CN110295053A - A kind of recycling processing method of coal chemical industry oil-containing solid slag - Google Patents
A kind of recycling processing method of coal chemical industry oil-containing solid slag Download PDFInfo
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- CN110295053A CN110295053A CN201910740132.0A CN201910740132A CN110295053A CN 110295053 A CN110295053 A CN 110295053A CN 201910740132 A CN201910740132 A CN 201910740132A CN 110295053 A CN110295053 A CN 110295053A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
Abstract
The present invention provides a kind of method of coal chemical industry oil-containing solid slag recycling treatment, the recycling processing method includes: (I) coal chemical industry oil-containing solid slag and distillate hybrid extraction, and separation of solid and liquid obtains level-one liquid-phase extraction object and level-one solid phase extract remainder；(II) the level-one solid phase extract remainder that step (I) obtains and crude benzol hybrid extraction, separation of solid and liquid obtain second level liquid-phase extraction object and second level solid phase extract remainder；(III) the second level solid phase extract remainder that step (II) obtains with plus hydrogen light petrol hybrid extraction, separation of solid and liquid obtain three-level liquid-phase extraction object and three-level solid phase extract remainder；(IV) the three-level solid phase extract remainder that step (III) obtains is dried to obtain desiccation inanimate matter component.Tar and asphaltic products can be made in extract organic component further processing after separation, and the inorganic component of desiccation then can be directly used for pyrolysis, gasification, combustion power generation, to realize the resource utilization of coal chemical industry oil-containing solid slag.
Description
Technical field
The invention belongs to Solid state fermentation fields, are related to a kind of recycling processing method of coal chemical industry oil-containing solid slag, especially relate to
And a kind of recycling processing method of the coal chemical industry oil-containing solid slag using three-level extraction.
Background technique
Coal chemical industry oil-containing solid slag is generated in the production processes such as coking, semi-coke, coal liquefaction, coal tar deep processing containing a large amount of
The solid residue of heavy oil ingredient, mainly by material compositions such as unreacted coal, pitch, mink cell focus, catalyst.Coal chemical industry oil-containing
Solid slag has corrosivity, adhesiveness, belongs to hazardous waste, deals with improperly and easily cause environmental pollution.It is extremely sticky under room temperature, it is difficult to
It directly utilizes, there is mobility at a certain temperature, but be easily adhered to equipment surface and result in blockage.Currently, coal chemical industry oil-containing
The general Land use systems of solid slag are that coal blending carries out burning processing, this undoubtedly causes the waste of high added value component in solid slag.
CN103275754A discloses a kind of separation liquefaction mink cell focus and bitumen from coal directly-liquefied residue
Method, comprising the following steps: coal directly-liquefied residue is mixed with the first extractant S1, is stirred, the extraction of level-one thermosol obtains
To the first extraction mixture；S2, the first extraction mixture is subjected to level-one separation of solid and liquid, obtains level-one extract liquor and level-one raffinate
Object；S3, level-one extract remainder is mixed with the second extractant, is stirred, the extraction of second level thermosol obtains the second extraction mixture；S4,
Second extraction mixture is subjected to second level separation of solid and liquid, obtains second level extract liquor and second level extract remainder；And S5, level-one extracted
Liquid carries out solvent recovery, obtains liquefaction mink cell focus；Second level extract liquor is subjected to solvent recovery, obtains bitumen；First extraction
It takes solvent and the second extractant is dead oil.Dead oil is from a wealth of sources reliable, low in cost, obtained drip
Green substance oil content is low, is ideal carbon materials raw material.
CN101962561A discloses the application of the extracting process and extract of a kind of coal directly-liquefied residue.The extraction
Method includes: that a) coal liquefaction residual powder and the first extractant are added in stirred tank to carry out level-one extraction；B) to step a's)
Extraction mixture is separated by solid-liquid separation, and the liquid portion made recycles the first extractant through solvent recovery unit and recycled
It uses；C) extract is obtained after recycling the first solvent, extract is mixed with the second extractant and carries out second level extraction；D) to step
Rapid extraction mixture c) is separated by solid-liquid separation, and liquid portion is made to obtain weight after solvent recovery unit recycles the second extractant
Then matter liquefaction oil enters coal liquefaction solvent hydrogenation unit together with other circulation solvents and carries out appropriateness plus hydrogen, as coal liquefaction
The circulation solvent of process；And e) bitumen obtained in step d) is heat-treated with the method for heating destructive distillation, is obtained
To mesophase pitch and oil product.
CN103509576A disclose it is a kind of from coal directly-liquefied residue separate inanimate matter method, include in order with
Lower step: 1) coal directly-liquefied residue is crushed and/or is ground, fine powder of the particle diameter less than 100 microns is obtained；It 2) will be above-mentioned
Fine powder is mixed with solvent, is reacted 0.5~20 hour under stirring in 20~300 DEG C, and the solvent includes that concentration is 1
The inorganic acid of~40 (weight) %；3) reaction product of step (2) is filtered and/or centrifugation obtains filter cake；4) by above-mentioned filter cake
It mixes with solvent, is reacted 0.5~20 hour under stirring in 20~300 DEG C, the solvent includes that concentration is 1~60
The inorganic base of (weight) %；5) reaction product of step (4) is filtered and/or centrifugation obtains filter cake, then dry filter cake.
Organic high added value component such as mink cell focus, pitch and coal, catalyst etc. in coal chemical industry oil-containing solid slag is inorganic low attached
Value added component separate and carry out respectively comprehensive utilization with significant economic benefit.But due to machine in coal chemical industry oil-containing solid slag
Tool impurity, fine particle and high viscosity component are higher, result in its be separated by solid-liquid separation difficulty it is big, low efficiency, it usually needs in high temperature
Solid-liquid is just able to achieve under condition of high voltage to efficiently separate, therefore, for coal chemical industry oil-containing solid slag, technical method disclosed above
It can not effectively realize that solid-liquid efficiently separates.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of recycling of coal chemical industry oil-containing solid slag
Processing method carries out three-level extraction to coal chemical industry oil-containing solid slag by using specific extractant, realizes coal chemical industry oil-containing
The harmless treatment and resource utilization of solid slag.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of recycling processing method of coal chemical industry oil-containing solid slag, the recycling
Processing method includes:
(I) coal chemical industry oil-containing solid slag and distillate hybrid extraction, separation of solid and liquid obtains level-one liquid-phase extraction object and level-one is solid
Phase extract remainder；
(II) the level-one solid phase extract remainder that step (I) obtains and crude benzol hybrid extraction, separation of solid and liquid obtain second level liquid phase extraction
Take object and second level solid phase extract remainder；
(III) the second level solid phase extract remainder that step (II) obtains with plus hydrogen light petrol hybrid extraction, separation of solid and liquid obtain three-level
Liquid-phase extraction object and three-level solid phase extract remainder；
(IV) the three-level solid phase extract remainder that step (III) obtains is dried to obtain desiccation inanimate matter component.
The present invention carries out three-level extraction to coal chemical industry oil-containing solid slag by using specific extractant, realizes coal chemical industry
The harmless treatment and resource utilization of oil-containing solid slag.
Present invention oil-containing solid slag to be dealt with is produced in the production processes such as coking, semi-coke, coal liquefaction, coal tar deep processing
The raw solid residue containing a large amount of heavy oil ingredients, mainly by material compositions such as unreacted coal, pitch, mink cell focus, catalyst,
Belong to hazardous waste, deals with improperly and easily cause environmental pollution.
Those skilled in the art should be noted that improvement of the invention is to have selected specific extractant to coal
Chemical industry oil-containing solid slag has carried out three-level extraction process, realizes the recycling treatment of oil-containing solid slag, and so-called recycling treatment refers to
Be that the extract generated in entire three-level extraction process and extract remainder are realized and made full use of, such as to finally obtained solid
Phase extract remainder (insoluble matters such as main most of residue including in oil-containing solid slag) is dried, and obtained desiccation solid slag can
For power generation by waste combustion, residual solvent therein can be recycled for obtained liquid-phase extraction objects at different levels and recycled, in addition may be used also
To be used to prepare pitch or tar by hydrotreating, to realize to the thorough harmless treatment of oil-containing solid slag and recycling
It utilizes.
Specifically how resource utilization is carried out to obtained liquid-phase extraction objects at different levels as subsequent, the present invention is not spy herein
It is different to limit.
In addition, the present invention and non-selected conventional extractant, level-one extraction process has selected distillate molten as extracting
Agent, it is therefore intended that extract the organic matter fractions such as condensed-nuclei aromatics in solid slag, pitch class, liquefaction oil product；Reextraction process choosing
Crude benzol is as extractant, it is therefore intended that extracts the organic matters groups such as aromatic compound in solid slag, pitch alkenes, liquefaction oil product
Point；Three-level extraction process has selected plus hydrogen light petrol is as extractant, it is therefore intended that extracts remaining liquefaction oil product in solid slag
Organic matter fraction.Be conducive to improve the dissolution of the different organic matter fractions in oil-containing solid slag using above-mentioned special extractant
Degree completes the additional recycling of oil product and bitumen in oil-containing solid slag to realize the solid-liquid separation efficiency of oil-containing solid slag.
As a preferred technical solution of the present invention, the desiccation inanimate matter group is divided into coal chemical industry desiccation solid slag.
It include coal, pitch, mink cell focus in the coal chemical industry oil-containing solid slag as a preferred technical solution of the present invention
One of catalyst or at least two combination.
As a preferred technical solution of the present invention, the quality of step (I) the coal chemical industry oil-containing solid slag and distillate
Than for 1:(0.5~10), such as can be 1:0.5,1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9 or 1:10.
Preferably, the distillate is the dead oil that true boiling-point (TBP) boiling range is 180~300 DEG C, further preferably
Ground, the distillate are the dead oil that true boiling-point (TBP) boiling range is 180~230 DEG C.
Preferably, the extraction temperature be 60~120 DEG C, such as can be 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C,
110 DEG C or 120 DEG C.
Preferably, the extraction time be 1~60min, such as can be 5min, 10min, 15min, 20min,
25min, 30min, 35min, 40min, 45min, 50min or 55min.
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably centrifugated.
Preferably, the temperature of the separation of solid and liquid be 20~100 DEG C, such as can be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C,
60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C.
As a preferred technical solution of the present invention, the mass ratio of step (II) the coal chemical industry oil-containing solid slag and crude benzol
For 1:(1~10), such as can be 1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9 or 1:10.
Preferably, the extraction temperature be 40~100 DEG C, such as can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C,
90 DEG C or 100 DEG C.
Preferably, the extraction time be 1~60min, such as can be 5min, 10min, 15min, 20min,
25min, 30min, 35min, 40min, 45min, 50min or 55min.
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably centrifugated.
Preferably, the temperature of the separation of solid and liquid be 20~100 DEG C, such as can be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C,
60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C.
As a preferred technical solution of the present invention, step (III) the coal chemical industry oil-containing solid slag with plus hydrogen light petrol
Mass ratio is 1:(1~10), such as can be 1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9 or 1:10.
Preferably, the extraction temperature be 20~100 DEG C, such as can be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C,
70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C.
Preferably, the extraction time be 1~60min, such as can be 5min, 10min, 15min, 20min,
25min, 30min, 35min, 40min, 45min, 50min or 55min.
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably filtered by vacuum.
Preferably, the temperature of the separation of solid and liquid be 20~100 DEG C, such as can be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C,
60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C.
As a preferred technical solution of the present invention, the temperature of step (IV) described drying is 100~300 DEG C, such as
It can be 100 DEG C, 125 DEG C, 150 DEG C, 175 DEG C, 200 DEG C, 225 DEG C, 250 DEG C, 275 DEG C or 300 DEG C.
Preferably, the drying time be 10~100min, such as can be 10min, 20min, 30min, 40min,
50min, 60min, 70min, 80min, 90min or 100min.
Preferably, the drying mode is spray drying, heated-air drying, vacuum drying, and further preferably vacuum is dry
It is dry.
As a preferred technical solution of the present invention, the recycling processing method further includes to the coal chemical industry
Desiccation solid slag is pyrolyzed, is gasified or is burnt for generating electricity.
As a preferred technical solution of the present invention, the recycling processing method further includes from liquid-phase extractions at different levels
Residual solvent therein is recycled in object and is recycled.
Preferably, remaining distillate and recycling are recycled from level-one liquid-phase extraction object.
Preferably, remaining crude benzol and recycling are recycled from second level liquid-phase extraction object.
Preferably, adding hydrogen light petrol and being recycled for remnants is recycled from three-level liquid-phase extraction object.
Preferably, it obtains adding hydrogen light petrol in three-level solid phase extract remainder drying process and be recycled.
Second aspect, the present invention provides a kind of isolated liquid phases at different levels extractions of the method for basis as described in relation to the first aspect
The purposes of object is taken, the liquid-phase extraction objects at different levels are used to prepare tar or pitch.
Numberical range of the present invention not only includes enumerated point value, further includes the above-mentioned numerical value not included
Arbitrary point value between range, as space is limited and for concise consideration, range described in the present invention no longer exclusive list includes
Specific point value.
Compared with prior art, the invention has the benefit that
1, the present invention provides a kind of novel dissolvent three-level extractant group technologies, compared to conventional extractant, originally
Invention has chosen specific extractant, it is advantageous that selecting three kinds of different types of extractants to oil-containing solid slag and its solid phase
Raffinate item is extracted step by step, has carried out selective extraction to the organic matter fraction in oil-containing solid slag to the greatest extent, same with this
When, extractant is from a wealth of sources and cheap, and extraction efficiency is high and is easily recycled, to realize coal chemical industry oil-containing solid slag
The efficient quick separating of middle solid-liquid two-phase.
2, the present invention provides a kind of method of novel dissolvent three-level extraction coal chemical industry oil-containing solid slag, there is unit after separation
Divide further processing that tar and asphaltic products can be made, the inorganic component of desiccation then can be directly used for pyrolysis, gasification, burn and send out
Electricity, to realize the resource utilization of coal chemical industry oil-containing solid slag.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
Embodiment 1
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using centrifugal filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:1, used dead oil true boiling-point (TBP) boiling range is 180~300 DEG C, and extraction temperature is 60 DEG C, and extraction time is
60min, filtration temperature are 40 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using centrifugal filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:1, and the second solvent is crude benzol, and extraction temperature is 40 DEG C, extraction time 60min, and filtration temperature is
40℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Centrifugal filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:2, and extraction temperature is 40 DEG C, extraction time 60min, and filtration temperature is 800 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 100 DEG C, drying time 100min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 2
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:3, used distillate is 200~300 DEG C of distillates, and extraction temperature is 70 DEG C, extraction time 60min, filtering temperature
Degree is 40 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:3, and the second solvent is crude benzol, and extraction temperature is 50 DEG C, extraction time 60min, and filtration temperature is
40℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:3, and extraction temperature is 30 DEG C, extraction time 60min, and filtration temperature is 40 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 100 DEG C, drying time 80min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 3
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:4, used distillate is 200~300 DEG C of distillates, and extraction temperature is 80 DEG C, extraction time 50min, filtering temperature
Degree is 60 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:4, and the second solvent is crude benzol, and extraction temperature is 60 DEG C, extraction time 50min, and filtration temperature is
60℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:4, and extraction temperature is 40 DEG C, extraction time 50min, and filtration temperature is 60 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 150 DEG C, drying time 60min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 4
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:5, used distillate is 200~300 DEG C of distillates, and extraction temperature is 90 DEG C, extraction time 50min, filtering temperature
Degree is 60 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:5, and the second solvent is crude benzol, and extraction temperature is 70 DEG C, extraction time 50min, and filtration temperature is
60℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:5, and extraction temperature is 50 DEG C, extraction time 50min, and filtration temperature is 60 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 150 DEG C, drying time 50min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 5
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:6, used distillate is 200~300 DEG C of distillates, and extraction temperature is 100 DEG C, extraction time 40min, filtering temperature
Degree is 90 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:6, and the second solvent is crude benzol, and extraction temperature is 80 DEG C, extraction time 40min, and filtration temperature is
80℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:6, and extraction temperature is 60 DEG C, extraction time 40min, and filtration temperature is 80 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 200 DEG C, drying time 40min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 6
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:7, used distillate is 280 DEG C of distillates, and extraction temperature is 110 DEG C, extraction time 40min, and filtration temperature is
80℃；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:7, and the second solvent is crude benzol, and extraction temperature is 90 DEG C, extraction time 40min, and filtration temperature is
80℃；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:7, and extraction temperature is 70 DEG C, extraction time 40min, and filtration temperature is 80 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 200 DEG C, drying time 30min.
The residue extraction yield being calculated is shown in Table 1.
Embodiment 7
The present invention provides a kind of processing methods of coal chemical industry oil-containing solid slag high efficient solid and liquid separation, comprising:
(I) coal chemical industry oil-containing solid slag is mixed with distillate, extraction process, using vacuum filtration to extraction mixture
Be separated by solid-liquid separation and obtains level-one liquid-phase extraction object and level-one solid phase extract remainder, the mass ratio of coal chemical industry oil-containing solid slag and distillate
For 1:10, used distillate is 200~300 DEG C of distillates, and extraction temperature is 120 DEG C, extraction time 30min, filtering
Temperature is 80 DEG C；
(II) a solid phase extract remainder for obtaining (I) mixed again with crude benzol, extraction process, using vacuum filtration
Extraction mixture be separated by solid-liquid separation and obtains second level liquid-phase extraction object and second level solid phase extract remainder, level-one solid phase extract remainder and the
The mass ratio of two solvents is 1:10, and the second solvent is crude benzol, and extraction temperature is 100 DEG C, extraction time 30min, filtration temperature
It is 80 DEG C；
(III) by secondary solid-phase extract remainder that (II) obtains with plus hydrogen light petrol finally mixed, extraction process, use
Vacuum filtration, which be separated by solid-liquid separation to extraction mixture, obtains three-level liquid-phase extraction object and three-level solid phase extract remainder, second level solid phase extraction
The mass ratio of excess and third solvent is 1:10, and extraction temperature is 80 DEG C, extraction time 30min, and filtration temperature is 80 DEG C；
(IV) the three-level solid phase extract remainder that step (III) obtains is further dried, it is remaining in removal extract remainder to have on a small quantity
Machine component, drying temperature are 200 DEG C, drying time 30min.
The residue extraction yield being calculated is shown in Table 1.
Table 1
| Project | Oil-containing solid slag extraction yield |
| Embodiment 1 | 50.62% |
| Embodiment 2 | 54.21% |
| Embodiment 3 | 58.22% |
| Embodiment 4 | 59.25% |
| Embodiment 5 | 62.52% |
| Embodiment 6 | 64.85% |
| Embodiment 7 | 65.02% |
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of recycling processing method of coal chemical industry oil-containing solid slag, which is characterized in that the recycling processing method includes:
(I) coal chemical industry oil-containing solid slag and distillate hybrid extraction, separation of solid and liquid obtain level-one liquid-phase extraction object and level-one solid phase extraction
Excess；
(II) the level-one solid phase extract remainder that step (I) obtains and crude benzol hybrid extraction, separation of solid and liquid obtain second level liquid-phase extraction object
With second level solid phase extract remainder；
(III) the second level solid phase extract remainder that step (II) obtains with plus hydrogen light petrol hybrid extraction, separation of solid and liquid obtain three-level liquid phase
Extract and three-level solid phase extract remainder；
(IV) the three-level solid phase extract remainder that step (III) obtains is dried to obtain desiccation inanimate matter component.
2. recycling processing method according to claim 1, which is characterized in that the desiccation inanimate matter group is divided into coalification
Work desiccation solid slag.
3. recycling processing method according to claim 1 or 2, which is characterized in that in the coal chemical industry oil-containing solid slag
Combination including one of coal, pitch, mink cell focus or catalyst or at least two.
4. recycling processing method according to claim 1-3, which is characterized in that step (I) described coal chemical industry
The mass ratio of oil-containing solid slag and distillate is 1:(0.5~10)；
Preferably, the distillate is the dead oil that true boiling-point (TBP) boiling range is 180~300 DEG C, it is further preferred that institute
The distillate stated is the dead oil that true boiling-point (TBP) boiling range is 180~230 DEG C；
Preferably, the extraction temperature is 60~120 DEG C；
Preferably, the extraction time is 1~60min；
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably centrifugated；
Preferably, the temperature of the separation of solid and liquid is 20~100 DEG C.
5. recycling processing method according to claim 1-4, which is characterized in that step (II) described coal chemical industry
The mass ratio of oil-containing solid slag and crude benzol is 1:(1~10)；
Preferably, the extraction temperature is 40~100 DEG C；
Preferably, the extraction time is 1~60min；
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably centrifugated；
Preferably, the temperature of the separation of solid and liquid is 20~100 DEG C.
6. recycling processing method according to claim 1-5, which is characterized in that step (III) described coal chemical industry
Oil-containing solid slag is 1:(1~10 with the mass ratio for adding hydrogen light petrol)；
Preferably, the extraction temperature is 20~100 DEG C；
Preferably, the extraction time is 1~60min；
Preferably, the separation of solid and liquid is centrifuge separation, filters pressing or vacuum filtration, is further preferably filtered by vacuum；
Preferably, the temperature of the separation of solid and liquid is 20~100 DEG C.
7. recycling processing method according to claim 1-6, which is characterized in that step (IV) described drying
Temperature is 100~300 DEG C；
Preferably, the drying time is 10~100min；
Preferably, the drying mode is spray drying, heated-air drying, vacuum drying, is further preferably dried in vacuo.
8. recycling processing method according to claim 1-7, which is characterized in that the recycling treatment side
Method further includes that the coal chemical industry desiccation solid slag is pyrolyzed, is gasified or is burnt for generating electricity.
9. recycling processing method according to claim 1-8, which is characterized in that the recycling treatment side
Method further includes recycling residual solvent therein from liquid-phase extraction objects at different levels and being recycled；
Preferably, remaining distillate and recycling are recycled from level-one liquid-phase extraction object；
Preferably, remaining crude benzol and recycling are recycled from second level liquid-phase extraction object；
Preferably, adding hydrogen light petrol and being recycled for remnants is recycled from three-level liquid-phase extraction object；
Preferably, it obtains adding hydrogen light petrol in three-level solid phase extract remainder drying process and be recycled.
10. a kind of purposes of the isolated liquid-phase extraction objects at different levels of -9 described in any item methods according to claim 1, special
Sign is that the liquid-phase extraction objects at different levels are used to prepare tar or pitch.
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