CN109294285A - A kind of conduction method of producing black pigment - Google Patents
A kind of conduction method of producing black pigment Download PDFInfo
- Publication number
- CN109294285A CN109294285A CN201811435332.7A CN201811435332A CN109294285A CN 109294285 A CN109294285 A CN 109294285A CN 201811435332 A CN201811435332 A CN 201811435332A CN 109294285 A CN109294285 A CN 109294285A
- Authority
- CN
- China
- Prior art keywords
- oil
- extraction
- water
- acid
- refined filtration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/50—Furnace black ; Preparation thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of conductive method of producing black pigment, using fuel gas with low heat value as fuel, obtain the environment of temperature and hypoxemia needed for cracking；By coal liquefaction residue after organic solvent extracts, obtain extract liquor and extract remainder, after the carbon black raw oil is preheating to 160 DEG C -300 DEG C, spray into reacting furnace at a high speed after being atomized, the feedstock oil of atomization is sufficiently mixed under the shear action of low-oxygen high-temperature combustion gas stream occurs efficient cracking reaction, the invention uses carbolineum to produce carbon black as raw material, improves carbon black yield and the quality of production.
Description
Technical field
The present invention relates to the technical fields of coal-burning chemical production.
Specifically, being to be related to a kind of low-oxygen environment using carbolineum as the production method of raw material production carbon black.
Background technique
Carbon black is to make raw material with hydrocarbon through a kind of carbon material obtained by Pintsch process.Kind of carbon black presses carbon black mass
Kind is divided with effect, there is hard (carbon) black, soft carbon, colour carbon black, special carbon black etc. kind, the carbon black of different cultivars
It needs to manufacture using variety classes, the raw material of different quality and different process.Now, the production of carbon black in China is mainly adopted
With Audit For Process, that is, use liquid aromatic hydrocarbon oil as the primary raw material of production carbon black, (also referred to as carbon black is former for suitable liquid aromatic hydrocarbon oil at present
Material oil) there are mainly three types of: catalytic cracked oil pulp, ethylene bottom oil and coal tar system.Coal tar is the ointment obtained when coal coking
Shape substance, coal tar system include: coal tar (mainly density be greater than 1000kg/m3 high temperature coal-tar), carbolineum (or de- crystalline substance again
Carbolineum) and carbon black oil.Carbon black oil is to be composed of carbolineum or de- brilliant carbolineum with coal tar pitch allotment, it can be considered that carbon black is former
Material is distinguished from the appearance, the carbon black raw oil including liquid and the solid asphalt for deploying carbon black raw oil.Carbon black oil is because of it
Cost performance is high, it has also become the primary raw material of Audit For Process production of carbon black.
Production of carbon black in addition to requiring feedstock oil to have the suitable index of correlation (or aromaticity) and density, also require its viscosity,
The index values such as asphalitine, free carbon, moisture content, ash, sulfur content, alkali metal content are as small as possible, and more lower better, carbon black enterprise
Consider from economic and practical angle, the carbon black raw oil of different quality is generally selected according to different kind of carbon black.Carbon black enterprise exists
When producing super-normal structure black, it is desirable that K+ content is less than 2PPm in feedstock oil, and Na+ content is less than 20PPm.Potassium ion is to carbon black structure
Influence be 10 times of sodium ion.
Coal is that archaeophyte is imbedded in underground and experienced complicated biochemistry and physicochemical change and gradually forms
Solid combustible mineral are a kind of solid combustible Organic carbons.Whatsoever coal, wherein all contain Determination of multiple metal elements, as sodium,
Potassium, calcium, magnesium, iron, vanadium etc., and these metallic elements existence form multiplicity in coal, have inorganic mineral shape metal, there is also phases
When the metallo-organic compound of quantity, coal district is different, and often its composition is also different, and single separation method can not be by these
Metal impurities are all kept completely separate with carbon and hydrocarbon.As coal rank changes, the metallo-organic compound content in coal
Change it is different, if metallic sodium organic compound in coal content with coal price change and be basically unchanged, metallic potassium organic compound exists
Content is reduced with coal price and is increased in coal.Metallo-organic compound has the spy for being insoluble in water and being soluble in organic solvent in coal
Point.
Ash is a quality index of coal and its deep processed product, and ash is divided into inherent ash and external ash again.
External ash be mainly dissolved in water metal salt and/or not soluble in water and density be greater than coal solid mineral substance, external ash can
To be removed by physical methods such as washing, sedimentation, filterings.The main ingredient of inherent ash is metal oxide and inorganic
Salt, metal oxide therein mainly have two part sources, and some after metallo-organic compound completely burned by forming, separately
Outer is formed by the inherent inorganic salts thermal decomposition in part.Therefore, inherent ash and organic compound form under certain condition
Tenor there are positive correlation, so as to characterize the tenor of organic compound form indirectly with inherent ash
Just.
DCL/Direct coal liquefaction is that coal is broken for 100~200 mesh particles and under the action of catalyst, passes through high temperature, high pressure
Add hydrogen and is directly translated into a kind of coalification technology of light liquid fuel.Coal is separated by solid-liquid separation during direct liquefaction through decompression
It can a kind of residue (also known as coal directly-liquefied residue or liquid for having temperature flowing of by-product while obtaining light liquid fuel
Change residue).Coal liquefaction residue is mainly made of inanimate matter and organic matter two parts, organic matter therein include: heavy coal liquids,
Bitumen and unconverted coal, inorganic matter include metal, nonmetallic mineral and additional catalyst in coal.Liquefaction
Heavy coal liquids and bitumen content account for about 50% of mass of residue or so, unconverted coal and account for about 30%, ash in residue
Account for about 20%.The mixture of heavy coal liquids and bitumen composition is solid under room temperature, shows drip because softening point is higher
Green character.DCL/Direct coal liquefaction considers from its economy, general to select low-middle metamorphic coal as feed coal, therefore inevitable in liquefaction coal
There are a large amount of metallo-organic compound, enters together with unconverted coal and constitute heavy coal liquids and pitch class object in liquefied residue
The component of matter.Liquefied residue generally accounts for about 30% or so of coal input quantity, rationally utilizes this part by-product, helps to improve liquefaction
The economic benefit of factory.
How coal liquefaction residue is rationally and efficiently used, is always an important topic in coal liquefaction field, now to coal liquid
The Land use systems for changing residue mainly have burning, coking liquefaction, gasification hydrogen-producing, solvent extraction back end hydrogenation and prepare carbon raw etc..
It directly burns in furnace using liquefied residue as fuel, is a kind of simplest using method, but cause the wasting of resources.Coking
Liquefaction be by residue can not distilled oil be partially converted to retortable oil, can must so remove heavy coal liquids and bitumen
In part metal and nonmetallic substance, but because of high temperature action, the heavy coal liquids and bitumen for having quite part turn
Coke is turned to, to reduce the utilization rate of heavy coal liquids and bitumen.By coal liquefaction residue gasification hydrogen-producing, result
It is suitable with burning, also heavy coal liquids and bitumen can be made by low value-added utilization.It is extracted and is liquefied by organic solvent
Residue, after heavy coal liquids and bitumen are more fully extracted, or as the circulation solvent of DCL/Direct coal liquefaction
Or as hydrogenating materials or as carbon raw, but all can be because of metallo-organic compound and oil-soluble inorganic salts by organic solvent
Extraction birth together enters in these products and increases the tenor and ash of product, so that circulation solvent viscosity increases
Greatly, by catalysis oxidation etc., these problems all reduce organic solvent extract for hydrogenation catalyst metal inactivation, carbon materials
Value, and because extract (heavy coal liquids and bitumen) has very high alkali metal content, it is straight to cannot achieve coal
Connect scale application of the liquefied residue on carbon black industry raw material.Furthermore organic solvent extracts coal directly-liquefied residue, finally all
It needs to be separated by solid-liquid separation to remove the solvent insolubles in liquefied residue mixture, is suitable for organic solvent extraction process separation of solid and liquid
Basic skills include: settling methods, centrifugal process, vortex method and filtration method etc..Settling methods are using between solid-liquid
Density contrast reaches solid-liquid separation effect, and must to be so greater than liquid organic molten for the density of organic solvent insoluble matter in liquefied residue
Agent extracts that mixture, but density difference very little, and the system viscosity of heavy hydrocarbon organic solvent extraction mixture be big, insoluble composition granule
Size is small (differing from less than 1 micron to tens microns), according to Stokes' law, to realize the application of settling methods, needs
Want the harsh conditions of high temperature, high pressure.Centrifugal process and cyclonic separation method impose centrifugal force also with density contrast between solid-liquid to reach
Solid-liquid separation effect is arrived, but the solid material solid content that the method is isolated is low, also needs to be aided with filtration method separation, and aforementioned three kinds
Separation method is generally used biggish solvent mass of residue ratio to reduce system viscosity, thus organic solvent usage amount it is big,
Cost recovery is high.Filtration method is to reach solid-liquid separation effect using material particular diameter size difference, and filter device need to only select one
The filter material of set aperture size can reach separating effect, and filtration method requires relatively the solid phase or liquid concentration of raw material
It is low, so be widely adopted.But filtration method has a problem that, is exactly in the identical situation of other conditions, consolidating for filter residue contains
Amount reduces with the increase of solidliquid mixture system viscosity.The solidliquid mixture filtering gained filter of liquefied residue organic solvent extraction
Slag solid content is generally 60%~80%.The organic solvent in filter residue can must be so recycled using filtration method, but excessive in filter residue
The presence of residual heavy liquefaction oil and bitumen can reduce solvent residue recovery rate, i.e. influence solvent extraction economy,
It also easily causes when recycling the organic solvent in filter residue, causes the adverse consequences such as material agglomeration, bonding apparatus in equipment, less serious case's drop
The low organic solvent rate of recovery, severe one can not operate normally filter residue solvent reclaimer, production system of paralysing.Therefore solvent is used
Extract liquefied residue, it is necessary to ensure that high heavy coal liquids, bitumen recovery rate.But it is primary to the level-one of liquefied residue
Property organic solvent extraction filtering, can not accomplish to obtain heavy coal liquids, bitumen in the case of low solvent mass of residue ratio
High extraction.
Petrochemical industry is to remove organic metal salt in crude oil and inorganic metal salt and use and add de- gold into crude oil
Belong to the technique that agent fills the water simultaneously and cooperates electrical desalting and dewatering device removing metal impurities, which has high production efficiency, production capacity
Greatly, the low advantage of oily water content after taking off.But crude oil and coal directly-liquefied residue and and heavy coal liquids and drip in liquefied residue
Green substance nature difference is big, the metal species and every kind of metal in the two wherein content and each metal in organic matter
It is other that existing forms also have day to push up, and influence of the various metals to following process (or product) is also different, the direction of desalination, purpose
It is also completely different with target level of product quality, have no the desalination demetalization treatment process of crude oil for handling the direct liquid of coal so far
Change the relevant report of residue and its extract.
The desalination process for demetalizating of coalification product is mainly applied in coal tar pretreatment.It is existing that coal tar is taken off
Salt process for demetalizating includes: filtering, standing, centrifugation, distillation plus hydrogen, electro-desalting etc..Filtration method processing coal tar can only remove coal
Solid mechanical impurity in tar is invalid to deliquescent metal salt.The effect and filtering of settled process and centrifugal process processing coal tar
Method is identical, there is a problem of same.Way of distillation processing coal tar can must so achieve the purpose that partial removal metal, but this is to damage
Losing the organic components such as 50% or more pitch is cost.Hydrogenation method processing coal tar can also reach the mesh of removing metal impurities
, but equipment investment is big, and operating cost is high, and security risk is high.Coal tar technology of electric de-salting with reference to crude oil demetal process, but
There is different processing methods again.China Patent Publication No. CN100999675A has invented a kind of using three-level crude oil electric desalting dress
It sets, and density is higher than or forms miscella close to the coal tar addition low-density flux oil of 1000kg/m3, keep electro-desalting former
Expect density be less than 1000kg/m3, then add commercially available crude oil metal remover and using water filling etc. crude oil be dehydrated, desalinating process come
Metal and solid impurity and moisture content in removing coal tar, but the invention is to produce light-weight fuel oil as mesh using coal tar hydrogenating
, it is not directed to the removing research of alkali metal potassium, sodium.China Patent Publication No. 103102933A has invented a kind of suitable treatment density
Coal tar electro-desalting, dehydration, de- slag method and apparatus greater than 1000kg/m3, the invention carry out crude electric desalter
Adaptability reform design, and with addition sodium carbonate liquor make solvent, note softened water or purified water to coal tar desalination, dehydration, take off
The de- processing of the electricity of slag, the invention can remove solid ammonium-salt in coal tar, but the sodium salt residual added necessarily increases coal tar pitch sodium and contains
Amount, influences coal tar pitch quality, which is not directed to removing alkali metal measure, and can not be completely suitable for property has other coal direct
Liquefied residue processing.
Therefore, at present there is an urgent need to a kind of method using coal directly-liquefied residue occur, this method wants that extraction can be made to have
Solvent more saves, solvent recovery cost is lower, extract alkali metal content and other quality index meet production of carbon black to raw material
Quality requirement.
Summary of the invention
It is an object of the invention to overcome the shortcoming of above-mentioned traditional technology, a kind of conduction production of carbon black is provided
Method.
The purpose of the present invention is what is reached by following technical measures: a kind of conductive method of producing black pigment, feature
Be: using fuel gas with low heat value as fuel, the combustion gas is coke oven combustion gas, obtains the environment of temperature and hypoxemia needed for cracking；It will
Coal liquefaction residue obtains extract liquor and extract remainder after organic solvent extracts, and filters to extract liquor, obtains refined filtration oil and refined filtration
Slag carries out the dealkalize oil obtained after dealkalize, desalination, drop ash processing, as the liquid carbon black feedstock oil to refined filtration oil；It is combustion-supporting
Gas regulation: using the oxygen rich gas of oxygen content 30% as combustion-supporting gas, combustion-supporting gas is supplied, the oxygen rich gas of oxygen content 30% is
Combustion-supporting gas is each led into fuel gas with low heat value reacts stove heating, carry out full combustion, reacting furnace temperature control 1500 DEG C-
2000℃；After the carbon black raw oil is preheating to 160 DEG C -300 DEG C, reacting furnace, the feedstock oil of atomization are sprayed at a high speed after being atomized
It is sufficiently mixed under the shear action of low-oxygen high-temperature combustion gas stream and efficient cracking reaction occurs.
A kind of improvement as above-mentioned technical proposal: the calorific value of the fuel gas with low heat value is in 900-1500kcal/Nm3 range
It is interior.
A kind of improvement as above-mentioned technical proposal: the reaction time of the efficient cracking reaction is 5ms-50ms, described
Carbon black smoke is generated in reaction process, the carbon black smoke collects carbon black after cooling, and further separation obtains
Carbon black and low-heating-value tail gas.
A kind of improvement as above-mentioned technical proposal: the organic solvent is that density is greater than or close to 1000kg/m3's
Heavy aromatic solvent, comprising: the coal tar such as carbolic oil, naphtalene oil, washing oil, carbolineum or other tar cuts oil or evaporate oil reprocessed oils and
The coalifications such as catalytic cracked oil pulp or one of petrochemical industry mink cell focus or the miscella based on these mink cell focuses or a variety of, it is described to have
When solvent extracts coal directly-liquefied residue, the additional amount of organic solvent are as follows: organic solvent mass of residue is than 0.6~5: 1.
A kind of improvement as above-mentioned technical proposal: adopted in the cooling procedure be water-cooled, air cooling or oily cooling side
Any one in formula, the carbon black is collected to be combined using one or both of cyclone separator or bag filter.
A kind of improvement as above-mentioned technical proposal: the mode of the organic solvent extraction cells processing is to be stirred extraction
It takes and is separated by solid-liquid separation, the organic solvent extraction cells include that single-stage extraction unit, two-stage and two or more extraction cells etc. are a variety of
Extraction mode, when using two-stage and the above extraction cells of two-stage, preferably counter-current extraction, the refined filtration oil dealkalize, desalination, drop ash
The method of processing is that the metal ions such as alkali metal in inorganic solvent extraction refined filtration oil are simultaneously removed, and the inorganic solvent is
Inorganic acid and deionized water.
A kind of improvement as above-mentioned technical proposal: the inorganic acid should be configured to weak solution before and it is made to contain 10
The water-soluble demulsifier of~40PPm, the inorganic acid are the inorganic acid including hydrochloric acid, sulfuric acid, nitric acid, preferably salt
Acid；Deionized water therein includes demineralized water, pure water, ultrapure water；Dilute hydrochloric acid prepares 10%~20% that water consumption is refined filtration oil,
The separation water of use of water is preferred washing procedure.
A kind of improvement as above-mentioned technical proposal: the method to the dealkalize of refined filtration oil, desalination, drop ash processing includes step
It is rapid: acid extraction first, i.e., with dilute hydrochloric acid extraction refined filtration oil, with metal ions such as alkali metal in salt acid extraction refined filtration oil, in conjunction with
Static pipeline mixer be dissolved in refined filtration oil and the metal ions such as alkali metal not soluble in water be converted to be dissolved in the metal of water from
Son obtains oleic acid mixture, and the oleic acid mixture obtains acid extraction oil after the de- device of electricity carries out water-oil separating；Then it washes
It washs, i.e., oil is extracted to acid and carry out water washing extraction, in conjunction with static pipeline mixer, acid extraction oil obtains oil water mixture through water washing,
The oil water mixture obtains dealkalize oil after the de- device of electricity carries out water-oil separating；
A kind of improvement as above-mentioned technical proposal: the salt acid extraction refined filtration oil technique is two-stage and two-stage or more adverse current
Extraction process, obtaining acid extraction oil quality should meet: moisture content is less than 0.3WT%, while acid extraction oil distillation surplus materials figureofmerit is answered
Meet K+ content and be less than 20PPm less than 2PPm, Na+ content, otherwise, acid extraction series, deionized water washing acid extraction oil should be increased
Before should add 10 1 40PPm water-soluble demulsifiers and appropriate antalkali, the antalkali is included as ammonia or ammonium hydroxide, has
Metal-free alkali compounds such as machine amine, preferably ethylenediamine.
A kind of improvement as above-mentioned technical proposal: the hydrochloric acid additional amount is by hydrochloric acid and refined filtration putty part mass ratio 1~2
: 1, and make acid extraction terminal pH value less than 1.5, preferably 1~1.5；Prepare dilute hydrochloric acid water be mutually all with the water of washing
The 10%~20% of refined filtration oil quality, in diluted hydrochloric acid dissolution extraction refined filtration oil under conditions of alkali metal and other inorganic impurities
Are as follows: pressure drop, that is, mixing intensity before and after static pipeline mixer is 60~120KPa, dissolution extraction temperature is identical as the de- temperature of electricity
It is 120 DEG C~140 DEG C, electric de- tank forceful electric power field intensity is 500~2000v/cm, and action time is 40~120min, electricity takes off pressure
For 0.6~1.5MPa；
The condition of water washing acid extraction oil is identical as diluted hydrochloric acid dissolution extraction refined filtration deep-fried twisted dough sticks part, gained dealkalize oil after water washing
Amount meets: moisture content be less than 0.3WT%, pH value be 6.5~8.0, free chlorine contents are less than 0.3PPm, the index of correlation be 110~
175, K+ content be less than 1PPm, Na+ content be less than 10PPm, asphalt content be 5.0~25.0WT%, ash be 0.01~
0.04WT%, viscosity (E80) they are 2.0~4.0, density (d420) is 1.05~1.17g/cm3, free carbon content be 2.0~
8.0WT%.
By adopting the above-described technical solution, compared with prior art, the invention has the advantages that environment of the invention in hypoxemia
It is lower that coal is used to produce carbon black as raw material, coal burning in production process is avoided, carbon black yield reduces, and secondly the invention passes through organic
Solvent extracts coal, improves the output and the quality of production of carbon black.
The invention is further illustrated in conjunction with specific embodiments.
Specific embodiment
Embodiment:
A kind of conductive method of producing black pigment, using fuel gas with low heat value as fuel, temperature and low needed for obtaining cracking
The environment of oxygen；
By coal liquefaction residue after organic solvent extracts, extract liquor and extract remainder are obtained, extract liquor is filtered, refined filtration is obtained
Oil and refined filtration slag, the dealkalize oil obtained after dealkalize, desalination, drop ash processing is carried out to refined filtration oil, and the as liquid carbon black is former
Material oil；
Combustion-supporting gas is adjusted: using the oxygen rich gas of oxygen content 30% as combustion-supporting gas, supplying combustion-supporting gas, oxygen content 30%
Oxygen rich gas be that combustion-supporting gas each leads into fuel gas with low heat value and reacts stove heating, progress full combustion, reacting furnace temperature control
System is at 1500 DEG C -2000 DEG C；
After the carbon black raw oil is preheating to 160 DEG C -300 DEG C, reacting furnace, the feedstock oil of atomization are sprayed at a high speed after being atomized
It is sufficiently mixed under the shear action of low-oxygen high-temperature combustion gas stream and efficient cracking reaction occurs.
The calorific value of the fuel gas with low heat value is within the scope of 900-1500kcal/Nm3.When the reaction of the efficient cracking reaction
Between be 5ms-50ms, generate carbon black smoke in the reaction process, the carbon black smoke collects carbon black after cooling, and
And further separation obtains carbon black and low-heating-value tail gas.
The organic solvent be density be greater than or close to 1000kg/m3 heavy aromatic solvent, comprising: carbolic oil, is washed naphtalene oil
The coal tar such as oil, carbolineum or coalifications or the petrochemical industry heavy such as other tar cuts oil or the reprocessed oils and the catalytic cracked oil pulp that evaporate oil
One of oil or the miscella based on these mink cell focuses are a variety of, when the organic solvent extracts coal directly-liquefied residue,
The additional amount of organic solvent are as follows: organic solvent mass of residue is than 0.6~5: 1.
Adopted in the cooling procedure be water-cooled, any one in air cooling or the oily type of cooling, the carbon black is collected
It is combined using one or both of cyclone separator or bag filter.
The mode of the organic solvent extraction cells processing is to be stirred extraction and separation of solid and liquid, the organic solvent extraction
Taking unit includes a variety of extraction modes such as single-stage extraction unit, two-stage and two or more extraction cells, more than two-stage and two-stage
When extraction cells, preferably counter-current extraction, the method that the refined filtration oil dealkalize, desalination, drop ash are handled are inorganic solvent extraction essence
The metal ions such as the alkali metal in oil strain are simultaneously removed, and the inorganic solvent is inorganic acid and deionized water.
The inorganic acid is described using the preceding water-soluble demulsifier that should be configured to weak solution and it is made to contain 10~40PPm
Inorganic acid is the inorganic acid including hydrochloric acid, sulfuric acid, nitric acid, preferably hydrochloric acid；Deionized water therein include demineralized water,
Pure water, ultrapure water；Dilute hydrochloric acid prepare water consumption be refined filtration oil 10%~20%, it is preferable to use water washing process separation water.
The method to the dealkalize of refined filtration oil, desalination, drop ash processing includes step:
Acid extraction first, i.e., with dilute hydrochloric acid extraction refined filtration oil, with metal ions such as alkali metal in salt acid extraction refined filtration oil,
In conjunction with static pipeline mixer being dissolved in refined filtration oil and the metal ions such as alkali metal not soluble in water are converted to and are dissolved in the gold of water
Belong to ion, obtain oleic acid mixture, the oleic acid mixture obtains acid extraction oil after the de- device of electricity carries out water-oil separating；
Then water washing extracts oil to acid and carries out water washing extraction, in conjunction with static pipeline mixer, acid extraction oil is through water washing
Oil water mixture is obtained, the oil water mixture obtains dealkalize oil after the de- device of electricity carries out water-oil separating；
The salt acid extraction refined filtration oil technique is two-stage and the above counter-current extraction technique of two-stage, and obtaining acid extraction oil quality should expire
Foot: moisture content be less than 0.3WT%, while acid extraction oil distillation surplus materials figureofmerit should meet K+ content less than 2PPm, Na+ content it is small
In 20PPm, otherwise, acid extraction series should be increased, 10 1 40PPm water-soluble demulsifiers should be added before deionized water washing acid extraction oil
With appropriate antalkali, the antalkali is included as metal-free alkali compounds such as ammonia or ammonium hydroxide, organic amine, excellent
It is selected as ethylenediamine.
The hydrochloric acid additional amount is less than acid extraction terminal pH value by hydrochloric acid and refined filtration putty part mass ratio 1~2: 1
1.5, preferably 1~1.5；The water of preparation dilute hydrochloric acid is mutually all the 10%~20% of refined filtration oil quality with the water of washing, institute
It states in diluted hydrochloric acid dissolution extraction refined filtration oil under conditions of alkali metal and other inorganic impurities are as follows: the pressure before and after static pipeline mixer
Drop i.e. mixing intensity is 60~120KPa, dissolution extraction temperature and the de- temperature of electricity are mutually all 120 DEG C~140 DEG C, and electricity takes off tank forceful electric power
Field intensity is 500~2000v/cm, and action time is 40~120min, the de- pressure of electricity is 0.6~1.5MPa；
The condition of water washing acid extraction oil is identical as diluted hydrochloric acid dissolution extraction refined filtration deep-fried twisted dough sticks part, gained dealkalize oil after water washing
Amount meets: moisture content be less than 0.3WT%, pH value be 6.5~8.0, free chlorine contents are less than 0.3PPm, the index of correlation be 110~
175, K+ content be less than 1PPm, Na+ content be less than 10PPm, asphalt content be 5.0~25.0WT%, ash be 0.01~
0.04WT%, viscosity (E80) they are 2.0~4.0, density (d420) is 1.05~1.17g/cm3, free carbon content be 2.0~
8.0WT%.
Claims (10)
1. a kind of conductive method of producing black pigment, it is characterised in that: using fuel gas with low heat value as fuel, temperature needed for obtaining cracking
With the environment of hypoxemia；
By coal liquefaction residue after organic solvent extracts, obtain extract liquor and extract remainder, to extract liquor filter, obtain refined filtration oil and
Refined filtration slag carries out the dealkalize oil obtained after dealkalize, desalination, drop ash processing, as the liquid carbon black feedstock oil to refined filtration oil；
Combustion-supporting gas is adjusted: using the oxygen rich gas of oxygen content 30% as combustion-supporting gas, supplying combustion-supporting gas, the richness of oxygen content 30%
Carrier of oxygen, which each leads into for combustion-supporting gas with fuel gas with low heat value, reacts stove heating, carries out full combustion, and reacting furnace temperature control exists
1500℃-2000℃；
After the carbon black raw oil is preheating to 160 DEG C -300 DEG C, reacting furnace is sprayed at a high speed after being atomized, the feedstock oil of atomization is low
It is sufficiently mixed under the shear action of oxygen high-temperature fuel gas stream and efficient cracking reaction occurs.
2. a kind of conductive method of producing black pigment according to claim 1, it is characterised in that: the heat of the fuel gas with low heat value
Value is within the scope of 900-1500kcal/Nm3.
3. a kind of conductive method of producing black pigment according to claim 1, it is characterised in that: the efficient cracking reaction
Reaction time is 5ms-50ms, carbon black smoke is generated in the reaction process, the carbon black smoke is after cooling by carbon black
It collects, and further separation obtains carbon black and low-heating-value tail gas.
4. a kind of conductive method of producing black pigment according to claim 3, it is characterised in that: the organic solvent is density
Be greater than or close to 1000kg/m3 heavy aromatic solvent, comprising: the coal tar such as carbolic oil, naphtalene oil, washing oil, carbolineum or other tar
Coalifications or the petrochemical industry mink cell focus such as fraction oil or the reprocessed oils and the catalytic cracked oil pulp that evaporate oil are mixed based on these mink cell focuses
One of oil or a variety of is closed, when the organic solvent extracts coal directly-liquefied residue, the additional amount of organic solvent are as follows: You Jirong
Agent mass of residue is than 0.6~5: 1.
5. a kind of conductive method of producing black pigment as claimed in claim 3, it is characterized in that: using water cooling in the cooling procedure
But, any one in air cooling or the oily type of cooling, the carbon black is collected using in cyclone separator or bag filter
One or both combination.
6. claim 1-5 its any one of as described in a kind of conductive method of producing black pigment, it is characterized in that: described organic
The mode of solvent extraction unit processing is to be stirred extraction and separation of solid and liquid, and the organic solvent extraction cells include single-stage extraction
A variety of extraction modes such as unit, two-stage and two or more extraction cells are taken, when using two-stage and the above extraction cells of two-stage, preferably
Counter-current extraction, the method that the refined filtration oil dealkalize, desalination, drop ash are handled are that inorganic solvent extracts alkali metal etc. in refined filtration oil
Metal ion is simultaneously removed, and the inorganic solvent is inorganic acid and deionized water.
7. a kind of conductive method of producing black pigment as claimed in claim 6, it is characterized in that: should be prepared before the inorganic acid use
At weak solution and the water-soluble demulsifier that makes it contain 10~40PPm, the inorganic acid is including hydrochloric acid, sulfuric acid, nitric acid
Inorganic acid, preferably hydrochloric acid；Deionized water therein includes demineralized water, pure water, ultrapure water；Dilute hydrochloric acid prepares water consumption
Refined filtration oil 10%~20%, it is preferable to use water washing process separation water.
8. a kind of conductive method of producing black pigment as claimed in claim 7, it is characterized in that: it is described to the dealkalize of refined filtration oil, desalination,
The method of drop ash processing includes step:
Acid extraction first, i.e., with dilute hydrochloric acid extraction refined filtration oil, with metal ions such as alkali metal in salt acid extraction refined filtration oil, in conjunction with
Static pipeline mixer be dissolved in refined filtration oil and the metal ions such as alkali metal not soluble in water be converted to be dissolved in the metal of water from
Son obtains oleic acid mixture, and the oleic acid mixture obtains acid extraction oil after the de- device of electricity carries out water-oil separating；
Then water washing extracts oil to acid and carries out water washing extraction, in conjunction with static pipeline mixer, acid extraction oil is obtained through water washing
Oil water mixture, the oil water mixture obtain dealkalize oil after the de- device of electricity carries out water-oil separating.
9. a kind of conductive method of producing black pigment as claimed in claim 8, it is characterized in that: the salt acid extraction refined filtration oil technique
For two-stage and the above counter-current extraction technique of two-stage, obtaining acid extraction oil quality should meet: moisture content is less than 0.3WT%, while acid extraction oil
Otherwise distillation surplus materials figureofmerit, which should meet K+ content, should increase acid extraction grade less than 20PPm less than 2PPm, Na+ content
Number should add 10 1 40PPm water-soluble demulsifiers and appropriate antalkali before deionized water washing acid extraction oil, in the alkalinity
It is included as metal-free alkali compounds such as ammonia or ammonium hydroxide, organic amine, preferably ethylenediamine with agent.
10. a kind of conductive method of producing black pigment as claimed in claim 9, it is characterized in that: the hydrochloric acid additional amount presses hydrochloric acid
With refined filtration putty part mass ratio 1~2: 1, and make acid extraction terminal pH value less than 1.5, preferably 1~1.5；Prepare dilute hydrochloric acid
Water is mutually all the 10%~20% of refined filtration oil quality with the water of washing, alkali metal in the diluted hydrochloric acid dissolution extraction refined filtration oil
And under conditions of other inorganic impurities are as follows: pressure drop, that is, mixing intensity before and after static pipeline mixer is 60~120KPa, dissolution
Extraction temperature is mutually all 120 DEG C~140 DEG C with the de- temperature of electricity, and the de- tank forceful electric power field intensity of electricity is 500~2000v/cm, action time
It is 0.6~1.5MPa for 40~120min, the de- pressure of electricity；
The condition of water washing acid extraction oil is identical as diluted hydrochloric acid dissolution extraction refined filtration deep-fried twisted dough sticks part, and gained dealkalize oil quality is full after water washing
Foot: moisture content is less than 0.3WT%, pH value is 6.5~8.0, free chlorine contents are less than 0.3PPm, the index of correlation is 110~175, K+
Content be less than 1PPm, Na+ content be less than 10PPm, asphalt content be 5.0~25.0WT%, ash be 0.01~0.04WT%,
Viscosity (E80) is 2.0~4.0, density (d420) is 1.05~1.17g/cm3, free carbon content is 2.0~8.0WT%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811435332.7A CN109294285A (en) | 2018-11-28 | 2018-11-28 | A kind of conduction method of producing black pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811435332.7A CN109294285A (en) | 2018-11-28 | 2018-11-28 | A kind of conduction method of producing black pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109294285A true CN109294285A (en) | 2019-02-01 |
Family
ID=65144091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811435332.7A Pending CN109294285A (en) | 2018-11-28 | 2018-11-28 | A kind of conduction method of producing black pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109294285A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111337645A (en) * | 2020-02-05 | 2020-06-26 | 中国人民解放军63921部队 | Earthquake liquefaction judgment method and device suitable for fine-grained soil sand |
| CN111662733A (en) * | 2020-06-10 | 2020-09-15 | 营口辽滨炭黑有限公司 | Method for producing carbon black by blending biological tar |
| CN112210233A (en) * | 2019-07-11 | 2021-01-12 | 中国石油化工股份有限公司 | Preparation method of conductive carbon black |
| CN113698797A (en) * | 2021-09-05 | 2021-11-26 | 周华良 | Vaporization tower for producing carbon black by gas mixing |
| CN115304936A (en) * | 2022-08-22 | 2022-11-08 | 青岛黑猫新材料研究院有限公司 | Production process of carbon black for magnetic resistance |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831205A (en) * | 2010-04-30 | 2010-09-15 | 曲靖众一精细化工股份有限公司 | Method for producing carbon black from carbon black raw oil in relatively anaerobic state |
| CN102492316A (en) * | 2011-12-15 | 2012-06-13 | 成都宝迪加航科技发展有限公司 | Method and equipment for producing carbon black with carbon black off-gas by means of supporting combustion of oxygen-enriched air and circulating oxygen debt combustion |
| CN105273734A (en) * | 2015-06-24 | 2016-01-27 | 刘毅 | Carbon black raw material, method for utilizing direct coal liquefaction residue for producing the carbon black raw material |
| CN108659579A (en) * | 2018-07-20 | 2018-10-16 | 宁波德泰化学有限公司 | A kind of manufacturing method of environmentally-friecarbon carbon black |
-
2018
- 2018-11-28 CN CN201811435332.7A patent/CN109294285A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831205A (en) * | 2010-04-30 | 2010-09-15 | 曲靖众一精细化工股份有限公司 | Method for producing carbon black from carbon black raw oil in relatively anaerobic state |
| CN102492316A (en) * | 2011-12-15 | 2012-06-13 | 成都宝迪加航科技发展有限公司 | Method and equipment for producing carbon black with carbon black off-gas by means of supporting combustion of oxygen-enriched air and circulating oxygen debt combustion |
| CN105273734A (en) * | 2015-06-24 | 2016-01-27 | 刘毅 | Carbon black raw material, method for utilizing direct coal liquefaction residue for producing the carbon black raw material |
| CN108659579A (en) * | 2018-07-20 | 2018-10-16 | 宁波德泰化学有限公司 | A kind of manufacturing method of environmentally-friecarbon carbon black |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210233A (en) * | 2019-07-11 | 2021-01-12 | 中国石油化工股份有限公司 | Preparation method of conductive carbon black |
| CN112210233B (en) * | 2019-07-11 | 2022-07-12 | 中国石油化工股份有限公司 | Preparation method of conductive carbon black |
| CN111337645A (en) * | 2020-02-05 | 2020-06-26 | 中国人民解放军63921部队 | Earthquake liquefaction judgment method and device suitable for fine-grained soil sand |
| CN111662733A (en) * | 2020-06-10 | 2020-09-15 | 营口辽滨炭黑有限公司 | Method for producing carbon black by blending biological tar |
| CN111662733B (en) * | 2020-06-10 | 2021-04-06 | 营口辽滨炭黑有限公司 | Method for producing carbon black by blending biological tar |
| CN113698797A (en) * | 2021-09-05 | 2021-11-26 | 周华良 | Vaporization tower for producing carbon black by gas mixing |
| CN115304936A (en) * | 2022-08-22 | 2022-11-08 | 青岛黑猫新材料研究院有限公司 | Production process of carbon black for magnetic resistance |
| CN115304936B (en) * | 2022-08-22 | 2023-08-04 | 青岛黑猫新材料研究院有限公司 | Production process of carbon black for magnetic resistance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109294285A (en) | A kind of conduction method of producing black pigment | |
| JP4045229B2 (en) | Production method of ashless coal | |
| KR20110085839A (en) | Metal recovery from hydroconverted heavy effluent | |
| CN103242881B (en) | The method of separate bitumen class material from coal directly-liquefied residue | |
| CN103013566B (en) | A kind of technique utilizing coal-tar pitch to prepare needle-shape coke raw material | |
| CN103275754B (en) | Method for separating liquefied heavy oil and asphalt substrate from direct coal liquefaction residues | |
| CN102115674A (en) | Coal liquefaction and petroleum refining combined method | |
| CN103275744A (en) | Asphalt substance separated from direct coal liquefaction residues and method and application thereof | |
| CN105778968A (en) | Method for preparing impregnating pitch, impregnating pitch and application thereof | |
| CN105316018A (en) | Pretreatment method for deep processing of coal tar | |
| CN104099171A (en) | Continuous distillation technology used for regeneration of spent lubrication oil | |
| CN105273734A (en) | Carbon black raw material, method for utilizing direct coal liquefaction residue for producing the carbon black raw material | |
| CN109868180A (en) | A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection | |
| CN105713658A (en) | Low-temperature coal tar pretreatment technology | |
| CN103254933B (en) | Method for separating liquefied heavy oil and asphalt substances from direct coal liquefaction residues | |
| CN103102933A (en) | Electric desalting, dewatering and deslagging method for coal tar | |
| US7128767B2 (en) | Method to upgrade low rank coal stocks | |
| CN109181730B (en) | Method for preparing needle coke from kerosene co-refining residues | |
| CN110157478B (en) | Pretreatment method of coal tar raw material | |
| CN109575974A (en) | A kind of method of the efficient deliming of coal liquefaction residue | |
| CN210765178U (en) | System for needle coke raw materials preliminary treatment | |
| CN103740393A (en) | Modified asphalt, method for preparing modified asphalt by utilizing coal direct liquefaction residue and application of modified asphalt | |
| CN113061452A (en) | Coal tar pitch quinoline insoluble extractant and extraction method thereof | |
| CN117304987B (en) | Method for preparing biological oil by utilizing kitchen waste through hydrothermal treatment | |
| KR101466495B1 (en) | Method for preparing coal pitch having improved property |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190201 |
|
| RJ01 | Rejection of invention patent application after publication |