CN106589717A - Mechanochemical preparation method of polyphenol amine-polytetrafluoroethylene composite material - Google Patents
Mechanochemical preparation method of polyphenol amine-polytetrafluoroethylene composite material Download PDFInfo
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- CN106589717A CN106589717A CN201611079832.2A CN201611079832A CN106589717A CN 106589717 A CN106589717 A CN 106589717A CN 201611079832 A CN201611079832 A CN 201611079832A CN 106589717 A CN106589717 A CN 106589717A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention provides a mechanochemical preparation method of a polyphenol amine-polytetrafluoroethylene composite material. The method comprises the following steps: (1) adding phenol and amine into pure water or water with a certain pH value according to a certain molar ratio, stirring and uniformly mixing; (2) transferring the phenol amine solution into a mortar and adding a proper amount of polytetrafluoroethylene; (3) grinding the blend in the mortar until polytetrafluoroethylene is completely changed to be dark brown and is not floated on the liquid surface; (4) after the reaction is finished, washing with water and absolute ethanol separately and freeze-drying until constant weight to obtain the polyphenol amine-polytetrafluoroethylene composite material. The preparation method provided by the invention is simple and convenient, short in preparation time, low in preparation cost and simple in aftertreatment; the hydrophilcity of polytetrafluoroethylene is obviously improved and the application range of polytetrafluoroethylene is wider.
Description
Technical field
The present invention relates to a kind of method that mechanochemistry polymerization prepares poly- phenol amine-ptfe composite.
Background technology
Low consumption, low-carbon (LC), environmental protection, sustainable development are the calls of current era, are also the national following selection of relation.So
And, a kind of wear phenomenon, natural phenomena of the generally existing caused by friction is generally deposited as the main cause of condemned MAT'L
Great riches is being caused to lose.Therefore, the destruction for study tribology, reducing fretting wear, material is reduced or avoided, be both
Energy saving and the maximally effective means of material, are again the inevitable choices in accordance with era development.
Politef（PTFE）It is a kind of important macromolecular material, with extremely excellent performance, such as high lubrication
Property, chemical stability, against weather etc., be widely used in the industrial departments such as Aero-Space, machinery, building, have become existing
Many key technologies are solved in generation science and technology and the indispensable material of production technology level is improved.However, its own surface
Extremely low, the surface wettability extreme difference of energy so that its terrifically hydrophobic, oleophobic, hardly possible is combined with other materials, limits its potential
Play, also limit its micro-nano powder as the application of high-performance lubricating additive.
To solve the problems, such as the surface inertness of PTFE, scientist is modified its surface to increase by various means
Plus its wettability and the compatibility with other materials.Current method mainly has：Sodium-naphthalene chemistry of complex etching processing method, height
Energy via radiation grafting modification method, laser emission modified method, ion implantation modification and plasma modification method etc..Although these methods are all
Energy preferably modified ptfe, but, the medicine of costliness, complicated process and special instrument limit these methods extensive
Using.
Politef is modified with mechanochemical reaction, so far it has not been found that similar report.
The content of the invention
For overcome the shortcomings of prior art there are problems that and, it is an object of the invention to provide a kind of mechanochemistry prepare it is poly-
The method of phenol amine-ptfe composite, the preparation time is short, preparation process environmental protection, prepare it is simple etc. excellent
Point, is a kind of polymerization that is gentle, easily operating and realize industrialized production.
To realize the purpose of the present invention, there is provided technical scheme below：
A kind of method that mechanochemistry prepares poly- phenol amine-ptfe composite, it is characterised in that following steps：
（1）The phenol of certain mol proportion and amine are added in the water of pure water or certain pH value, stirring, mix homogeneously；
（2）The phenol amine aqueous solution is proceeded to into mortar, and adds appropriate politef；
（3）Blend is ground in mortar, politef is ground to and is changed into dark brown completely, and no longer float on liquid level
On；
（4）After the completion of reaction, respectively with water and absolute ethanol washing, lyophilization obtains poly- phenol amine-politef to constant weight
Composite.
Preparation method is simple of the present invention, preparation time is short, and preparation cost is low, and post processing is simple；Significantly improve polytetrafluoro
The hydrophilic of ethylene, makes being more widely applied for politef.
Further, phenol is at least one in catechol, hydroquinone, pyrogallol in the step.
Further, in the step amine be diethylenetriamine, triethylene tetramine, TEPA or structural formula be
NH2(CH2)nNH2Fatty amine（N represents 2 to 12 integer）In at least one.
Further, the mol ratio of phenol and amine is 0.8 ~ 1.2 in the step: 1.
Further, the mass ratio of politef and phenol is 1 in the step: 0.02~1.
Further, certain pH value is pH=7.0 ~ 9.9 in the step.
Further, milling time is 1 ~ 4 hour in the step.
The present invention proposes a kind of brand-new scheme for preparing modified Teflon, i.e., pass through mechanochemistry using phenol and amine
The method of polymerization is modified.Conventional electrochemistry and chemical polymerization are compared in mechanochemistry polymerization, had that preparation time is short, are prepared
The advantages of process environmental protection, simple preparation method, simple technological process and higher polymerization efficiency, machinery polymerization is by outer
Plus mechanical force enable to be polymerized faster in be polymerized very slow poly- phenol amine of ptfe surface under other reaction conditions
In ptfe surface.So that politef can be dispersed in water, solid friction field is preferably applied to.
Compared with other technologies, the invention has the advantages that：
（1）Preparing raw material by poly- phenol amine-ptfe composite of the present invention is with low cost, is easy to popularization to make
With the politef after modification has hydrophilic, in can apply to wider solid friction system.
（2）Preparation process is simple of the present invention, preparation process environmental protection is adapted to scale industrial production.
Specific embodiment
Technical scheme is further elaborated with reference to specific embodiment, these embodiments are intended merely to explain
State technical scheme and the restriction to the claims in the present invention content can not be considered as.It is raw materials used in embodiment to be often
Rule commercial products device therefor is conventional equipment method of testing and is conventional method.
Embodiment 1
Catechol and triethylene tetramine are added in pure water so as to which mol ratio is 0.9:1, stirring, mix homogeneously；Then will
The phenol amine aqueous solution proceeds to mortar, and adds politef so as to the mass ratio of catechol be 10:1, grind 2 hours
Afterwards, separated, washed, being dried, you can poly- phenol amine-ptfe composite is obtained.
Embodiment 2
Hydroquinone and hexamethylene diamine are added in the water of pH value 8.0 so as to which mol ratio is 1:1, stirring, mix homogeneously；Then
The phenol amine aqueous solution is proceeded to into mortar, and adds politef so as to the mass ratio of catechol be 5:1, grind 3 hours
Afterwards, separated, washed, being dried, you can poly- phenol amine-ptfe composite is obtained.
Embodiment 3
（1）During 0.035 catechol and 0,037g1,6- hexamethylene diamine are added containing the mortar that 5mL pH are 8.5 buffer, to the greatest extent
Amount stirs.
（2）Add 0.420g politef.
（3）Blend is ground into 4 h in agate mortar, politef is ground to and is changed into dark brown completely, and not
Float on again on buffer；
（4）It is neutrality to pH value of solution respectively with water and absolute ethanol washing after the completion of reaction, is dried to constant weight, obtains poly- phenol
Amine-ptfe composite.
Embodiment 4
（1）During 0.070g catechols and 0,074g1,6- hexamethylene diamine are added containing the mortar that 5mL pH are 9.0 buffer, to the greatest extent
Amount stirs.
（2）Add 0.420g politef.
（3）Blend is ground into 3 h in agate mortar, politef is ground to and is changed into dark brown completely, and not
Float on again on buffer；
（4）It is neutrality to pH value of solution respectively with water and absolute ethanol washing after the completion of reaction, is dried to constant weight, obtains poly- phenol
Amine-ptfe composite.
Claims (7)
1. a kind of method that use mechanochemistry polymerization prepares poly- phenol amine-ptfe composite；Method and step is as follows：
The phenol of certain mol proportion and amine are added in the water of pure water or certain pH value, mix homogeneously；After proceed to mortar, add appropriate
Politef, be ground, be ground to politef and be changed into dark brown completely, and no longer float on liquid level；Wash
Drying is washed, poly- phenol amine-ptfe composite is obtained.
2. one kind as claimed in claim 1 prepares poly- phenol amine-micron order politef composite wood with mechanochemistry polymerization
The method of material, it is characterised in that described phenol is at least one in catechol, hydroquinone, pyrogallol.
3. a kind of use mechanochemistry polymerization as claimed in claim 1 prepares the side of poly- phenol amine-ptfe composite
Method, it is characterised in that described amine is diethylenetriamine, triethylene tetramine, TEPA or structural formula are NH2(CH2)
nNH2Fatty amine（N represents 2 to 12 integer）In at least one.
4. a kind of use mechanochemistry polymerization as claimed in claim 1 prepares the side of poly- phenol amine-ptfe composite
Method, it is characterised in that described phenol and the mol ratio of amine is 0.8 ~ 1.2: 1.
5. a kind of use mechanochemistry polymerization as claimed in claim 1 prepares the side of poly- phenol amine-ptfe composite
Method, it is characterised in that described politef and the mass ratio of phenol is 1: 0.02~1.
6. a kind of use mechanochemistry polymerization as claimed in claim 1 prepares the side of poly- phenol amine-ptfe composite
Method, it is characterised in that described certain pH value is pH=7.0 ~ 9.9.
7. a kind of use mechanochemistry polymerization as claimed in claim 1 prepares the side of poly- phenol amine-ptfe composite
Method, it is characterised in that described milling time is 1 ~ 4 hour.
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| CN201611079832.2A CN106589717B (en) | 2016-11-30 | 2016-11-30 | A kind of method that mechanochemistry prepares poly- phenol amine-ptfe composite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020166988A1 (en) * | 2019-02-15 | 2020-08-20 | 성균관대학교산학협력단 | Modified polytetrafluoroethylene, manufacturing method therefor, ion exchange membrane using same, and method for manufacturing ion exchange membrane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262664A (en) * | 2014-09-10 | 2015-01-07 | 齐鲁工业大学 | Preparation method of poly(phenol-amine) superhydrophilic particulates |
-
2016
- 2016-11-30 CN CN201611079832.2A patent/CN106589717B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262664A (en) * | 2014-09-10 | 2015-01-07 | 齐鲁工业大学 | Preparation method of poly(phenol-amine) superhydrophilic particulates |
Non-Patent Citations (3)
| Title |
|---|
| 刘晓玲，等: "pH响应性聚酚胺微胶囊制备及其吸附性能研究", 《齐鲁工业大学学报》 * |
| 王琪 等: "高分子力化学研究进展", 《高分子通报》 * |
| 阮子宁，等: "聚（邻苯二酚-己二胺）-聚苯乙烯复合材料的亲疏水性能研究", 《齐鲁工业大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020166988A1 (en) * | 2019-02-15 | 2020-08-20 | 성균관대학교산학협력단 | Modified polytetrafluoroethylene, manufacturing method therefor, ion exchange membrane using same, and method for manufacturing ion exchange membrane |
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| CN106589717B (en) | 2018-12-21 |
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Effective date of registration: 20210419 Address after: No.13, 3rd floor, building 1, No.1, Tidu street, Qingyang District, Chengdu, Sichuan 610041 Patentee after: Chengdu yishenrui Technology Co.,Ltd. Address before: 250353 Ji'nan University, Changqing, Shandong Road, No. 3501 Patentee before: Qilu University of Technology Effective date of registration: 20210419 Address after: 215600 Zhujiang Road, modern agriculture demonstration park, Zhangjiagang City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Chi Knight Anticorrosive Technology Co.,Ltd. Address before: No.13, 3rd floor, building 1, No.1, Tidu street, Qingyang District, Chengdu, Sichuan 610041 Patentee before: Chengdu yishenrui Technology Co.,Ltd. |