CN113234460A - Analysis method of oil-rich coal - Google Patents
Analysis method of oil-rich coal Download PDFInfo
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- CN113234460A CN113234460A CN202110453585.2A CN202110453585A CN113234460A CN 113234460 A CN113234460 A CN 113234460A CN 202110453585 A CN202110453585 A CN 202110453585A CN 113234460 A CN113234460 A CN 113234460A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
Abstract
The invention relates to the field of evaluation of rich-oil coal resources and extraction of oil products, in particular to an analysis method of rich-oil coal; the analysis method comprises the steps of carrying out industrial analysis, total sulfur analysis, hydrocarbon analysis, ash component analysis, nitrogen analysis, kudzu low-temperature dry distillation analysis, vitrinite reflectivity analysis, microscopic component classification analysis, scanning electron microscope analysis, energy spectrum quantitative analysis and X-ray diffraction whole rock analysis on the oil-rich coal, and then carrying out pyrolysis treatment; the pyrolysis treatment conditions are as follows: heating from room temperature, raising the temperature to 550-650 ℃ at the speed of 15 +/-0.5 ℃/min, and keeping the temperature for 25-35 min. The pyrolysis treatment condition of the oil-rich coal is determined through analysis of the oil-rich coal, and the oil-rich coal is subjected to pyrolysis treatment under the condition, so that high-quality pyrolysis coke, pyrolysis liquid and pyrolysis gas can be obtained.
Description
Technical Field
The invention relates to the field of evaluation of rich-oil coal resources and extraction of oil products, in particular to an analysis method of rich-oil coal.
Background
The oil-rich coal refers to coal resources with the tar yield of 7-12%, and is classified into high-oil coal (T) according to the tar yield of the coalar，d>12.00%), oil-rich coal (T)ar，d>7.00% -12.00%) and oil-bearing coal (T)ar，dLess than or equal to 7.00 percent). Coal is used as main energy, wherein the low-rank coal accounts for 46 percent of the total coal resources, and the resource evaluation, development and utilization research on the rich oil-rich low-rank coal resources has great significance for guaranteeing the energy safety. The method develops the potential survey of rich oil coal resources and the extraction, test and analysis of oil products, expands the new field of oil gas exploration and exploitation, continuously improves the continuous guarantee capability of oil gas resources, and makes new contributions to the guarantee of energy resource safety and the optimization of energy structures.
By processing the oil-rich coal, relatively rich coal resources can be converted into relatively short oil and gas resources and semicoke capable of replacing anthracite and partial coking coal, and the current research foundation and technology restrict the large-scale development of the oil-rich coal.
In the prior art, according to the characteristics of high volatile components and high hydrogen content of low-rank coal, the quality-based utilization of coal resources can be realized through graded conversion and utilization; the process is that tar, coal crude gas and semicoke can be formed through pyrolysis; the tar can be first extracted into phenol and then hydrogenated into light aromatic hydrocarbon, naphtha and other oil products, and the raw gas can be converted into CH4CO and H2The semicoke is used as clean energy and can be used for blast furnace injection and gasification raw materials. The comprehensive energy efficiency of the low-rank coal in quality-based utilization is higher than that of direct power generation of the low-rank coal, the economic competitiveness is higher than that of direct power generation, the efficient comprehensive utilization of coal resources is realized, the emission of sulfur dioxide is also obviously reduced, and the environmental pollution caused by coal burning is reduced.
However, the coal classification and quality separation utilization level is still low, the problems of insufficient conceptual recognition, lagged systematic matching technology and the like still face, and a test analysis method for an oil-rich coal resource system is short of a system flow.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide an analysis method of oil-rich coal, which is used for performing systematic analysis on coal quality of coal rock of the oil-rich coal and performing qualitative and quantitative analysis on a pyrolysis product of the oil-rich coal.
Specifically, the invention provides the following technical scheme:
the invention provides an analysis method of rich-oil coal, which comprises the steps of carrying out industrial analysis, total sulfur analysis, hydrocarbon analysis, ash component analysis, nitrogen analysis, kudzuvine root gold low-temperature dry distillation analysis, vitrinite reflectivity analysis, micro-component classification analysis, scanning electron microscope analysis, energy spectrum quantitative analysis and X-ray diffraction whole rock analysis on the rich-oil coal, and then carrying out pyrolysis treatment;
the pyrolysis treatment conditions are as follows: heating from room temperature, raising the temperature to 550-650 ℃ at the speed of 15 +/-0.5 ℃/min, and keeping the temperature for 25-35 min.
The invention discovers that the rich-oil coal is subjected to pyrolysis treatment after being subjected to industrial analysis, total sulfur analysis, hydrocarbon analysis, ash component analysis, nitrogen analysis, kudzu low-temperature dry distillation analysis, vitrinite reflectance analysis, micro-component classification analysis, scanning electron microscope analysis, energy spectrum quantitative analysis and X-ray diffraction total rock analysis in sequence/respectively, and the pyrolysis condition can be determined accurately. Namely, according to industrial analysis, total sulfur analysis, hydrocarbon analysis, ash component analysis, nitrogen analysis, kudzu low-temperature dry distillation analysis, vitrinite reflectivity analysis, micro-component classification analysis, scanning electron microscope analysis, energy spectrum quantitative analysis and X-ray diffraction whole rock analysis, the coal-rock coal quality characteristics, the coal geochemical characteristics and the mineralogical characteristics of the oil-rich coal sample can be systematically mastered, and a material analysis basis is provided for a pyrolysis experiment.
In addition, the thermal decomposition temperature (Td) is around 300 ℃ for most coals; while the apparent shape and structure of the coal are not significantly changed in the course of increasing the temperature from room temperature to the thermal decomposition temperature (Td). Specifically, dehydration reaction is mainly carried out before 120 ℃, and CH adsorbed on the surface and in pores of coal is basically removed at about 200 DEG C4、CO2、N2And the like; the molecular structures of the bituminous coal and the anthracite coal do not have a large amount of thermal decomposition reaction in the process, only have a small amount of condensation, and when the temperature of the lignite rises above 200 ℃, the decarboxylation reaction starts to be carried out, and the thermal decomposition reaction starts to be carried out at about 300 ℃.
The invention also discovers that the pyrolysis efficiency of the oil-rich coal can be improved by changing the experimental conditions of the pyrolysis treatment; the pyrolysis efficiency is improved by 7.69%.
Preferably, the industrial analysis is performed according to GB/T212-2008 to obtain data of moisture, ash, volatile matter, coke breeze characteristics, total moisture and fixed carbon of the oil-rich coal.
Preferably, the total sulfur analysis is performed according to GB/T214-2007 to obtain the oil-rich coal total sulfur data.
Preferably, the hydrocarbon analysis is carried out according to GB/T476-2008, so as to analyze the content of C, H elements in the oil-rich coal.
Preferably, the ash composition analysis is performed according to GB/T1574-2007 for analyzing the oxide content in the oil-rich coal ash.
Preferably, the nitrogen analysis is carried out according to GB/T19227-2008, and the content of the N element in the oil-rich coal is analyzed;
preferably, the low-temperature dry distillation analysis of the kudzuvine root is carried out according to GB/T1341-2007 to obtain the data of the yield of semicoke, the yield of tar and the yield of total moisture in the oil-rich coal, and the specific conditions are as follows: raising the temperature from 300 ℃ to 550-650 ℃ at the speed of 5 +/-0.5 ℃/min and keeping the temperature for 10-20 min.
Preferably, the vitrinite reflectance analysis is performed according to GB/T6948-2008, so as to obtain vitrinite reflectance data in oil-rich coal.
Preferably, the microscopic component classification analysis is carried out according to GB/T15588-2013, and organic components and inorganic components in the oil-rich coal are analyzed.
Preferably, the scanning electron microscope analysis is carried out according to SY/T5162-2014 so as to analyze the structural morphology of components in the oil-rich coal and the contained minerals.
Preferably, the quantitative analysis of the energy spectrum is carried out according to SY/T6189-2018 so as to analyze the content of minerals contained in the oil-rich coal.
Preferably, the X-ray diffraction whole rock analysis is carried out according to SY/T5163-2018 to determine the type of minerals contained in the oil-rich coal.
In the invention, the rich-oil coal is pyrolyzed to generate pyrolysis coke, pyrolysis liquid and pyrolysis gas; the pyrolysis products can be recycled. In particular, the method of manufacturing a semiconductor device,
(1) pyrolytic coke
The coke is mainly used for blast furnace ironmaking and blast furnace smelting of nonferrous metals such as copper, lead, zinc, titanium, antimony, mercury and the like, and plays roles of a reducing agent, a heating agent and a material column framework; the pyrolysis coke generated by pyrolysis can be directly combusted to utilize the heat energy thereof; pyrolytic coke (biochar) generated by biomass pyrolysis has a high specific surface area, so that the pyrolytic coke can be prepared into an adsorption material; in addition, the biochar can also be used as a soil conditioner.
(2) Pyrolysis liquid
The pyrolysis liquid comprises pyrolysis oil obtained by pyrolysis and partial condensed water, and oil-water separation is a big problem in the application of the pyrolysis liquid; pyrolysis oil can be used as a substitute for fossil fuels to generate heat, electricity, and chemicals, and is applicable to boiler-burning and thermoelectric power generation in a short period of time and to turbine and diesel engines in a long-term consideration. Upgrading pyrolysis oil to transportation oil is technically feasible, but requires further development. A wide variety of chemicals are available through pyrolysis oil refining and derivatization. The pyrolysis oil contains a considerable portion of water, and the calorific value of the pyrolysis oil is lower than that of fossil fuel; however, flame combustion experiments indicate that fast pyrolysis oil can be used in industrial boilers instead of heavy oil and light oil; the fuel used as boiler/furnace is the most direct application of pyrolysis oil; meanwhile, the pyrolysis oil can be suitable for boiler power generation co-fired with coal. The bio-oil can also be used as an alternative fuel of a diesel engine. The pyrolysis oil can also be used directly for power generation; over the past few years, the experimental operation of pyrolysis oil on different diesel engines and modified dual oil engines has been for hundreds of hours, and the operation of the engines and the results of the tests have been encouraging. However, some of the problems of pyrolysis oil replacing diesel oil, especially its acidic (pH 3) soot formation and repolymerization, remain to be solved. Only biomass can produce "green" hydrocarbons. The comparison of the production of synthesis gas from solid biomass and pyrolysis oil shows that large scale production by gasification of pyrolysis oil is more encouraging. It is technically and economically feasible to gasify pyrolysis oil with pure oxygen to produce synthesis gas and then produce hydrocarbons through fischer-tropsch synthesis. The bio-oil is used for extracting chemicals, can be used for preparing special chemicals, and can also be used for preparing polyphenol, chemical fertilizer, pesticide and chemicals with environmental protection requirements; the production of high value chemicals can improve the economic benefits of bio-oil utilization.
(3) Pyrolysis gas
Directly burning pyrolysis gas for producing steam and preheating air; secondly, the pyrolysis gas is purified, condensed and dedusted, and water, residual oil and other impurities are used for producing the gas fuel with higher purity.
The beneficial effect of this application lies in:
the pyrolysis treatment condition of the oil-rich coal is determined through analysis of the oil-rich coal, and the oil-rich coal is subjected to pyrolysis treatment under the condition, so that high-quality pyrolysis coke, pyrolysis liquid and pyrolysis gas can be obtained. In addition, the invention also improves the pyrolysis efficiency of the oil-rich coal and improves the tar yield by 7.69%.
Drawings
FIG. 1 is an X-ray spectrum of an oil-rich coal;
FIG. 2 is a spectrum of analysis of pyrolysis products of oil-rich coal.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides an analysis method of oil-rich coal, which comprises the following steps:
(1) performing industrial analysis (according to GB/T212-2008), total sulfur analysis (according to GB/T214-2007), hydrocarbon analysis (according to GB/T476-2008), ash component analysis (according to GB/T1574-2007), nitrogen analysis (according to GB/T19227-2008), Kudzuvine gold low-temperature dry distillation analysis (according to GB/T1341-2007), vitrinite reflectance analysis (according to GB/T6948-2008), micro-component classification analysis (according to GB/T15588-2013), scanning electron microscope analysis (according to SY/T5162-2014), energy spectrum quantitative analysis (according to SY/T6189-2018) and X-ray diffraction total rock analysis (according to SY/T5163-2018) on oil-rich coal;
wherein the results of each analysis are shown in tables 1, 2, 3, 4 and 5;
TABLE 1
TABLE 2
TABLE 3
TABLE 4
TABLE 5
In addition, the results of the microscopic component test were as follows:
(ii) organic component
Vitrinite group: taking matrix vitrinite (cementing hemifilament, filament fragment, clastic inert body, chitin group, clay, etc.) as main material; occasionally homogeneous vitrinite and agglomerate vitrinite;
inertinite group: taking a hemifusome as a main material, oxidizing the mitoplast, chipping the inert plastid again, and occasionally generating a coarse mitochondrion and a fire-burned mitochondrion;
chitin group: microsporidia are occasionally observed.
(ii) inorganic Components
Clay: filling the semiprotonic body cavities or fissures;
sulfide: filling cracks with pyrite;
carbonate salt: not shown;
silicon oxide: not shown;
other minerals: not shown;
the scanning electron microscope test results are as follows:
quartz is seen to be in an obvious crystal form (an angular form and a secondary angular form);
most of the filamentous bodies with different angles can be seen, obvious cell cavities and plant ducts (nearly circular, oval and flat) can be seen, and worm-shaped cross sections can be seen;
filling inert group fragments and quartz particles in the cell cavity;
fourthly, the asphaltene with stronger granular feeling (the components with oil-producing potential are more available);
lens body is filled in the cavity in a cylindrical shape;
sixthly, the strawberry-shaped pyrite (non-filled) can be seen.
The results of the X-ray analysis are shown in FIG. 1;
(2) carrying out pyrolysis treatment on the oil-rich coal; the pyrolysis experimental instrument mainly comprises a pyrolysis furnace, a thermocouple, a temperature controller, a quartz pyrolysis tube, a condenser, a flowmeter, an air bag collecting device and the like. And (3) 20g of a rich coal sample (the quality of the experimental sample can be adjusted according to actual conditions). Firstly, putting a rich-oil coal sample into a quartz tube, flatly spreading the sample to ensure that the sample is uniformly heated, then putting the rich-oil coal sample into a fixed bed reactor, and setting the heating rate of a furnace to heat to a set pyrolysis final temperature (starting heating from room temperature, heating to 600 ℃ at the rate of 15 ℃/min, and keeping the temperature for 30 min). Solid residues remained in the quartz tube after the pyrolysis reaction are pyrolysis coke of a pyrolysis solid-phase product; condensing the pyrolysis reaction volatile matter in a collection bottle to obtain pyrolysis liquid phase product pyrolysis liquid through an ice water condensation system; the generated non-condensable gas passes through a filter and other purification devices, then passes through a gas flowmeter, and is finally collected into pyrolysis gas phase product pyrolysis gas by a gas bag.
The results of the pyrolysis and three-phase yield analysis are shown in table 6;
TABLE 6
| Serial number | Solid phase | Liquid phase | Gas phase |
| 1 | 54.75％ | 36.39％ | 8.86％ |
The water content and the pH value of the pyrolysis tar are shown in Table 7;
TABLE 7
| Serial number | pH | Water content ratio | Tar yield |
| 1 | 10.31 | 69.2％ | 11.2％ |
As can be seen from Table 2, the yield of tar produced by dry distillation of Kudzuvine root is 10.4%; as can be seen from Table 7, the tar yield of the pyrolysis treatment was 11.2%.
The results of the pyrolysis product analysis of the oil-rich coal are shown in fig. 2 and table 8;
TABLE 8
As can be seen from FIG. 2 and Table 8, the present invention quantitatively measures the components and contents of tar while increasing the yield of pyrolysis tar.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The analysis method of the rich oil coal is characterized in that the rich oil coal is subjected to industrial analysis, total sulfur analysis, hydrocarbon analysis, ash component analysis, nitrogen analysis, kudzu low-temperature dry distillation analysis, vitrinite reflectance analysis, micro-component classification analysis, scanning electron microscope analysis, energy spectrum quantitative analysis and X-ray diffraction whole rock analysis, and then is subjected to pyrolysis treatment;
the pyrolysis treatment conditions are as follows: heating from room temperature, raising the temperature to 550-650 ℃ at the speed of 15 +/-0.5 ℃/min, and keeping the temperature for 25-35 min.
2. An assay method according to claim 1, wherein the industrial assay is performed in accordance with GB/T212-2008.
3. An assay method according to claim 1 or 2, wherein the total sulphur assay is performed according to GB/T214-2007.
4. An analysis method according to any one of claims 1 to 3, wherein the hydrocarbon analysis is performed in accordance with GB/T476-2008.
5. An assay method according to any one of claims 1 to 4, wherein the ash component assay is performed according to GB/T1574-2007.
6. An assay method according to any one of claims 1 to 5 wherein the nitrogen assay is performed according to GB/T19227-2008.
7. The analysis method according to any one of claims 1 to 6, wherein the low-temperature dry distillation analysis of the Pueraria lobata is carried out according to GB/T1341-2007, and the specific conditions are as follows: raising the temperature from 300 ℃ to 550-650 ℃ at the speed of 5 +/-0.5 ℃/min and keeping the temperature for 10-20 min.
8. An assay method according to any one of claims 1 to 7 wherein the vitrinite reflectance assay is performed in accordance with GB/T6948-2008.
9. An assay method according to any one of claims 1 to 8 wherein the micro-component classification assay is carried out in accordance with GB/T15588-2013.
10. The analytical method according to any one of claims 1 to 9, wherein the scanning electron microscope analysis is performed according to SY/T5162-2014;
and/or, the quantitative analysis of the energy spectrum is carried out according to SY/T6189-2018;
and/or, the X-ray diffraction whole rock analysis is carried out according to SY/T5163-2018.
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| CN117665041A (en) * | 2024-02-01 | 2024-03-08 | 中海石油气电集团有限责任公司 | Radio frequency heating oil-rich coal in-situ pyrolysis simulation test device and method |
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| CN117665041A (en) * | 2024-02-01 | 2024-03-08 | 中海石油气电集团有限责任公司 | Radio frequency heating oil-rich coal in-situ pyrolysis simulation test device and method |
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