relates to organic porous material preparation field, specifically in a kind of system for template for high internal phase ratio emulsions
The method preparing organic porous material using polymerisable surfactant.
Background technology
Porous material is made up of continuous solid skeleton and hole.The border of hole or surface are by compound or chemical combination
Thing is constituted for main body.Because porous material structure is to be formed in space clustering by polyhedron-shaped hole, so being referred to as " bubble
Foam " material；Further, since being shaped like in honeycomb texture, also referred to as " cellular material ".
Porous material is big because of cell volume, thus has the advantages that density is low, porosity is high, specific surface area is big.Always with
Come, porous material is used as two phase structure material, thermal insulation heat-barrier material, catalyst carrier material, adsorption and separation material and biology
Tissue substitute product material etc..Porous material mainly includes metal polyporous material and non-metal porous material.Wherein, polyalcohol stephanoporate
Material causes paying close attention to emphatically of people because having more excellent physical and chemical performance and be widely applied prospect.Porous is gathered
Compound traditional preparation methods have antiphase method, phase separation method, solvent pore method etc., but these methods all can not accurately control hole and
The size of passage and distribution.
High internal phase ratio emulsions [High Internal Phase Emulsion (HIPE)], also known as high concentrated emulsions, refer to interior
Phase（Dispersion phase）Volume fraction more than 74%, even as high as 99% emulsion.High internal phase emulsion as template prepares porous
Material is as polymerization phase using the continuous phase of high internal phase ratio emulsions, carries out polyreaction at a certain temperature, is polymerized warp after terminating
Washing, drying can get the polymeric material of loose structure.The method preparing porous material with other（As antiphase method, phase are divided
From method, solvent pore method etc.）Compare, high internal phase emulsion as template has the size being accurately controlled hole and channel diameter and divides
The advantage of cloth.High internal phase ratio emulsions system is by vinyl monomer, initiator, porogen, cross-linking agent, salt（Generally use calcium chloride）, table
Face activating agent, water composition.
In high internal phase ratio emulsions, surfactant is extremely important.Conventional surfactants are simply adsorbed onto polymeric material
On, rather than with firm covalent bonding.In some cases（As freeze-thaw cycle, impose high shear force etc.）, general surface
Activating agent easily gets off from latex particle surface desorption, makes latex become unstable, and surfactant is easily sent out in film
Raw migration, forms aggregation and reduces the resistance to water of product, lead to the plasticization being caused by water.
Polymerisable surfactant has surface activity and polymerizability, is had a series of excellent with the polymer that it is prepared
Point：（1）Polymerisable surfactant, while playing conventional surfactant effect, also has the function of participating in emulsion polymerization,
And it is firmly bonded to the surface of polymer particle in the way of covalent bond, become a part for polymer, make prepared grain
Son not only has preferable particle diameter distribution, and has the distinctive performance of surfactant molecule；（2）Polymerisable surfactant with
Monomer copolymerization, decreases the surfactant of residual in emulsion clear liquid, is easy to purification；（3）Can easily be accommodated and be dissolved in emulsion dispersion
Monomer composition in phase, can prepare the changeable macromolecular material of composition.
Content of the invention
It is an object of the invention to provide a kind of method that high internal phase ratio emulsions prepare organic porous material for template.
The present invention relates to a kind of method that high internal phase ratio emulsions prepare organic porous material for template.It is characterized in that in horse
Carry out sour single methanol ester sodium salt（Maleic acid list lauryl alcohol ester sodium salt, maleic acid list hexadecanol ester sodium salt, maleic acid list octadecyl sodium
Salt, maleic acid list fatty alcohol-polyoxyethylene ether ester sodium salt）Polymerisable surfactant carries out polyreaction system under conditions of existing
Standby organic porous material.
High internal phase ratio emulsions prepare organic porous material for template, and its step is as described below：It is vinyl monomer, pore first
Agent, cross-linking agent, salt（Typically refer to calcium chloride）, maleic acid single methanol ester sodium salt polymerisable surfactant and water be positioned over three mouthfuls of burnings
In bottle, stirring；Next to that high pure nitrogen replaces the air in reaction bulb；Add initiator under nitrogen protection；In uniform temperature
Under carry out polyreaction；Reaction is purified to organic porous material with apparatus,Soxhlet'ses after terminating, solvent absolute methanol.
The present invention has the special feature that：Using polymerizable maleic acid list lauryl alcohol ester sodium salt, maleic acid list hexadecanol ester sodium salt,
Maleic acid list octadecyl sodium salt, maleic acid list fatty alcohol-polyoxyethylene ether ester sodium salt polymerisable surfactant replace traditional
Surfactant, the organic porous material physical and chemical stability obtaining is good, uniform pore diameter, and specific surface area is big.
Specific embodiments
Embodiment 1：Take 7.8 ml acrylonitrile, 4.6 ml toluene, 3.5 g maleic acid list lauryl alcohol ester sodium salts（Polymerizable table
Face activating agent）, 1 ml divinylbenzene be positioned over 250 ml there-necked flasks, stir 30 min；Deca 100 ml CaCl2Aqueous solution；
Continue stirring 30 min；Separately weigh 0.8 g azodiisobutyronitrile and be positioned over there-necked flask, stir 10 min, then nitrogen charging deoxygenation, 70
8 h are reacted at DEG C.After the completion of reaction, extract 48 h with absolute methanol in apparatus,Soxhlet'ses, with the unreacted in removing system
Monomer and impurity, finally wash, vacuum drying, obtain polyacrylonitrile.
Embodiment 2：Take 7.8 ml acrylonitrile, 4.6 ml toluene, 3 g maleic acid list hexadecanol ester sodium salts（Polymerizable surface
Activating agent）, 1 ml divinylbenzene be positioned over 250 ml there-necked flasks, stir 30 min；Deca 100 ml CaCl2Aqueous solution；Continue
Continuous stirring 30 min；Separately weigh 0.8 g azodiisobutyronitrile and be positioned over there-necked flask, stir 10 min, then nitrogen charging deoxygenation, 70 DEG C
Lower reaction 8 h.After the completion of reaction, extract 48 h with absolute methanol in apparatus,Soxhlet'ses, with unreacted in removing system
Monomer and impurity, finally wash, vacuum drying, obtain polyacrylonitrile.
Embodiment 3：Take 7.8 ml acrylonitrile, 4.6 ml toluene, 2.8 g maleic acid list octadecyl sodium salts（Polymerizable table
Face activating agent）, 1 ml divinylbenzene be positioned over 250 ml there-necked flasks, stir 30 min；Deca 100 ml CaCl2Aqueous solution；
Continue stirring 30 min；Separately weigh 0.8 g azodiisobutyronitrile and be positioned over there-necked flask, stir 10 min, then nitrogen charging deoxygenation, 70
8 h are reacted at DEG C.After the completion of reaction, extract 48 h with absolute methanol in apparatus,Soxhlet'ses, with the unreacted in removing system
Monomer and impurity, finally wash, vacuum drying, obtain polyacrylonitrile.
Embodiment 4：Take 7.8 ml acrylonitrile, 4.6 ml toluene, 2.5 g maleic acid list fatty alcohol-polyoxyethylene ether ester sodium salts
（Polymerisable surfactant）, 1 ml divinylbenzene be positioned over 250 ml there-necked flasks, stir 30 min；Deca 100 ml
CaCl2Aqueous solution；Continue stirring 30 min；Separately weigh 0.8 g azodiisobutyronitrile and be positioned over there-necked flask, stir 10 min, so
Nitrogen charging deoxygenation afterwards, reacts 8 h at 70 DEG C.After the completion of reaction, extract 48 h with absolute methanol in apparatus,Soxhlet'ses, to remove body
Unreacted monomer in system and impurity, finally wash, vacuum drying, obtain polyacrylonitrile.
Claims (3)
1. a kind of high internal phase ratio emulsions system prepares the method for organic porous material it is characterised in that using polymerizable table for template
Face activating agent substitutes traditional surfactant, comprises the following steps：
（1）Vinyl monomer, initiator, porogen, cross-linking agent, calcium chloride, polymerisable surfactant are mixed together in water;
（2）Under nitrogen protection, it is warming up to and is polymerized at a temperature of certain, be polymerized the porous material obtaining and adopt surname extraction
Device purifies.
2. vinyl monomer according to claim 1 refer to styrene, methyl methacrylate, acrylonitrile, methacrylic acid-
Beta-hydroxy ethyl ester, acrylamide.
3. surfactant according to claim 1 is it is characterised in that described surfactant is polymerizable maleic acid
Single lauryl alcohol ester sodium salt, maleic acid list hexadecanol ester sodium salt, maleic acid list octadecyl sodium salt, maleic acid list fatty alcohol polyoxy second
Alkene ether-ether sodium salt.
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| CN201610870507.1A CN106478866A (en) | 2016-10-07 | 2016-10-07 | A kind of preparation method of organic porous material |
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| CN201610870507.1A CN106478866A (en) | 2016-10-07 | 2016-10-07 | A kind of preparation method of organic porous material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417853A (en) * | 2017-09-14 | 2017-12-01 | 湖南理工学院 | A kind of preparation method of porous polypropylene nitrile |
| CN110330584A (en) * | 2019-07-02 | 2019-10-15 | 陕西师范大学 | A kind of flame-retardant smoke inhibition high-strength light high molecular material and preparation method thereof |
| CN113929814A (en) * | 2021-09-24 | 2022-01-14 | 湖北大学 | Preparation method and application of polyacrylonitrile/silicon dioxide porous composite material |
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| CN1217003A (en) * | 1996-03-27 | 1999-05-19 | 诺瓦提斯公司 | Process for mfg. porous polymer from a mixture |
| CN1265678A (en) * | 1997-08-15 | 2000-09-06 | 陶氏化学公司 | High internal phase emulsions and porous materials prepared therefrom |
| CN1433444A (en) * | 2000-06-05 | 2003-07-30 | 陶氏环球技术公司 | Continuous process for polymerizing, curing and drying high internal phase emulsions |
| CN102199242A (en) * | 2011-03-26 | 2011-09-28 | 鲁东大学 | Preparation method of porous high-oil-absorbing resin |
| CN104710554A (en) * | 2015-01-05 | 2015-06-17 | 泰山医学院 | Preparation method of interpenetrating network porous polymer composite material |
| CN105330780A (en) * | 2015-11-20 | 2016-02-17 | 同济大学 | Styrene base resin porous material capable of adsorbing polycyclic aromatic hydrocarbon and preparation method of styrene base resin porous material |
| US20170114244A1 (en) * | 2014-06-18 | 2017-04-27 | Lubrizol Advanced Materials, Inc. | Peelable composition |
-
2016
- 2016-10-07 CN CN201610870507.1A patent/CN106478866A/en active Pending
Patent Citations (7)
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| CN1217003A (en) * | 1996-03-27 | 1999-05-19 | 诺瓦提斯公司 | Process for mfg. porous polymer from a mixture |
| CN1265678A (en) * | 1997-08-15 | 2000-09-06 | 陶氏化学公司 | High internal phase emulsions and porous materials prepared therefrom |
| CN1433444A (en) * | 2000-06-05 | 2003-07-30 | 陶氏环球技术公司 | Continuous process for polymerizing, curing and drying high internal phase emulsions |
| CN102199242A (en) * | 2011-03-26 | 2011-09-28 | 鲁东大学 | Preparation method of porous high-oil-absorbing resin |
| US20170114244A1 (en) * | 2014-06-18 | 2017-04-27 | Lubrizol Advanced Materials, Inc. | Peelable composition |
| CN104710554A (en) * | 2015-01-05 | 2015-06-17 | 泰山医学院 | Preparation method of interpenetrating network porous polymer composite material |
| CN105330780A (en) * | 2015-11-20 | 2016-02-17 | 同济大学 | Styrene base resin porous material capable of adsorbing polycyclic aromatic hydrocarbon and preparation method of styrene base resin porous material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417853A (en) * | 2017-09-14 | 2017-12-01 | 湖南理工学院 | A kind of preparation method of porous polypropylene nitrile |
| CN110330584A (en) * | 2019-07-02 | 2019-10-15 | 陕西师范大学 | A kind of flame-retardant smoke inhibition high-strength light high molecular material and preparation method thereof |
| CN113929814A (en) * | 2021-09-24 | 2022-01-14 | 湖北大学 | Preparation method and application of polyacrylonitrile/silicon dioxide porous composite material |
| CN113929814B (en) * | 2021-09-24 | 2023-03-03 | 湖北大学 | Preparation method and application of polyacrylonitrile/silicon dioxide porous composite material |
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Application publication date: 20170308 |