CN101624532B - Method for hydrogenating and liquefying coal with high content of inert components - Google Patents

Method for hydrogenating and liquefying coal with high content of inert components Download PDF

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CN101624532B
CN101624532B CN 200910113414 CN200910113414A CN101624532B CN 101624532 B CN101624532 B CN 101624532B CN 200910113414 CN200910113414 CN 200910113414 CN 200910113414 A CN200910113414 A CN 200910113414A CN 101624532 B CN101624532 B CN 101624532B
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swelling
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马凤云
郭靖
周岐雄
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Xinjiang University
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Abstract

The invention relates to a method for hydrogenating and liquefying coal with high content of inert components, comprising the steps of swelling treatment, hydrogenation and liquefaction reaction as well as solid-liquid separation. The invention has the advantages that under the conditions of higher content of inert components, lower content of hydrogen and carbon elements and lower content of volatiles in Wucaiwan coal with consideration to the liquefaction cost, the oil yield of hydrogenation liquefaction of the Wucaiwan coal is obviously improved, thereby changing the current well-known view that only low liquefaction rate of coal can be obtained when the coal has high content of inert components and low content of hydrogen and carbon elements and volatiles.

Description

The hydrogenation liquefaction method of high-content inertinite part coal
Technical field
The present invention relates to the technical field of DCL/Direct coal liquefaction, is a kind of hydrogenation liquefaction method of high-content inertinite part coal.
Background technology
The Xinjiang Coal resource is very abundant, and its prognostic reserves reach 2.19 trillion tons, surpasses 40% of national total amount.
Five colours gulf coal is positioned at area, accurate east, is first of the large coal electricity Coal Chemical Base of Xinjiang five, just will build up maximum in the world open coal mine.The characteristics such as this mining area coal has that the coal seam number of plies is many, thickness is large, it is shallow to bury, high-moisture, low ash and low-sulfur.The coal analysis of five colours gulf coal is in Table 1.Its Coal Characteristics can be summarized as " three height ", i.e. high inertinite content, high-moisture, high oxidation calcium; " three is low ", i.e. low hydrogen carbon element ratio, low ash and low-sulfur.Five colours gulf coal hydrogen carbon element, than low, illustrate in coal and contains more aromatic structure; The inertinite optimal reaction temperature is more than 450 ℃, and the inertinite volume percent content of multicolored gulf coal is 75% to 85%, is the liquefaction effect obtained, and the temperature of reacting required is just high; Five colours gulf coal fugitive constituent is 32.57%, and hydrogen carbon element ratio is 0.59.The fugitive constituent of coal and hydrogen carbon element are than larger (oil hydrogen charcoal ratio is 1.5 to 1.6), and ature of coal is better, more is easy to hydrogenation liquefaction, and according to grade of coal national standard (GB5751-86), multicolored gulf coal belongs to the bituminous coal that degree of coalification is higher.
The characteristics of coal direct liquefaction need the high pressure-temperature condition exactly.Therefore, to equipment performance and processing condition, require harsh.Therefore, at oily productive rate under high as far as possible prerequisite, further gentle liquefaction reaction condition and to reduce costs be the focus of gelatin liquefaction research always.
The swelling mechanism of coal, its theoretical basis is the coal macromolecule two phase model.This model thinks, the structure of coal can be regarded as by the small molecules embedded between three-dimensional cross-linked cancellated macromole and network and be formed.Exist the interaction of hydrogen bond, charge transfer or Van der Waals force etc. between the two.Coal is light year by year, and internetwork small molecules the more.The molecular structure characteristics of coal are both to have had hydrogen supply capacity, have again the Hydrogen Energy of being subject to power.Therefore, nucleophilic or close electric solvent can rupture hydrogen bond between the two of molecular structure of coal and weak chemical bond, reduce its degree of crosslinking, and it is fully stretched.From the eighties in last century, by swelling equilibrium theoretical investigation coal macromolecule cross-link bond structure in polymer Neo-Confucianism.With polar organic solvent, coal is processed, can destroy crosslinked hydrogen bond in molecular structure of coal, change the chemical structure of coal, reduce the associative structure of free energy, improve the chemical reactivity of coal, can higher oily productive rate and transformation efficiency arranged than direct liquefaction under mild conditions.
At present, have and in a large number the swelling coal is carried out to the research of direct liquefaction.The coal analysis of different coals, in Table 1, for the hydrogen carbon element ratio of coal, only has multicolored gulf coal less than 0.6, and other coals are all between 0.7 to 0.8; And for fugitive constituent, except the coal of Mei He South Africa, multicolored gulf all 37% to 46%.Hydrogen carbon element ratio and the fugitive constituent of coal are higher, more are easy to liquefaction.Therefore, with regard to liquidation of coal, prosperous coal and northern place coal are the most liquescent, and multicolored gulf coal is the most difficult liquefaction.
In table 3:
F.Pinto [1]etc (Pinto F, GulyurtluI, Lobo LS et al.Effect of coal pre-treatmentwith swelling solvents on coal liquefaction[J] (impact of swelling pretreatment on gelatin liquefaction) .fuel, 1999,78:629-634 discloses with tetrahydrofuran (THF) swelling South Africa coal, hydrogenation liquefaction under hydrogen first pressing 7.9MPa (measuring under normal temperature), 400 ℃ of liquefaction temperatures and reaction times 30min condition, oily productive rate reaches 27% by original 24%.On the one hand, although South Africa coal hydrogen carbon element higher be 0.71, under above-mentioned reaction conditions, oily productive rate is lower; On the other hand, with liquefaction oil productive rate after tetrahydrofuran (THF) swelling coal, only improve 3 percentage points, the swelling effect is not remarkable.
Haoquan Hu [2](Hu Haoquan (Hu Haoquan), Sha Guangyan, Chen Guohua.Effect of solventswelling on liquefaction of Xinglong coal at less severe conditions[J] (impact of swelling treatment on prosperous gelatin liquefaction under mild conditions) .fuel, 2000, 68:33-43 discloses and has used respectively tetrahydrofuran (THF) and the prosperous coal of pyridine swelling, at molten coal than 2: 1 (quality of naphthane and the mass ratio of coal), hydrogen first pressing 4MPa (measuring under normal temperature), hydrogenation liquefaction under 350 ℃ of liquefaction temperatures and reaction times 30min condition, transformation efficiency is by original 20%, reach respectively 29% and 28%, 9 and 8 percentage points have been improved.The fugitive constituent of prosperous coal is 40.72%, and hydrogen charcoal ratio is 0.78, belongs to the high-quality coal that is easy to liquefaction.But, because liquefaction temperature is low, prosperous coal transformation efficiency is only 20%, with prosperous coal transformation efficiency after tetrahydrofuran (THF) and pyridine swelling,<30%, the swelling effect is still not remarkable yet.
Hengfu Shui [3]etc (Shui Hengfu, Wang Zhicai, Cao Meixia.Effect ofpre-treatment of coal on its solvent extraction and liquefaction properties[J] (impact of swelling pretreatment on solvent extraction and Performance of Hydrogenation Liquefaction of Coal) .fuel, 2008.04.28:1-6 disclose and used respectively tetrahydrofuran (THF) and N-Methyl pyrrolidone swelling Firing Shenhua Coal, at molten coal than 3: 1 (quality of naphthane and the mass ratio of coal), hydrogen first pressing 4MPa (measuring under normal temperature), hydrogenation liquefaction under 400 ℃ of liquefaction temperatures and reaction times 30min condition, hydrocarbon yield is by original 21%, reach respectively 24% and 18%, improved respectively 3 and reduced by 3 percentage points.Now, swelling is not obvious to the Firing Shenhua Coal action effect, and the N-Methyl pyrrolidone solvent is by negative effect, and hydrocarbon yield has reduced before than swelling on the contrary.
Ni Xianzhi [4]deng (Ni Xianzhi, Wang Li, Chen Lihui etc. the research [J] of Young Coal solvent-swollen back end hydrogenation liquefaction performance. University Of Science and Technology Of Shandong's journal, 2003,22 (3): 97-100 discloses the coal with pyridine swelling Sun Cun, molten coal than 1.5 to 2: 1 (quality of naphthane and the mass ratio of coal), hydrogen first pressing 10MPa (measuring under normal temperature), 400 ℃ of liquefaction temperatures and reaction times 60min condition under hydrogenation liquefaction, oily productive rate reaches 40% by original 18%, improves 22 percentage points.With pyridine swelling north place coal [6] (Ni Xianzhi, Wang Li, Chen Lihui etc. Swelled With Solvent Under The Radiation of Ultrasonic Wave improves the research [J] of Performance of Hydrogenation Liquefaction of Coal. coal conversion, 2003,26 (4): 37-41 disclose molten coal than 7: 1 (quality of naphthane and the mass ratio of coal), hydrogen first pressing (7MPa to 8MPa) (measuring under normal temperature), 400 ℃ of liquefaction temperatures and reaction times 90min condition under, the oil productive rate reaches 70% by original 57%, has improved 13 percentage points.Two kinds of swelling coals, although oily productive rate has improved the first pressing of 10 percentage points of ,Dan Sun village gelatin liquefaction hydrogen up to 10MPa (measuring under normal temperature) before with respect to swelling, high like this pressure, make the final pressure of its liquefaction reaction higher, cause the material of conversion unit to be required high, cost is corresponding uprises in liquefaction; Large (molten coal was than 7: 1) (quality of naphthane and mass ratio of coal) of quantity of solvent that place, north coal not only used, and the reaction times of liquefaction is long.
Hou Yuchi [6]deng (Hou Yuchi, Lu Jichang, Malaysian's treasured. swelling is on deifying the impact [J] of texture of coal and liquefaction performance. Liaoning chemical industry, 2008,37 (6): 381-384 discloses by pyridine swelling Firing Shenhua Coal, molten coal than 3: 1 (quality of naphthane and the mass ratio of coal), hydrogen first pressing 7MPa (measuring under normal temperature), 420 ℃ of liquefaction temperatures and reaction times 60min condition under hydrogenation liquefaction, hydrocarbon yield (oily gentle productive rate and) reaches 62% by original 45%, improves 17 percentage points.On the one hand Firing Shenhua Coal is one of good coal of 14 kinds of liquefaction properties filtering out of Coal Mining Research Institute; Quantity of solvent used large (molten coal was than 3: 1) on the other hand.This two aspect cost that makes to liquefy is high.
Summary of the invention
The invention provides a kind of hydrogenation liquefaction method of high-content inertinite part coal, it has overcome the deficiency of prior art, solve the problem of the more difficult liquefaction of multicolored gulf coal, specifically solved multicolored gulf coal because inertinite content is higher, the hydrogen carbon element is lower, the lower problem that productive rate (comprising oily productive rate, hydrocarbon yield, transformation efficiency) is lower, cost is higher that liquefies that causes of fugitive constituent.
Technical scheme of the present invention is achieved like this: a kind of hydrogenation liquefaction method of high-content inertinite part coal, and it carries out in the steps below:
The first step swelling treatment: by N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) mixed solution with the ratio of multicolored gulf coal with 2 to 10: 1, mix while stirring, the standing swelling of room temperature lower seal 0.5 hour to 24 hours, vacuum filtration also will obtain the swelling coal after filter residue and drying; Wherein, N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) take volume ratio as 1 to 2: 0 to 1: 1 formation mixed solution, the ratio unit of above-mentioned mixed solution and multicolored gulf coal is ml/g;
Second step hydrogenation liquefaction reaction: above-mentioned swelling coal, catalyzer ferric oxide, promotor elemental sulfur and the hydrogen supply dissolvent naphthane of requirement are mixed and pour reactor into by four, sealed reactor to after being replaced with hydrogen in still, be charged at normal temperatures 5MPa to 7MPa, control 4 ℃ of heat-up rates/min to 5 ℃/min, constant temperature 30min to 60min after being 400 ℃ to 460 ℃ to temperature of reaction, then reactor is forced rapidly to be cooled in 200 ℃ in 15min at 10min, be cooled to again room temperature, obtain reaction product; Wherein, above-mentioned swelling coal 20 weight parts, catalyzer ferric oxide 0.57 weight part to 1.43 weight part, promotor elemental sulfur 0.46 weight part to 1.15 weight part, the mass ratio of hydrogen supply dissolvent naphthane and swelling coal is 1.5 to 2: 1 (instant coal ratio);
The 3rd step solid-liquid separation: the solid, liquid phase product of reaction product is carried out respectively to extracting with normal hexane, toluene and tetrahydrofuran solvent by Soxhlet extractor successively, (during by the Soxhlet extractor extracting: the normal hexane solvend is defined as liquefaction oil to obtain respectively successively liquefaction oil, asphaltene, preasphaltene and liquefied residue, the insoluble toluene solvend of normal hexane is defined as asphaltene, toluene insoluble tetrahydrofuran (THF) solvend is defined as preasphaltene, and tetrahydrofuran insoluble is defined as liquefied residue).
Below further optimization and/or the selection to technique scheme:
In above-mentioned the first step swelling treatment, the vacuum-drying of gained filter residue obtains the swelling coal in 12 hours.
In above-mentioned the first step swelling treatment, the gained filter residue first rinses with 5 ml distilled waters with 5 milliliters of dehydrated alcohols and every gram coal with every gram coal, then vacuum-drying obtains the swelling coal in 12 hours.
In above-mentioned the 3rd step solid-liquid separation, the extracting time is respectively with normal hexane extracting 48 hours, with toluene extracting 48 hours with tetrahydrofuran (THF) extracting 24 hours.
In the reaction of above-mentioned second step hydrogenation liquefaction, sealed reactor to the hydrogen exchange that is 99.99% by purity in still 3 to 5 times.
In above-mentioned second step hydrogenation liquefaction reaction, in reactor, stirring velocity is 300rad/min to 350rad/min.
The technology of the present invention effect: in the situation that take into account the liquefaction cost, inertinite content at multicolored gulf coal is higher, the hydrogen carbon element is lower, fugitive constituent hangs down in situation, the oily productive rate of multicolored gulf Coal Liquefaction is significantly improved, thereby change at present generally acknowledged viewpoint: when the inertinite content of coal is high and the hydrogen carbon element than and fugitive constituent while all hanging down, can only obtain the low liquefied fraction of coal.
Embodiment
Embodiment 1: the hydrogenation liquefaction method of this high-content inertinite part coal carries out in the steps below:
The first step swelling treatment: by N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) mixed solution with the ratio of multicolored gulf coal with 2: 1, mix while stirring, the standing swelling of room temperature lower seal 0.5 hour, vacuum filtration also will obtain the swelling coal after filter residue and drying; Wherein, N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) take volume ratio as 1: 0: 1 formation mixed solution, the ratio unit of above-mentioned mixed solution and multicolored gulf coal is ml/g;
Second step hydrogenation liquefaction reaction: above-mentioned swelling coal, catalyzer ferric oxide, promotor elemental sulfur and the hydrogen supply dissolvent naphthane of requirement are mixed and pour reactor into by four, sealed reactor to after being replaced with hydrogen in still, be charged at normal temperatures 5MPa MPa, control 4 ℃/min of heat-up rate, constant temperature 30min after being 400 ℃ to temperature of reaction, then reactor is forced rapidly in 10min to be cooled in 200 ℃, then be cooled to room temperature, obtain reaction product; Wherein, above-mentioned swelling coal 20 weight parts, catalyzer ferric oxide 0.57 weight part, promotor elemental sulfur 0.46 weight part, the mass ratio of hydrogen supply dissolvent naphthane and swelling coal is 1.5: 1;
The 3rd step solid-liquid separation: the solid, liquid phase product of reaction product is carried out respectively to extracting with normal hexane, toluene and tetrahydrofuran solvent by Soxhlet extractor successively, obtain respectively successively liquefaction oil, asphaltene, preasphaltene and liquefied residue.
Embodiment 2: the hydrogenation liquefaction method of this high-content inertinite part coal is characterized in that carrying out in the steps below:
The first step swelling treatment: by N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) mixed solution with the ratio of multicolored gulf coal with 10: 1, mix while stirring, the standing swelling of room temperature lower seal 24 hours, vacuum filtration also will obtain the swelling coal after filter residue and drying; Wherein, N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) take volume ratio as 2: 0 to 1: 1 formation mixed solutions, the ratio unit of above-mentioned mixed solution and multicolored gulf coal is ml/g;
Second step hydrogenation liquefaction reaction: above-mentioned swelling coal, catalyzer ferric oxide, promotor elemental sulfur and the hydrogen supply dissolvent naphthane of requirement are mixed and pour reactor into by four, sealed reactor to after being replaced with hydrogen in still, be charged at normal temperatures 7MPa, control 5 ℃/min of heat-up rate, constant temperature 60min after being 460 ℃ to temperature of reaction, then reactor is forced rapidly in 15min to be cooled in 200 ℃, then be cooled to room temperature, obtain reaction product; Wherein, above-mentioned swelling coal 20 weight parts, catalyzer ferric oxide 1.43 weight parts, promotor elemental sulfur 1.15 weight parts, the mass ratio of hydrogen supply dissolvent naphthane and swelling coal is 2: 1;
The 3rd step solid-liquid separation: the solid, liquid phase product of reaction product is carried out respectively to extracting with normal hexane, toluene and tetrahydrofuran solvent by Soxhlet extractor successively, obtain respectively successively liquefaction oil, asphaltene, preasphaltene and liquefied residue.
Embodiment 3: the hydrogenation liquefaction method of this high-content inertinite part coal carries out in the steps below:
The first step swelling treatment: by N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) mixed solution with the ratio of multicolored gulf coal with 2 to 10: 1, mix while stirring, the standing swelling of room temperature lower seal 0.5 hour to 24 hours, vacuum filtration also will obtain the swelling coal after filter residue and drying; Wherein, N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) take volume ratio as 1 to 2: 0 to 1: 1 formation mixed solution, the ratio unit of above-mentioned mixed solution and multicolored gulf coal is ml/g;
Second step hydrogenation liquefaction reaction: above-mentioned swelling coal, catalyzer ferric oxide, promotor elemental sulfur and the hydrogen supply dissolvent naphthane of requirement are mixed and pour reactor into by four, sealed reactor to after being replaced with hydrogen in still, be charged at normal temperatures 5MPa to 7MPa, control 4 ℃ of heat-up rates/min to 5 ℃/min, constant temperature 30min to 60min after being 400 ℃ to 460 ℃ to temperature of reaction, then reactor is forced rapidly to be cooled in 200 ℃ in 15min at 10min, be cooled to again room temperature, obtain reaction product; Wherein, above-mentioned swelling coal 20 weight parts, catalyzer ferric oxide 0.57 weight part to 1.43 weight part, promotor elemental sulfur 0.46 weight part to 1.15 weight part, the mass ratio of hydrogen supply dissolvent naphthane and swelling coal is 1.5 to 2: 1;
The 3rd step solid-liquid separation: the solid, liquid phase product of reaction product is carried out respectively to extracting with normal hexane, toluene and tetrahydrofuran solvent by Soxhlet extractor successively, obtain respectively successively liquefaction oil, asphaltene, preasphaltene and liquefied residue.
Below the hydrogenation liquefaction method of above-mentioned high-content inertinite part coal is done further optimize or select:
In the first step swelling treatment: the vacuum-drying of gained filter residue obtains the swelling coal in 12 hours; Perhaps, in the first step swelling treatment, the gained filter residue first rinses with 5 ml distilled waters with 5 milliliters of dehydrated alcohols and every gram coal with every gram coal, then vacuum-drying obtains the swelling coal in 12 hours.
In the 3rd step solid-liquid separation, the extracting time is respectively with normal hexane extracting 48 hours, with toluene extracting 48 hours with tetrahydrofuran (THF) extracting 24 hours.
In second step hydrogenation liquefaction reaction, sealed reactor to the hydrogen exchange that is 99.99% by purity in still 3 to 5 times.
In the reaction of second step hydrogenation liquefaction, in reactor, stirring velocity is 300rad/min to 350rad/min.
The test result contrast of the present invention and prior art is as follows:
1. pass through coal analysis, five colours gulf coal inertinite volume percent content is 75% to 85%, and hydrogen carbon element ratio<0.6 and fugitive constituent<37% belongs to the coal of more difficult liquefaction, but still can, considerably beyond the effect of high-quality coal liquefaction, refer to table 3 by swelling treatment.
2. in the lower liquefaction of low first pressing 5MPa to 7MPa (measuring under normal temperature), hydrogen usage is low on the one hand, and consumption only has 5% (volume percent) left and right; React on the other hand final pressure low (13MPa to 17MPa) (measuring) under 400 ℃ to 460 ℃ of temperature of reaction.Reduce the liquefaction cost from above-mentioned two aspects.
3. use N-Methyl pyrrolidone (NMP), DMF (DMF) and dithiocarbonic anhydride (CS 2) [V 1: V 2: V 3=(1 to 2): (0 to 1): 1] liquefaction effect obviously strengthens after the coal of swelling five colours gulf, show as molten coal than 1.5 to 2: 1, low hydrogen first pressing 5 to 7MPa (measuring under normal temperature), 460 ℃ of temperature of reaction and reaction times 30min to 60min condition under hydrogenation liquefaction, the oil productive rate changes into 70% to 75% by 55% original raising, has improved 5 to 20 percentage points; Hydrocarbon yield rises to 73% to 75% by 65%, has improved 8 to 10 percentage points; Transformation efficiency rises to 80% to 85% by 77%, has improved 3 to 8 percentage points, refers to table 2 and table 4.
4. changing generally acknowledged inertinite volume percent content at present is 75% to 85%, and the hydrogen carbon element than and fugitive constituent while all hanging down, can only obtain the viewpoint of low liquefied fraction.
Figure G2009101134144D00062
Figure G2009101134144D00071
Figure G2009101134144D00081

Claims (1)

1. the hydrogenation liquefaction method of high-content inertinite part five colours gulf coal is characterized in that carrying out in the steps below:
The first step swelling treatment: by N-Methyl pyrrolidone, N, the mixed solution of dinethylformamide and dithiocarbonic anhydride and multicolored gulf coal mix while stirring with 2 to 10:1 ratio, the standing swelling of room temperature lower seal 0.5 hour to 24 hours, vacuum filtration also will obtain the swelling coal after filter residue and drying; Wherein, N-Methyl pyrrolidone, DMF and dithiocarbonic anhydride be take volume ratio and are formed mixed solution as 1 to 2:0 to 1:1, and the ratio unit of above-mentioned mixed solution and multicolored gulf coal is ml/g;
Second step hydrogenation liquefaction reaction: above-mentioned swelling coal, catalyzer ferric oxide, promotor elemental sulfur and the hydrogen supply dissolvent naphthane of requirement are mixed and pour reactor into by four, sealed reactor to after being replaced with hydrogen in still, be charged at normal temperatures 5 MPa to 7 MPa, control 4 ℃ of heat-up rates/min to 5 ℃/min, constant temperature 30 min to 60min after being 400 ℃ to 460 ℃ to temperature of reaction, then reactor is forced rapidly to be cooled in 200 ℃ in 15min at 10min, be cooled to again room temperature, obtain reaction product; Wherein, above-mentioned swelling coal 20 weight parts, catalyzer ferric oxide 0.57 weight part to 1.43 weight part, promotor elemental sulfur 0.46 weight part to 1.15 weight part, the mass ratio of hydrogen supply dissolvent naphthane and swelling coal is 1.5 to 2:1;
The 3rd step solid-liquid separation: the solid, liquid phase product of reaction product is carried out respectively to extracting with normal hexane, toluene and tetrahydrofuran solvent by Soxhlet extractor successively, obtain respectively successively liquefaction oil, asphaltene, preasphaltene and liquefied residue;
Wherein:
In the first step swelling treatment, the gained filter residue first rinses with 5 ml distilled waters with 5 milliliters of dehydrated alcohols and every gram coal by every gram coal, then vacuum-drying obtains the swelling coal in 12 hours;
In the 3rd step solid-liquid separation, the extracting time is respectively with normal hexane extracting 48 hours, with toluene extracting 48 hours with tetrahydrofuran (THF) extracting 24 hours;
In second step hydrogenation liquefaction reaction, sealed reactor to the hydrogen exchange that is 99.99% by purity in still 3 to 5 times;
In the reaction of second step hydrogenation liquefaction, in reactor, stirring velocity is 300rad/min to 350rad/min.
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