CN109536190B - Method for separating liquefiable and non-liquefiable components from coal inert matter microscopic components - Google Patents

Method for separating liquefiable and non-liquefiable components from coal inert matter microscopic components Download PDF

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CN109536190B
CN109536190B CN201910022990.1A CN201910022990A CN109536190B CN 109536190 B CN109536190 B CN 109536190B CN 201910022990 A CN201910022990 A CN 201910022990A CN 109536190 B CN109536190 B CN 109536190B
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蔺华林
王叶函
叶伟林
连俊
韩生
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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
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    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
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Abstract

The invention discloses a method for separating liquefiable and non-liquefiable components from inert component micro-components of coal. The method comprises the following specific steps: firstly, selecting coal with dark grey black and color by naked eyes from a coal sample, wherein the content of inert components in the coal is relatively enriched; then, carrying out a floating-sinking experiment on the inerter group, and collecting 1.35-1.50 g/cm3Coal samples between densities were subjected to liquefaction experiments and it was found from the liquefaction data that both liquefiable and non-liquefiable portions of the inertinite group could be defined. The method can promote the separation of the coal inert micro-components and improve the content of the liquefiable part of the coal inert micro-components, and has practical industrial and application values.

Description

Method for separating liquefiable and non-liquefiable components from coal inert matter microscopic components
Technical Field
The invention particularly relates to a separation method for liquefiable and non-liquefiable coal in inert matter micro-components, and belongs to the technical field of separation of coal and the micro-components thereof.
Background
The coal resource reserves of China are the second place in the world, coal is also the main energy of China, and will not change for a long time in the future, so holding the properties of coal, fully researching the composition structure of coal is a very key foundation, the structure and composition of coal directly determine the properties of coal, and all coal conversions are inevitably related to the change of the composition structure of coal. The coal is a complex mixture composed of organic microscopic components with different properties and a small amount of inorganic mineral substances, and the organic microscopic components can be divided into a microscopic component, an inert component and a chitin component according to the optical properties of the coal. The inert group can be divided into mitoplasts, hemimitoplasts, fungi, secretes, mitochondria, microsomes, and clastic inert bodies. Although China has abundant coal resources, the coal reserves with high content of inert components are abundant, which seriously restricts the development of coal cleaning technology.
The direct coal liquefaction technology is a deep conversion process for removing heteroatoms such as oxygen, nitrogen, sulfur and the like in coal through a series of hydrogenation reactions under certain pressure, catalyst and temperature conditions to generate liquid gas hydrocarbon and hydrocarbon, and is an important means for realizing clean utilization of coal. Generally, vitrinite and chitinous group in coal macerals are liquefied active components, vitrinite and chitinous group in three components of inertinite and chitinous group are "active components" in coal macerals, play an important role in the coal liquefaction conversion process and oil yield, and directly determine the conversion rate and oil yield of coal, and inertinite is inert in the coal liquefaction process and difficult to liquefy, and the increase of the content thereof can cause adverse effects on the liquefied oil yield. However, direct liquefaction tests on some high-inertinite raw coals indicate that high-inertinite raw coals may also have better liquefied oil yields and coal conversions. The premise of researching the components forming the inertinite group and exploring the influence of the components on the direct coal liquefaction is to separate and enrich the components forming the inertinite group. Abundant coal resources in China are fully utilized, the situation that alternative liquid fuel is needed in a certain period of the future can be predicted along with the gradual reduction of oil reserves, and due to the global coal reserves and the abundance of the coal reserves, coal liquefaction can be used as one of alternative liquid fuel sources.
Disclosure of Invention
The invention aims to provide a method for separating liquefiable and non-liquefiable components from inert component micro-components of coal. The present invention divides the micro-constituents of coal inerts into two parts, liquefiable and non-liquefiable, by density definition. According to the invention, more intensive and careful research work is carried out on the basic research of the coal inert group and the liquefaction reaction mechanism, and the separation and enrichment of coal rock components are carried out by utilizing heavy liquid separation so as to further reveal the liquefaction performance of the inert group.
The technical scheme of the invention is realized in such a way.
A method for separating liquefiable and non-liquefiable components in inert component microscopic components of coal comprises the following steps:
(1) selecting a coal sample which is grey black and dark in color by hand;
(2) crushing the hand-selected coal sample, and screening and collecting the inert-rich group particles with smaller particle size;
(3) grinding the inert group enrichment to prepare coal powder, performing chemical deashing treatment, and crushing by using a rod mill to obtain a coal powder sample;
(4) taking a plurality of coal powder samples for a sink-float centrifugal experiment, wherein each coal powder sample is 20-30 g, and the density range of the specific gravity liquid is 1.35-1.50 g/cm3And the density interval is set to be 0.02g/cm3The centrifugation time is 20-30 min, and the centrifugation rotating speed is 2000-3000 r/min; obtaining the distribution data condition of each density range of the coal powder sample and collecting the density of 1.35-1.50 g/cm3Coal samples of various density ranges in between;
(5) carrying out liquefaction experiments on the collected coal samples in each density range;
(6) on the basis of liquefaction data, when the yield of the liquefied product oil reaches more than 60%, considering that the liquefied product oil can be liquefied, defining a density boundary line between a liquefied part and a non-liquefiable part, and determining the density range of the liquefiable part;
(7) performing a floating and sinking centrifugation experiment on the coal powder sample obtained in the step (3), and collecting the coal powder sample with the density of 1.35-1.43 g/cm3To obtain the liquefiable components of the inert component.
In the invention, in the step (2), a jaw crusher is used for crushing the coal sample to 0.5-3 mm, and the inert-rich particles with smaller particle size are screened and collected.
In the present invention, in the step (3), the chemical deashing treatment method is as follows: respectively carrying out acid pickling treatment twice by using hydrochloric acid and hydrofluoric acid under an inert atmosphere, filtering after each acid pickling, and washing a coal sample by using warm water; and finally, vacuum drying.
In the invention, in the step (3), the granularity of the pulverized coal sample crushed by the rod mill is 0.15-0.20 mm.
In the invention, in the step (4), the specific gravity liquid is subjected to centrifugal floating and sinking from low to high. The zinc chloride used for the experiment is used as a floating and sinking medium, and the density range of the prepared specific gravity liquid is 1.35-1.50 g/cm through calibration of a densimeter3And the density interval is set to be 0.02g/cm3。
In the invention, in the step (5), the liquefaction experimental conditions are as follows: weighing 20-30 g of collected inert group enriched coal powder samples of each density group, wherein the initial hydrogen pressure is 10.0MPa, adding a coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60-90 min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished.
In the invention, in the step (6), based on the liquefaction data, the density range is 1.35-1.50 g/cm3The pulverized coal sample is divided into two grades, 1.35-1.43 g/cm3And 1.44 to 1.50g/cm3。
In the invention, in the step (7), the sample obtained in the step (3) is subjected to a sink-float centrifugal experiment, and the collection density is 1.35-1.43 g/cm3To obtain the liquefiable components of the inert component.
Compared with the prior art, the invention has the beneficial effects that: the invention initiatively proposes and successfully divides the micro-components of the inert component into liquefiable components and non-liquefiable components, ensures that the inert component is not completely 'inert', draws a boundary line in the inert micro-components, can better utilize the liquefying performance of coal, has wide application prospect and market potential from the perspective of resource utilization and economy, and promotes the forward development of the coal liquefying technology.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
A method for separating liquefiable and non-liquefiable components in inert component microscopic components of coal specifically comprises the following steps:
(1) manually selecting a large willow tower coal sample to obtain a coal sample with the content of inert components of more than 80%;
(2) crushing the coal sample to 0.5-3 mm by using a jaw crusher, and screening and collecting inert-rich particles with smaller particle sizes;
(3) grinding the inert group enrichment to prepare coal powder, performing chemical deashing treatment, and crushing by using a rod mill to obtain a coal powder sample;
(4) performing centrifugal floating and sinking experiment on the coal powder sample, performing centrifugal floating and sinking experiment on the specific gravity liquid with a ratio from low to high, and obtaining and collecting a series of samples (1.35 g/cm) with density3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3，1.50g/cm3). The density of the specific gravity liquid is 1.35-1.50 g/cm3And the density interval is set to 0.02g/cm3And centrifuging for 30min at the rotating speed of 2500r/min, selecting 7g of an inertinite enriched coal powder sample, placing the inertinite enriched coal powder sample in 8 centrifuge tubes of 50ml for centrifugal test, standing the centrifuge tubes for 2h after the centrifugal test is finished at the rotating speed of 2500r/min, and finally washing and drying the products of the specific gravity components respectively, cooling and weighing. (surfactant Brij-35 is added into the specific gravity liquid according to actual requirements, because the coal powder has poor hydrophilicity, in order to avoid that the coal powder cannot be fully dissolved into the specific gravity liquid to cause that the expected separation effect cannot be achieved, the surfactant Brij-35 is added according to actual requirements);
(5) collecting a series of density range coal dust samples (1.35 g/cm)3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3，1.50g/cm3) Respectively carrying out liquefaction experiments, wherein the standard liquefaction experiment conditions are as follows: weighing 28g of collected inert group enriched coal powder samples of each density group, wherein the initial hydrogen pressure is 10.0MPa, adding a coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished;
(6) the liquefaction data results show a density of 1.35g/cm3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3The yield of the liquefied product oil is over 60 percent, and the density is 1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3The oil yield of the liquefied product is below 60 percent. Aiming at the inert micro-components (1.35-1.50 g/cm) in the big willow tower coal3) At 1.44g/cm3Dividing the separation line into liquefiable and non-liquefiable;
(7) performing a centrifugal floating and sinking experiment on a coal powder sample, performing the centrifugal floating and sinking experiment on a specific gravity liquid with a low-to-high ratio, and collecting 1.35-1.43 g/cm3And 1.44 to 1.50g/cm3Density range samples were subjected to liquefaction experiments. The standard experimental conditions for liquefaction were: weighing 28g of collected coal dust sample with the required density range enriched, wherein the initial hydrogen pressure is 10.0MPa, adding the coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished;
(8) the density of the obtained liquefied product is 1.35-1.43 g/cm3The yield of the liquefied product oil is 70%, the liquefied product oil is liquefiable, and the density is in a range of 1.44-1.50 g/cm3The yield of liquefied product oil of (2) was 34% and was not liquefiable. Specific results are shown in table 1.
TABLE 1 big willow tower coal sample
Figure BDA0001941458370000041
Example 2
A method for separating liquefiable and non-liquefiable components in inert component microscopic components of coal specifically comprises the following steps:
(1) manually selecting a coal sample of the connecting tower to obtain a coal sample with the content of inert components of more than 80%;
(2) crushing the coal sample to 0.5-3 mm by using a jaw crusher, and screening and collecting inert-rich particles with smaller particle sizes;
(3) grinding the inert group enrichment to prepare coal powder, performing chemical deashing treatment, and crushing by using a rod mill to obtain a coal powder sample;
(4) performing centrifugal floating and sinking experiment on the coal powder sample, performing centrifugal floating and sinking experiment on the specific gravity liquid with a ratio from low to high, and obtaining and collecting a series of samples (1.35 g/cm) with sample density3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3，1.50g/cm3). The density of the specific gravity liquid is 1.35-1.50 g/cm3And the density interval is set to 0.02g/cm3Centrifuging for 30min at 2500r/min, and selecting inert coalAnd 7g of powder sample is divided into 8 centrifugal tubes of 50ml for centrifugal test, the centrifugal time is 30min, the centrifugal speed is 2500r/min, the centrifugal tubes are kept stand for 2h after the centrifugal test is finished, and finally products of each specific gravity component are respectively washed, dried, cooled and weighed. (surfactant Brij-35 is added into the specific gravity liquid according to actual requirements, because the coal powder has poor hydrophilicity, in order to avoid that the coal powder cannot be fully dissolved into the specific gravity liquid to cause that the expected separation effect cannot be achieved, the surfactant Brij-35 is added according to actual requirements);
(5) collecting a series of density coal dust samples (1.35 g/cm)3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3，1.50g/cm3) Respectively carrying out liquefaction experiments, wherein the standard liquefaction experiment conditions are as follows: weighing 28g of collected inert group enriched coal powder samples of each density group, wherein the initial hydrogen pressure is 10.0MPa, adding a coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished;
(6) the liquefaction data results show a density of 1.35g/cm3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3The yield of the liquefied product oil is over 60 percent, and the density is 1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3The oil yield of the liquefied product is below 60 percent. Aiming at inert micro-components (1.35-1.50 g/cm) in coal of a make-up tower3) At 1.44g/cm3Dividing the separation line into liquefiable and non-liquefiable;
(7) performing a centrifugal floating and sinking experiment on a coal powder sample, performing the centrifugal floating and sinking experiment on a specific gravity liquid with a low-to-high ratio, and collecting 1.35-1.43 g/cm3And 1.44 to 1.50g/cm3Density range samples were subjected to liquefaction experiments. The standard experimental conditions for liquefaction were: weighing 28g of collected coal dust sample with required density range enrichment, adding the coal sample and a solvent according to the mass ratio of 1:1.5, and adding ferric oxide, wherein the initial hydrogen pressure is 10.0MPaCatalyzing, wherein the mass of the catalyst is 3% of that of the coal sample, S is used as a cocatalyst, the reaction temperature is kept constant for 60min after rising to a constant temperature section, and the temperature is cooled to 200 ℃ within 30min after the constant temperature is finished;
(8) the density of the obtained liquefied product is 1.35-1.43 g/cm3The yield of the liquefied product oil is 75 percent and is liquefiable, and the density ranges from 1.44 to 1.50g/cm3The yield of the liquefied product oil of (2) was 40% and was not liquefiable. The specific results are shown in Table 2.
TABLE 2 coal sample of make-up tower
Figure BDA0001941458370000051
Example 3
A method for separating liquefiable and non-liquefiable components in inert component microscopic components of coal specifically comprises the following steps:
(1) manually selecting a Renbebel coal sample to obtain a coal sample with the inert component content of more than 80%;
(2) crushing the coal sample to 0.5-3 mm by using a jaw crusher, and screening and collecting inert-rich particles with smaller particle sizes;
(3) grinding the inert group enrichment to prepare coal powder, performing chemical deashing treatment, and crushing by using a rod mill to obtain a coal powder sample;
(4) and (3) carrying out a centrifugal floating and sinking experiment on the coal powder sample, carrying out the centrifugal floating and sinking experiment on the specific gravity liquid with a ratio from low to high, obtaining the distribution data condition of each density range of the sample, and collecting the sample in each density range. The density of the specific gravity liquid is 1.35-1.50 g/cm3And the density interval is set to 0.02g/cm3And centrifuging for 30min at the rotating speed of 2500r/min, selecting 7g of an inertinite enriched coal powder sample, placing the inertinite enriched coal powder sample in 8 centrifuge tubes of 50ml for centrifugal test, standing the centrifuge tubes for 2h after the centrifugal test is finished at the rotating speed of 2500r/min, and finally washing and drying the products of the specific gravity components respectively, cooling and weighing. (surfactant Brij-35 is added into the specific gravity liquid according to actual requirements, because the coal powder has poor hydrophilicity, in order to avoid that the coal powder is not fully dissolved into the specific gravity liquid to cause unexpected separationThe effect is that the surfactant Brij-35) is added according to the actual requirement;
(5) collecting a series of density range coal dust samples (1.35 g/cm)3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3，1.50g/cm3) Respectively carrying out liquefaction experiments, wherein the standard liquefaction experiment conditions are as follows: weighing 28g of collected inert group enriched coal powder samples of each density group, wherein the initial hydrogen pressure is 10.0MPa, adding a coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished;
(6) the liquefaction data results show a density of 1.35g/cm3，1.37g/cm3，1.39g/cm3，1.41g/cm3，1.43g/cm3The yield of the liquefied product oil is over 60 percent, and the density is 1.43g/cm3，1.45g/cm3，1.47g/cm3，1.49g/cm3The oil yield of the liquefied product is below 60 percent. Aiming at the inert micro-components (1.35-1.50 g/cm) in the Renbell coal3) At 1.44g/cm3Dividing the separation line into liquefiable and non-liquefiable;
(7) performing a centrifugal floating and sinking experiment on a coal powder sample, performing the centrifugal floating and sinking experiment on a specific gravity liquid with a low-to-high ratio, and collecting 1.35-1.43 g/cm3And 1.44 to 1.50g/cm3Density range samples were subjected to liquefaction experiments. The standard experimental conditions for liquefaction were: weighing 28g of collected coal dust sample with the required density range enriched, wherein the initial hydrogen pressure is 10.0MPa, adding the coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished;
(8) the density of the obtained liquefied product is 1.35-1.43 g/cm3The yield of the liquefied product oil is 65%, the liquefied product oil is liquefiable, and the density is in a range of 1.44-1.50 g/cm3With a 40% yield of liquefied product oil of (A) is notCan be liquefied. The specific results are shown in Table 3.
TABLE 3 Renbell coal samples
Figure BDA0001941458370000061
The above description is only a basic description of the present invention, and any equivalent changes made according to the technical solution of the present invention should fall within the protection scope of the present invention.

Claims (7)

1. A method for separating liquefiable and non-liquefiable components in inert component micro-components of coal is characterized by comprising the following specific steps:
(1) selecting a coal sample which is grey black and dark in color by hand;
(2) crushing the hand-selected coal sample, and screening and collecting the inert-rich group particles with smaller particle size;
(3) grinding the inert-rich group particles to prepare coal powder, performing chemical deashing treatment, and crushing by using a rod mill to obtain a coal powder sample;
(4) taking a plurality of coal powder samples for a sink-float centrifugal experiment, wherein each coal powder sample is 20-30 g, and the density range of the specific gravity liquid is 1.35-1.50 g/cm3And the density interval is set to be 0.02g/cm3The centrifugation time is 20-30 min, and the centrifugation rotating speed is 2000-3000 r/min; obtaining the distribution data condition of each density range of the coal powder sample and collecting the density of 1.35-1.50 g/cm3Coal samples of various density ranges in between;
(5) carrying out liquefaction experiments on the collected coal samples in each density range;
(6) based on liquefaction data, when the yield of the liquefied product oil is more than 60%, the liquefied product oil is considered to be liquefiable, a density boundary between a liquefied part and a non-liquefiable part is defined, and the density range of the liquefiable part is determined to be 1.35-1.43 g/cm3；
(7) Performing a floating and sinking centrifugation experiment on the coal powder sample obtained in the step (3), and collecting the coal powder sample with the density of 1.35-1.43 g/cm3To obtain the liquefiable components of the inert component.
2. The separation method according to claim 1, characterized in that: in the step (2), a jaw crusher is used for crushing the coal sample to 0.5-3 mm, and the inert-rich particles with small particle size are screened and collected.
3. The separation method according to claim 1, characterized in that: in the step (3), the chemical deashing treatment method comprises the following steps: respectively carrying out acid cleaning treatment twice by using hydrochloric acid and hydrofluoric acid under the inert atmosphere of nitrogen, filtering after each acid cleaning, and washing the coal sample by using warm water; and finally, vacuum drying.
4. The separation method according to claim 1, characterized in that: in the step (3), the granularity of the pulverized coal sample crushed by the rod mill is 0.15-0.20 mm.
5. The separation method according to claim 1, characterized in that: in the step (4), a centrifugal floating and sinking experiment is carried out on the specific gravity liquid in a ratio from low to high; zinc chloride is selected as a floating and sinking medium.
6. The separation method according to claim 1, characterized in that: in the step (5), the liquefaction experimental conditions are as follows: weighing 20-30 g of collected inert group enriched coal powder samples of each density group, wherein the initial hydrogen pressure is 10.0MPa, adding a coal sample and a solvent according to the mass ratio of 1:1.5, catalyzing by ferric oxide, taking S as a cocatalyst, keeping the reaction temperature constant for 60-90 min after the reaction temperature rises to reach a constant temperature section, and cooling the temperature to 200 ℃ within 30min after the constant temperature is finished.
7. The separation method according to claim 1, characterized in that: in the step (6), based on the liquefaction data, the density range is 1.35-1.50 g/cm3The pulverized coal sample is divided into two grades, 1.35-1.43 g/cm3And 1.44 to 1.50g/cm3。
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