CN108047495A - A kind of in-situ preparation method of carbon nanotubes and the superpower compounded mix of carbon black - Google Patents
A kind of in-situ preparation method of carbon nanotubes and the superpower compounded mix of carbon black Download PDFInfo
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- CN108047495A CN108047495A CN201711279620.3A CN201711279620A CN108047495A CN 108047495 A CN108047495 A CN 108047495A CN 201711279620 A CN201711279620 A CN 201711279620A CN 108047495 A CN108047495 A CN 108047495A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention belongs to technical fields prepared by compounded mix, more particularly to carbon nanotubes and the in-situ preparation method of the superpower compounded mix of carbon black, quantitative carbon nanotubes is blended into the carbon nanotubes prepared again through high-temp in-situ after the liquid material for preparing carbon black and the superpower compounded mix of carbon black in advance.Carbon nanotubes is added in advance in the liquid material for preparing carbon black, the superpower compounded mix of carbon nano-tube in situ and carbon black, the carbon nanotubes for preparing to be premixed into is served as theme, the perfect class grape string structure in the form of the carbon black particle generated is a beading.The superpower compounded mix being formed in situ can freely control the composition ratio of carbon nanotubes and carbon black, play conductive and reinforcing effect well, can substitute the superconduction carbon black of import completely.Present invention process simple and stable, it is easy to operation, without the existing carbon black production device of change and equipment.
Description
Technical field
The invention belongs to technical fields prepared by compounded mix, and in particular to carbon nanotubes and the superpower compounded mix of carbon black
Quantitative carbon nanotubes is blended into what is prepared again through high-temp in-situ after the liquid material for preparing carbon black by in-situ preparation method in advance
Carbon nanotubes and the superpower compounded mix of carbon black.
Background technology
Carbon nanotubes has excellent physical mechanical property, mainly has hexagonal row as monodimension nanometer material
The carbon atom of row forms several layers to tens of layers of coaxial pipe.It has very big draw ratio, diameter usually 1-100nm it
Between, length is at a few micrometers to hundreds of microns.Just because of its big draw ratio, carbon nanotubes is in mechanics, electricity, electrical and thermal conductivity
Energy aspect all shows very excellent.Since it is with excellent performance, carbon nanotubes is in catalyst carrier, rubber plastic composite wood
The numerous areas such as material, electrochemical material, photoelectric sensing all have wide, potential application prospect.
Carbon nanotubes compounded with carbon black after can the microcosmic lower conductive structure for forming similar thyrsiform, Points And lines
Organic assembling forms three-dimensional conductive network, conductive capability is greatly improved, reinforcing effect also has very big promotion.With the hair of technology
The compounding filler of exhibition and the reduction of cost, carbon nanotubes and carbon black will obtain more widely should in plastics and rubber
With.
Patent CN201410693341.1 discloses a kind of multi-factor structure complex conductive fillers.Its invention is to light inorganic
One layer of powder (hollow glass micropearl, mica, carbon fiber, flake graphite etc.) coating surface suction ripple magnetic material (such as Ni, Fe,
Co, Ni-P, Co-P, Ni-Co-P, Co-W-P, barium ferrite, ferroso-ferric oxide, carbonyl iron etc.), then plating layer of conductive material
(such as inorganic oxides such as silver, nickel, copper metal or doped stannum oxide, doped indium oxide, doping zinc-oxide, titanium dioxide), system
Obtain new multicomponent structure composite conductive filler-inorganic particle kernel/magnetic material coating/conductive material coating.Such composite guide
Electric filler can further improve the reflecting properties of electromagnetic wave the absorbent properties and conductive material of electromagnetic wave using absorbing material
Its capability of electromagnetic shielding has many advantages, such as light weight, at low cost, shielding bandwidth, advantages of good shielding performance, compound being electromagnetically shielded
Material Field has very big application value.But its is complicated for operation, and technique is cumbersome not easy to control, is unfavorable for directly promoting amplification industry
Change.
Patent CN201610469431.1 discloses a kind of preparation method of sulfenyl product carbon complex conductive fillers, belongs to
In conductive filler preparing technical field.The invention in alkaline conditions, using microwave irradiation, makes peach gum initial hydrolysis that peach be made
Gummy slurry is spare, recycles acid methane-generating pit supernatant processing petrochemical industry product carbon, dissolves ash content therein, obtain carbon black
It to purifying, is mixed with spare peach gum slurry, adds in yeast fermentation, make mixture that there is porous structure, then pass through screw extruding
The uniformity of filler is improved, addition sublimed sulfur is compound, through calcining peach gum adhesive is made to be carbonized, and remaining carbon is fixed as skeleton
Complex conductive fillers are made in sulphur and carbon black in filler.Its step of preparation process is still cumbersome, and requirement to equipment is high, cost compared with
It is high.
Patent CN201610898391.2 discloses a kind of aqueous, environmental protective conductive carbon based on graphene-carbon black compounded mix
Starch preparation method, it is characterised in that its mass percentage composition is：Binding agent：5-20%, mixed solvent：65-85%, graphene：
0.1-5%, carbon black：1-15%, dispersant：0.05-1%, antifoaming agent：0.1-1%, crosslinking agent：0.1-1%, thickener：0.1-1%.It should
Invention still needs carbon black product later stage and graphene, dispersant etc. to carry out, and external force is compound to get to corresponding requirements.
Although the preparation process and mode of conductive filler are improved, still remain can not be prepared in situ, carbon black needs
Later stage and other conductive agents compounding, preparation process complexity is cumbersome, technology controlling and process is difficult, is not easy the problems such as scale amplification, therefore,
It is badly in need of a kind of on carbon nanotubes and the in-situ preparation method of the superpower compounded mix of carbon black.
The content of the invention
It is an object of the invention to for it is of high cost existing for the existing preparation process of current conductive filler, processing step is complicated
It is cumbersome, the problems such as carbon nanotubes and carbon black superpower compounded mix method is not prepared in situ, provide a kind of carbon nanotubes and carbon black
The in-situ preparation method of superpower compounded mix, carbon nanotubes is added in advance in the liquid material for preparing carbon black, in original charcoal
Under black preparation process and appointed condition, the superpower compounded mix of carbon nano-tube in situ and carbon black.The present invention can be achieved certainly
By controlling（It needs to add in carbon nanotubes in advance so as to be calculated according to final proportioning by the quantity for the carbon black for precalculating generation
The mode of quantity realize）The composition ratio of carbon nanotubes and carbon black, simple production process, flow is easily operated, at low cost,
It is easy to large-scale promotion.
The technical scheme is that：
Carbon nanotubes, is blended into the liquid for preparing carbon black by the in-situ preparation method of a kind of carbon nanotubes and the superpower compounded mix of carbon black
Carbon nanotubes and the superpower compounded mix of carbon black are prepared through high-temp in-situ again after state raw material, in carbon black feed stock through high temperature generation carbon black
Meanwhile the carbon nanotubes for preparing to be premixed into is served as theme, the perfect class Portugal in the form of the carbon black particle generated is a beading
Grape string structure.
The in-situ preparation method of a kind of carbon nanotubes and the superpower compounded mix of carbon black, is as follows：
（1）Carbon nanotubes is mixed into the liquid material for preparing carbon black, the weight ratio of carbon nanotubes and liquid material is received for carbon
Mitron：Liquid material=0.1:100-500:100；
（2）The mixture of carbon nanotubes and liquid material is warming up to 50-110 DEG C of dehydration；
（3）Carbon nanotubes and liquid starting material mixture are preheated to 600-650 DEG C, in atomized spray to reacting furnace；
（4）After progressive solution, at a temperature of 1000 DEG C -2300 DEG C, the superpower of carbon nanotubes and carbon black is prepared in situ and compound fills out
Material；
（5）To 800 DEG C -860 DEG C, point three-level carries out being cooled to 230 DEG C -240 DEG C quench zone spray cooling；
（6）Separation is collected, 70 DEG C of -120 DEG C of dryings.
The features of the present invention also has：
The weight ratio of carbon nanotubes and liquid material is carbon nanotubes：Liquid material=10:100-50:100, preferred section
Effective grape cluster conductive structure is more readily formed.
The liquid material for preparing carbon black is the one or more of coal tar, pitch, clarified oil, ethylene bottom oil
Mixture, wherein, clarified oil is that Catalytic Cracking Unit of Measure passes through simply dealt catalytic slurry at once, and clarification oil density is big, hydrogen content
Low, saturated hydrocarbons and arene content account for 50%-60%.
The carbon nanotubes is single-walled carbon nanotube, double-walled carbon nano-tube, the one or more of multi-walled carbon nanotube
Mixture, the particle size range of the carbon nanotubes is 50nm-500 μm, is preferably 100nm-50 μm, more preferable 1 μm of -20 μ
M, suitable carbon nanotubes grain size can provide more suitably space and match combination with the carbon black formed.
The mixture of the carbon nanotubes and liquid material heating dehydration temperaturre is 80-90 DEG C, suitable temperature range,
Efficiency improves during drying, and is not easy to form caking with high hardness.
The step（4）Progressive solution, for three-level heat（Three sections of heating, temperature gradually rise, temperature are avoided to rise sharply and is drawn
The carbon distribution risen）；Temperature is prepared in situ as 1400-1700 DEG C, the agraphitic carbon ratio of the too low formation of temperature raises, temperature too Gao Ze
It is too fast to form speed, thyrsiform structure forms insufficient, all has detrimental effect to the conduction and reinforcing property of composite material.
The carbon nanotubes obtained by the carbon nanotubes of the present invention and the in-situ preparation method of the superpower compounded mix of carbon black
With the superpower compounded mix of carbon black, have and served as theme with the carbon nanotubes being premixed into, in the form of the carbon black particle generated is a beading
Perfect class grape string structure.
The superpower compounded mix of carbon nanotubes and carbon black of acquisition is for the conduction of plastics and rubber, heat conduction, reinforcement.
Beneficial effects of the present invention are：The present invention is filled in advance using a certain proportion of carbon nanotubes into the liquid for preparing carbon black
In state raw material；When preparing carbon black, the superpower composite conducting material of carbon nano-tube in situ and carbon black；By controlling carbon nanotubes
Additional proportion, realization obtain the conductive filler of preferable thyrsiform；Current traditional handicraft is compared, greatly improves original charcoal
The electric conductivity of black product, improves the competitiveness of product in market.It can realize the seamless incision of existing carbon black Preparation equipment, nothing
It must change, it is at low cost, it is easy to accomplish large-scale production.
In short, the superpower compounded mix that is formed in situ of the present invention, the ratio of components of carbon nanotubes and carbon black can be freely controlled
Example plays conductive and reinforcing effect well, can substitute the superconduction carbon black of import completely；And stabilization simple for process, is convenient for
Operation, without the existing carbon black production device of change and equipment.
Description of the drawings
The carbon nanotubes and the SEM pictures of carbon black beading compounded mix that Fig. 1 is prepared in situ.
The carbon nanotubes and the SEM pictures of carbon black beading compounded mix that Fig. 2 is prepared in situ.
Specific embodiment
Below in conjunction with the content in the embodiment of the present invention, apparent and completion is carried out to technical scheme and is explained
It states.Obviously, described embodiment is only the part of the embodiment of the present invention, and is not whole experiment case studies.It is based on
The embodiment of the present invention.Remaining embodiment that others skilled in the art are obtained, all belong to the scope of protection of the present invention within.
Embodiment 1：
（1）Carbon nanotubes is mixed into the liquid material for preparing carbon black, it is 5-15 μm that carbon nanotubes, which selects powder particle diameter, and weight is
110g；The weight of liquid material is 1000g；
（2）The mixture of carbon nanotubes and liquid material is warming up to 90 DEG C of dehydrations；
（3）Carbon nanotubes and liquid starting material mixture are preheated to 650 DEG C, in atomized spray to reacting furnace；
（4）After progressive solution, at a temperature of 1700 DEG C, the superpower compounded mix of carbon nanotubes and carbon black is prepared in situ；
（5）Quench zone spray cooling divides three-level to 850 DEG C（It is specific to set）Carry out 240 DEG C of cooling；
（6）Separation is collected, 110 DEG C of dryings；
（7）Samples weighing, weight 525g；Sample SEM is Fig. 1
Embodiment 2：
（1）Carbon nanotubes is mixed into the liquid material for preparing carbon black, it is 15-20 μm that carbon nanotubes, which selects powder particle diameter, weight
For 90g；The weight of liquid material is 900g；
（2）The mixture of carbon nanotubes and liquid material is warming up to 85 DEG C of dehydrations；
（3）Carbon nanotubes and liquid starting material mixture are preheated to 640 DEG C, in atomized spray to reacting furnace；
（4）After progressive solution, at a temperature of 1650 DEG C, the superpower compounded mix of carbon nanotubes and carbon black is prepared in situ；
（5）Quench zone spray cooling divides three-level to 840 DEG C（It is specific to set）Carry out 230 DEG C of cooling；
（6）Separation is collected, 120 DEG C of dryings；
（7）Samples weighing, weight 457g；Sample SEM is Fig. 2
1 identical rubber compounding of test example, adds in the rubber compound of different fillers, and performance compares.
In this comparative example, using conventional natural rubber formulations, reinforced filling comparison is respectively：The A present invention is prepared in situ
Carbon nanotubes and carbon black compounded mix（Using the product of embodiment 2）；B does not add the conventional carbon black that carbon nanotubes is handled（Card is rich
Special company N220 carbon blacks）, specific formula is as shown in table 1.
1 natural gum mixing formula of table
Concrete operations are：Two natural rubber rubber compound formulas are plasticated, mixer on a mill by identical equipment and technique
Mixing, mill mixing are parked, the finished composition after bottom sheet are vulcanized 15 on vulcanizing press under 150 DEG C, 10MPa pressure
Minute, you can it obtains and is each kneaded vulcanizate.
The vulcanizate that A and B is obtained carries out quantitative measurement, and obtained test result is as shown in table 2.
2 vulcanizating glue physical performance test result of table
As can be known from Table 2, under identical formulation condition, the objects such as tensile strength, tearing strength, elongation at break of A rubber compounds
Rationality can be significantly improved compared with B rubber compounds；The Mooney viscosity of A rubber compounds has bright compared with B rubber compounds
It is aobvious to reduce；Degree of scatter of the A rubber compounds filler described above in rubber substantially improves；The vulcanization course of A rubber compounds substantially contracts
Short, a large amount of energy consumptions can be saved by improving curing efficiency；A is kneaded tan δ of the vulcanizate under the conditions of 25 DEG C and is obviously reduced, explanation
, with relatively low hysteresis loss, relatively low rolling resistance can be had by making tyre surface with it for it.
Test example 2
It in this comparative example, is formulated using plastics PE, conductive filler comparison is respectively：The carbon nanotubes that the C present invention is prepared in situ
With carbon black compounded mix；D does not add the conventional carbon black that carbon nanotubes is handled（Cabot Co., Ltd's N220 carbon blacks）, E addition imports Czech
The conductive filler of carbon black（The highly conductive carbon black CHEZACARB Type Bs of Czech）, specific formula is as shown in table 3.
3 PE plastic formulas of table
Concrete operations are：C, tri- PE of D and E formulas, under conditions of by identical equipment and technique, material after mixing,
It is added in double screw extruder, controls 180 DEG C -220 DEG C of head temperature, extrusion plastic adhesive tape.
C, the plastics batten that D and E is obtained carries out conducting performance test, and obtained test result is as shown in table 4.
4 performance data of table
As can be known from Table 4, under identical formulation condition, volume resistance, sheet resistance, elongation at break of C plastics battens etc.
Physical property is significantly improved compared with D plastics battens, and especially there are the differences of the nearly 4-5 order of magnitude for resistance
Not；The compounded mix of the present invention has extremely apparent advantage and stability, can be produced completely with import outside surrogate from data
Product E.
In conclusion by means of the above-mentioned technical proposal of the present invention, by the way that the carbon nanotubes quantified is blended into liquid original
Method through being prepared in situ again after material while carbon black feed stock generates carbon black through high temperature, prepares the carbon nanometer being premixed into
Pipe is served as theme, and is the perfect class grape string structure in the form of a beading by the carbon black particle that generates, have it is conductive well and
Reinforcing effect can substitute the superconduction carbon black of import completely.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God and any modification, equivalent substitution, improvement and etc. within principle, done, should all be included in the protection scope of the present invention.
Claims (10)
1. the in-situ preparation method of a kind of carbon nanotubes and the superpower compounded mix of carbon black, carbon nanotubes is blended into and prepares carbon black
Carbon nanotubes and the superpower compounded mix of carbon black are prepared through high-temp in-situ again after liquid material, carbon black is generated through high temperature in carbon black feed stock
While, the carbon nanotubes for preparing to be premixed into is served as theme, the perfect class in the form of the carbon black particle generated is a beading
Grape string structure.
2. the in-situ preparation method of carbon nanotubes according to claim 1 and the superpower compounded mix of carbon black, specific steps are such as
Under：
（1）Carbon nanotubes is mixed into the liquid material for preparing carbon black, the weight ratio of carbon nanotubes and liquid material is received for carbon
Mitron：Liquid material=0.1:100-500:100；
（2）The mixture of carbon nanotubes and liquid material is warming up to 50-110 DEG C of dehydration；
（3）Carbon nanotubes and liquid starting material mixture are preheated to 600-650 DEG C, in atomized spray to reacting furnace；
（4）After progressive solution, at a temperature of 1000 DEG C -2300 DEG C, the superpower of carbon nanotubes and carbon black is prepared in situ and compound fills out
Material；
（5）To 800 DEG C -860 DEG C, point three-level carries out being cooled to 230 DEG C -240 DEG C quench zone spray cooling；
（6）Separation is collected, 70 DEG C of -120 DEG C of dryings.
3. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The weight ratio of carbon nanotubes and liquid material is carbon nanotubes：Liquid material=10:100-50:100.
4. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The liquid material for preparing carbon black is coal tar, one or more kinds of mixtures of pitch, clarified oil, ethylene bottom oil,
Wherein, clarified oil is that Catalytic Cracking Unit of Measure passes through simply dealt catalytic slurry at once, and clarification oil density is big, and hydrogen content is low, saturation
Hydrocarbon and arene content account for 50%-60%.
5. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The carbon nanotubes is single-walled carbon nanotube, one or more kinds of mixtures of double-walled carbon nano-tube, multi-walled carbon nanotube.
6. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The particle size range of the carbon nanotubes is 50nm-500 μm, is preferably 100nm-50 μm, more preferable 1 μm -20 μm.
7. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The mixture of the carbon nanotubes and liquid material heating dehydration temperaturre is 80-90 DEG C.
8. the in-situ preparation method of carbon nanotubes according to claim 2 and the superpower compounded mix of carbon black, which is characterized in that
The step（4）Progressive solution, for three-level heat；Temperature is prepared in situ as 1400-1700 DEG C.
9. the side of being prepared in situ of the carbon nanotubes and the superpower compounded mix of carbon black according to claim 1-8 any claims
The superpower compounded mix of carbon nanotubes and carbon black that method is obtained is had and is served as theme with the carbon nanotubes being premixed into, with what is generated
Carbon black particle is the perfect class grape string structure of beading form.
10. carbon nanotubes and the superpower compounded mix of carbon black according to claim 1-8 any claims are prepared in situ
The superpower compounded mix of carbon nanotubes and carbon black that method is obtained is for the conduction of plastics and rubber, heat conduction, reinforcement.
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| CN109467783A (en) * | 2018-11-08 | 2019-03-15 | 上海应用技术大学 | A kind of polyethylene/carbon nanotube conducting material and preparation method thereof |
| CN109651700A (en) * | 2018-11-28 | 2019-04-19 | 江苏松上科技有限公司 | A kind of permanent conductive plastics particle and preparation method thereof |
| CN110330794A (en) * | 2019-04-08 | 2019-10-15 | 绍兴文理学院元培学院 | A kind of pressure sensitive composite material and preparation method thereof in flexible sensor |
| CN110684375A (en) * | 2019-11-01 | 2020-01-14 | 青岛科技大学 | Pyrolytic carbon black modification method for loading carbon nano tube on surface of pyrolytic carbon black |
| CN110721699A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Gasoline hydrodesulfurization catalyst and preparation method and application thereof |
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| CN110721699A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Gasoline hydrodesulfurization catalyst and preparation method and application thereof |
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| CN110330794A (en) * | 2019-04-08 | 2019-10-15 | 绍兴文理学院元培学院 | A kind of pressure sensitive composite material and preparation method thereof in flexible sensor |
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| CN111795764B (en) * | 2019-04-09 | 2021-11-09 | 绍兴文理学院元培学院 | Sandwich type large-area high-density flexible array sensor and preparation method thereof |
| CN110684375A (en) * | 2019-11-01 | 2020-01-14 | 青岛科技大学 | Pyrolytic carbon black modification method for loading carbon nano tube on surface of pyrolytic carbon black |
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