CN109232967A - A method of lipophilic fiber element aeroge is prepared based on gas-solid phase interface molecular regulation mechanism - Google Patents
A method of lipophilic fiber element aeroge is prepared based on gas-solid phase interface molecular regulation mechanism Download PDFInfo
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- CN109232967A CN109232967A CN201810581138.3A CN201810581138A CN109232967A CN 109232967 A CN109232967 A CN 109232967A CN 201810581138 A CN201810581138 A CN 201810581138A CN 109232967 A CN109232967 A CN 109232967A
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- 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
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- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- 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
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- 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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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Abstract
A method of lipophilic fiber element aeroge is prepared based on gas-solid phase interface molecular regulation mechanism, is to provide one kind using waste paper as raw material, after its dissolution is prepared hydrogel, is further modified preparation green, lightweight, the method for high specific surface area porous material.The method comprises the following steps: the dissolution and purification of one, waste paper；Two, the preparation of cellulose aerogels；Three, the preparation of cellulose aerogels oil absorption material.The present invention is simple with the cellulose aerogels preparation method that waste paper is basic material preparation, and novel in design, biodegradable properties are good, and absorption efficiency is high, can be used repeatedly.A variety of organic solvents and oil product can be absorbed extensively by hydrophobic fibre element aeroge prepared by this technique, and there is excellent recuperability and selectivity, have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of lipophile material, and in particular to one kind is based on gas-solid phase interface molecular regulation
The method that mechanism prepares lipophilic fiber element aeroge.
Background technique
Oil spills is to seriously threaten one of disaster of marine ecology, when meeting is in petroleum preparation, storage and transportational process
There is generation.In view of popularity and importance of the petroleum resources in mankind's activity, Oil spills is necessarily to face and must solve
Major issue.The traditional means of cleaning leakage petroleum mainly have three kinds of approach such as chemical method, bioanalysis and physical method, wherein changing
The means such as light degradation, burning, solidification precipitating are maximally efficient in method, also become the leakage most commonly used processing mode of crude oil.But
Chemical Treatment means, which are easy to cause, causes the secondary pollutions such as catabolite, incineration ashes, is unfavorable for the purification of environment；Micro- life
Object facture thoroughly but takes long time, inefficiency crude Treatment, and microorganism is to the pH of living environment, temperature, oxygen content
Deng there is strict demand, there is significant limitations；And the common oil skimmer oil-water separation of physical method is poor, purification efficiency compared with
It is low.In numerous processing means, absorption cleaning mode is considered as that crude oil clears up one of maximally efficient, thorough mode.
Currently, existing multiple material can be used for leaking the absorption cleaning of crude oil, mainly there are the inorganic species of mineral, synthesis organic
Species and natural organic matter class.The oily adsorption capacity of inorganic material is low；Synthetic organic material have good oil absorption, but by
It is difficult to the shortcomings that degrading in itself, is easy to cause secondary pollution；Natural organic derives from plant or animal body, has good
Reproducibility and biodegradability, but most natural organic has lower crude oil adsorptivity and absorbs and holds
Amount, therefore, developing novel there is environmentally friendly oil absorption material to become industry requirement.
As leakage crude oil absorbing material, high oil absorption content, it is highly selective, inexpensive be prerequisite feature.Gas
Gel is minimum one of the material of world's upper density, and internal 99.98% volume is air, has porous structure and keeps good
Good rigidity, can be worth by multiple material.Cellulosic material is main at present to use with biomass, environment reserves greatly main feature
In preparing paper products.With the increase year by year of paper consumption figure, waste paper already takes up in solid refuse 25%~40% ratio,
If realize waste paper effective use, on the one hand advantageously account for problem of environmental pollution, on the other hand can efficent use of resources, subtract
The destruction of few forest reserves.The main means of cellulose aerogels product are freeze-drying, by being dried in vacuo under cryogenic conditions,
It removes all moisture and prepares more hollow fiber network structures of pure cellulose matter.There are many researchs to focus on fiber at present
Cellulosic material oil suction is modified, such as prepares high lipophilic aeroge using bacteria cellulose as raw material, and achieve good oleophylic
Performance, but bacteria cellulose preparation process is complicated, and production efficiency is low, it is difficult to meet the needs of large-scale application.It is with waste paper
The research that raw material prepares aeroge often uses the processing modes such as solution modification method, liquid phase deposition, during hydrophobic modification
Solvent, the aeroge surface residual solvent used be easy to cause the chemical reagent pollution in modified and application process.Therefore, it uses
Waste paper as raw material prepare aeroge applied to crude oil leakage processing research direction in, high waste paper utilization rate, high-specific surface area,
Research emphasis of the easy modification mode, high oil absorption efficiency as cellulose aerogels.
Summary of the invention
The object of the present invention is to provide one kind using waste paper as raw material, prepares oleophylic based on gas-solid phase interface molecular regulation mechanism
Property cellulose aerogels method, waste paper is processed and be modified become aeroge oil absorption material.
The purpose of the present invention is achieved through the following technical solutions:
A method of lipophilic fiber element aeroge, concrete operations step are prepared based on gas-solid phase interface molecular regulation mechanism
It is rapid as follows:
One, the dissolution of waste paper and the preparation of dispersion liquid
Sodium hydroxide/urea liquid (solution mixing ratio is dispersed according to the ratio that solid content is 1%~2.5% by waste paper
Example is sodium hydroxide: urea=(0.15~0.2): in 1), and carrying out ultrasonic treatment 5min~10min, then sets dispersion liquid
It is freezed in refrigerator blocking.
Two, the preparation of cellulose aerogels
Blocking dispersion liquid will be freezed and be placed in thaw at RT, and be submerged in the solution that concentration of alcohol is 98.5%~99.5%
In solidified.Sample after solidification is placed in progress solvent displacement 45h~50h in deionized water, later -100 DEG C~-90
Cellulose aerogels are obtained after carrying out freeze-drying process 45h~50h under the conditions of DEG C temperature.
Three, the hydrophobic modification of cellulose aerogels
Cellulose aerogels after drying are put into the large container equipped with methyltrimethoxysilane (MTMS) to be placed in
Heating is sealed in bulk container, reaction temperature is 65 DEG C~75 DEG C, and the reaction time is 1h~3h to complete cellulose aerogels
The silylating reagent on surface；Cellulose aerogels after hydrophobic modification are placed in vacuum drying oven at 70 DEG C~75 DEG C and carry out heat
10h~12h is handled, to remove extra MTMS modifying agent.
The invention has the following beneficial effects:
1, cellulose aerogels are prepared by raw material of waste paper, can effectively solve the problem that the waste paper pollution in environment, reduces gloomy
Woods consumption and energy waste, and aeroge uses rear degradable recycling, for maintaining the ecological balance and environment sustainable development to have
There is good facilitation.
2, invention product has that large specific surface area, microfibril diameter be thin, microcosmic knot with cellulose aerogels for final pattern
Structure is regular, and number is recycled up to 5~10 times in the high feature of uniform pore diameter, porosity inside aeroge.
3, the present invention take silanes gas-solid phase interface regulation cellulose aerogels hydrophobic modification mode it is easy to operate,
Secondary pollution problem is not present in novel design, and the lipophilic fiber element aeroge oil suction multiplying power of preparation can reach own wt
50~300 times, there is good selectivity to finish class in oil mixing with water environment, there is very strong application value.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the scope of the present invention.
Specific embodiment 1
According to the ratio that solid content is 1% dispersing sodium hydroxide/urea liquid for waste paper, (solution mixed proportion is hydrogen-oxygen
Change sodium: in urea=0.15:1, and carry out ultrasonic treatment 5min, then dispersion liquid is placed in refrigerator freeze it is blocking.It will frost
Blocking dispersion liquid is placed in thaw at RT, and is submerged in the solution that concentration of alcohol is 98.5% and is solidified.After solidification
Sample is placed in progress solvent displacement 45h in deionized water, after carrying out freeze-drying process 45h under the conditions of -90 DEG C of temperature later
Obtain cellulose aerogels.
Cellulose aerogels after drying are put into the large container equipped with methyltrimethoxysilane (MTMS) to be placed in
Heating is sealed in bulk container, reaction temperature is 65 DEG C, and the reaction time is silane of the 1h to complete cellulose aerogels surface
Change and is modified；Cellulose aerogels after hydrophobic modification are placed in vacuum drying oven at 70 DEG C and carry out heat treatment 10h, it is more to remove
Remaining MTMS modifying agent.
Number is recycled up to 5 times in oil-absorption fiber element aeroge manufactured in the present embodiment, and oil suction multiplying power can reach itself
50 times of weight.
Specific embodiment 2
According to the ratio that solid content is 2.5% dispersing sodium hydroxide/urea liquid for waste paper, (solution mixed proportion is hydrogen
Sodium oxide molybdena: in urea=0.2:1, and carrying out ultrasonic treatment 10min, then dispersion liquid is placed in refrigerator freeze it is blocking.By ice
The dispersion liquid for being frozen into block is placed in thaw at RT, and is submerged in the solution that concentration of alcohol is 99.5% and is solidified.After solidifying
Sample be placed in deionized water progress solvent displacement 50h, progress freeze-drying process 50h under the conditions of -100 DEG C of temperature later
After obtain cellulose aerogels.
Cellulose aerogels after drying are put into the large container equipped with methyltrimethoxysilane (MTMS) to be placed in
Heating is sealed in bulk container, reaction temperature is 75 DEG C, and the reaction time is silane of the 3h to complete cellulose aerogels surface
Change and is modified；Cellulose aerogels after hydrophobic modification are placed in vacuum drying oven at 75 DEG C and carry out heat treatment 12h, it is more to remove
Remaining MTMS modifying agent.
Number is recycled up to 10 times in oil-absorption fiber element aeroge manufactured in the present embodiment, and oil suction multiplying power can reach itself
300 times of weight.
Specific embodiment 3
According to the ratio that solid content is 1.5% dispersing sodium hydroxide/urea liquid for waste paper, (solution mixed proportion is hydrogen
Sodium oxide molybdena: in urea=0.17:1, and carrying out ultrasonic treatment 8min, then dispersion liquid is placed in refrigerator freeze it is blocking.By ice
The dispersion liquid for being frozen into block is placed in thaw at RT, and is submerged in the solution that concentration of alcohol is 99% and is solidified.After solidification
Sample is placed in progress solvent displacement 48h in deionized water, after carrying out freeze-drying process 49h under the conditions of -95 DEG C of temperature later
Obtain cellulose aerogels.
Cellulose aerogels after drying are put into the large container equipped with methyltrimethoxysilane (MTMS) to be placed in
Heating is sealed in bulk container, reaction temperature is 70 DEG C, and the reaction time is silane of the 2h to complete cellulose aerogels surface
Change and is modified；Cellulose aerogels after hydrophobic modification are placed in vacuum drying oven at 73 DEG C and carry out heat treatment 12h, it is more to remove
Remaining MTMS modifying agent.
Number is recycled up to 8 times in oil-absorption fiber element aeroge manufactured in the present embodiment, and oil suction multiplying power can reach itself
80 times of weight.
Claims (4)
1. a kind of method for preparing lipophilic fiber element aeroge based on gas-solid phase interface molecular regulation mechanism, which is characterized in that
The method and step is as follows:
One, it the dissolution of waste paper and the preparation of dispersion liquid: disperses waste paper in sodium hydroxide/urea liquid, and carries out ultrasonic place
Reason form dispersion liquid, then the dispersion liquid is placed in refrigerator freeze it is blocking；
Two, the preparation of cellulose aerogels: blocking dispersion liquid will be freezed and be placed in thaw at RT, and be submerged in ethyl alcohol and coagulated
Gu；Sample after solidification is placed in progress solvent displacement in deionized water, obtains cellulose after carrying out freeze-drying process later
Aeroge；
Three, the hydrophobic modification of cellulose aerogels: the cellulose aerogels after drying are put into equipped with methyl trimethoxy oxygroup silicon
The large container of alkane, which is placed in bulk container, is sealed heat treatment, completes the silylating reagent on cellulose aerogels surface；
Cellulose aerogels after hydrophobic modification are placed in vacuum drying oven and are heat-treated, to remove extra methyl trimethoxy oxygroup
Silane.
2. a kind of as described in claim 1 prepare lipophilic fiber element aeroge based on gas-solid phase interface molecular regulation mechanism
Method, which is characterized in that
Solid content of the waste paper in sodium hydroxide/urea liquid is 1%~2.5%；
The sodium hydroxide/urea liquid configuration proportion is sodium hydroxide and urea quality ratio is 0.15~0.20:1；
The sonication treatment time is 5min~10min.
3. a kind of as described in claim 1 prepare lipophilic fiber element aeroge based on gas-solid phase interface molecular regulation mechanism
Method, which is characterized in that
The concentration of alcohol is 98.5%~99.5%；
The time that sample after the solidification carries out solvent displacement in deionized water is 45h~50h；
The freeze-drying process condition is -100 DEG C~-90 DEG C, 45h~50h.
4. a kind of as described in claim 1 prepare lipophilic fiber element aeroge based on gas-solid phase interface molecular regulation mechanism
Method, which is characterized in that
The cellulose aerogels hydrophobic modification reaction temperature is 65 DEG C~75 DEG C, and the reaction time is 1h~3h；
The vacuum drying oven heat treatment temperature is 70 DEG C~75 DEG C, and the processing time is 10h~12h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851839A (en) * | 2019-01-22 | 2019-06-07 | 仲恺农业工程学院 | A kind of aerogel material and the preparation method and application thereof |
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| CN105924686A (en) * | 2016-04-13 | 2016-09-07 | 四川大学 | Biology base polymer aerogel oil absorption material and preparation method thereof |
| CN107365423A (en) * | 2017-08-07 | 2017-11-21 | 武汉大学 | A kind of hydrophobically modified method of cellulose |
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| US20140130710A1 (en) * | 2011-05-06 | 2014-05-15 | Upm-Kymmene Corporation | Hydrophobic coating and a method for producing hydrophobic surface |
| CN103980547A (en) * | 2014-05-27 | 2014-08-13 | 哈尔滨工业大学 | Method for preparing magnetic cellulose aerogel from wastepaper |
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