CN106565947B - A kind of pore creating material and preparation method thereof for reticulated porous materials - Google Patents
A kind of pore creating material and preparation method thereof for reticulated porous materials Download PDFInfo
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Abstract
The invention discloses a kind of pore creating materials of reticulated porous materials and preparation method thereof, and the molecular structural formula of the pore creating material is as follows：Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or hydrophobic grouping, polyoxyethylene ether and hydrophobic grouping must exist simultaneously in each pore-creating agent molecule.The present invention is hydrophobic grouping and polyoxyethylene ether to be introduced by reaction on its hydroxyl, using anhydrous sorbitol as precursor structure to obtain preparing the pore creating material of reticulated porous materials.The method of the invention has widened the selection range of reaction raw materials, while can introduce a variety of functional groups, increases the specificity of pore creating material；Its pore-creating mode is using micella occupy-place method, during removing pore creating material micella, it is only necessary to which simple pure water impregnates, and meets energy-saving and environment-friendly requirement.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of preparation and application of novel pore creating material, and in particular to Yi Zhongyong
In the pore creating material and preparation method thereof of reticulated porous materials.
Background technology
Since the surface of porous material has abundant pore structure and larger specific surface area, so porous material is often made
Sorbing material is used, such as common toxic gas filter device；Meanwhile the porous material chemical stability after carbonization
Height, the carrier that can be used for making chemical catalyst are used；Because carbon material is conductive, and charge and discharge number is to using the longevity
Life influences very little, therefore the porous material after being carbonized usually is regarded excellent electrode material and used, particularly with emerging super electricity
Container, porous carbon electrodes are even more with advantage that is cheap, lasting a long time.
Include for the boring technique of porous material at present：Raw material activation method, hard template method, soft template method etc..Former material
Expect that activation method, the natural materials used, such as cellulose, coal and its derivative, these materials itself have pore structure, so
It is relatively simple to prepare porous material, but pore-size distribution is uneven, it is difficult to meet actual demand；And hard template method, although can be with
Ideal control pore structure, but step cumbersome due to the costliness of its template price and when removing removing template, at present
Example and few that is more to be present in experiment, being really applied in production.
Soft template method, usually using surfactant as pore creating material, when the concentration of surfactant in the solution is more than
Critical micelle concentration (CMC), will form small micellar structure.It is right using the hydrophilic and oleophilic attribute of micella outer layer group
Small molecule material is attracted, to allow small-molecule substance to be coated on micellar surface.After small molecule material polymerizing curable, elution
Surfactant can be obtained porous material.Such as：CN1926181A discloses a kind of water soluble polymer material and surface
Activating agent, the method for preparing the water dispersible or water-soluble porous body of three-dimensional open pores lattice；CN101332421A discloses one
The method that kind prepares nucleocapsid type microgel composite microsphere with polymerisable surfactant；CN100584880C discloses a kind of activity
The method that agent split-phase prepares porous material.
The above method, for raw material activation method and hard template method, there are certain uncontrollable factors.Activating agent
The size of molecular weight and the quantity of hydrophilic radical can all influence the HLB value of activating agent, and then influence critical micelle concentration and glue
The aggregation number of beam, this will have a direct impact on the hole size and pattern finally obtained.So the porous material that at present prepared by soft template method
Material, aperture are difficult to control between being distributed in 1nm~1 μm mostly, and are easy to reunite between micella, form larger hole, it is difficult to
Obtain reticulated porous structures.Use more polyethers kind block polymer, cost of material higher in soft template method at present simultaneously
Every kilogram needs hundreds of members, can only can just bear such cost in laboratory or high repayment industry.In process aspect, going
When except soft template, common method is high-temperature calcination or the extraction of strong acid, highly basic, these methods are not only to porous material
Structure can cause certain damage, and to the technical staff of Attended Operation, there is also certain danger.
Invention content
The technical issues of solution：In order to overcome the deficiencies of existing technologies, it is wide to obtain a kind of raw material selection range, functional group's kind
Class is more, and specificity is high, can increase the specific surface area and porosity of unit mass, simplifies construction procedure energy-saving and environment-friendly pore-creating again
Agent, the pore creating material and preparation method thereof that the present invention provides a kind of for reticulated porous materials.
Technical solution：The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or hydrophobic grouping, polyoxyethylene ether and hydrophobic group
Group must exist simultaneously in each pore-creating agent molecule.
Preferably, the hydrophobic grouping is carboxylic acids, alcohols or phosphoric acid ester.
Further, the hydrophobic grouping is octanoic acid, capric acid, oleic acid, linoleic acid, ricinoleic acid, linolenic acid, palmitin
Acid, stearic acid, lauric acid, myristic acid, octanol, decyl alcohol, oleyl alcohol, sub- oleyl alcohol, soft lipidol, stearyl alcohol, laruyl alcohol, cardanol, two
Isooctyl phosphoric acid ester, diisooctyl phosphite ester, diisooctyl pyrophosphate or diisooctyl pyrophosphite.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and mixture quality 1.0%~3.0% is added by the first stage
Sodium hydroxide is stirred to react 9~10h as catalyst in 120~150 DEG C of oil bath pan；
Hydrophobic grouping is added in second stage in the reaction product of previous step, and be added mixture quality 0.5%~
Then 1.0% sodium hydroxide is stirred to react 4~5h, to obtain pore creating material as catalyst at a temperature of 60~90 DEG C.
Preferably, every 1mol anhydrous sorbitols, need 1~2mol polyoxyethylene ether and 4~5mol it is hydrophobic
Group participates in reaction.
Further, by taking carboxylic-acid substance as an example, a kind of pore creating material for reticulated porous materials, preparation method it is anti-
The principle is answered to be：
Wherein：R-OH is anhydrous sorbitol, and R '-COOH is carboxylic-acid substance, and the two is by esterification, by long chain alkane
Molecule is linked on anhydrous sorbitol.
Further, by taking alcohols material as an example, a kind of pore creating material for reticulated porous materials, the reaction of preparation method
Principle is：
R-OH+R'-OH→R-O-R'+H2O
Wherein：R-OH is anhydrous sorbitol, and R '-OH is alcohols material, and the two will be grown by double hydroxyls dehydrate condensation reactions
Paraffin molecules are linked on anhydrous sorbitol.
Further, by taking phosphoric acid ester substance as an example, a kind of pore creating material for reticulated porous materials, preparation method
Reaction principle is：
In formula：R-OH is anhydrous sorbitol, R '-COO-R " it is phosphoric acid ester substance, the two will be grown by ester exchange reaction
Paraffin molecules are linked on anhydrous sorbitol.
Advantageous effect：(1) present invention is obtained by anhydrous sorbitol and polyoxyethylene ether and hydrophobic grouping two-step reaction, due to
Anhydrous sorbitol has 4 hydroxyls, can link a variety of groups, increase the specificity of pore creating material；(2) pore creating material of the present invention
Hydrophily is strong, during eluting occupy-place micella, avoids the high-temperature calcination of traditional handicraft or the immersion of strong acid and strong base, no
Only energy conservation and environmental protection also reduces the danger of practitioner；(3) pore creating material of the present invention, existing porosity of porous material meeting
Change because of different process, on average in 40% level, porosity of the present invention is higher, can be more than 60%；Occur at present
Porous material specific surface area be about 1000~1500m2/ g, the reticulated porous materials specific surface area that the present invention makes can be more than
2000m2/g。
Description of the drawings
Fig. 1 prepares design drawing for net porous structure material of the invention.
Fig. 2 is surface electronic microscope photo after the embodiment of the present invention 1 elutes pore creating material.
Fig. 3 is surface electronic microscope photo after the embodiment of the present invention 2 elutes pore creating material.
Fig. 4 is surface electronic microscope photo after the embodiment of the present invention 3 elutes pore creating material.
Fig. 5 is surface electronic microscope photo after the embodiment of the present invention 4 elutes pore creating material.
Fig. 6 is surface electronic microscope photo after the embodiment of the present invention 5 elutes pore creating material.
Fig. 7 is surface electronic microscope photo after the embodiment of the present invention 6 elutes pore creating material.
Specific implementation mode
The content that following embodiment further illustrates the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit of that invention and essence, to changing and replacing made by the method for the present invention, step or condition, the present invention is belonged to
Range.Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4The polyoxyethylene ether linked with parent or diisooctyl phosphoric acid ester, polyoxyethylene ether and
Diisooctyl phosphoric acid ester must exist simultaneously in each pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 3.0% is added by the first stage
As catalyst, 9h is stirred to react in 120 DEG C of oil bath pan；
Diisooctyl phosphoric acid ester is added in the reaction product of previous step, and mixture quality 0.5% is added for second stage
Sodium hydroxide as catalyst, then 5h is stirred to react at a temperature of 60 DEG C, to obtain pore creating material.
The anhydrous sorbitol, polyoxyethylene ether, the molar ratio of diisooctyl phosphoric acid ester are 1:2:4.
Embodiment 2
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or cardanol, polyoxyethylene ether and cardanol exist
It must be existed simultaneously in each pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 2.0% is added by the first stage
As catalyst, 9.5h is stirred to react in 140 DEG C of oil bath pan；
Cardanol is added in second stage in the reaction product of previous step, and the hydroxide of mixture quality 0.8% is added
Then sodium is stirred to react 4h, to obtain pore creating material as catalyst at a temperature of 70 DEG C.
The anhydrous sorbitol, polyoxyethylene ether, the molar ratio of cardanol are 1:2:4.
Embodiment 3
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or decyl alcohol, polyoxyethylene ether and decyl alcohol are each
It must be existed simultaneously in a pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 2.5% is added by the first stage
As catalyst, 9h is stirred to react in 140 DEG C of oil bath pan；
Decyl alcohol is added in second stage in the reaction product of previous step, and the sodium hydroxide of mixture quality 0.7% is added
As catalyst, it then is stirred to react 4.5h at a temperature of 85 DEG C, to obtain pore creating material.
The anhydrous sorbitol, polyoxyethylene ether, the molar ratio of decyl alcohol are 1:1:4.
Embodiment 4
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or lauric acid, polyoxyethylene ether and lauric acid exist
It must be existed simultaneously in each pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 1.0% is added by the first stage
As catalyst, 10h is stirred to react in 150 DEG C of oil bath pan；
Lauric acid is added in second stage in the reaction product of previous step, and the hydroxide of mixture quality 0.5% is added
Then sodium is stirred to react 4h, to obtain pore creating material as catalyst at a temperature of 80 DEG C.
The anhydrous sorbitol, polyoxyethylene ether, lauric molar ratio are 1:1:5.
Embodiment 5
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or stearic acid, polyoxyethylene ether and stearic acid exist
It must be existed simultaneously in each pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 2.0% is added by the first stage
As catalyst, 9h is stirred to react in 130 DEG C of oil bath pan；
Stearic acid is added in second stage in the reaction product of previous step, and the hydroxide of mixture quality 1.0% is added
Then sodium is stirred to react 4h, to obtain pore creating material as catalyst at a temperature of 90 DEG C.
The anhydrous sorbitol, polyoxyethylene ether, stearic molar ratio are 1:2:5.
Embodiment 6
The molecular structural formula of a kind of pore creating material for reticulated porous materials, the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or oleic acid, polyoxyethylene ether and oleic acid are each
It must be existed simultaneously in a pore-creating agent molecule.
A kind of preparation method of pore creating material for reticulated porous materials, uses anhydrous sorbitol for precursor structure, at it
It by reactive grafting polyoxyethylene ether in part of hydroxyl, adds hydrophobic grouping and is reacted with residual hydroxyl, to obtain for making
The pore creating material of standby reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the sodium hydroxide of mixture quality 1.5% is added by the first stage
As catalyst, 9h is stirred to react in 135 DEG C of oil bath pan；
Oleic acid is added in second stage in the reaction product of previous step, and the sodium hydroxide of mixture quality 0.5% is added
As catalyst, it then is stirred to react 4h at a temperature of 75 DEG C, to obtain pore creating material.
The anhydrous sorbitol, polyoxyethylene ether, the molar ratio of oleic acid are 1:2:5.
Above-mentioned pore creating material is used to prepare porous material, tests its aperture and specific surface area, the results are shown in table below：
Claims (5)
1. a kind of pore creating material for reticulated porous materials, which is characterized in that the molecular structural formula of the pore creating material is as follows：
Wherein：R1、R2、R3、R4It is the polyoxyethylene ether linked with parent or hydrophobic grouping, polyoxyethylene ether and hydrophobic grouping are every
It must be existed simultaneously in one pore-creating agent molecule.
2. a kind of pore creating material for reticulated porous materials according to claim 1, which is characterized in that the hydrophobic group
Group is carboxylic acids, alcohols or phosphoric acid ester substance.
3. a kind of pore creating material for reticulated porous materials according to claim 2, which is characterized in that the carboxylic acids
Substance is octanoic acid, capric acid, oleic acid, linoleic acid, ricinoleic acid, linolenic acid, palmitic acid, stearic acid, lauric acid or myristic acid；Institute
The alcohols material stated is octanol, decyl alcohol, oleyl alcohol, sub- oleyl alcohol, soft lipidol, stearyl alcohol, laruyl alcohol or cardanol；The phosphate
Substance is diisooctyl phosphoric acid ester, diisooctyl phosphite ester, diisooctyl pyrophosphate or diisooctyl pyrophosphite.
4. a kind of preparation method of pore creating material according to claims 1 to 3 any one of them for reticulated porous materials, special
Sign is, uses anhydrous sorbitol for precursor structure, by reactive grafting polyoxyethylene ether in its part of hydroxyl, adds thin
Water base group reacts with residual hydroxyl, to obtain the pore creating material for being used to prepare reticulated porous materials, is as follows：
Anhydrous sorbitol is mixed with polyoxyethylene ether, and the hydrogen-oxygen of mixture quality 1.0%~3.0% is added by the first stage
Change sodium as catalyst, 9~10h is stirred to react in 120~150 DEG C of oil bath pan；
Hydrophobic grouping is added in second stage in the reaction product of previous step, and mixture quality 0.5%~1.0% is added
Then sodium hydroxide is stirred to react 4~5h, to obtain pore creating material as catalyst at a temperature of 60~90 DEG C.
5. a kind of preparation method of pore creating material for reticulated porous materials according to claim 4, which is characterized in that institute
The every 1mol anhydrous sorbitols stated, it is anti-by needing the polyoxyethylene ether of 1~2mol and the hydrophobic grouping of 4~5mol to participate in per 1mol
It answers.
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| CN107331878B (en) * | 2017-05-31 | 2020-07-14 | 惠州亿纬锂能股份有限公司 | Pore-forming agent for lithium-manganese dioxide battery positive electrode, porous positive electrode prepared from pore-forming agent and lithium-manganese dioxide battery |
| CN107399958A (en) * | 2017-08-08 | 2017-11-28 | 湖南省醴陵市玉果电瓷有限公司 | A kind of porcelain bushing shell and preparation method thereof |
| CN108062185B (en) * | 2018-01-31 | 2022-02-01 | 京东方科技集团股份有限公司 | Touch control assembly, manufacturing method thereof and display device |
| CN111994893A (en) * | 2020-07-24 | 2020-11-27 | 盐城工学院 | Preparation method of nitrogen-doped carbon material |
| CN116102763A (en) * | 2023-01-07 | 2023-05-12 | 合肥学院 | Pore-forming agent, high-tensile-strength breathable film and preparation method thereof |
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| CN101831283A (en) * | 2010-04-02 | 2010-09-15 | 河南大学 | Water-base nano polysilicon particles, preparation method thereof and use thereof |
| CN102717064A (en) * | 2012-07-06 | 2012-10-10 | 厦门大学 | Hyperbranched nano-silver taking amphiphilic polymer as stabilizing agent and preparation method thereof |
| CN103183832A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for magnetic cellulose-chitosan composite microsphere |
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| CN101831283A (en) * | 2010-04-02 | 2010-09-15 | 河南大学 | Water-base nano polysilicon particles, preparation method thereof and use thereof |
| CN103183832A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for magnetic cellulose-chitosan composite microsphere |
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