CN107502996A - A kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material - Google Patents

A kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material Download PDF

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Publication number
CN107502996A
CN107502996A CN201710537206.1A CN201710537206A CN107502996A CN 107502996 A CN107502996 A CN 107502996A CN 201710537206 A CN201710537206 A CN 201710537206A CN 107502996 A CN107502996 A CN 107502996A
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oil
parts
weight
carbon fiber
useless
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朱明�
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02Composition of linings ; Methods of manufacturing

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)
  • Water Treatment By Sorption (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material, it is after at least two waste liquid state oil respective pretreatments are cleaned, 58 ° of fixed oils, ms emulsifying agents, dimeric dibasic acid, SA dioctyl ester, oleic acid, blue or green oil, tung oil are added to carry out cross-mixing emulsification, after the effects such as modified and copolymerization, standing is layered, floor portions, which by wire drawing pre-oxidize charing black leadization surface treatment and the step such as batch, is made carbon fiber, and top section can be used for making composite nano materials.The energy has been saved by the recycling for the fluid oil that gives up, has realized sustainable development, while reduce the manufacturing cost of carbon fiber.The method treatment conditions of the present invention are gentle, can be carried out under normal temperature, suitable for production application, extend raw material sources prepared by carbon fiber, high financial profit.

Description

A kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material
Technical field
The present invention relates to the regeneration technology of useless fluid oil, and carbon fiber is prepared as raw material using useless fluid oil more particularly to one kind With the method for nano material.
Background technology
Useless fluid oil refers to gear oil, machinery oil, hydraulic oil, the useless machine changed from various machineries, vehicle, ship etc. Oil, transformer oil, lubricating oil, rubber oil, plastic oil, coal tar etc., mostly higher boiling, high-molecular weight hydrocarbon and non-hydrocarbons mixing Thing.Due to being mixed into dust during use, the impurity such as metal dust caused by other miscellaneous oil and mechanical wears and cause color Blackening, viscosity become big and gradually gone bad, and generate organic acid, colloid etc., it is difficult to be continuing with.It is annual to have largely useless fluid oil Produce and abandoned as waste material, cause environmental pollution, waste of resource.
At present useless fluid oil be mostly washed by soda acid or with a large amount of carclazytes to decolourize the methods of realize regeneration or production Diesel oil.Soda acid, which is washed, needs substantial amounts of severe corrosive industrial chemicals, and the carclazyte of decolouring and the sediment filtered out belong to secondary pollutant, Secondary pollution is easily caused, processing cost is higher.
Carbon fiber is a kind of one of photoelectricity basic material found in modern age, and the one kind being mainly made up of carbon is extraordinary fine Dimension, its phosphorus content is different and different with species, typically more than 90%.Carbon fiber has light and strong, light and firm, high temperature resistant, corrosion resistant Erosion, endurance, construction size stability is good and design is good, can large area aggressiveness shaping etc. the advantages that, obtained extensive Using its demand is also increasing.The preparation of carbon fiber at present, mostly be using some carbon containing organic fiber such as nylon yarns, Acrylics filament, artificial silk etc. are raw material, and organic fiber and plastic resin are combined together into charing is made carbon fiber, costly. If useless fluid oil can be applied to the preparation of carbon fiber, huge economic value will be realized.
The content of the invention
The invention provides a kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material, waste liquid is realized The regeneration of state oil.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method that carbon fiber is prepared using useless fluid oil as raw material, comprises the following steps:
1) at least two waste liquid state oils are not stood into 12-24h, filters off top layer scum silica frost and bottom sediment, then passed through Filter, adsorb to remove suspended impurity, then decolourize and remove mechanical admixture;
2) at least two useless fluid oils that will be handled through step 1) are mixed with same volume, take mixed useless fluid oil 20-60 parts by weight, 58 DEG C of fixed oils of 5-20 parts by weight and the MS-1 emulsifying agents of 0.5-5.0 parts by weight are added in stirring and is stirred 0.5-2h is mixed, then sequentially adds dimeric dibasic acid, SA dibutyl ester, the 0.5- of 0.5-3.0 parts by weight of 0.5-5.0 parts by weight Oleic acid, the green grass or young crops oil of 0.01-0.1 parts by weight and the tung oil of 0.01-1 parts by weight of 3.0 parts by weight, stirring 2-5h intersect and mixed Close emulsification;
3) by mixture stratification at 10 DEG C -35 DEG C obtained by step 2), the floor portions after layering are taken to make in high pressure To be weaved to obtain precursor under, precursor pre-oxidizes at 200 DEG C -500 DEG C, is then carbonized at 1000 DEG C -2000 DEG C, then at Graphitization at 2500 DEG C -3000 DEG C, the fiber after graphitization carry out starching after liquid phase oxidation, carbon fiber are made;After taking layering Top section is used to make composite nano materials.
Optionally, the waste liquid state grease separation from useless gear oil, useless machinery oil, waste hydraulic oil, used oil, useless transformer oil, Waste lubricating oil, waste rubber oil, converting plastic waste to oil and waste coal tar.
Optionally, in step 2), mixed useless fluid oil 20-60 parts by weight are taken, 8-15 parts by weight are added in stirring 58 DEG C of fixed oils and 1.0-2.0 parts by weight MS-1 emulsifying agents and stir 0.5-2h, then sequentially add 1.0-2.0 parts by weight Dimeric dibasic acid, the SA dibutyl ester of 0.5-1.0 parts by weight, the oleic acid of 0.5-1.0 parts by weight, 0.01-0.5 parts by weight green grass or young crops oil And the tung oil of 0.01-0.7 parts by weight, stirring 2-5h carry out cross-mixing emulsification.
Optionally, the time of the cross-mixing emulsification is 3h.
Optionally, the temperature of the cross-mixing emulsification is 10 DEG C -35 DEG C.
Optionally, the preparation method of the composite nano materials is:The upper strata after the layering of 30-60 parts is taken by weight Partly, 30-60 parts ceramic clay and 10 parts of water mix 20-60 minutes, by mould molding, by the base substrate after shaping in 800- Sinter and pressurize 1-3 hours at 900 DEG C, finishing is taken out after cooling.
Optionally, the composite nano materials are used to make brake block.
Compared to prior art, the invention has the advantages that:
1. useless fluid oil adds 58 ° of fixed oils, MS- emulsifying agents, dimeric dibasic acid, SA after the removal of impurity is gone in pretreatment Dibutyl ester, oleic acid, blue or green oil, tung oil are to carry out cross-mixing emulsification, and after the effects such as modified and copolymerization, standing is divided Layer, floor portions the step such as are surface-treated-batched by wire drawing-pre-oxidation-charing-graphitization-and carbon fiber is made, and pass through waste liquid The recycling of state oil has saved the energy, realizes sustainable development, while reduce the manufacturing cost of carbon fiber.
The process such as wash to carry out soda acid 2. the industrial chemicals of severe corrosive need not be added, do not produce secondary pollution, and handle Mild condition, it can carry out under normal temperature, suitable for production application, high financial profit.
3. materials are extensive, strong applicability, the raw material sources of carbon fiber preparation are extended.
4. top section can be used to make composite nano materials with metal, Ceramic Composite, it is widely used.
Following examples are described in further detail to the present invention;But a kind of of the present invention is prepared using useless fluid oil as raw material The method of carbon fiber and nano material is not limited to embodiment.
Embodiment
Embodiment 1
Used oil and waste lubricating oil are stood into 12h respectively, filter off top layer scum silica frost and bottom sediment, then by filtering, adsorbing To remove suspended impurity, then carry out decolorization, then remove because during use with metal machinery friction and caused by clay Deng mechanical admixture, then by treated used oil and waste lubricating oil with volume ratio 1:1 mixing carries out cross-mixing emulsification, utilizes Composition in all kinds of useless fluid oils is condensed, and specifically takes the mixed parts by weight of useless fluid oil 50,10 weights are added in stirring Measure 58 DEG C of fixed oils of part and the MS-1 emulsifying agents of 1.5 parts by weight and stir 1h, wait 58 DEG C of fixed oils to dissolve in useless fluid oil again The dimeric dibasic acid of 1.5 parts by weight is sequentially added to mineral oil modification and bonding, the SA dibutyl ester of 0.5 parts by weight, 0.5 parts by weight Oleic acid promote the tung oil of copolymerization, the green grass or young crops oil of 0.1 parts by weight and 0.5 parts by weight to be used for coagulative precipitation layering, stir under normal temperature 3h, the then stratification at 25 DEG C.
The floor portions after layering are taken to be weaved to obtain precursor under high pressure effect, precursor pre-oxidizes at 300 DEG C To heat-resisting and insoluble fiber, then it is carbonized at 1500 DEG C, the graphitization at 2500 DEG C, the fiber after graphitization carries out liquid Phase oxidation finally carries out starching processing to prevent stopping loss wound, carbon fiber is made to increase the compatibility to resin.
Top section 30%, ceramic clay 60% and water 10% after layering is taken to put into mixer stirring 30 by mass percentage Minute forms the material of leather hard to be well mixed, and is molded in press-in die, the base substrate after shaping is sintered and applied at 900 DEG C Plus-pressure extrudes 2 hours, takes out finishing after cooling, obtains composite nano materials brake block.
Embodiment 2
By useless gear oil, useless machinery oil, waste hydraulic oil, useless transformer oil, waste rubber oil, converting plastic waste to oil and waste coal tar point 24h is not stood, filters off top layer scum silica frost and bottom sediment, then removes suspended impurity by filtering, adsorbing, then is carried out at decolouring Reason, then remove because during use with metal machinery friction and caused by the mechanical admixture such as clay, then will be treated upper Oil is stated with volume ratio 1:1:……1:1 mixing carries out cross-mixing emulsification, is condensed using the composition in all kinds of useless fluid oils, Specifically take the mixed parts by weight of useless fluid oil 60, the 58 DEG C of fixed oils and 2.0 parts by weight of 15 parts by weight are added in stirring MS-1 emulsifying agents simultaneously stir 1.5h, then sequentially add the dimeric dibasic acids of 2.0 parts by weight, 1.0 parts by weight SA dibutyl ester, The oleic acid of 1.0 parts by weight, the green grass or young crops oil of 0.5 parts by weight and the tung oil of 0.7 parts by weight, stir 3h under normal temperature, then at 25 DEG C Stratification.
The floor portions after layering are taken to be weaved to obtain precursor under high pressure effect, precursor pre-oxidizes at 500 DEG C To heat-resisting and insoluble fiber, then it is carbonized at 2000 DEG C, the graphitization at 3000 DEG C, the fiber after graphitization carries out liquid Phase oxidation finally carries out starching processing to prevent stopping loss wound, carbon fiber is made to increase the compatibility to resin.
Top section 40%, ceramic clay 50% and water 10% after layering is taken to put into mixer stirring 30 by mass percentage Minute forms the material of leather hard to be well mixed, and is molded in press-in die, the base substrate after shaping is sintered and applied at 850 DEG C Plus-pressure extrudes 2 hours, takes out finishing after cooling, obtains composite nano materials brake block.
Embodiment 3
Waste hydraulic oil, used oil and useless transformer oil are stood into 18h respectively, filter off top layer scum silica frost and bottom sediment, then lead to Filtering, adsorb to remove suspended impurity, then carry out decolorization, then remove because during use with metal machinery friction and The mechanical admixtures such as caused clay, then by treated waste hydraulic oil, used oil and useless transformer oil with volume ratio 1:1:1 is mixed Close and carry out cross-mixing emulsification, be condensed using the composition in all kinds of useless fluid oils, specifically take mixed useless fluid oil 20 Parts by weight, 58 DEG C of fixed oils of 8 parts by weight and the MS-1 emulsifying agents of 1 parts by weight are added in stirring and stirs 1h, wait 58 DEG C firmly Carburetion dissolves in useless fluid oil the dimeric dibasic acid for sequentially adding 1 parts by weight to mineral oil modification and bonding, the certain herbaceous plants with big flowers two of 0.5 parts by weight Sour dibutyl ester, the oleic acid of 0.5 parts by weight promote the tung oil of copolymerization, the green grass or young crops oil of 0.01 parts by weight and 0.01 parts by weight to be used to condense Precipitated and separated, 3h is stirred under normal temperature, then the stratification at 25 DEG C.
The floor portions after layering are taken to be weaved to obtain precursor under high pressure effect, precursor pre-oxidizes at 200 DEG C To heat-resisting and insoluble fiber, then it is carbonized at 1000 DEG C, the graphitization at 2500 DEG C, the fiber after graphitization carries out liquid Phase oxidation finally carries out starching processing to prevent stopping loss wound, carbon fiber is made to increase the compatibility to resin.
Top section 60%, ceramic clay 30% and water 10% after layering is taken to put into mixer stirring 30 by mass percentage Minute forms the material of leather hard to be well mixed, and is molded in press-in die, the base substrate after shaping is sintered and applied at 800 DEG C Plus-pressure extrudes 2 hours, takes out finishing after cooling, obtains composite nano materials brake block.
Above-described embodiment is only used for further illustrating that a kind of of the present invention prepares carbon fiber as raw material using useless fluid oil and received The method of rice material, but the invention is not limited in embodiment, every technical spirit according to the present invention is to above example institute Any simple modification, equivalent change and modification made, each falls within the protection domain of technical solution of the present invention.

Claims (7)

  1. A kind of 1. method that carbon fiber and nano material are prepared using useless fluid oil as raw material, it is characterised in that comprise the following steps:
    1) at least two waste liquid state oils are not stood into 12-24h, top layer scum silica frost and bottom sediment is filtered off, then by filtering, inhaling Removing suspended impurity is accompanied by, then decolourizes and removes mechanical admixture;
    2) at least two useless fluid oils that will be handled through step 1) are mixed with same volume, take mixed useless fluid oil 20-60 Parts by weight, 58 DEG C of fixed oils of 5-20 parts by weight and the MS-1 emulsifying agents of 0.5-5.0 parts by weight are added in stirring and is stirred 0.5-2h, then sequentially add dimeric dibasic acid, SA dibutyl ester, the 0.5-3.0 of 0.5-3.0 parts by weight of 0.5-5.0 parts by weight Oleic acid, the green grass or young crops oil of 0.01-0.1 parts by weight and the tung oil of 0.01-1 parts by weight of parts by weight, stirring 2-5h carry out cross-mixing Emulsification;
    3) by mixture stratification at 10 DEG C -35 DEG C obtained by step 2), the floor portions after layering are taken under high pressure effect Weaved to obtain precursor, precursor pre-oxidizes at 200 DEG C -500 DEG C, is then carbonized at 1000 DEG C -2000 DEG C, then at 2500 Graphitization at DEG C -3000 DEG C, the fiber after graphitization carry out starching after liquid phase oxidation, carbon fiber are made;Take the upper strata after layering Part is used to make composite nano materials.
  2. 2. according to the method for claim 1, it is characterised in that:The certainly useless gear oil of the waste liquid state grease separation, useless machinery oil, give up Hydraulic oil, used oil, useless transformer oil, waste lubricating oil, waste rubber oil, converting plastic waste to oil and waste coal tar.
  3. 3. according to the method for claim 1, it is characterised in that:In step 2), mixed useless fluid oil 20-60 weight is taken Part, 58 DEG C of fixed oils of 8-15 parts by weight and the MS-1 emulsifying agents of 1.0-2.0 parts by weight are added in stirring and stirs 0.5-2h, Then the dimeric dibasic acids of 1.0-2.0 parts by weight, the SA dibutyl ester of 0.5-1.0 parts by weight, 0.5-1.0 parts by weight are sequentially added Oleic acid, the green grass or young crops oil of 0.01-0.5 parts by weight and the tung oil of 0.01-0.7 parts by weight, stirring 2-5h carry out cross-mixing emulsification.
  4. 4. according to the method for claim 3, it is characterised in that:The time of the cross-mixing emulsification is 3h.
  5. 5. according to the method for claim 1, it is characterised in that:The temperature of the cross-mixing emulsification is 10 DEG C -35 DEG C.
  6. 6. according to the method for claim 1, it is characterised in that:The preparation method of the composite nano materials is:By weight Part takes the top section after the layering of 30-60 parts, 30-60 parts ceramic clay and 10 parts of water to mix 20-60 minutes, passes through mould Tool shaping, the base substrate after shaping is sintered at 800-900 DEG C and pressurizeed 1-3 hours, and finishing is taken out after cooling.
  7. 7. according to the method for claim 6, it is characterised in that:The composite nano materials are used to make brake block.
CN201710537206.1A 2017-07-04 2017-07-04 A kind of method that carbon fiber and nano material are prepared using useless fluid oil as raw material Pending CN107502996A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105544019A (en) * 2015-12-16 2016-05-04 华南理工大学 High oil-absorbing polyacrylonitrile hollow activated carbon fiber and preparation method thereof
CN106582520A (en) * 2016-12-17 2017-04-26 清华大学 Carbon nanomaterial macro body, preparing method and particle adsorption filter properties

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105544019A (en) * 2015-12-16 2016-05-04 华南理工大学 High oil-absorbing polyacrylonitrile hollow activated carbon fiber and preparation method thereof
CN106582520A (en) * 2016-12-17 2017-04-26 清华大学 Carbon nanomaterial macro body, preparing method and particle adsorption filter properties

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
理查德•范•巴斯怀森: "《缸内直喷式汽油机 ***•原理•研发与前景 原书第3版》", 31 July 2016, 机械工业出版社 *
贺福: "《碳纤维及石墨纤维》", 31 July 2010, 化学工业出版社 *

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