CN108276790A - A kind of preparation method of the special dipping agent bitumen of Carbon Materials - Google Patents
A kind of preparation method of the special dipping agent bitumen of Carbon Materials Download PDFInfo
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- CN108276790A CN108276790A CN201810264372.3A CN201810264372A CN108276790A CN 108276790 A CN108276790 A CN 108276790A CN 201810264372 A CN201810264372 A CN 201810264372A CN 108276790 A CN108276790 A CN 108276790A
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- carbon materials
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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
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/023—Working-up pitch, asphalt, bitumen by chemical means reaction with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/026—Working-up pitch, asphalt, bitumen by chemical means reaction with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
Abstract
The invention discloses a kind of preparation methods of the special dipping agent bitumen of Carbon Materials, belong to technical field of petrochemical industry.The present invention is first by coal tar pitch solvent extraction impurity removal and purification; refined bitumen is made; electric tank cathode room is added in the electrolytic bath configured again by refined bitumen and voluntarily; constant temperature stirring electrolysis is carried out under argon gas guard mode; catholyte product is made; it after being mixed again with water, is filtered, washed, dries, removal of impurities catholyte product is made；To clean catholyte product and polyacrylamide, phosphatide mixed melting again, and be continually fed into carbon dioxide gas, after cooling, discharge to get the special dipping agent bitumen of Carbon Materials.The special dipping agent bitumen of Carbon Materials prepared by technical solution of the present invention obtains mobility, and the feature that coking ability is high in dipping process with excellent.The special dipping agent bitumen of Carbon Materials prepared by technical solution of the present invention obtains mobility, and the feature that coking ability is high in dipping process with excellent.
Description
Technical field
The invention discloses a kind of preparation methods of the special dipping agent bitumen of Carbon Materials, belong to technical field of petrochemical industry.
Background technology
Dipping agent bitumen is a kind of common density reinforcing agent in Carbon Materials production, is mainly used for high power and ultra high power
The raw materials for production etc. of the impregnation technology and high-tech product of graphite electrode such as aerospace, artificial skelecton and needle coke；In height
In the performance Carbon Materials such as preparation process of C/C composite materials high-density high-strength carbon block, effect is even more irreplaceable.Dipping
The quality of agent quality directly influences the production cost and material property of high-performance carbon material, therefore Carbon Materials manufacturer is very heavy
Depending on the R and D of impregnating agent.Pitch is one of raw material most important, most basic in various Carbon Materials, is generally also used for preparing
Binder and impregnating agent.The characteristics of dipping agent bitumen is quinoline insolubles（QI components）Content is especially low, about 0.1%~
Between 0.5%.Pitch immersion rate is reduced because QI can form impervious filter cake at the pore entrance of carbon product, directly
Influence dipping effect.In addition, also having higher coking carbon residue and lower softening point, this is a pair of property mutually restricted
Matter.In order to solve this problem, it is necessary to processing is modified to dipping agent bitumen, so that dipping agent bitumen has good rheology
Performance is more conducive to the raising of pickling efficiency.
Coal tar pitch abundance at present, using coal tar pitch be raw material prepare dipping agent bitumen can fully, effectively utilize money
Source meets the needs of market is to dipping agent bitumen.But the QI contained by coal tar pitch forms impermeability during Carbon Materials impregnate
Filter cake makes osmotic resistance increase, and reduces dipping effect.Therefore, the impregnation of Carbon Materials should use the impregnating agent of low QI contents
Coal tar pitch.The quality of impregnating agent coal tar pitch performance directly influences the production cost and material property of high-performance carbon material.Tradition
Most of charcoal ink factory substitutes impregnating agent coal tar pitch using mid temperature pitch.Since the QI contents in mid temperature pitch are up to 2% ~ 10%,
QI easily blocks stomata in production process, reduces pitch immersion rate, seriously affects dipping effect, the carbon product matter produced
Amount is poor, and of high cost and service life is shorter.Dipping agent bitumen is larger in market potential, but also can increase year by year, property
The excellent dipping agent bitumen of energy can also not only be exported goods and earned foreign currency with import substitutes, good market prospect.
Therefore, how to improve traditional dipping agent bitumen poor fluidity, coking ability and the bad disadvantage of dipping effect, to obtain
The dipping agent bitumen for taking more high combination property is that it is promoted and applies, meets industrial production demand urgent problem to be solved.
Invention content
The present invention solves the technical problem of：For traditional dipping agent bitumen poor fluidity, coking ability and dipping
Ineffective disadvantage provides a kind of preparation method of the special dipping agent bitumen of Carbon Materials.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It counts in parts by weight, takes 40~50 parts of acetonitriles successively, 70~80 parts of absolute ethyl alcohols, 4~8 parts of tetrabutylammonium bromide, 8
~10 parts of saltcake, 8~10 parts of boron oxides, 2~4 parts of magnesium hydroxides, 3~5 parts of aluminium hydroxides, 4~6 parts of calcium bicarbonates, 0.6~
0.8 part of emulsifier, is stirred, obtains electrolytic bath；
（2）It is 1 in mass ratio by refined bitumen and electrolytic bath：20~1：The cathode chamber of 30 addition separated type electrolytic tanks, and to
The electrolytic bath of 3~5 times of refined bitumen quality is added in anode chamber, under argon gas guard mode, constant temperature stirring electrolysis obtains cathode
Electrolysate；
（3）It is 1 in mass ratio by catholyte product and water：10~1：It after 20 are stirred, filters, washing, vacuum refrigeration is dry
Dry, must clean catholyte product；
（4）It counts in parts by weight, takes 80~100 parts of removal of impurities catholyte products, 3~5 parts of polyacrylamides, 4~6 parts of phosphorus successively
Fat heats melting, obtains fusant, and be continually fed into carbon dioxide gas into fusant after mixing, discharge, then through natural cooling
To room temperature, the special dipping agent bitumen of Carbon Materials is obtained.
Step（1）The emulsifier preparation process is：It counts in parts by weight, takes 70~80 parts successively（N- amidino groups）Dodecane
Base acrylamide, 30~35 parts of polyethylene glycol phosphates, 3~4 parts of ferrocene, 6~8 parts of paracide, constant temperature is stirred to react 3~
5h obtains emulsifier.
Step（2）The refined bitumen preparation process is：Coal tar pitch complex solvent is extracted 4~8 times, then through distilling back
Solvent is received, refined bitumen is obtained；The complex solvent is compounded by the raw material of following parts by weight：10~30 parts of kerosene, 8~
10 parts of toluene, 10~20 parts of quinoline.
Step（2）The constant temperature stirs electrolytic condition：Electrolysis temperature is 55~60 DEG C, and decomposition voltage is 20~30V, is stirred
Mix rotating speed is 300~500r/min.
Step（4）The polyacrylamide is the anionic polyacrylamide that molecular weight is 600~20,000,000.
Step（4）The phosphatide is any one in egg yolk lecithin, soybean lecithin or milk lecithin.
The beneficial effects of the invention are as follows：
（1）The present invention is handled refined bitumen by using electrolysis process, and in electrolytic process, the crystallization water changes in saltcake
At free water, and using this free water as hydrogen supply agent, in electrolytic process, realization adds hydrogen to refined bitumen, makes asphaltene molecule structure
By partial destruction, aromatic moiety is opened, and so that the reduction of pitch armaticity, fatty is increased, macromolecular structure Partial digestion is
Small molecule, the degree of polymerization reduce, to make refined bitumen softening point decline, to enable product mobility in dipping process to have
Effect improves；Furthermore after saltcake dehydration, sodium sulfate crystal is gradually precipitated in system, in follow-up water-washing process, sodium sulphate is dissolved in
Water is removed, and abundant diffusion admittance is left inside system, this diffusion admittance can also effectively will be closed inside system
Bubble is got through, to be conducive to other active ingredients diffusion profile inside asphalt system；
（2）The present invention is by adding boron oxide, magnesium hydroxide, aluminium hydroxide and calcium bicarbonate, in preparation process, carbonic acid first
Hydrogen calcium can decompose at a temperature of relative reduction, generate water, carbon dioxide and calcium carbonate, water and can be used as in electrolytic process
Hydrogen supply agent, and the generation of carbon dioxide gas, advantageously reduce viscosity of the system in preparation process, prepared by raising system
Mobility in journey improves reaction efficiency, and magnesium hydroxide and hydrogen to be conducive to improve reactant molecule effective collision probability
Aluminium oxide can be gradually dehydrated during following process, generate corresponding metal oxide, and be used as and fill out with calcium carbonate and boron oxide
Agent is filled, the porosity of Carbon Materials in dipping process is reduced, improves the coking value of pitch, secondly, calcium carbonate, boron oxide, magnesia
It is smooth with Membranes On Alumina Particles Surface, in addition system after, can play lubricating action, reduce the binding force between asphaltene molecule, to
Its softening point is reduced, in addition, the addition of boron oxide, can be such that magnesia and aluminium oxide melts in high temperature dipping process, from
And mobility of the product in dipping process is effectively improved, in addition, partial oxidation aluminium can be used as catalyst and be present in inside system,
The coking reaction of catalytic asphalt occurs, and to improve the coking ability of product, and part inorganic, metal oxide can be with calcium carbonate
It is sintered under the high temperature conditions, and inorganic skeleton is formed in Carbon Materials pore interior, realize reinforcing and filling to Carbon Materials,
It is that Carbon Materials mechanical property further increases, porosity effectively reduces；
（3）The present invention makes emulsifier by oneself by addition, which can form small imitated vesicle structure inside system, and
With carbon dioxide reversible action can occur for the amidine group in the imitated vesicle structure, to realize the expansion to vesicle system and shrink
Journey with the addition of carbon dioxide, can be such that vesicle system expands, in use, in hot conditions in preparation process
Under, carbon dioxide release, to form the motive force needed for diffusion in system, in addition, after carbon dioxide release, vesica volume
It shrinks, to form negative relative state inside Carbon Materials, is conducive to impregnating agent and further penetrates into inside Carbon Materials, make
Carbon Materials porosity is effectively reduced.
Specific implementation mode
It counts in parts by weight, takes 70~80 parts successively（N- amidino groups）Dodecylacrylamide, 30~35 parts of polyethylene glycol
Phosphate, 3~4 parts of ferrocene, 6~8 parts of paracide are added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 45~50 DEG C in temperature, under the conditions of rotating speed is 300~500r/min, constant temperature is stirred to react 3~5h, and discharging is naturally cold
But to room temperature, emulsifier is obtained；It counts in parts by weight, 10~30 parts of kerosene, 8~10 parts of toluene, 10~20 parts of quinoline is taken to stir successively
20~50min of mixing is mixed, obtains complex solvent, then by after pitch powder use gained complex solvent extraction 4~8 times, be distilled to recover molten
Agent obtains refined bitumen；It counts in parts by weight, takes 40~50 parts of acetonitriles, 70~80 parts of absolute ethyl alcohols, 4~8 parts of tetrabutyl bromines successively
Change ammonium, 8~10 parts of saltcake, 8~10 parts of boron oxides, 2~4 parts of magnesium hydroxides, 3~5 parts of aluminium hydroxides, 4~6 parts of calcium bicarbonates,
0.6~0.8 part of emulsifier, is poured into batch mixer, under the conditions of rotating speed is 1200~1800r/min, is stirred 2~4h, is gone out
Material, obtains electrolytic bath；It is then 1 in mass ratio by refined bitumen and electrolytic bath：20~1：30 are added separated type electrolytic tank
Cathode chamber, and to the electrolytic bath of 3~5 times of refined bitumen quality used in separated type electrolytic tank anode chamber addition cathode chamber, then with
80~150mL/min rates are passed through argon gas into separated type electrolytic tank, under argon gas guard mode, in temperature be 55~60 DEG C,
Decomposition voltage is 20~30V, under the conditions of speed of agitator is 300~500r/min, constant temperature stirring electrolysis 12~for 24 hours, discharging obtains cloudy
Pole electrolysate；It is 1 in mass ratio by catholyte product and deionized water：10~1：20 pour into three-necked flask, with stirring
After device is stirred 45~60min with 600~800r/min rotating speeds, filtering obtains filter residue, and filter residue 3~5 is washed with deionized
It is secondary, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 2~3h, discharging, must clean catholyte product；By weight
Number meter is measured, takes 80~100 parts of removal of impurities catholyte products successively, 3~5 parts of polyacrylamides, 4~6 parts of phosphatide, mixing pours into
In reaction kettle, be heated to material melts in reaction kettle, obtain fusant, and into the reaction kettle for fill fusant with 100~
150mL/min rates are passed through carbon dioxide gas, after being continually fed into 45~60min, stop heating and are passed through carbon dioxide gas,
It discharges while hot, after naturally cool to room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide is that molecular weight is
600~20,000,000 anionic polyacrylamide.The phosphatide is in egg yolk lecithin, soybean lecithin or milk lecithin
Any one.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 6 parts of carbon
Sour hydrogen calcium, 0.8 part of emulsifier, is poured into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, is discharged, obtain electric
Solve slurries；It is then 1 in mass ratio by refined bitumen and electrolytic bath：30 be added separated type electrolytic tanks cathode chamber, and to every
From formula electrolyzer anode chamber be added cathode chamber used in 5 times of refined bitumen quality electrolytic bath, then with 150mL/min rates to every
It it is 60 DEG C, decomposition voltage 30V in temperature, speed of agitator is under argon gas guard mode from argon gas is passed through in formula electrolytic cell
Under the conditions of 500r/min, for 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；Catholyte product and deionized water are pressed
Mass ratio is 1：20 pour into three-necked flask, and after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue,
And filter residue is washed with deionized 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging must clean
Catholyte product；Count in parts by weight, take successively 100 parts removal of impurities catholyte products, 5 parts of polyacrylamides, 6 parts of phosphatide,
Mixing is poured into reaction kettle, and material melts in reaction kettle are heated to, and obtains fusant, and into the reaction kettle for fill fusant with
150mL/min rates are passed through carbon dioxide gas, after being continually fed into 60min, stop heating and are passed through carbon dioxide gas, while hot
Discharging, after naturally cool to room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide be molecular weight be 800~
15000000 anionic polyacrylamide.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 6 parts of calcium bicarbonates, 0.8
Part emulsifier, is poured into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, is discharged, obtain electrolytic bath；Then
It is 1 in mass ratio by refined bitumen and electrolytic bath：30 are added the cathode chamber of separated type electrolytic tank, and positive to separated type electrolytic tank
The electrolytic bath of 5 times of refined bitumen quality used in cathode chamber is added in pole room, then with 150mL/min rates into separated type electrolytic tank
It is passed through argon gas, is 60 DEG C, decomposition voltage 30V in temperature, speed of agitator is 500r/min conditions under argon gas guard mode
Under, for 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；It is 1 in mass ratio by catholyte product and deionized water：20
It pours into three-necked flask, after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue, deionized water is used in combination
It washs filter residue 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging, the catholyte that must clean production
Object；It counts in parts by weight, takes 100 parts of removal of impurities catholyte products successively, 5 parts of polyacrylamides, 6 parts of phosphatide, mixing is poured into anti-
It answers in kettle, is heated to material melts in reaction kettle, obtain fusant, and into the reaction kettle for fill fusant with 150mL/min speed
Rate is passed through carbon dioxide gas, after being continually fed into 60min, stops heating and is passed through carbon dioxide gas, discharge while hot, wait for nature
It is cooled to room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide be molecular weight be 800~15,000,000 it is cloudy from
Sub- polyacrylamide.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 6 parts of calcium bicarbonates, 0.8 part
Emulsifier pours into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, discharges, obtain electrolytic bath；Then will
Refined bitumen and electrolytic bath are 1 in mass ratio：30 are added the cathode chamber of separated type electrolytic tanks, and to separated type electrolytic tank anode
The electrolytic bath of 5 times of refined bitumen quality used in cathode chamber is added in room, then is led into separated type electrolytic tank with 150mL/min rates
Enter argon gas, under argon gas guard mode, in temperature be 60 DEG C, decomposition voltage 30V, speed of agitator be 500r/min under the conditions of,
For 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；It is 1 in mass ratio by catholyte product and deionized water：20 fall
Enter in three-necked flask, after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue, and be washed with deionized water
It washs filter residue 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging, must clean catholyte product；
It counts in parts by weight, 100 parts of removal of impurities catholyte products, 5 parts of polyacrylamides, 6 parts of phosphatide is taken to mix and pour into reaction kettle successively
In, material melts in reaction kettle are heated to, obtain fusant, and logical with 150mL/min rates into the reaction kettle for fill fusant
Enter carbon dioxide gas, after being continually fed into 60min, stops heating and be passed through carbon dioxide gas, discharge while hot, wait for natural cooling
To room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide is that the anion that molecular weight is 800~15,000,000 is poly-
Acrylamide.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 6 parts of calcium bicarbonates, 0.8 part of emulsifier pour into mixed
In material machine, under the conditions of rotating speed is 1800r/min, it is stirred 4h, discharges, obtains electrolytic bath；Then by refined bitumen and electricity
It is 1 to solve slurries in mass ratio：30 are added the cathode chamber of separated type electrolytic tank, and cathode chamber is added to separated type electrolytic tank anode chamber
The electrolytic bath of 5 times of refined bitumen quality used, then argon gas is passed through into separated type electrolytic tank with 150mL/min rates, in argon
It it is 60 DEG C, decomposition voltage 30V in temperature, under the conditions of speed of agitator is 500r/min, constant temperature stirring is electrolysed under gas shielded state
For 24 hours, it discharges, obtains catholyte product；It is 1 in mass ratio by catholyte product and deionized water：20 pour into three-necked flask,
After being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue, and filter residue is washed with deionized 5 times, then
Filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging, must clean catholyte product；It counts in parts by weight,
100 parts of removal of impurities catholyte products, 5 parts of polyacrylamides, 6 parts of phosphatide are taken to mix and pour into reaction kettle, be heated to reacting successively
Material melts in kettle obtain fusant, and are passed through carbon dioxide gas into the reaction kettle for fill fusant with 150mL/min rates
Body, after being continually fed into 60min, stop heating and be passed through carbon dioxide gas, discharge while hot, after naturally cool to room temperature to get
The special dipping agent bitumen of Carbon Materials.The polyacrylamide is the anionic polyacrylamide that molecular weight is 800~15,000,000.Institute
It is egg yolk lecithin to state phosphatide.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 0.8 part
Emulsifier pours into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, discharges, obtain electrolytic bath；Then will
Refined bitumen and electrolytic bath are 1 in mass ratio：30 are added the cathode chamber of separated type electrolytic tanks, and to separated type electrolytic tank anode
The electrolytic bath of 5 times of refined bitumen quality used in cathode chamber is added in room, then is led into separated type electrolytic tank with 150mL/min rates
Enter argon gas, under argon gas guard mode, in temperature be 60 DEG C, decomposition voltage 30V, speed of agitator be 500r/min under the conditions of,
For 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；It is 1 in mass ratio by catholyte product and deionized water：20 fall
Enter in three-necked flask, after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue, and be washed with deionized water
It washs filter residue 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging, must clean catholyte product；
It counts in parts by weight, 100 parts of removal of impurities catholyte products, 5 parts of polyacrylamides, 6 parts of phosphatide is taken to mix and pour into reaction kettle successively
In, material melts in reaction kettle are heated to, obtain fusant, and logical with 150mL/min rates into the reaction kettle for fill fusant
Enter carbon dioxide gas, after being continually fed into 60min, stops heating and be passed through carbon dioxide gas, discharge while hot, wait for natural cooling
To room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide is that the anion that molecular weight is 800~15,000,000 is poly-
Acrylamide.The phosphatide is egg yolk lecithin.
It counts in parts by weight, 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline is taken to be stirred 50min, must compound molten successively
Agent, then by after pitch powder use gained complex solvent extraction 8 times, be distilled to recover solvent, obtain refined bitumen；It counts in parts by weight,
Take 50 parts of acetonitriles successively, 80 parts of absolute ethyl alcohols, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5
Part aluminium hydroxide, 6 parts of calcium bicarbonates pour into batch mixer, under the conditions of rotating speed is 1800r/min, are stirred 4h, discharge,
Obtain electrolytic bath；It is then 1 in mass ratio by refined bitumen and electrolytic bath：30 are added the cathode chamber of separated type electrolytic tank, and
The electrolytic bath of 5 times of refined bitumen quality used in cathode chamber is added to separated type electrolytic tank anode chamber, then with 150mL/min rates
Argon gas is passed through into separated type electrolytic tank, under argon gas guard mode, in temperature be 60 DEG C, decomposition voltage 30V, speed of agitator
Under the conditions of 500r/min, for 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；By catholyte product and deionized water
It is 1 in mass ratio：20 pour into three-necked flask, and after being stirred 60min with blender with 800r/min rotating speeds, filtering must filter
Slag, and filter residue is washed with deionized 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging obtains
Clean catholyte product；It counts in parts by weight, takes 100 parts of removal of impurities catholyte products, 5 parts of polyacrylamides, 6 parts of phosphorus successively
Fat, mixing pour into reaction kettle, are heated to material melts in reaction kettle, obtain fusant, and into the reaction kettle for filling fusant
It is passed through carbon dioxide gas with 150mL/min rates, after being continually fed into 60min, stops heating and is passed through carbon dioxide gas, take advantage of
Heat discharging, after naturally cool to room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide is that molecular weight is 800
~1,500 ten thousand anionic polyacrylamide.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 100 parts of refined drips successively
Blueness, 5 parts of polyacrylamides, 6 parts of phosphatide, mixing pour into reaction kettle, are heated to material melts in reaction kettle, obtain fusant, and
Carbon dioxide gas is passed through with 150mL/min rates into the reaction kettle for fill fusant, after being continually fed into 60min, stops adding
Heat and be passed through carbon dioxide gas, discharge while hot, after naturally cool to room temperature to get the special dipping agent bitumen of Carbon Materials.It is described
Polyacrylamide is the anionic polyacrylamide that molecular weight is 800~15,000,000.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 6 parts of carbon
Sour hydrogen calcium, 0.8 part of emulsifier, is poured into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, is discharged, obtain electric
Solve slurries；It is then 1 in mass ratio by refined bitumen and electrolytic bath：30 be added separated type electrolytic tanks cathode chamber, and to every
From formula electrolyzer anode chamber be added cathode chamber used in 5 times of refined bitumen quality electrolytic bath, then with 150mL/min rates to every
It it is 60 DEG C, decomposition voltage 30V in temperature, speed of agitator is under argon gas guard mode from argon gas is passed through in formula electrolytic cell
Under the conditions of 500r/min, for 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；Catholyte product and deionized water are pressed
Mass ratio is 1：20 pour into three-necked flask, and after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue,
And filter residue is washed with deionized 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging must clean
Catholyte product；It counts in parts by weight, 100 parts of removal of impurities catholyte products, 6 parts of phosphatide, mixing is taken to pour into reaction kettle successively
In, material melts in reaction kettle are heated to, obtain fusant, and logical with 150mL/min rates into the reaction kettle for fill fusant
Enter carbon dioxide gas, after being continually fed into 60min, stops heating and be passed through carbon dioxide gas, discharge while hot, wait for natural cooling
To room temperature to get the special dipping agent bitumen of Carbon Materials.The phosphatide is egg yolk lecithin.
It counts in parts by weight, takes 80 parts successively（N- amidino groups）Dodecylacrylamide, 35 parts of polyethylene glycol phosphates, 4
Part ferrocene, 8 parts of paracide are added in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 50
DEG C, under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 5h, and discharging, cooled to room temperature obtains emulsifier；By weight
Number meter, takes 30 parts of kerosene, 10 parts of toluene, 20 parts of quinoline to be stirred 50min, obtains complex solvent, then pitch powder is used successively
After gained complex solvent extracts 8 times, it is distilled to recover solvent, obtains refined bitumen；It counts in parts by weight, takes 50 parts of acetonitriles successively, 80
Part absolute ethyl alcohol, 8 parts of tetrabutylammonium bromide, 10 parts of saltcake, 10 parts of boron oxides, 4 parts of magnesium hydroxides, 5 parts of aluminium hydroxides, 6 parts of carbon
Sour hydrogen calcium, 0.8 part of emulsifier, is poured into batch mixer, under the conditions of rotating speed is 1800r/min, is stirred 4h, is discharged, obtain electric
Solve slurries；It is then 1 in mass ratio by refined bitumen and electrolytic bath：30 be added separated type electrolytic tanks cathode chamber, and to every
From formula electrolyzer anode chamber be added cathode chamber used in 5 times of refined bitumen quality electrolytic bath, then with 150mL/min rates to every
It it is 60 DEG C, decomposition voltage 30V in temperature, speed of agitator is under argon gas guard mode from argon gas is passed through in formula electrolytic cell
Under the conditions of 500r/min, for 24 hours, discharging obtains catholyte product for constant temperature stirring electrolysis；Catholyte product and deionized water are pressed
Mass ratio is 1：20 pour into three-necked flask, and after being stirred 60min with blender with 800r/min rotating speeds, filtering obtains filter residue,
And filter residue is washed with deionized 5 times, then the filter residue after washing is transferred to vacuum freezing drying oven, dry 3h, discharging must clean
Catholyte product；It counts in parts by weight, 100 parts of removal of impurities catholyte products, 5 parts of polyacrylamides, mixing is taken to pour into successively
In reaction kettle, material melts in reaction kettle are heated to, obtain fusant, and into the reaction kettle for fill fusant with 150mL/min
Rate is passed through carbon dioxide gas, after being continually fed into 60min, stops heating and is passed through carbon dioxide gas, discharge while hot, wait for certainly
So it is cooled to room temperature to get the special dipping agent bitumen of Carbon Materials.The polyacrylamide is the moon that molecular weight is 800~15,000,000
Cationic polyacrylamide.
Comparative example：The dipping agent bitumen of Jining Co., Ltd production.
The special dipping agent bitumen of Carbon Materials of 1 to 9 gained of example and comparative example product are subjected to performance detection, it is specific to detect
Method is as follows：
1. mobility：After measuring test specimen softening point temperature using ring and ball method, with reference to formula（1）（The formula be softening point to softening point with
Existing relationship between viscosity and temperature within the scope of upper 150 DEG C）Calculate viscosity；
lgηt=-4.175+711.8/（（86.1-ts）+t）（1）
In formula：ηtFor test specimen again temperature t when viscosity, Pas；tsFor test specimen softening point；
2. coking ability：Test specimen coking value is measured according to GB8727.
Specific testing result is as shown in table 1：
Table 1
| Detection project | Viscosity/Pas | Coking value/% |
| Example 1 | 0.098 | 63.1 |
| Example 2 | 0.273 | 59.2 |
| Example 3 | 0.467 | 58.7 |
| Example 4 | 0.584 | 58.3 |
| Example 5 | 0.982 | 57.6 |
| Example 6 | 1.141 | 56.9 |
| Example 7 | 1.032 | 57.2 |
| Example 8 | 1.365 | 55.3 |
| Example 9 | 1.433 | 53.8 |
| Comparative example | 2.035 | 48.3 |
By 1 testing result of table it is found that the special dipping agent bitumen of Carbon Materials prepared by technical solution of the present invention has in dipping process
There are excellent mobility, and the feature that coking ability is high, has broad prospects in the development of asphalt industry.
Claims (6)
1. a kind of preparation method of the special dipping agent bitumen of Carbon Materials, it is characterised in that specifically preparation process is：
（1）It counts in parts by weight, takes 40~50 parts of acetonitriles successively, 70~80 parts of absolute ethyl alcohols, 4~8 parts of tetrabutylammonium bromide, 8
~10 parts of saltcake, 8~10 parts of boron oxides, 2~4 parts of magnesium hydroxides, 3~5 parts of aluminium hydroxides, 4~6 parts of calcium bicarbonates, 0.6~
0.8 part of emulsifier, is stirred, obtains electrolytic bath；
（2）It is 1 in mass ratio by refined bitumen and electrolytic bath：20~1：The cathode chamber of 30 addition separated type electrolytic tanks, and to
The electrolytic bath of 3~5 times of refined bitumen quality is added in anode chamber, under argon gas guard mode, constant temperature stirring electrolysis obtains cathode
Electrolysate；
（3）It is 1 in mass ratio by catholyte product and water：10~1：It after 20 are stirred, filters, washing, vacuum refrigeration is dry
Dry, must clean catholyte product；
（4）It counts in parts by weight, takes 80~100 parts of removal of impurities catholyte products, 3~5 parts of polyacrylamides, 4~6 parts of phosphorus successively
Fat heats melting, obtains fusant, and be continually fed into carbon dioxide gas into fusant after mixing, discharge, then through natural cooling
To room temperature, the special dipping agent bitumen of Carbon Materials is obtained.
2. a kind of preparation method of the special dipping agent bitumen of Carbon Materials according to claim 1, it is characterised in that：Step
（1）The emulsifier preparation process is：It counts in parts by weight, takes 70~80 parts successively（N- amidino groups）Dodecylacrylamide,
30~35 parts of polyethylene glycol phosphates, 3~4 parts of ferrocene, 6~8 parts of paracide, constant temperature are stirred to react 3~5h, must emulsify
Agent.
3. a kind of preparation method of the special dipping agent bitumen of Carbon Materials according to claim 1, it is characterised in that：Step
（2）The refined bitumen preparation process is：Coal tar pitch complex solvent is extracted 4~8 times, then through being distilled to recover solvent, is obtained smart
Pitch processed；The complex solvent is compounded by the raw material of following parts by weight：10~30 parts of kerosene, 8~10 parts of toluene, 10
~20 parts of quinoline.
4. a kind of preparation method of the special dipping agent bitumen of Carbon Materials according to claim 1, it is characterised in that：Step
（2）The constant temperature stirs electrolytic condition：Electrolysis temperature is 55~60 DEG C, and decomposition voltage is 20~30V, speed of agitator 300
~500r/min.
5. a kind of preparation method of the special dipping agent bitumen of Carbon Materials according to claim 1, it is characterised in that：Step
（4）The polyacrylamide is the anionic polyacrylamide that molecular weight is 600~20,000,000.
6. a kind of preparation method of the special dipping agent bitumen of Carbon Materials according to claim 1, it is characterised in that：Step
（4）The phosphatide is any one in egg yolk lecithin, soybean lecithin or milk lecithin.
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Application publication date: 20180713 |