CN104530293A - Preparation method of polyacrylate-graphene oxide composites - Google Patents
Preparation method of polyacrylate-graphene oxide composites Download PDFInfo
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- CN104530293A CN104530293A CN201410754101.8A CN201410754101A CN104530293A CN 104530293 A CN104530293 A CN 104530293A CN 201410754101 A CN201410754101 A CN 201410754101A CN 104530293 A CN104530293 A CN 104530293A
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Abstract
The invention discloses a preparation method of polyacrylate-graphene oxide composites, which belongs to the field of chemical industry. The method is implemented by taking graphene oxide as a filling body, taking N,N methylene bisacrylamide as a crosslinking agent and taking ammonium persulfate as an initiator through polymerizing the materials above and an acrylic acid by using an aqueous solution polymerization method so as to prepare a super-absorbent composite material. The method disclosed by the invention achieves the beneficial effect that polyacrylate-graphene oxide composites prepared according to the method are good in compatibility, water absorption and salt tolerance.
Description
Technical field
The invention belongs to chemical field, be specifically related to the preparation method of a kind of polyacrylic acid-graphene oxide mixture.
Background technology
In recent years, Graphene and graphene-based material, because of the electrical property of its excellence, stable thermal characteristics and good mechanical property, cause worldwide research interest.Graphene can occur to reunite and can not form the stable aqueous solution in water, limits its applicability widely.And the graphene oxide preparing Graphene can classify as the compound between graphite layers 177l of covalent linkage, because the electrostatic repulsion of himself wetting ability and interlayer can form the stable aqueous solution.In preparation process, the layer that different oxy radicals can embed graphite as carboxyl, hydroxyl, carbonyl etc. is asked or layer edge, and cause the expansion of its interlamellar spacing, this makes graphene oxide in " intercalation chemistry ", show application background.Also result on the other hand the avidity of graphite oxide to water and polar solvent.By water solution polymerization process, graphene oxide as inorganic laminated obturator can with all heteropolymer compounds, as polyaniline, polyvinyl alcohol, poly-(e. caprolactone) etc.Due to adding of graphene oxide, the thermal characteristics of mixture or mechanical property etc. all improve, but also there is not been reported graphene oxide to be applied to the research of superabsorbent water Material Field.
Since super water-absorbing material came out from 1 938 years, there is a lot of product success industrialization at present, be widely used in fields such as agricultural, medicine, environmental protection.Super water-absorbing material can adsorb and be equivalent to oneself weight tens to the hundred times even water of thousands of times or the aqueous solution.Its surprising water-retaining capacity comes from the repulsion effect in material structure on macromolecular chain between electric charge and the osmotic pressure effect inside and outside gel network.In addition, the degree of crosslinking of gel network and the wetting ability of material itself are also two important influence factors.The people such as Wang have prepared sodium alginate grafted polyacrylic acid/sodium sulfonate superabsorbent water complex by grafting copolymerization process; The people such as Leel have synthesized polyacrylamide/hectorite gel for Liquidity limit type dye.In recent years, a lot of research starts concern laminated inorganic matter, as super water-absorbing material to improve mixture absorption property with this prepared by clay, Muscovitum.
Summary of the invention
In order to overcome the above problems, the invention provides the preparation method of a kind of polyacrylic acid-graphene oxide mixture.
A preparation method for polyacrylic acid-graphene oxide mixture, said method comprising the steps of:
(1) taking 5-10 part vinylformic acid joins in 20-50 part graphene oxide dispersion of having prepared, and rapid stirring is to entirely molten;
(2), under room temperature, in above-mentioned mixed solution, add 16-20 part N, N. methylene-bisacrylamide, keeps rapid stirring simultaneously, passes into N
220-40min carries out gas displacement;
(3) after gas displacement, be warming up to 50-55 DEG C, fast 0.05-0.20 part ammonium persulphate joined in reaction system, be warming up to 70 DEG C of reaction 3-5h simultaneously;
(4) reaction system is down to room temperature, sample is washed with distilled water to neutrality, 60-80 DEG C of dry 24h;
(5) sample carries out grinding and crosses 400-500 mesh sieve and namely obtains described polyacrylic acid-graphene oxide mixture.
Further, the concentration of step (1) described graphene oxide dispersion is 0.05wt%-0.15wt%.
The beneficial effect that the present invention reaches is:
(1) polyacrylic acid prepared-graphene oxide mixture presents amorphous state, and graphene oxide, in complex systems, obvious agglomeration does not occur, and has good compatibility with polyacrylic acid-graphite oxide alkene polymer;
(2) graphene oxide add the water-retaining capacity drastically increasing polyacrylic acid-graphite oxide alkene polymer, water regain can reach 5099, active group in graphene oxide structure can be combined by-COOH the group on polyacrylic acid macromolecular chain, forms more closely knit polymer network structure and can hold more water molecules;
(3) stannic oxide/graphene nano lamella plays the effect of " nonionic " property obturator in macromolecule network, thus effectively prevent caving in of network structure, improves the salt tolerance of polyacrylic acid-graphene oxide mixture.
Embodiment
Embodiment 1
A preparation method for polyacrylic acid-graphene oxide mixture, said method comprising the steps of:
(1) taking 5 parts of vinylformic acid, to join the 20 parts of concentration prepared be in 0.15wt% graphene oxide dispersion, and rapid stirring is to entirely molten;
(2), under room temperature, in above-mentioned mixed solution, add 16 parts of N, N. methylene-bisacrylamides, keep rapid stirring simultaneously, pass into N
220min carries out gas displacement;
(3) after gas displacement, be warming up to 50-55 DEG C, fast 0.05 part of ammonium persulphate joined in reaction system, be warming up to 70 DEG C of reaction 3h simultaneously;
(4) reaction system is down to room temperature, sample is washed with distilled water to neutrality, 60-80 DEG C of dry 24h;
(5) sample carries out grinding and crosses 400-500 mesh sieve and namely obtains described polyacrylic acid-graphene oxide mixture.
Embodiment 2
A preparation method for polyacrylic acid-graphene oxide mixture, said method comprising the steps of:
(1) taking 10 parts of vinylformic acid, to join the 50 parts of concentration prepared be in 0.05wt% graphene oxide dispersion, and rapid stirring is to entirely molten;
(2), under room temperature, in above-mentioned mixed solution, add 20 parts of N, N. methylene-bisacrylamides, keep rapid stirring simultaneously, pass into N
240min carries out gas displacement;
(3) after gas displacement, be warming up to 50-55 DEG C, fast 0.20 part of ammonium persulphate joined in reaction system, be warming up to 70 DEG C of reaction 5h simultaneously;
(4) reaction system is down to room temperature, sample is washed with distilled water to neutrality, 60-80 DEG C of dry 24h;
(5) sample carries out grinding and crosses 400-500 mesh sieve and namely obtains described polyacrylic acid-graphene oxide mixture.
Embodiment 3
A preparation method for polyacrylic acid-graphene oxide mixture, said method comprising the steps of:
(1) taking 8 parts of vinylformic acid, to join the 40 parts of concentration prepared be in 0.10wt% graphene oxide dispersion, and rapid stirring is to entirely molten;
(2), under room temperature, in above-mentioned mixed solution, add 18 parts of N, N. methylene-bisacrylamides, keep rapid stirring simultaneously, pass into N
230min carries out gas displacement;
(3) after gas displacement, be warming up to 50-55 DEG C, fast 0.10 part of ammonium persulphate joined in reaction system, be warming up to 70 DEG C of reaction 4h simultaneously;
(4) reaction system is down to room temperature, sample is washed with distilled water to neutrality, 60-80 DEG C of dry 24h;
(5) sample carries out grinding and crosses 400-500 mesh sieve and namely obtains described polyacrylic acid-graphene oxide mixture.
Claims (2)
1. a preparation method for polyacrylic acid-graphene oxide mixture, is characterized in that, said method comprising the steps of:
(1) taking 5-10 part vinylformic acid joins in 20-50 part graphene oxide dispersion of having prepared, and rapid stirring is to entirely molten;
(2), under room temperature, in above-mentioned mixed solution, add 16-20 part N, N. methylene-bisacrylamide, keeps rapid stirring simultaneously, passes into N
220-40min carries out gas displacement;
(3) after gas displacement, be warming up to 50-55 DEG C, fast 0.05-0.20 part ammonium persulphate joined in reaction system, be warming up to 70 DEG C of reaction 3-5h simultaneously;
(4) reaction system is down to room temperature, sample is washed with distilled water to neutrality, 60-80 DEG C of dry 24h;
(5) sample carries out grinding and crosses 400-500 mesh sieve and namely obtains described polyacrylic acid-graphene oxide mixture.
2. the preparation method of the polyacrylic acid according to right 1-graphene oxide mixture, is characterized in that, the concentration of step (1) described graphene oxide dispersion is 0.05wt%-0.15wt%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105270077A (en) * | 2015-11-26 | 2016-01-27 | 张正西 | Ink painting drawing plate made of graphene and manufacturing method of ink painting drawing plate |
| CN105601850A (en) * | 2015-12-24 | 2016-05-25 | 吉首大学 | Preparation method of graphene oxide composite gel applicable to heavy metal adsorption |
| CN105949361A (en) * | 2016-06-15 | 2016-09-21 | 湖州超能生化有限公司 | Preparation method of solid sodium polyacrylate |
| CN106380544A (en) * | 2016-09-09 | 2017-02-08 | 河南农业大学 | Preparation method of graphene oxide doped environment-friendly super absorbent resin |
| CN106890626A (en) * | 2015-12-18 | 2017-06-27 | 财团法人工业技术研究院 | The formed method of sorbing material and adsorption type heat pump |
| CN107522996A (en) * | 2017-10-09 | 2017-12-29 | 浙江卫星新材料科技有限公司 | A kind of preparation method of Graphene antibiosis composition and antibacterial super absorbent resin |
| CN107556677A (en) * | 2017-10-09 | 2018-01-09 | 浙江卫星新材料科技有限公司 | A kind of super absorbent resin of high antibiotic property and high-salt tolerance and preparation method and application |
| CN108048542A (en) * | 2017-12-25 | 2018-05-18 | 信利光电股份有限公司 | The method of application and the PCR of graphene oxide polyacrylic acid composite |
| CN110563877A (en) * | 2019-09-29 | 2019-12-13 | 中国石油大学(华东) | preparation method of composite salt-resistant super absorbent resin |
| CN110790856A (en) * | 2019-11-14 | 2020-02-14 | 淄博宏达助剂有限公司 | Graphene oxide/polyacrylic acid composite hydrogel and preparation method thereof |
| CN112191235A (en) * | 2019-11-29 | 2021-01-08 | 南京工程学院 | Preparation method of porous compound capable of adsorbing calcium and magnesium ions |
| CN113929965A (en) * | 2020-11-23 | 2022-01-14 | 航天特种材料及工艺技术研究所 | Self-adaptive water loss composite water storage material and preparation method and application thereof |
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| CN103435951A (en) * | 2013-09-09 | 2013-12-11 | 江南大学 | Nanometer composite high-molecular dual-network hydrogel and preparation method thereof |
| CN103897093A (en) * | 2014-04-04 | 2014-07-02 | 武汉理工大学 | Graphene/polymer composite hydrogel thin film and preparation method thereof |
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| CN102580633A (en) * | 2011-12-31 | 2012-07-18 | 青岛大学 | Preparation method of graphene oxide/poly(N-isopropylacrylamide) composite hydrogel |
| CN103435951A (en) * | 2013-09-09 | 2013-12-11 | 江南大学 | Nanometer composite high-molecular dual-network hydrogel and preparation method thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105270077A (en) * | 2015-11-26 | 2016-01-27 | 张正西 | Ink painting drawing plate made of graphene and manufacturing method of ink painting drawing plate |
| CN106890626A (en) * | 2015-12-18 | 2017-06-27 | 财团法人工业技术研究院 | The formed method of sorbing material and adsorption type heat pump |
| CN105601850A (en) * | 2015-12-24 | 2016-05-25 | 吉首大学 | Preparation method of graphene oxide composite gel applicable to heavy metal adsorption |
| CN105949361A (en) * | 2016-06-15 | 2016-09-21 | 湖州超能生化有限公司 | Preparation method of solid sodium polyacrylate |
| CN105949361B (en) * | 2016-06-15 | 2018-04-13 | 湖州超能生化有限公司 | A kind of preparation method of solid-state Sodium Polyacrylate |
| CN106380544A (en) * | 2016-09-09 | 2017-02-08 | 河南农业大学 | Preparation method of graphene oxide doped environment-friendly super absorbent resin |
| CN107522996B (en) * | 2017-10-09 | 2019-12-20 | 浙江卫星新材料科技有限公司 | Preparation method of graphene composition for enhancing absorption performance of super absorbent resin |
| CN107522996A (en) * | 2017-10-09 | 2017-12-29 | 浙江卫星新材料科技有限公司 | A kind of preparation method of Graphene antibiosis composition and antibacterial super absorbent resin |
| CN107556677A (en) * | 2017-10-09 | 2018-01-09 | 浙江卫星新材料科技有限公司 | A kind of super absorbent resin of high antibiotic property and high-salt tolerance and preparation method and application |
| CN107556677B (en) * | 2017-10-09 | 2019-12-20 | 浙江卫星新材料科技有限公司 | High-pressure absorption and high-water-retention super absorbent resin and preparation method and application thereof |
| CN108048542A (en) * | 2017-12-25 | 2018-05-18 | 信利光电股份有限公司 | The method of application and the PCR of graphene oxide polyacrylic acid composite |
| CN110563877A (en) * | 2019-09-29 | 2019-12-13 | 中国石油大学(华东) | preparation method of composite salt-resistant super absorbent resin |
| CN110790856A (en) * | 2019-11-14 | 2020-02-14 | 淄博宏达助剂有限公司 | Graphene oxide/polyacrylic acid composite hydrogel and preparation method thereof |
| CN112191235A (en) * | 2019-11-29 | 2021-01-08 | 南京工程学院 | Preparation method of porous compound capable of adsorbing calcium and magnesium ions |
| CN113929965A (en) * | 2020-11-23 | 2022-01-14 | 航天特种材料及工艺技术研究所 | Self-adaptive water loss composite water storage material and preparation method and application thereof |
| CN113929965B (en) * | 2020-11-23 | 2023-09-26 | 航天特种材料及工艺技术研究所 | Self-adaptive water loss composite water storage material and preparation method and application thereof |
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