CN110358139A - Polyacrylamide/nano-cellulose composite aerogel and preparation method thereof - Google Patents
Polyacrylamide/nano-cellulose composite aerogel and preparation method thereof Download PDFInfo
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- CN110358139A CN110358139A CN201910793317.8A CN201910793317A CN110358139A CN 110358139 A CN110358139 A CN 110358139A CN 201910793317 A CN201910793317 A CN 201910793317A CN 110358139 A CN110358139 A CN 110358139A
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- nano
- polyacrylamide
- cellulose
- preparation
- composite aerogel
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Classifications
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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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
-
- 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
-
- 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
- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
-
- 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
Abstract
The present invention relates to a kind of polyacrylamide/nano-cellulose composite aerogels and preparation method thereof, belong to nano-cellulose field of compound material.This method is after mixing acrylamide solution with nano-cellulose, the gel that polyacrylamide is chemically crosslinked network interpenetrating nano-cellulose structure is formed by atom transition free radical polymerization reaction (ATRP), rear freeze-drying prepares polyacrylamide/nano-cellulose composite aerogel.The polyacrylamide that the present invention synthesizes/nano-cellulose composite aerogel shows the microcosmic Hierarchical porosity structure with macropore nesting micropore, is provided simultaneously with mild condition, easily operated feature.
Description
Technical field
The present invention relates to one kind using acrylamide as monomer, by atom transition free radical polymerization reaction (ATRP) and compound
Nano-cellulose prepares the method for aeroge under certain conditions.The present invention relates to a kind of polyacrylamide/nano-celluloses
Composite aerogel and preparation method thereof belongs to nano-cellulose field of compound material.
Background technique
Aeroge be it is a kind of accumulated as nano-scale particle made of, the lightweight solid material with nanoscale hole hole, therefore
With high porosity, specific surface area, the characteristics of excellent chemical stability, in energy-storing thermal insulation material, catalytic carrier, sound-absorbing
Material and high efficiency composition material etc. are all widely used.
Native cellulose has the characteristics such as from a wealth of sources, renewable, degradable and green non-pollution, and nano-cellulose is
Cellulosic molecule is manipulated in nano-scale range and carries out Modification design, prepares the novel nano material with excellent functionality
Material, nanometer fine chemical product, since it is with good biocompatibility and biodegradability, mechanical property equal spies by force
Point, and it is widely used in the preparation of composite material as nanometer reinforcing phase.Nano-cellulose is mutually embedded into polyacrylamide gel
In network, physical crosslinking is formed, and aeroge is made, can largely increase the intensity of polyacrylamide aeroge,
And make its being more widely applied in terms of load.
Summary of the invention
The object of the present invention is to provide a kind of polyacrylamide/nano-cellulose composite aerogel and preparation method thereof, with
Acrylamide is monomer, and the polyacrylamide gel of chemical crosslinking is formed by atom transition free radical polymerization reaction (ATRP),
Composite nano fiber element forms physical crosslinking, and the method for preparing aeroge under certain conditions simultaneously.
The present invention also provides a kind of polyacrylamide/nano-cellulose composite aerogel preparation method, this method packets
It includes:
(1) acrylamide is dissolved in DMSO, is uniformly mixed with CNF (cellulose nanometer fibril), obtains composite dispersion liquid；
(2) initiator, catalyst are added in the environment of nitrogen protection, is uniformly mixed, plural gel is made, and through dialysing
Processing removes impurity；
(3) plural gel is subjected to freeze-drying process, obtains polyacrylamide/nano-cellulose composite aerogel.
Above-mentioned technical proposal, in step (1), the raw material sources of CNF include at least one in timber, careless class and linen-cotton class
Kind.
Above-mentioned technical proposal, in step (1), the preparation method of CNF is high pressure homogenization method.
Above-mentioned technical proposal, in step (2), initiator is ethyl-alpha-bromopropionate, the ratio of acrylamide and initiator
For 15~25: 1 (w/w).
Above-mentioned technical proposal, in step (2), catalyst is cuprous bromide, the ratio of acrylamide and catalyst is 15~
25∶1(w/w)。
Above-mentioned technical proposal, in step (2), the reaction temperature and time for preparing plural gel can be selected in a wider range
It takes, preferable reaction temperature is 60~80 DEG C, and the reaction time is 12~24 hours.
Above-mentioned technical proposal, in step (3), freeze-drying temperature is -60 DEG C.
In the polyacrylamide of preparation/nano-cellulose plural gel, nano-cellulose is embedded in polypropylene as reinforced phase
In the porous network structure of amide, closely it is crosslinked with substrate；It is poly- after adding nano-cellulose compared with polyacrylamide gel
Acrylamide plural gel mechanical strength dramatically increases.
The present invention relates to polyacrylamide/nano-cellulose composite aerogel preparation method, the system of the aeroge
The characteristics of Preparation Method is simple, easy to implement, strong operability.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, following embodiment be it is descriptive,
It is not restrictive, these specific embodiments cannot be limited the invention to.In following embodiments, unless otherwise specified, institute
The experimental method used is conventional method, and reagent used etc. can chemically or biological reagent company is bought.
The present invention provides a kind of polyacrylamide/nano-cellulose composite aerogel preparation methods, which is characterized in that
Its method includes:
(1) acrylamide is dissolved in DMSO, is uniformly mixed with CNF (cellulose nanometer fibril), obtains composite dispersion liquid；
(2) initiator, catalyst are added in the environment of nitrogen protection, is uniformly mixed, plural gel is made, and through dialysing
Processing removes impurity；
(3) plural gel is subjected to freeze-drying process, obtains polyacrylamide/nano-cellulose composite aerogel.
Above-mentioned technical proposal, in step (1), the raw material of CNF is including timber, careless at least one of class and linen-cotton class.
Above-mentioned technical proposal, in step (1), the preparation method of CNF is high pressure homogenization method.
Above-mentioned technical proposal, in step (2), initiator is ethyl-alpha-bromopropionate, the ratio of acrylamide and initiator
For 15~25: 1 (w/w).
Above-mentioned technical proposal, in step (2), catalyst is cuprous bromide, the ratio of acrylamide and catalyst is 15~
25∶1(w/w)。
Above-mentioned technical proposal, in step (2), the reaction temperature and time for preparing plural gel can be selected in a wider range
It takes, preferable reaction temperature is 60~80 DEG C, and the reaction time is 12~24 hours.
Above-mentioned technical proposal, in step (3), freeze-drying temperature is -60 DEG C.
Embodiment 1
(1) it weighs 1.5g acrylamide to be dissolved in 10mlDMSO, mixes, obtain compound with 0.05g (over dry) CNF suspension
Dispersion liquid；
(2) 0.075g cuprous bromide is weighed, 54 μ L ethyl-alpha-bromopropionates is measured, is codissolved in compound point in a nitrogen environment
It in dispersion liquid, stirs evenly, is warming up to 80 DEG C and reacts 24 hours, obtain plural gel；
(3) to plural gel dialysis treatment 3 days, unreacted drug is removed；
(4) plural gel is placed in -40 DEG C of low temperature refrigerators and is saved 12 hours, is finally freeze-dried under the conditions of -60 DEG C
Obtain polyacrylamide/nano-cellulose composite aerogel.
Embodiment 2
(1) it weighs 1.5g acrylamide to be dissolved in 10mlDMSO, mixes, obtain compound with 0.05g (over dry) CNF suspension
Dispersion liquid；
(2) 0.1g cuprous bromide is weighed, 72 μ l ethyl-alpha-bromopropionates is measured, is codissolved in composite diffusion in a nitrogen environment
It in liquid, stirs evenly, is warming up to 80 DEG C and reacts 24 hours, obtain plural gel；
(3) to plural gel dialysis treatment 3 days, unreacted drug is removed；
(4) plural gel is placed in -40 DEG C of low temperature refrigerators and is saved 12 hours, is finally freeze-dried under the conditions of -60 DEG C
Obtain polyacrylamide/nano-cellulose composite aerogel.
Claims (4)
1. a kind of polyacrylamide/nano-cellulose composite aerogel and preparation method thereof, it is characterized in that in order including as follows
Step:
(1) acrylamide is dissolved in DMSO, is uniformly mixed with CNF (cellulose nanometer fibril), obtains composite dispersion liquid；
(2) initiator, catalyst are added in the environment of nitrogen protection, is uniformly mixed, plural gel is made, and through dialysis treatment
Remove impurity；
(3) plural gel is subjected to freeze-drying process, obtains polyacrylamide/nano-cellulose composite aerogel.
2. according to the method described in claim 1, wherein, in the step (1) raw material sources of CNF include timber, careless class and
At least one of linen-cotton class；The preparation method of CNF is high pressure homogenization method.
3. according to the method described in claim 1, wherein, initiator is ethyl-alpha-bromopropionate, acryloyl in the step (2)
The ratio of amine and initiator is 15~25: 1 (w/w)；Catalyst is cuprous bromide, the ratio of acrylamide and catalyst is 15~
25∶1(w/w)。
4. according to the method described in claim 1, wherein, reaction temperature and the time of plural gel are prepared in the step (2)
It can choose in a wider range, preferable reaction temperature is 60~80 DEG C, and the reaction time is 12~24 hours；In the step (3)
Being freeze-dried temperature is -60 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910793317.8A CN110358139A (en) | 2019-08-27 | 2019-08-27 | Polyacrylamide/nano-cellulose composite aerogel and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300419A (en) * | 2020-09-28 | 2021-02-02 | 浙江理工大学 | Preparation method of cellulose aerogel with environmental responsiveness |
| CN112851860A (en) * | 2021-01-08 | 2021-05-28 | 杭州所予科技有限公司 | Degradable cellulose-polyacrylamide composite water-retaining agent and preparation method thereof |
| CN114452948A (en) * | 2022-01-10 | 2022-05-10 | 安徽农业大学 | Modified cellulose aerogel and preparation method and application thereof |
-
2019
- 2019-08-27 CN CN201910793317.8A patent/CN110358139A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300419A (en) * | 2020-09-28 | 2021-02-02 | 浙江理工大学 | Preparation method of cellulose aerogel with environmental responsiveness |
| CN112300419B (en) * | 2020-09-28 | 2023-02-03 | 浙江理工大学 | Preparation method of cellulose aerogel with environmental responsiveness |
| CN112851860A (en) * | 2021-01-08 | 2021-05-28 | 杭州所予科技有限公司 | Degradable cellulose-polyacrylamide composite water-retaining agent and preparation method thereof |
| CN114452948A (en) * | 2022-01-10 | 2022-05-10 | 安徽农业大学 | Modified cellulose aerogel and preparation method and application thereof |
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Application publication date: 20191022 |
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