CN109880215A - A kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhancing vinyon and preparation method thereof - Google Patents
A kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhancing vinyon and preparation method thereof Download PDFInfo
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Abstract
A kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhancing vinyon, it is characterised in that it is 40~85 parts of substrate that the plastics, which include by components by weight percent, 4~50 parts of phenol-formaldehyde resin modified in-situ reducing coats graphene oxide, 2.5~11 parts of crosslinking agent three parts form；It is that 95 ~ 100 parts of phenol-formaldehyde resin modified and 1 ~ 8% graphene oxide form that the phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide, which includes by components by weight percent, wherein phenol-formaldehyde resin modified in-situ polymerization, which is grown on graphene oxide active site, forms uniform phenolic resin clad, and by graphene oxide partial reduction.Usefulness of the present invention are as follows: (1) excellent fireproof performance；(2) at low cost, technology environmental protection.
Description
Technical field
The present invention relates to a kind of polythene materials and preparation method thereof, go back in situ more particularly to a kind of phenol-formaldehyde resin modified
Original cladding graphene oxide enhancing vinyon and preparation method thereof.
Background technique
Polyethylene has excellent chemical stability, lower temperature resistance, dielectric properties, easily molded processing and enough mechanical property
Energy and its powerful competitiveness, it has also become the resins for universal use that output is big, the wide one kind of purposes is important.Its manufactured goods is from thin
Film, tubing, daily necessities to electric wire and cable jacket material etc. have been seen everywhere, but the oxygen index (OI) of PE is 17.3, belongs to combustible material,
In burning, heat release rate is big, and calorific value is high, flame propagation speed, decomposes and generates fuel gas CO etc., is not easy to extinguish, easily
Fire is caused, huge threat is formed to the safety of life and property of people, this just makes PE product in electric appliance, skyscraper, coal
The application in many fields such as mine, tunnel, decoration is restricted, therefore just has especially important meaning to the fire-retardant research of polyethylene
Justice.
Two-dimentional carbon element crystal of the graphene as discovered in recent years has prominent and excellent heating conduction and mechanical property
Can, nanostructure is also very unique, and graphene has biggish specific surface area, and a small amount of additional amount can be to polymer matrix
Body performance generates significant impact.However graphene surface has inert state, it is poor with the interface compatibility of other media, and stone
Black alkene has stronger Van der Waals force between layers, is easy to produce aggregation each other, and graphene enhances polymer composites
It can be highly dependent on the raising of interface bond strength, the key factor of control interface intensity is surface-treated to graphene,
The effective extension for increasing graphene surface can be rolled into a ball, and different functional groups be introduced by surface treatment method, to effectively improve
The interface cohesion of graphene and resin, but to the generally organic matter that graphene is surface-treated, such as coupling agent, crosslinking agent
Deng flame retardant property is not generally high, reduces the flame retardant property of material again instead.Graphene oxide is due to a large amount of polar group
Group, with organic matrix and solvent it is easy to form it is good dispersion is blended, be the excellent selection of resin tooth material, but organic group
The appearance of group can cause the high-temperature stability of condensation material to be deteriorated.Method using reduction is by can be by the oxidation stone as reinforced phase
Black alkene is reduced into reduced graphene, but the removing of reducing agent not only higher cost, but also is easy pollution environment.
The Chinese invention patent that application notification number is 108148244 A of CN discloses a kind of flame retardant polyethylene material, leads to
Addition dispersing agent TAS-2A, technical white oil 10#, the copolymer of ethylene-octene, coupling agent, inorganic fillings etc. are crossed, polyethylene is obtained
The mechanical property of flame-retardant materials can reach using standard, and the flame retardant property of polythene material can be greatly improved, and make
Polythene material improves security performance when in use.
The Chinese invention patent that application notification number is 105237847 A of CN discloses a kind of preparation side of silvering graphite alkene
Method and its application in conductive Flame-retardant Hdpe explosion-suppressing material, pass through " the purification process of graphene；The acid of graphene
Change, silanization treatment；The preparation of graphene suspension；The preparation of silver ammino solution；These steps of the chemical silvering of graphene ", obtain
The graphene silver-plated to surface chemistry.Silvering graphite alkene and high molecular material are coextruded again, obtain conductive flame-retardant high-molecular/plating
The silver-colored compound explosion-suppressing material of graphene.With excellent electric conductivity, chemically, anti-flammability and datonation-inhibition function can overcome existing suppression
The defects of quick-fried material.
The Chinese invention patent that application notification number is 105733145 A of CN discloses a kind of oxidation that amion acetic acid is modified
Graphene, halogen-free flame retardance of polyvinyl alcohol material and preparation method thereof, by the way that amion acetic acid molecule is grafted to graphene oxide sheet
On layer, on the one hand, graphene sheet layer has certain air barrier and anti-flammability；On the other hand, elecrtonegativity carboxyl then can be used
In targeted induction MgAl-LDH lamella, to realize that MgAl-LDH's is evenly dispersed, the collaboration of graphene and MgAl-LDH is played
Fire retardation improves the flame retardant effect of PVA matrix.
Currently, domestic and foreign scholars and enterprise have carried out a large amount of research to the raising of graphene reinforced plastics heat resistance,
Research shows that the heat resistance of composite material is largely determined by the dispersibility of graphene, graphene reinforced phase at present
The raising of dispersion performance is mostly to have the surface of graphene modified and also realized originally by the subsequent chemistry of graphene oxide, still
Two kinds of means have certain defect.Modified graphene surface is just mostly the poor polymer material of heat resistance, and aoxidizes stone
The sequential reduction process of black alkene not only higher cost, and the removing environmental pollution of reducing agent is larger, is unfavorable for graphene material
Expect further genralrlization and application.
Summary of the invention
It is an object of the invention to overcome graphene to enhance polythene material bad dispersibility, graphene oxide sequential reduction is needed
The problem of adding and remove the cost and pollution of additional reducing agent.By the way that redox occurs before phenol and graphene oxide
Reaction solves needs additional the step of adding reducing agent, has saved cost and be also beneficial to environmental protection.In addition, melamine and urine
Plain phenol-formaldehyde resin modified in-situ polymerization is simultaneously grown on redox graphene surface and forms interspersed dispersion to graphene oxide sheet,
And redox graphene is formed and uniformly wraps layer, the redox graphene piece after not only contributing to reduction is in resin
In uniform dispersion；And for wrapping phenolic resin in layer, a large amount of rigid structure is also solved in melamine resin
The poor problem of other modifying agent flame retardant properties.The graphene oxide shell core knot that melamine and urea modified phenolic resin wrap
Structure can be evenly dispersed in polythene material, forms excellent flame retarding construction, is conducive to mentioning for polythene material flame retardant property
It is high.
To achieve the purpose of the present invention, used technical solution is: a kind of phenol-formaldehyde resin modified in-situ reducing cladding oxygen
Graphite alkene enhance vinyon, it is characterised in that the plastics include by components by weight percent be 40~85 parts substrate, 4~50
The phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide, 2.5~11 parts of crosslinking agent three parts composition of part；The substrate is
High density polyethylene (HDPE)；It is 95 ~ 100 parts that the phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide, which includes by components by weight percent,
Phenol-formaldehyde resin modified and 1 ~ 8% graphene oxide composition, wherein it is living to be grown on graphene oxide for phenol-formaldehyde resin modified in-situ polymerization
Form uniform phenolic resin clad on property site, and by graphene oxide partial reduction；The crosslinking agent is 2,5- diformazan
Base -2,5- bis(t-butylperoxy) hexane or cumyl peroxide.
The graphene oxide number of plies is 1 ~ 4 layer, 10 ~ 50 μm of piece diameter.
The phenol-formaldehyde resin modified is urea and cyanurotriamide modified thermoplastic phenolic resin, the phenol-formaldehyde resin modified
Preparation method include the steps that following sequences:
(1) it takes graphene oxide to add deionized water compound concentration 2 ~ 10wt% aqueous solution according to condition described in claim 1 ~ 2, surpasses
It is spare that 1 ~ 2h of sound obtains graphene oxide solution；
(2) 45~60 parts of phenol, 44~77 parts of formaldehyde, 2~7 parts of NaOH described in claim 1 ~ 2 are added according to mass ratio
It with graphene oxide solution described in 15 ~ 55 parts of steps (1), is uniformly mixed, is warming up to 65 ~ 75 DEG C, stirred under constant temperature anti-
1.5 ~ 2.5h is answered, 80 ~ 90 DEG C is then heated to, is stirred to react 2 ~ 3h under constant temperature, phenolic resin in-situ reducing cladding is made
Graphene oxide solution, wherein graphene oxide is partially reduced；
(3) 16~18 parts of melamines and 30~50 parts of urea are added in example in mass ratio in the solution obtained to step (2), 45
Then 1 ~ 1.5h of isothermal reaction under the conditions of ~ 60 DEG C is quickly cooled to 10 ~ 20 DEG C, obtain phenol-formaldehyde resin modified in-situ reducing cladding
Graphene oxide solution；
(4) solution for obtaining step (3) is under the conditions of 70 DEG C, -0.1 ~ -0.2MPa, the straight sample drying of vaccum dewatering, obtains
Phenol-formaldehyde resin modified in-situ reducing coats graphene oxide.
Usefulness of the present invention are as follows: (1) excellent fireproof performance, graphene oxide and phenol-formaldehyde resin modified form in situ poly-
Symphysis is long, interts dispersion, and formed to redox graphene and uniformly wrap layer, the oxygen reduction after not only contributing to reduction
Uniform dispersion of the graphite alkene piece in resin, and it is used to wrap phenolic resin in layer, it is a large amount of in melamine resin
Rigid structure also solves the problems, such as that other modifying agent flame retardant properties are poor；(2) phenol-formaldehyde resin modified can directly and graphite oxide
Alkene forms redox reaction, solves the problems, such as the application of reducing agent and removing, reduces cost, technology is more environmentally-friendly.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
It is as defined in the appended claims that the modification of form falls within the application.
Embodiment 1
A kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhancing vinyon, it is characterised in that the plastics
Including by components by weight percent be 40 parts substrate, 4 parts phenol-formaldehyde resin modified in-situ reducing coat graphene oxide, 2.5 parts of friendship
Join agent three parts composition；The substrate is high density polyethylene (HDPE)；The phenol-formaldehyde resin modified in-situ reducing coats graphene oxide
Including being that 95 parts of phenol-formaldehyde resin modified and 1% graphene oxide form by components by weight percent, wherein phenol-formaldehyde resin modified is poly- in situ
Symphysis, which is longer than on graphene oxide active site, forms uniform phenolic resin clad, and by graphene oxide partial reduction；
The crosslinking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane.
The graphene oxide number of plies is 1 layer, 10 ~ 50 μm of piece diameter.
The phenol-formaldehyde resin modified is urea and cyanurotriamide modified thermoplastic phenolic resin, the phenol-formaldehyde resin modified
Preparation method include the steps that following sequences:
(1) graphene oxide is taken to add deionized water compound concentration 2wt% aqueous solution, ultrasonic 1h according to condition described in claim 1 ~ 2
It is spare to obtain graphene oxide solution；
(2) according to mass ratio addition 45 parts of phenol described in claim 1,44 parts of formaldehyde, 2 parts of NaOH and 15 part of steps (1)
The graphene oxide solution is uniformly mixed, is warming up to 65 DEG C, is stirred to react 1.5h under constant temperature, then heats to 80
DEG C, it is stirred to react 2h under constant temperature, phenolic resin in-situ reducing is made and coats graphene oxide solution, wherein graphene oxide
It is partially reduced；
(3) 16 parts of melamines and 30 parts of urea are added in example in mass ratio in the solution obtained to step (2), under the conditions of 45 DEG C
Then isothermal reaction 1h is quickly cooled to 10 DEG C, obtain phenol-formaldehyde resin modified in-situ reducing and coat graphene oxide solution；
(4) solution for obtaining step (3) is under the conditions of 70 DEG C, -0.1MPa, the straight sample drying of vaccum dewatering, obtains modified phenol
Urea formaldehyde in-situ reducing coats graphene oxide.
Embodiment 2
A kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhancing vinyon, it is characterised in that the plastic bag
Include the substrate for being 85 parts by components by weight percent, 50 parts of phenol-formaldehyde resin modified in-situ reducing coats graphene oxide, 11 parts of crosslinking
Agent three parts composition；The substrate is high density polyethylene (HDPE)；The phenol-formaldehyde resin modified in-situ reducing coats graphene oxide packet
Including by components by weight percent is that 100 parts of phenol-formaldehyde resin modified and 8% graphene oxide form, and wherein phenol-formaldehyde resin modified is poly- in situ
Symphysis, which is longer than on graphene oxide active site, forms uniform phenolic resin clad, and by graphene oxide partial reduction；
The crosslinking agent is cumyl peroxide.
The graphene oxide number of plies is 4 layers, 10 ~ 50 μm of piece diameter.
The phenol-formaldehyde resin modified is urea and cyanurotriamide modified thermoplastic phenolic resin, the phenol-formaldehyde resin modified
Preparation method include the steps that following sequences:
(1) graphene oxide is taken to add deionized water compound concentration 10wt% aqueous solution according to condition described in claim 1 ~ 2, ultrasound
It is spare that 2h obtains graphene oxide solution；
(2) 60 parts of phenol, 77 parts of formaldehyde, 7 parts of NaOH and 55 part of steps described in claim 1 ~ 2 are added according to mass ratio
(1) graphene oxide solution described in is uniformly mixed, is warming up to 75 DEG C, is stirred to react 2.5h under constant temperature, then heats to
90 DEG C, 3h is stirred to react under constant temperature, and phenolic resin in-situ reducing is made and coats graphene oxide solution, wherein graphite oxide
Alkene is partially reduced；
(3) 18 parts of melamines and 50 parts of urea are added in example in mass ratio in the solution obtained to step (2), under the conditions of 60 DEG C
Then isothermal reaction 1.5h is quickly cooled to 20 DEG C, obtain phenol-formaldehyde resin modified in-situ reducing and coat graphene oxide solution；
(4) solution for obtaining step (3) is under the conditions of 70 DEG C, -0.2MPa, the straight sample drying of vaccum dewatering, obtains modified phenol
Urea formaldehyde in-situ reducing coats graphene oxide.
It above are only two specific embodiments of the invention, but the design concept of the present invention is not limited to this, all benefits
It is made a non-material change to the present invention with this design, should belong to the behavior for invading the scope of protection of the invention.But it is all
Without departing from the content of technical solution of the present invention, according to the technical essence of the invention any type of letter to the above embodiments
Single modification, equivalent variations and remodeling, still fall within the protection scope of technical solution of the present invention.
Claims (3)
1. a kind of phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide enhances vinyon, it is characterised in that the plastics
It is made of, is formulated substrate, phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide and crosslinking agent three parts are as follows:
Substrate, 40~85 parts
Phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide, 4~50 parts
Crosslinking agent, 2.5~11 parts
Wherein, the substrate is high density polyethylene (HDPE)；Phenol-formaldehyde resin modified in-situ reducing cladding graphene oxide include by
Components by weight percent is 95 ~ 100 parts of phenol-formaldehyde resin modified and 1 ~ 8% graphene oxide composition, and wherein phenol-formaldehyde resin modified is poly- in situ
Symphysis, which is longer than on graphene oxide active site, forms uniform phenolic resin clad, and by graphene oxide partial reduction；
The crosslinking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane or cumyl peroxide.
2. plastics according to claim 1, it is characterised in that the graphene oxide number of plies is 1 ~ 4 layer, piece diameter 10 ~ 50
μm。
3. plastics according to claim 1, it is characterised in that the phenol-formaldehyde resin modified is that urea and melamine change
The thermoplastic phenolic resin of property, the preparation method of the phenol-formaldehyde resin modified include the steps that following sequences:
(1) it takes graphene oxide to add deionized water compound concentration 2 ~ 10wt% aqueous solution according to condition described in claim 1 ~ 2, surpasses
It is spare that 1 ~ 2h of sound obtains graphene oxide solution；
(2) 45~60 parts of phenol, 44~77 parts of formaldehyde, 2~7 parts of NaOH described in claim 1 ~ 2 are added according to mass ratio
It with graphene oxide solution described in 15 ~ 55 parts of steps (1), is uniformly mixed, is warming up to 65 ~ 75 DEG C, stirred under constant temperature anti-
1.5 ~ 2.5h is answered, 80 ~ 90 DEG C is then heated to, is stirred to react 2 ~ 3h under constant temperature, phenolic resin in-situ reducing cladding is made
Graphene oxide solution, wherein graphene oxide is partially reduced；
(3) 16~18 parts of melamines and 30~50 parts of urea are added in example in mass ratio in the solution obtained to step (2), 45
Then 1 ~ 1.5h of isothermal reaction under the conditions of ~ 60 DEG C is quickly cooled to 10 ~ 20 DEG C, obtain phenol-formaldehyde resin modified in-situ reducing cladding
Graphene oxide solution；
(4) under the conditions of 70 DEG C, -0.1 ~ -0.2MPa, vaccum dewatering obtains the solution for obtaining step (3) until sample drying
It obtains phenol-formaldehyde resin modified in-situ reducing and coats graphene oxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929947A (en) * | 2021-11-01 | 2022-01-14 | 湖北省疾病预防控制中心（湖北省预防医学科学院） | Graphene hot compress material for eye massager and preparation method thereof |
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| CN104627994A (en) * | 2015-02-06 | 2015-05-20 | 中国科学院山西煤炭化学研究所 | Preparation method of reduced graphene oxide/phenol formaldehyde resin-base activated carbon in-situ composite material |
| KR20160062530A (en) * | 2014-11-25 | 2016-06-02 | 롯데케미칼 주식회사 | Geothermal pipe |
| CN108943917A (en) * | 2018-08-20 | 2018-12-07 | 苏州宏久航空防热材料科技有限公司 | A kind of modification phenolic resin-based composite material and preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665519A (en) * | 2013-12-02 | 2014-03-26 | 常州大学 | Special insulating low temperature resistant submarine cable material and preparation method thereof |
| KR20160062530A (en) * | 2014-11-25 | 2016-06-02 | 롯데케미칼 주식회사 | Geothermal pipe |
| CN104627994A (en) * | 2015-02-06 | 2015-05-20 | 中国科学院山西煤炭化学研究所 | Preparation method of reduced graphene oxide/phenol formaldehyde resin-base activated carbon in-situ composite material |
| CN108943917A (en) * | 2018-08-20 | 2018-12-07 | 苏州宏久航空防热材料科技有限公司 | A kind of modification phenolic resin-based composite material and preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113929947A (en) * | 2021-11-01 | 2022-01-14 | 湖北省疾病预防控制中心（湖北省预防医学科学院） | Graphene hot compress material for eye massager and preparation method thereof |
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