CN106995719A - The method and thus obtained organic matter extract of organic matter in extracting coal directly-liquefied residue - Google Patents
The method and thus obtained organic matter extract of organic matter in extracting coal directly-liquefied residue Download PDFInfo
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- CN106995719A CN106995719A CN201610050065.6A CN201610050065A CN106995719A CN 106995719 A CN106995719 A CN 106995719A CN 201610050065 A CN201610050065 A CN 201610050065A CN 106995719 A CN106995719 A CN 106995719A
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- organic matter
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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
- C10G57/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one cracking process or refining process and at least one other conversion process
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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
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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
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
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- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
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- Materials Engineering (AREA)
- Extraction Or Liquid Replacement (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to the method for the organic matter in extracting coal directly-liquefied residue.Specifically, the method for the invention comprises the following steps：By coal directly-liquefied residue and solvent in mass ratio 1:(1-50) is mixed, the solvent is selected from the double solvents of water or water and organic solvent, obtained mixture is heated to temperature for more than 250 DEG C and reacted, and solid product and liquid product will be obtained after the reactant filtering of generation, it can obtain organic matter extract after atmospheric and vacuum distillation is carried out to liquid product.Method of the present invention, which has the advantages that low production cost, environmentally friendly, follow-up extract lock out operation simple and extracts obtained organic matter extract has high H/C ratios.
Description
Technical field
The invention belongs to direct coal liquefaction technology field, it is related to having in extracting coal directly-liquefied residue
The method of machine matter and thus obtained organic matter extract.Specifically, the present invention relates to selected from
The organic matter in a kind of extracting coal directly-liquefied residue in the double solvents of water or water and organic solvent
Method, and obtained organic matter extract is extracted by this method.
Background technology
Currently, worldwide economic development still depends critically upon the production and utilization of fossil energy,
China is no exception.Energy resource structure composition (rich coal few oil) and consumptive characteristics based on China and
The of a relatively high rate of economic development, the effective of the energy has seemed increasingly using with safety problem
It is important.However, for the oil as main energy sources, Chinese storage level is relatively low.To be true
The energy environment safety of China is protected, makes full use of the coal resources that China is rich in reduce to external stone
The dependence of oil inlet, has obtained the extensive common recognition of all circles.
It is used as the direct coal liquefaction technology of one of the conventional method currently with coal resources, Neng Gouchong
Divide and utilize China cleanly compared with the coal resources of horn of plenty.The liquefaction technology passes through to " rich carbon is poor
" solid " coal of hydrogen " directly adds " hydrogen ", produces the liquefaction products similar to " crude oil ".This
A little liquefaction products can pass through refining and the process similar to oil, obtain including hair so as to produce
Various chemicals including motivation fuel.In the technical process of the liquefaction technology, coal direct hydrogenation
Liquefaction reaction is key reaction unit therein.In the reaction member, except generation " liquid "
Purpose product outside, restricted by reactant activity and operating condition, also generation account for feedstock quality about
30% or so " solid-state " liquefied residue is used as accessory substance.The liquefied residue complicated component, wherein
30% unsegregated mink cell focus is accounted for containing quality and quality accounts for 30% or so pitch class and had
Machine matter.Main purpose in view of direct coal liquefaction technology is production liquid oil, so above-mentioned liquid
Whether the organic matter changed in residue can effectively reclaim, it will directly affect whole DCL/Direct coal liquefaction skill
The efficiency and economy of art.
Generally handled previously for coal liquefaction residue using means such as direct burning, coking liquefactions,
This not only brings environmental problem, and significantly reduces the economy of direct coal liquefaction technology.Cause
This, how effectively and reclaim at low cost the organic matter in above-mentioned liquefied residue turn into currently for coal
The preferred direction that Direct liquefaction technology is improved.
So far, in the prior art, those skilled in the art have studied molten using organic extraction
Agent is stripped to the organic matter in coal directly-liquefied residue.For example, Chinese patent CN
101885976B and CN 101962561B disclose the oil produced in itself with DCL/Direct coal liquefaction process
The method that product are extracted as extractant to coal liquefaction residue；Miao Qiang (coal directly-liquefied residues
Abstraction technique present situation and development trend,《Clean coal technology》, the 1st phase of volume 21,2015 1
Month, the 56-60 pages) mention in the prior art by quinoline, aromatic hydrocarbons mixture, imidazole-like ionic
The organic solvents such as liquid, DMAC N,N' dimethyl acetamide, tetrahydrofuran, furfural, pyridine as
The solvent being stripped to coal liquefaction residue；(Shenhua direct coal liquefaction residue is overcritical for Liu Pengfei etc.
Solvent extraction is studied,《Chemistry of fuel journal》, the 7th phase of volume 40, in July, 2012,776-781
Page) disclose straight to coal by supercritical solvent extraction method using toluene, benzene and three kinds of solvents of ethanol
Liquefied residue is connect to be extracted.
However, due to using these organic solvents higher as extraction solvent cost itself, moreover,
In order to avoid the corrosiveness of organic solvent also needs to the reaction unit using specific materials, this is also carried
High production cost.Further, since the problem of use of organic solvent is also easy to cause environmental pollution.
Therefore, new method for extracting is developed, having in coal directly-liquefied residue can either be effectively extracted
Machine matter, additionally it is possible to ensure extractant used it is with low cost and can pollution abatement and environmentally friendly,
Technical problem as pendulum urgent need to resolve in face of those skilled in the art.
The content of the invention
Although water is polar solvent at normal temperatures and pressures, with the rise of temperature, water is by polarity
Material is changed into apolar substance, and the solvability to organic matter progressively strengthens.In addition, adding in water
Plus a certain amount of organic solvent, it comparatively can further improve and take out under relatively low temperature conditionss
Put forward efficiency.For above-mentioned technical problem present in this area, the present inventor is had found by studying,
Carried out at high temperature with coal directly-liquefied residue using the double solvents of water or water and organic solvent anti-
Should, it can realize and the organic matter in coal directly-liquefied residue is stripped, so that there is provided one kind
Side that is with low cost, environment-friendly and can effectively extracting the organic matter in coal directly-liquefied residue
Method.
Therefore, in one aspect, the invention provides with solvent extraction coal directly-liquefied residue
The method of organic matter, wherein, this method comprises the following steps：
(1) by coal directly-liquefied residue and solvent in mass ratio 1:(1-50) is mixed, and is mixed
Compound；
(2) mixture obtained in step (1) is heated to temperature for more than 250 DEG C, and makes to mix
Compound reacts at such a temperature, obtains reactant；
(3) reactant in step (2) is filtered, obtains solid product and liquid product；
(4) liquid product is subjected to atmospheric and vacuum distillation, obtains organic matter extract and solvent；
(5) solvent is reclaimed and recycled；
Wherein, solvent is selected from the double solvents of water or water and organic solvent.
On the other hand, the invention provides the organic matter extract obtained according to above method extraction.
Technical scheme can be entered by following paragraph [1] to the content described in paragraph [28]
The exemplary explanation of row：
[1] method of the organic matter in a kind of use solvent extraction coal directly-liquefied residues of, its feature exists
In the described method comprises the following steps：
(1) by the coal directly-liquefied residue and the solvent in mass ratio 1:(1-50) is mixed,
Obtain mixture；
(2) mixture obtained in the step (1) is heated to temperature for more than 250 DEG C, and
The mixture is reacted at said temperatures, obtain reactant；
(3) reactant in the step (2) is filtered, obtains solid product and liquid phase
Product；
(4) liquid product is subjected to atmospheric and vacuum distillation, obtains organic matter extract and described molten
Agent；
(5) solvent is reclaimed and recycled；
Wherein, the solvent is selected from the double solvents of water or water and organic solvent.
[2] methods of the according to paragraph [1], it is characterised in that in the step (1), will
The coal directly-liquefied residue and the solvent in mass ratio 1:(10-50) is mixed.
[3] methods of the according to paragraph [2], it is characterised in that by the coal directly-liquefied residue
With the solvent in mass ratio 1:(10-35) is mixed.
[4] methods of the according to paragraph [3], it is characterised in that by the coal directly-liquefied residue
With the solvent in mass ratio 1:10、1:15 or 1:35 are mixed.
[5] methods of the according to either segment in paragraph [1]-[4], it is characterised in that in the step
(1) in, the coal directly-liquefied residue is mixed in the following way with the solvent：
High-temperature high-voltage reaction system is connected at coal directly-liquefied residue outlet, coal directly-liquefied residue is arranged
The temperature entered in the high-temperature high-voltage reaction system for being more than 4MPa to pressure is more than 250 DEG C
The solvent in.
[6] methods of the according to either segment in paragraph [1]-[4], it is characterised in that in the step
(1) in, the coal directly-liquefied residue is mixed in the following way with the solvent：Will
The coal directly-liquefied residue discharged at coal directly-liquefied residue outlet is mixed with the solvent
Slurry mixture, pressure is transported to for more than 4MPa, temperature by pump by the slurry mixture
For in more than 250 DEG C of high-temperature high-voltage reaction system.
[7] methods of the according to paragraph [1], it is characterised in that the organic solvent is that alcohols is molten
Agent, ether solvent, ketones solvent, furans solvent or their mixture.
[8] methods of the according to paragraph [7], it is characterised in that the alcohols solvent is selected from unitary
Alcohol, dihydric alcohol or their mixture.
[9] methods of the according to paragraph [8], it is characterised in that the monohydric alcohol be selected from methanol,
Ethanol or their mixture.
[10] methods of the according to paragraph [8], it is characterised in that the dihydric alcohol is ethylene glycol.
[11] methods of the according to paragraph [7], it is characterised in that the ether solvent is selected from ether.
[12] methods of the according to paragraph [7], it is characterised in that the ketones solvent is selected from acetone.
[13] methods of the according to paragraph [7], it is characterised in that the furans solvent is selected from four
Hydrogen furans.
[14] methods of the according to either segment in paragraph [1]-[13], it is characterised in that the solvent
For water and the double solvents of organic solvent, wherein, water and the organic solvent in mass ratio 1:(it is more than
0-1) mixed.
[15] methods of the according to paragraph [14], it is characterised in that water is pressed with the organic solvent
Mass ratio 1:(being more than 0-0.5) is mixed.
[16] methods of the according to paragraph [15], it is characterised in that water is pressed with the organic solvent
Mass ratio 1:0.1 is mixed.
[17] methods of the according to either segment in paragraph [1]-[16], it is characterised in that in the step
Suddenly in (2), the mixture obtained in the step (1) is heated under 4MPa-30MPa.
[18] methods of the according to paragraph [17], it is characterised in that will be obtained in the step (1)
The mixture arrived is heated under 4MPa-20MPa.
[19] methods of the according to either segment in paragraph [1]-[18], it is characterised in that in the step
Suddenly in (2), the mixture obtained in the step (1) is heated to 250 DEG C -400 DEG C.
[20] methods of the according to paragraph [19], it is characterised in that will be obtained in the step (1)
To mixture be heated to 250 DEG C -320 DEG C.
[21] methods of the according to paragraph [20], it is characterised in that will be obtained in the step (1)
To mixture be heated to 250 DEG C, 300 DEG C or 320 DEG C.
[22] methods of the according to either segment in paragraph [1]-[21], it is characterised in that in the step
Suddenly in (2), the mixture reaction is more than 0h and less than or equal to 5h.
[23] methods of the according to paragraph [22], it is characterised in that the mixture reacts 1h-5h.
[24] methods of the according to paragraph [23], it is characterised in that the mixture reacts 1h-3h.
[25] methods of the according to paragraph [24], it is characterised in that the mixture reaction 1h,
2h or 3h.
[26] methods of the according to either segment in paragraph [1]-[25], it is characterised in that in the step
Suddenly in (4), by the liquid product respectively in 0.08MPa-0.16MPa and 0.001MPa-0.019
Atmospheric and vacuum distillation is carried out under MPa.
[27] methods of the according to paragraph [26], it is characterised in that distinguish the liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa.
[28] methods of the according to either segment in paragraph [1]-[27] extracts obtained organic matter extracting
Thing.
Compared with the disclosed other methods being stripped to coal directly-liquefied residue in the prior art,
In method of the present invention, by DCL/Direct coal liquefaction consersion unit can be relatively easy to achieve by
The double solvents of water or water and organic solvent with coal directly-liquefied residue be mixed slurry mixture,
Or be discharged into coal directly-liquefied residue in the reactor under the conditions of high-temperature high-voltage reaction, therefore, this
The described method of invention can be coupled with direct coal liquefaction process.
In addition, compared with the Application way of disclosed coal directly-liquefied residue in the prior art, this hair
Bright described method is using the organic matter in water extracting coal directly-liquefied residue (by only containing C, H
The mixture composition of organic hydrocarbon and the in addition organic hydrocarbon also containing hetero atom N, S and O) so that
With following advantage：Due to mainly using green extractant cheap and easy to get and being capable of pollution abatement
(that is, the double solvents of water or water and a small amount of organic solvent), institute is with the inventive method not only
Production cost can be substantially reduced, but also it is environment-friendly.Also, method of the present invention is also
The organic matter in coal directly-liquefied residue can effectively be extracted.Simultaneously as being used as the water of extractant
Or the double solvents of water and organic solvent is between the organic matter as purpose product and unmixing, because
This, after the completion of extracting, easily separates purpose product (organic matter) from extractant,
So as to easily extract the organic matter in coal directly-liquefied residue.In addition, compared with DCL/Direct coal liquefaction
For residue, the present invention, which extracts obtained organic matter extract, has higher H/C ratios (to rub
You are than meter), therefore, advantageously approached in composition in using obtained organic matter as raw material production
In the liquefaction products of crude oil.
Brief description of the drawings
Fig. 1 is the process chart of the illustrative embodiments of the present invention.
Embodiment
In the present invention, term " coal directly-liquefied residue " refer to by coal by using this area
The direct coal liquefaction technology known solid residue resulting after being handled.Unless otherwise indicated,
Coal directly-liquefied residue of the present invention is mainly comprising mink cell focus, bitumen, unconverted
Mineral matter in coal and raw coal.
In the present invention, unless otherwise indicated, term " high temperature " refers to that temperature is more than 250 DEG C.
In the present invention, unless otherwise indicated, term " high pressure " is that finger pressure is more than 4MPa.
In the present invention, unless otherwise indicated, term " atmospheric and vacuum distillation " refers in normal pressure (about 1
Individual standard atmospheric pressure, for example, can be 0.08MP-0.16Mpa) and decompression (e.g., from about 0.001
MPa-0.019MPa distilled under), so as to obtain the different cut of boiling range.
In one embodiment, the present invention relates to having in solvent extraction coal directly-liquefied residue
The method of machine matter, wherein, this method comprises the following steps：
(1) by coal directly-liquefied residue and solvent in mass ratio 1:(1-50) is mixed, and is mixed
Compound；
(2) mixture obtained in step (1) is heated to temperature for more than 250 DEG C, and makes this
Mixture reacts at such a temperature, obtains reactant；
(3) reactant in step (2) is filtered, obtains solid product and liquid product；
(4) liquid product is subjected to atmospheric and vacuum distillation, obtains organic matter extract and solvent；
(5) solvent is reclaimed and recycled；
Wherein, solvent is selected from the double solvents of water or water and organic solvent.
In one preferred embodiment, in above-mentioned steps (1), by coal directly-liquefied residue
With solvent in mass ratio 1:(10-50) is mixed, and preferably in mass ratio 1:(10-35) is mixed,
More preferably in mass ratio 1:10、1:15 or 1:35 are mixed.
In one preferred embodiment, in above-mentioned steps (1), by coal directly-liquefied residue
Mixed in the following way with solvent：High temperature is connected at coal directly-liquefied residue outlet high
Reaction system is pressed, coal directly-liquefied residue is drained into the high temperature high pressure reverse that pressure is more than 4MPa
The temperature in system is answered in more than 250 DEG C of solvent.In another preferred embodiment, upper
State in step (1), coal directly-liquefied residue is mixed in the following way with solvent：Will be from
The coal directly-liquefied residue discharged at coal directly-liquefied residue outlet is mixed and made into slurry with solvent and mixed
Compound, by pump by slurry mixture be transported to pressure be more than 4MPa, temperature be 250 DEG C with
On high-temperature high-voltage reaction system in.
In one preferred embodiment, organic solvent is alcohols solvent, ether solvent, ketone
Solvent, furans solvent or their mixture.
In embodiment still more preferably, alcohols solvent is preferably selected from monohydric alcohol, dihydric alcohol
Or their mixture.Wherein, as monohydric alcohol of the present invention, preferably include, but is not limited to
Methanol, ethanol or their mixture；As dihydric alcohol of the present invention, preferably include but not
It is limited to ethylene glycol.
In embodiment still more preferably, ether solvent preferably includes, but is not limited to ether.
In embodiment still more preferably, ketones solvent preferably includes, but is not limited to acetone.
In embodiment still more preferably, furans solvent preferably includes, but is not limited to tetrahydrochysene
Furans.
In one preferred embodiment, the solvent in the present invention is the compound of water and organic solvent
Solvent, wherein, water and organic solvent in mass ratio 1:(being more than 0-1) is mixed.It is preferred that water is with having
Machine solvent in mass ratio 1:(being more than 0-0.5), more preferably in mass ratio 1:0.1 is mixed.
In one preferred embodiment, in above-mentioned steps (2), by the step (1)
In obtained mixture heat, preferably heated under 4MPa-20MPa under 4MPa-30MPa.
In one preferred embodiment, in above-mentioned steps (2), it will be obtained in step (1)
To mixture be heated to 250 DEG C -400 DEG C, be preferably heated to 250 DEG C -320 DEG C, more preferably heat
To 250 DEG C, 300 DEG C or 320 DEG C.
In one preferred embodiment, in above-mentioned steps (2), mixture reaction more than 0h,
And less than or equal to 5h, preferably react 1h-5h, more preferably react 1h-3h, further preferably reaction
1h, 2h or 3h.
In one preferred embodiment, in above-mentioned steps (4), by the liquid product point
Not atmospheric and vacuum distillation is carried out under 0.08MPa-0.16MPa and 0.001MPa-0.019MPa, it is excellent
Liquid product is carried out atmospheric and vacuum distillation by choosing under 0.1MPa and 0.001MPa respectively.
In another embodiment, taken out the present invention relates to the organic matter obtained according to above method extraction
Extract.
The organic matter extract that the present invention is obtained with solvent extraction is the lightweight in coal directly-liquefied residue
Component.Wherein, light components of the present invention are the organic hydrocarbon that includes in coal directly-liquefied residue
Mixture.
It will be appreciated by persons skilled in the art that residual in the above-mentioned DCL/Direct coal liquefaction listed of the present invention
The ratio that is mixed between hybrid mode, coal directly-liquefied residue and solvent between slag and solvent and
The non-limiting the scope of the invention of the selection in reaction temperature and reaction time, above range
Selection is intended merely to cost-effective while ensureing to reach optimum efficiency.To those skilled in the art
For it is understood that in the case of without departing from spirit of the invention, being carried out to the present invention program
Simple replacement, change or change each fallen within protection scope of the present invention.
In addition, unless otherwise stated, the extract content of organic matter extract of the present invention is pressed
Calculated according to equation below：
Extract content (%)=[(quality of quality-solid product of coal directly-liquefied residue) direct liquid of/coal
Change the quality of residue] × 100%
Below in conjunction with drawings and examples, the present invention is described in further detail, but the present invention
Protection domain be not limited in accompanying drawing and these following embodiments.
Embodiment
Embodiment 1
By 10g coal directly-liquefied residues and water in the following way in mass ratio 1:15 are mixed：
High-temperature high-voltage reaction system is connected at coal directly-liquefied residue outlet, by coal directly-liquefied residue
In the high-temperature water (250 DEG C) for being drained into the high-temperature high-voltage reaction system that pressure is 4MPa, obtain
To coal directly-liquefied residue and the mixture of water.
Then, the mixture of above-mentioned coal directly-liquefied residue and water is heated under 4MPa
250 DEG C, and mixture is reacted 2h at such a temperature, obtain reactant.Then, reactant is entered
Row filtering, obtains solid product and liquid product, wherein, the quality of the solid product is 9.62g.
Then, liquid product is subjected to atmospheric and vacuum distillation under 0.12MPa and 0.001MPa respectively, obtained
To organic matter extract and water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 3.8%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.99。
Embodiment 2
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:15 are mixed and made into grain slag
Pulp mixture, it is that 10MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 300 DEG C under 10MPa, and makes mixture
2h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 9.23g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 7.7%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.96。
Embodiment 3
By 10g coal directly-liquefied residues and water in the following way in mass ratio 1:15 are mixed：
High-temperature high-voltage reaction system is connected at coal directly-liquefied residue outlet, by coal directly-liquefied residue
In the high-temperature water (300 DEG C) for being drained into the high-temperature high-voltage reaction system that pressure is 10MPa,
Obtain the mixture of coal directly-liquefied residue and water.
Then, the mixture of above-mentioned coal directly-liquefied residue and water is heated under 10MPa
300 DEG C, and mixture is reacted 1h at such a temperature, obtain reactant.Then, reactant is entered
Row filtering, obtains solid product and liquid product, wherein, the quality of the solid product is 9.30g.
Then, liquid product is subjected to atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtained
To organic matter extract and water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 7.0%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.96。
Embodiment 4
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:15 are mixed and made into grain slag
Pulp mixture, it is that 10MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 300 DEG C under 10MPa, and makes mixture
3h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 9.20g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.16MPa and 0.019MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 8.0%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.96。
Embodiment 5
By 10g coal directly-liquefied residues and water in the following way in mass ratio 1:1 is mixed：
High-temperature high-voltage reaction system is connected at coal directly-liquefied residue outlet, by coal directly-liquefied residue
In the high-temperature water (320 DEG C) for being drained into the high-temperature high-voltage reaction system that pressure is 12MPa,
Obtain the mixture of coal directly-liquefied residue and water.
Then, the mixture of above-mentioned coal directly-liquefied residue and water is heated under 12MPa
320 DEG C, and mixture is reacted 2h at such a temperature, obtain reactant.Then, reactant is entered
Row filtering, obtains solid product and liquid product, wherein, the quality of the solid product is 9.70g.
Then, liquid product is subjected to atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtained
To organic matter extract and water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 3.0%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.98。
Embodiment 6
By 10g coal directly-liquefied residues and water in the following way in mass ratio 1:10 are mixed：
High-temperature high-voltage reaction system is connected at coal directly-liquefied residue outlet, by coal directly-liquefied residue
In the high-temperature water (320 DEG C) for being drained into the high-temperature high-voltage reaction system that pressure is 12MPa,
Obtain the mixture of coal directly-liquefied residue and water.
Then, the mixture of above-mentioned coal directly-liquefied residue and water is heated under 12MPa
320 DEG C, and mixture is reacted 2h at such a temperature, obtain reactant.Then, reactant is entered
Row filtering, obtains solid product and liquid product, wherein, the quality of the solid product is 9.03g.
Then, liquid product is subjected to atmospheric and vacuum distillation under 0.08MPa and 0.001MPa respectively, obtained
To organic matter extract and water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 9.7%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
0.94。
Embodiment 7
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:15 are mixed and made into grain slag
Pulp mixture, it is that 12MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 320 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 320 DEG C under 12MPa, and makes mixture
5h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 8.50g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 15.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.95.
Embodiment 8
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:15 are mixed and made into grain slag
Pulp mixture, it is that 12MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 320 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 320 DEG C under 12MPa, and makes mixture
2h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 8.49g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 15.1%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.95.
Embodiment 9
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:35 are mixed and made into grain slag
Pulp mixture, it is that 12MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 320 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 320 DEG C under 12MPa, and makes mixture
2h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 7.85g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 21.5%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.93.
Using Industry Analysis Method known in the art and elemental analysis method, in this embodiment
The coal directly-liquefied residue of use carries out Industrial Analysis and elementary analysis, and its result is as shown in table 1 below：
Table 1：The Industrial Analysis of coal directly-liquefied residue in embodiment 9 and elementary analysis result
Meanwhile, using elemental analysis method known in the art, to having for being obtained in this embodiment
The element composition of machine matter extract is analyzed, and result is shown in table 2 below.
Table 2：The element composition of organic matter extract in embodiment 9
Embodiment 10
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:50 are mixed and made into grain slag
Pulp mixture, it is that 12MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 320 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 320 DEG C under 12MPa, and makes mixture
2h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 7.50g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtains organic matter extract
And water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 25.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.90.
Embodiment 11
10g coal directly-liquefied residues are mixed in the following way with water：Will be from the direct liquid of coal
Change the coal directly-liquefied residue and water in mass ratio 1 discharged at sludge discharge tube:35 are mixed and made into grain slag
Pulp mixture, it is that 22MPa, temperature are that the grain slag pulp mixture is transported into pressure by pump
In 400 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned grain slag pulp mixture is heated to 400 DEG C under 22MPa, and makes mixture
2h is reacted at such a temperature, obtains reactant.Then, reactant is filtered, obtains solid phase
Product and liquid product, wherein, the quality of the solid product is 7.00g.Then, liquid phase is produced
Thing carries out atmospheric and vacuum distillation under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Water.Obtained water is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 30.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.85.
Embodiment 12
By 10g coal directly-liquefied residues with water and the double solvents (water of methanol:Methanol=1:0.1) lead to
Following manner is crossed to be mixed：The DCL/Direct coal liquefaction that will be discharged at coal directly-liquefied residue outlet
Double solvents in mass ratio 1 of the residue with water and methanol:15 are mixed and made into slurry mixture, pass through pump
The slurry mixture is transported to the high-temperature high-voltage reaction that pressure is 12MPa, temperature is 300 DEG C
In system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.18g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and methanol.Obtained water and the double solvents of methanol is reclaimed and circulated
Use.
Wherein, the extract content of the organic matter extract is 8.2%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
1.10。
Embodiment 13
Except using water:Methanol=1:Outside 0.5 water and the double solvents of methanol, according to embodiment 12
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
9.15g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and methanol.To obtained water and methanol
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 8.5%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
1.10。
Embodiment 14
Except using water:Methanol=1:Outside 1 water and the double solvents of methanol, according to embodiment 12
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
9.00g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and methanol.To obtained water and methanol
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.10.
Embodiment 15
By 10g coal directly-liquefied residues with water and the double solvents (water of ethanol:Ethanol=1:0.1) lead to
Following manner is crossed to be mixed：The DCL/Direct coal liquefaction that will be discharged at coal directly-liquefied residue outlet
Double solvents in mass ratio 1 of the residue with water and ethanol:15 are mixed and made into slurry mixture, pass through pump
The slurry mixture is transported to the high-temperature high-voltage reaction that pressure is 12MPa, temperature is 300 DEG C
In system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.20g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and ethanol.Obtained water and the double solvents of ethanol is reclaimed and circulated
Use.
Wherein, the extract content of the organic matter extract is 8.0%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
1.04。
Embodiment 16
Except using water:Ethanol=1:Outside 0.5 water and the double solvents of ethanol, according to embodiment 15
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
9.00g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and ethanol.To obtained water and ethanol
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.03.
Embodiment 17
Except using water:Ethanol=1:Outside 1 water and the double solvents of ethanol, according to embodiment 15
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
8.60g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and ethanol.To obtained water and ethanol
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 14.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.00.
Embodiment 18
By 10g coal directly-liquefied residues with water and the double solvents (water of ethylene glycol:Ethylene glycol=1:0.1)
Mixed in the following way：The direct liquid of coal that will be discharged at coal directly-liquefied residue outlet
Change double solvents in mass ratio 1 of the residue with water and ethylene glycol:15 are mixed and made into slurry mixture, lead to
Cross pump and the slurry mixture is transported to the HTHP that pressure is 12MPa, temperature is 300 DEG C
In reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.00g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and ethylene glycol.Obtained water and the double solvents of ethylene glycol is reclaimed simultaneously
Recycle.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.04.
Embodiment 19
Except using water:Ethylene glycol=1:Outside 0.5 water and the double solvents of ethylene glycol, according to implementation
Method described in example 18 obtains solid product and liquid product, wherein, the matter of the solid product
Measure as 8.90g.Then, liquid product is often subtracted under 0.1MPa and 0.001MPa respectively
Pressure distillation, obtains the double solvents of organic matter extract and water and ethylene glycol.To obtained water with
The double solvents of ethylene glycol is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 11.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.04.
Embodiment 20
Except using water:Ethylene glycol=1:Outside 1 water and the double solvents of ethylene glycol, according to embodiment
Method described in 18 obtains solid product and liquid product, wherein, the quality of the solid product
For 8.40g.Then, liquid product is subjected to Atmospheric vacuum under 0.1MPa and 0.001MPa respectively
Distillation, obtains the double solvents of organic matter extract and water and ethylene glycol.To obtained water and second
The double solvents of glycol is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 16.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.02.
Embodiment 21
By 10g coal directly-liquefied residues with water and the double solvents (water of ether:Ether=1:0.1) lead to
Following manner is crossed to be mixed：The DCL/Direct coal liquefaction that will be discharged at coal directly-liquefied residue outlet
Double solvents in mass ratio 1 of the residue with water and ether:15 are mixed and made into slurry mixture, pass through pump
The slurry mixture is transported to the high-temperature high-voltage reaction that pressure is 12MPa, temperature is 300 DEG C
In system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.10g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and ether.Obtained water and the double solvents of ether is reclaimed and circulated
Use.
Wherein, the extract content of the organic matter extract is 9.0%.Also, the organic matter extract
For organic hydrocarbon mixture, the elements such as C, H, N, S and O are mainly contained, H/C ratios therein are
1.01。
Embodiment 22
Except using water:Ether=1:Outside 0.5 water and the double solvents of ether, according to embodiment 21
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
8.80g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and ether.To obtained water and ether
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 12.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.00.
Embodiment 23
Except using water:Ether=1:Outside 1 water and the double solvents of ether, according to embodiment 21
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
8.50g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and ether.To obtained water and ether
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 15.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.99.
Embodiment 24
By 10g coal directly-liquefied residues with water and the double solvents (water of acetone:Acetone=1:0.1) lead to
Following manner is crossed to be mixed：The DCL/Direct coal liquefaction that will be discharged at coal directly-liquefied residue outlet
Double solvents in mass ratio 1 of the residue with water and acetone:15 are mixed and made into slurry mixture, pass through pump
The slurry mixture is transported to the high-temperature high-voltage reaction that pressure is 12MPa, temperature is 300 DEG C
In system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.00g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and acetone.Obtained water and the double solvents of acetone is reclaimed and circulated
Use.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.00.
Embodiment 25
Except using water:Acetone=1:Outside 0.5 water and the double solvents of acetone, according to embodiment 24
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
8.70g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and acetone.To obtained water and acetone
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 13.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.95.
Embodiment 26
Except using water:Acetone=1:Outside 1 water and the double solvents of acetone, according to embodiment 25
Described in method obtain solid product and liquid product, wherein, the quality of the solid product is
8.50g.Then, liquid product is subjected to Atmospheric vacuum steaming under 0.1MPa and 0.001MPa respectively
Evaporate, obtain the double solvents of organic matter extract and water and acetone.To obtained water and acetone
Double solvents is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 15.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.94.
Embodiment 27
By 10g coal directly-liquefied residues with water and the double solvents (water of tetrahydrofuran:Tetrahydrofuran
=1:0.1) mixed in the following way：The coal that will be discharged at coal directly-liquefied residue outlet
Double solvents in mass ratio 1 of the direct liquefaction residue with water and tetrahydrofuran:15, which are mixed and made into slurry, mixes
Compound, it is that 12MPa, temperature are 300 DEG C that the slurry mixture is transported into pressure by pump
In high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 8.80g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract with
And the double solvents of water and tetrahydrofuran.Obtained water and the double solvents of tetrahydrofuran is returned
Receive and recycle.
Wherein, the extract content of the organic matter extract is 12.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.95.
Embodiment 28
Except using water:Tetrahydrofuran=1:Outside 0.5 water and the double solvents of tetrahydrofuran, according to
Method described in embodiment 27 obtains solid product and liquid product, wherein, the solid product
Quality be 8.50g.Then, liquid product is carried out under 0.1MPa and 0.001MPa respectively
Atmospheric and vacuum distillation, obtains the double solvents of organic matter extract and water and tetrahydrofuran.To obtaining
Water and the double solvents of tetrahydrofuran reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 15.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.91.
Embodiment 29
Except using water:Tetrahydrofuran=1:Outside 1 water and the double solvents of tetrahydrofuran, according to reality
Apply the method described in example 27 and obtain solid product and liquid product, wherein, the solid product
Quality is 7.70g.Then, liquid product is carried out under 0.1MPa and 0.001MPa respectively normal
Vacuum distillation, obtains the double solvents of organic matter extract and water and tetrahydrofuran.To what is obtained
The double solvents of water and tetrahydrofuran is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 23.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.90.
Comparative example 1
10g coal directly-liquefied residues are mixed in the following way with methanol：Will be direct from coal
The coal directly-liquefied residue discharged at liquefied residue outlet and methanol in mass ratio 1:15 are mixed
Slurry mixture, it is that 12MPa, temperature are that the slurry mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 8.90g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Methanol.Obtained methanol is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 11.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.13.
Comparative example 2
10g coal directly-liquefied residues are mixed in the following way with ethanol：Will be direct from coal
The coal directly-liquefied residue discharged at liquefied residue outlet and ethanol in mass ratio 1:15 are mixed
Slurry mixture, it is that 12MPa, temperature are that the slurry mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 9.00g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Ethanol.Obtained ethanol is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.09.
Comparative example 3
10g coal directly-liquefied residues are mixed in the following way with ethylene glycol：Will be straight from coal
Connect the coal directly-liquefied residue and ethylene glycol in mass ratio 1 discharged at liquefied residue outlet:15 mixing
Slurry mixture is made, the slurry mixture is transported to for 12MPa, temperature by pressure by pump
For in 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 8.80g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Ethylene glycol.Obtained ethylene glycol is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 10.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.05.
Comparative example 4
10g coal directly-liquefied residues are mixed in the following way with ether：Will be direct from coal
The coal directly-liquefied residue discharged at liquefied residue outlet and ether in mass ratio 1:15 are mixed
Slurry mixture, it is that 12MPa, temperature are that the slurry mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 8.90g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Ether.Obtained ether is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 11.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 1.03.
Comparative example 5
10g coal directly-liquefied residues are mixed in the following way with acetone：Will be direct from coal
The coal directly-liquefied residue discharged at liquefied residue outlet and acetone in mass ratio 1:15 are mixed
Slurry mixture, it is that 12MPa, temperature are that the slurry mixture is transported into pressure by pump
In 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 8.00g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Ether.Obtained acetone is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 20.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.89.
Comparative example 6
10g coal directly-liquefied residues are mixed in the following way with tetrahydrofuran：Will be from coal
The coal directly-liquefied residue discharged at direct liquefaction sludge discharge tube and tetrahydrofuran in mass ratio 1:15
Be mixed and made into slurry mixture, by pump by the slurry mixture be transported to pressure for 12MPa,
Temperature is in 300 DEG C of high-temperature high-voltage reaction system.
Then, above-mentioned slurry mixture is heated to 300 DEG C under 12MPa, and mixture is existed
2h is reacted at this temperature, obtains reactant.Then, reactant is filtered, obtains solid phase production
Thing and liquid product, wherein, the quality of the solid product is 7.00g.Then, by liquid product
Atmospheric and vacuum distillation is carried out under 0.1MPa and 0.001MPa respectively, obtain organic matter extract and
Tetrahydrofuran.Obtained tetrahydrofuran is reclaimed and recycled.
Wherein, the extract content of the organic matter extract is 30.0%.Also, the organic matter is extracted
Thing is organic hydrocarbon mixture, mainly contains the elements such as C, H, N, S and O, H/C ratios therein
For 0.82.
Can be with by the comparative result of above-described embodiment 12- embodiments 29 and comparative example 1- comparative examples 6
Find out, compared with the extracting carried out only with organic solvent to coal directly-liquefied residue, the present invention is logical
Cross and coal directly-liquefied residue is stripped using the double solvents of water and organic solvent, substantially subtracting
(so as to reduce the dirt that organic solvent is brought to environment in the case of few consumption of organic solvent
Dye), additionally it is possible to obtain and only with organic matter extract content during organic solvent relatively.
In addition, the record of 1- embodiments 11 is understood according to embodiments of the present invention, side of the present invention
Method can also be further in the case where not using organic solvent completely, and realizes residual to DCL/Direct coal liquefaction
Effective extracting of organic matter in slag (extract content reaches more than 3.0%).
Also, the organic matter extract obtained by above-described embodiment 1- embodiments 29 is the direct liquid of coal
Change residue in light components (light components be organic hydrocarbon mixture, mainly comprising C, H,
N, S and O element).Wherein, the organic matter extracting obtained in above-described embodiment 1- embodiments 29
The H/C of thing has reached more than 0.85, it is clear that higher than the coal directly-liquefied residue known as raw material
In corresponding H/C ratios (average out to 0.74).
As can be seen here, method of the present invention is by using the compound molten of water or water and organic solvent
Agent is stripped to coal directly-liquefied residue, can not only reduce production cost, realize it is environment-friendly
Effective extracting, but also the separating treatment journey between subsequent extraction thing and extraction solvent can be simplified
Sequence.Meanwhile, the present invention, which extracts obtained organic matter extract, has higher H/C ratios, because
This, advantageously in subsequent treatment, and thus easily production obtains the liquid constituted closer to crude oil
Change product.
Claims (10)
1. a kind of method of the organic matter in use solvent extraction coal directly-liquefied residue, its feature exists
In the described method comprises the following steps：
(1) by the coal directly-liquefied residue and the solvent in mass ratio 1:(1-50) is mixed,
Obtain mixture；
(2) mixture obtained in the step (1) is heated to temperature for more than 250 DEG C, and
The mixture is reacted at said temperatures, obtain reactant；
(3) reactant in the step (2) is filtered, obtains solid product and liquid phase
Product；
(4) liquid product is subjected to atmospheric and vacuum distillation, obtains organic matter extract and described molten
Agent；
(5) solvent is reclaimed and recycled；
Wherein, the solvent is selected from the double solvents of water or water and organic solvent.
2. according to the method described in claim 1, it is characterised in that in the step (1),
By the coal directly-liquefied residue and the solvent in mass ratio 1:(10-50) is mixed.
3. method according to claim 1 or 2, it is characterised in that in the step (1)
In, the coal directly-liquefied residue is mixed in the following way with the solvent：It is straight in coal
Connection high-temperature high-voltage reaction system at liquefied residue outlet is connect, coal directly-liquefied residue is drained into
Temperature in the high-temperature high-voltage reaction system that pressure is more than 4MPa is more than 250 DEG C of institute
State in solvent.
4. method according to claim 1 or 2, it is characterised in that in the step (1)
In, the coal directly-liquefied residue is mixed in the following way with the solvent：Will be from coal
The coal directly-liquefied residue discharged at direct liquefaction sludge discharge tube is mixed and made into slurry with the solvent
Mixture, it is that more than 4MPa, temperature are that the slurry mixture is transported into pressure by pump
In more than 250 DEG C of high-temperature high-voltage reaction system.
5. according to the method described in claim 1, it is characterised in that the organic solvent is alcohols
Solvent, ether solvent, ketones solvent, furans solvent or their mixture.
6. the method according to any one of claim 1-5, it is characterised in that the solvent
For water and the double solvents of organic solvent, wherein, water and the organic solvent in mass ratio 1:(it is more than
0-1) mixed.
7. the method according to any one of claim 1-6, it is characterised in that in the step
Suddenly in (2), the mixture obtained in the step (1) is heated under 4MPa-30MPa.
8. the method according to any one of claim 1-7, it is characterised in that in the step
Suddenly in (2), the mixture reaction is more than 0h and less than or equal to 5h.
9. the method according to any one of claim 1-8, it is characterised in that in the step
Suddenly in (4), by the liquid product respectively in 0.08MPa-0.16MPa and 0.001MPa-0.019
Atmospheric and vacuum distillation is carried out under MPa.
10. the method according to any one of claim 1-9 extracts obtained organic matter extracting
Thing.
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| CN110129082A (en) * | 2019-04-12 | 2019-08-16 | 北京中科诚毅科技发展有限公司 | It is a kind of to prepare pitch technique using putty slag |
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Address after: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Zhongke synthetic oil Technology Co.,Ltd. Address before: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: SYNFUELS CHINA TECHNOLOGY Co.,Ltd. |