CN113716596B - Method for extracting various products by utilizing oil shale semicoke or oil shale ash in grading manner - Google Patents

Method for extracting various products by utilizing oil shale semicoke or oil shale ash in grading manner Download PDF

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Publication number
CN113716596B
CN113716596B CN202111079020.9A CN202111079020A CN113716596B CN 113716596 B CN113716596 B CN 113716596B CN 202111079020 A CN202111079020 A CN 202111079020A CN 113716596 B CN113716596 B CN 113716596B
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oil shale
reaction
filtrate
ammonia
raw materials
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CN113716596A (en
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郭洪范
王卓
刘云义
熊莉佳
窦泽伟
王志远
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Liaoning International Investment And Trade Promotion Center Liaoning E Port Service Center
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Liaoning International Investment And Trade Promotion Center Liaoning E Port Service Center
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid

Abstract

The invention discloses a method for extracting various products by utilizing oil shale semicoke or oil shale ash in a grading way, which comprises the following steps: collecting oil shale semicoke or oil shale ash as a raw material, and crushing the raw material for later use; and extracting a calcium carbonate product and/or a silicon dioxide product by using the crushed raw materials. The method can effectively separate calcium, silicon and other components in the oil shale solid waste, simultaneously obtain products such as calcium carbonate, silicon dioxide (white carbon black) and the like, recycle process materials, recycle intermediate product ammonium solution and ammonia gas, recycle and utilize the generated carbon dioxide with high value, extract the residual waste residue, and can be used in the fields of building materials, aluminum extraction raw materials and the like, and the method has the advantages of basically no three waste discharge and remarkable environmental benefit.

Description

Method for extracting various products by utilizing oil shale semicoke or oil shale ash in grading manner
Technical Field
The invention relates to the field of comprehensive utilization of oil shale resources, in particular to a method for extracting various products by utilizing oil shale semicoke or oil shale ash in a grading way.
Background
Oil shale is sedimentary rock containing combustible organic matters, and the organic matters can be converted into shale oil similar to crude oil through carbonization, or can be directly burnt as solid fuel to generate heat (steam generation) and generate electricity, so that the oil shale is the two main development directions of the oil shale industry.
Oil shale resources are of great reserves and are listed as one of the most important successor energy sources in the 21 st century, but the development of the oil shale industry presents a great bottleneck. Oil shale retorting oil refining produces oil shale semicoke and direct combustion produces oil shale ash, and the amount of the solid byproducts is extremely large, because the inorganic matter content in the oil shale is extremely high, and the oil shale is a high ash solid fuel, for example, about 10-30 tons of solid waste are simultaneously produced when 1 ton of shale oil is extracted. However, the utilization rate of the solid byproducts in the oil shale industry is not high, the solid byproducts are uniformly piled and abandoned as waste, the waste is rarely utilized, a large amount of land is occupied, and serious pollution is caused to the environment, for example, the oil shale semicoke contains water-soluble phenolic compounds, sulfur-containing compounds, semi-volatile substances, polycyclic aromatic hydrocarbons and other toxic pollutants, and exudates formed in the process of dumping and open air placement can form serious threat to groundwater.
The problem of disposal of solid byproducts from oil shale resource utilization severely constrains the development of the oil shale industry. If the solid waste of the oil shale industry is used as a raw material to prepare a product with high added value, the economy of oil shale resource utilization can be improved, the problem of environmental pollution can be effectively solved, and the comprehensive utilization of resources without solid waste emission can be realized.
Therefore, development of a utilization method of oil shale semicoke or oil shale ash is urgently required to solve the above problems.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for extracting various products by utilizing oil shale semicoke or oil shale ash in a grading way.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
a method for extracting a plurality of products by utilizing oil shale semicoke or oil shale ash in a grading way, which comprises the following steps:
s1, collecting oil shale semicoke or oil shale ash as raw materials, and crushing the raw materials for later use;
s2, extracting a calcium carbonate product and/or a silicon dioxide product by using the crushed raw materials.
Further, in the step S2, when only the calcium carbonate product is extracted, the specific steps are as follows:
S2A1, placing the crushed raw materials into a calciner for calcination treatment to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2A2, adding the calcined powder prepared in the step S2A1 into the circulating mother liquor A, heating to perform ammonia distillation reaction, recovering the generated ammonia gas into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain filtrate A rich in water-soluble calcium salt and solid residue I after calcium extraction;
S2A3, introducing the carbon dioxide gas prepared in the step S2A1 and the ammonia gas prepared in the step S2A2 into the filtrate A rich in water-soluble calcium salt, wherein Ca 2+ And (3) carrying out precipitation reaction on ions, wherein the precipitate is calcium carbonate, filtering a reaction solution after the reaction is finished, and collecting filter residues to obtain a calcium carbonate product.
Further, in the step S2, when only the silica product is extracted, the specific steps are as follows:
S2B1, placing the crushed raw materials into a calciner to be calcined to obtain calcined powder or directly adding the crushed raw materials into a circulating mother liquor B to perform ammonia distillation extraction reaction, recovering released ammonia into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain filtrate B and solid residues II, wherein the filtrate B is a solution rich in Si compounds;
S2B2, introducing the ammonia gas obtained in the step S2B1 into the filtrate B to obtain silica precipitate, filtering after the reaction is finished, and collecting filter residues to obtain a silica product.
Further, in the step S2, when extracting the calcium carbonate product and the silica product, the specific steps are as follows:
S2C1, placing the crushed raw materials into a calciner for calcination treatment to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2C2, adding the calcined powder prepared in the step S2C1 into the circulating mother liquor A, heating to perform ammonia distillation reaction, recovering the generated ammonia gas into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain filtrate A rich in water-soluble calcium salt and solid residue I after calcium extraction;
S2C3, adding the solid residue I obtained in the step S2C2 into the circulating mother liquor B, carrying out ammonia distillation and extraction reaction, recovering released ammonia into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain filtrate B and a solid residue II, wherein the filtrate B is a solution rich in Si compounds;
S2C4, introducing the carbon dioxide gas prepared in the step S2C1 and the ammonia gas prepared in the step S2C2 into the filtrate A rich in water-soluble calcium salt, wherein Ca 2+ The ions undergo a precipitation reaction, the precipitate is calcium carbonate, the reaction solution is filtered after the reaction is finished, and filter residues are collected to obtain a calcium carbonate product;
S2C5, introducing the ammonia gas obtained in the step S2C3 into the filtrate B to obtain silica precipitate, filtering after the reaction is finished, and collecting filter residues to obtain a silica product.
Further, the circulating mother solution A is an aqueous solution containing ammonium chloride or ammonium nitrate or ammonium acetate.
Further, the circulating mother solution B is an aqueous solution containing ammonium fluoride.
Further, the ammonia distillation reaction is carried out at 85-105 ℃.
Further, the Ca 2+ The ion precipitation reaction is carried out at 40-120 ℃.
Further, the silica precipitation is carried out at 40-90 ℃.
Compared with the prior art, the method can effectively separate calcium, silicon and other components in the oil shale solid waste, simultaneously obtain products such as calcium carbonate, silicon dioxide (white carbon black) and the like, recycle process materials, recycle intermediate products such as ammonium solution and ammonia, recycle the generated carbon dioxide, utilize the generated carbon dioxide in a high value, and finally the residual waste residue can be used in the fields of building materials and the like, basically has no three wastes discharge and has remarkable environmental benefit; in addition, the oil shale semicoke or oil shale ash grade extraction method provided by the invention not only realizes high-value utilization of a large amount of solid wastes and avoids serious problems such as resource waste, occupation of a large amount of land and environmental pollution, but also has strong raw material adaptability of the process, and can flexibly regulate and control reaction steps according to the components of the oil shale industrial solid wastes, thereby realizing flexible regulation and control of the types of process products.
Drawings
Fig. 1 is a section distribution schematic diagram of the oil shale semicoke or oil shale ash classification extraction method of the invention.
FIG. 2 is a detailed flow chart of the method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. The specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
When the silicon content in the collected oil shale semicoke or oil shale ash is very low and no silicon extraction is necessary, only the calcium carbonate product is required to be extracted, as shown in fig. 1 and 2, the embodiment provides a method for extracting various products by utilizing the oil shale semicoke or the oil shale ash in a grading way, which comprises the following steps:
s1, collecting oil shale semicoke or oil shale ash as raw materials, and crushing the raw materials for later use;
S2A1, placing the crushed raw materials into a calciner for calcination treatment, controlling the temperature to 850-1100 ℃, and calcining for 1-2 hours to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2A2, adding the calcined powder obtained in the step S2A1 into a circulating mother liquor A (in the embodiment, the circulating mother liquor A uses an aqueous solution containing ammonium chloride), wherein NH in the aqueous solution containing ammonium chloride 4 The Cl concentration is 1.0-2.0mol/L, ammonia distillation reaction is carried out at the temperature of 85-105 ℃, the generated ammonia gas is recovered into an ammonia gas collecting tank, and after the reaction is finished, the filtration is carried out to obtain filtrate A rich in water-soluble calcium salt and solid residue I after calcium extraction;
S2A3, introducing the carbon dioxide gas obtained in the step S2A1 and the ammonia gas obtained in the step S2A2 into the filtrate A rich in water-soluble calcium salt, and stirring at 200-1000rpm and at 40-120deg.C to obtain Ca 2+ And (3) carrying out precipitation reaction on ions, wherein the precipitate is calcium carbonate, filtering a reaction solution after the reaction is finished, and the filtrate is a circulating mother solution A and is circularly used in the step S2A2, and washing, filtering, drying and grinding the collected filter residues to obtain a calcium carbonate powdery product.
Example 2
When the content of calcium in the collected shale semicoke or oil shale ash is very low and the silicon extraction is not necessary, only the silicon dioxide product is required to be extracted, as shown in fig. 1 and 2, the embodiment provides a method for extracting various products by utilizing the oil shale semicoke or the oil shale ash in a grading way, which comprises the following steps:
s1, collecting oil shale semicoke or oil shale ash as raw materials, and crushing the raw materials for later use;
S2B1, placing the crushed raw materials into a calciner to be calcined (850-1100 ℃ for 1-2 hours) to obtain calcined powder or directly adding the crushed raw materials into a circulating mother liquor B (the circulating mother liquor B in the embodiment uses an aqueous solution containing ammonium fluoride), carrying out ammonia distillation extraction reaction at 85-105 ℃, recovering released ammonia into an ammonia gas collecting tank, filtering after the reaction is finished to obtain a filtrate B and a solid residue II, wherein the filtrate B is rich in Si compounds (NH 4 )SiF 6 State present) of the solution;
S2B2, introducing ammonia gas obtained in the step S2B1 into filtrate B, reacting at 40-90 ℃ to obtain silicon dioxide precipitate, filtering after the reaction is finished, wherein the filtrate is circulating mother liquor B which can be recycled in the step S2B1, and the filter residue is silicon dioxide, and washing, filtering, drying and grinding to obtain a silicon dioxide powder product.
Example 3
When the calcium and silicon contents in the collected oil shale semicoke or oil shale ash need to be extracted, as shown in fig. 1 and 2, the embodiment provides a method for extracting various products by utilizing the oil shale semicoke or the oil shale ash in a grading way, which comprises the following steps:
s1, collecting oil shale semicoke or oil shale ash as raw materials, and crushing the raw materials for later use;
S2C1, placing the crushed raw materials into a calciner for calcination treatment, controlling the temperature to 850-1100 ℃, and calcining for 1-2 hours to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2C2 the calcined powder obtained in the step S2C1 is added to the circulating mother liquor A (in this example, the circulating mother liquor A uses an aqueous solution containing ammonium chloride), wherein NH in the aqueous solution containing ammonium chloride 4 The Cl concentration is 1.0-2.0mol/L, ammonia distillation reaction is carried out at the temperature of 85-105 ℃, the generated ammonia gas is recovered into an ammonia gas collecting tank, and after the reaction is finished, the filtration is carried out to obtain filtrate A rich in water-soluble calcium salt and solid residue I after calcium extraction;
S2C3, adding the solid residue obtained in the step S2C2 into a circulating mother solution B (the circulating mother solution B in the embodiment uses ammonium salt water solution containing ammonium fluoride), carrying out ammonia distillation and extraction reaction at 85-105 ℃, recovering released ammonia into an ammonia collecting tank, filtering after the reaction is finished to obtain a filtrate B and a solid residue II, wherein the filtrate B is rich in Si compounds (in (NH) 4 )SiF 6 State present) of the solution;
S2C4, introducing carbon dioxide gas obtained in the step S2C1 and ammonia gas obtained in the step S2C2 into filtrate A rich in water-soluble calcium salt, and stirring at 200-1000rpm and at 40-120deg.C to obtain Ca 2+ The ions undergo a precipitation reaction, the precipitate is calcium carbonate, the reaction solution is filtered after the reaction is finished, the filtrate is a circulating mother solution A and is circularly used in the step S2C2, and the collected filter residues are washed, filtered, dried and ground to obtain a calcium carbonate powdery product;
S2C5, introducing ammonia gas obtained in the step S2C3 into filtrate B, reacting at 40-90 ℃ to obtain silicon dioxide precipitate, filtering after the reaction is finished, wherein the filtrate is circulating mother liquor B which can be recycled in the step S2C3, and the filter residue is silicon dioxide, and washing, filtering, drying and grinding to obtain a silicon dioxide powder product.
For example 1, example 2 and example 3, according to the different extraction difficulties and compositions of different components of the oil shale industrial solid waste, the number of times of ammonium evaporation extraction can be increased appropriately, and the extraction effect and the cost of ammonium evaporation can be selected.
In addition, in the above embodiment, the solid residues after the process extraction in the step S2A2, S2B1 or S2C3 and the impurities such as Al, mg and the like in the step S2A3, S2B2, S2C4 or S2C5 can be removed (precipitated) by adjusting and controlling the pH value of the circulating mother liquor, and the solid residues can be used as building materials or aluminum-smelting raw materials, etc., so as to reduce the emission of process waste and further increase the utilization rate of resources.
The invention can utilize the oil pageThe principle of the method for extracting and preparing various high added value products by using the solid waste in the rock industry as the raw material in a grading way is as follows: firstly, calcining oil shale semicoke or oil shale ash to remove organic matters and carbon components in raw materials, and preventing the organic matters and the carbon components from reducing subsequent CaCO (CaCO) 3 And SiO 2 Whiteness of the products, and simultaneously, calcium carbonate is decomposed into calcium oxide and CO 2 Gas (reaction equation: caCO) 3 →CaO+CO 2 ∈) and the calcium carbonate is converted into calcium oxide, so that the subsequent extraction of calcium element from solid raw materials is facilitated; then the calcined raw material is reacted with ammonium salt solution for several times, the ammonium salt selectivity is regulated and controlled to react with different components in the oil shale solid waste raw material for several times by regulating and controlling the composition of ammonium salt anions, firstly the ammonium salt (circulating mother liquor A) is reacted with calcium oxide (first extraction; the reaction equation is CaO+H) 2 O→Ca(OH) 2 And Ca (OH) 2 +2NH 4 Cl→2NH 3 ↑+CaCl 2 +2H 2 O，NH 4 Cl can also be replaced by NH 4 NO 3 And NH 4 Ac) and then the calcium element in the solid raw material is treated by water-soluble Ca 2+ Extracting ion form into water solution, releasing ammonia gas, recovering, filtering to obtain Ca-containing solution 2+ Filtering the ion filtrate and the oil shale solid waste filter residue with calcium removed, and then carrying out the reaction to obtain carbon dioxide and NH 3 Introducing Ca into the gas 2+ The calcium carbonate (reaction equation: ca) is prepared in the solution under alkaline condition 2+ +2NH 3 +H 2 O+CO 2 →CaCO 3 ↓+2NH 4 + ) Filtering the reaction solution to obtain a calcium carbonate product, wherein the filtrate is a circulating mother solution A, and the recovered circulating mother solution A is recycled; then extracting silicon component in the oil shale solid waste for the second time, adding the filter residue obtained after the first extraction into another ammonium salt solution (circulating mother solution B), performing a second ammonia distillation reaction, recovering distilled ammonia gas, and filtering to obtain a solution rich in water-soluble silicon compound (SiF) 6 - ) Introducing ammonia gas into the obtained filtrate rich in silicon compounds to prepare silicon dioxide, and filtering to obtain filtrate which is recycled as a circulating mother liquor B, wherein the filter residue is a silicon dioxide product; in the above reaction, ammonium saltBy NH 4 + →NH 3 ∈and inverse process NH thereof 3 ↑→NH 4 + Recycling, CO 2 The gas is recycled, and solid residues such as components which cannot be extracted in the raw materials can be used as building materials, aluminum smelting raw materials and the like, so that the process basically has no byproducts, and the reaction process is green.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.

Claims (4)

1. A method for extracting a plurality of products by utilizing oil shale semicoke or oil shale ash in a grading way, which is characterized by comprising the following steps:
s1, collecting oil shale semicoke or oil shale ash as raw materials, and crushing the raw materials for later use;
s2, extracting a calcium carbonate product and/or a silicon dioxide product by using the crushed raw materials;
in the step S2, when only the calcium carbonate product is extracted, the specific steps are as follows:
S2A1, placing the crushed raw materials into a calciner for calcination treatment to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2A2, adding the calcined powder prepared in the step S2A1 into a circulating mother liquor A, wherein the circulating mother liquor A is an aqueous solution containing ammonium chloride or ammonium nitrate or ammonium acetate, heating to perform an ammonia distillation reaction, recovering the generated ammonia gas into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain a filtrate A rich in water-soluble calcium salt and a solid residue I after calcium extraction;
S2A3, introducing the carbon dioxide gas prepared in the step S2A1 and the ammonia gas prepared in the step S2A2 into the filtrate A rich in water-soluble calcium salt, wherein Ca 2+ The ions undergo a precipitation reaction, the precipitate is calcium carbonate, the reaction solution is filtered after the reaction is finished, and filter residues are collected to obtain a calcium carbonate product;
in the step S2, when only the silica product is extracted, the specific steps are as follows:
S2B1, placing the crushed raw materials into a calciner to be calcined to obtain calcined powder or directly adding the crushed raw materials into a circulating mother liquor B, wherein the circulating mother liquor B is an aqueous solution containing ammonium fluoride, carrying out ammonia distillation and extraction reaction, recovering released ammonia into an ammonia gas collecting tank, filtering after the reaction is finished to obtain a filtrate B and a solid residue II, and the filtrate B is a solution rich in Si compounds;
S2B2, introducing the ammonia gas obtained in the step S2B1 into the filtrate B to obtain silica precipitate, filtering after the reaction is finished, and collecting filter residues to obtain a silica product;
in the step S2, when extracting the calcium carbonate product and the silicon dioxide product, the specific steps are as follows:
S2C1, placing the crushed raw materials into a calciner for calcination treatment to obtain calcined powder, and recovering carbon dioxide gas generated in the calcination process;
S2C2, adding the calcined powder prepared in the step S2C1 into a circulating mother liquor A, wherein the circulating mother liquor A is an aqueous solution containing ammonium chloride or ammonium nitrate or ammonium acetate, heating to perform an ammonia distillation reaction, recovering the generated ammonia gas into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain a filtrate A rich in water-soluble calcium salt and a solid residue I after calcium extraction;
S2C3, adding the solid residue I obtained in the step S2C2 into a circulating mother liquor B, wherein the circulating mother liquor B is an aqueous solution containing ammonium fluoride, carrying out an ammonia distillation extraction reaction, recovering released ammonia into an ammonia gas collecting tank, and filtering after the reaction is finished to obtain a filtrate B and a solid residue II, and the filtrate B is a solution rich in Si compounds;
S2C4, introducing the carbon dioxide gas prepared in the step S2C1 and the ammonia gas prepared in the step S2C2 into the filtrate A rich in water-soluble calcium salt, wherein Ca 2+ The ions undergo a precipitation reaction, the precipitate is calcium carbonate, the reaction solution is filtered after the reaction is finished, and filter residues are collected to obtain a calcium carbonate product;
S2C5, introducing the ammonia gas obtained in the step S2C3 into the filtrate B to obtain silica precipitate, filtering after the reaction is finished, and collecting filter residues to obtain a silica product.
2. The method for extracting a plurality of products by utilizing oil shale semicoke or oil shale ash classification as claimed in claim 1, wherein the method comprises the following steps of: the ammonia distillation reaction is carried out at 85-105 ℃.
3. The method for extracting a plurality of products by utilizing oil shale semicoke or oil shale ash classification as claimed in claim 1, wherein the method comprises the following steps of: the Ca is 2+ The ion precipitation reaction is carried out at 40-120 ℃.
4. The method for extracting a plurality of products by utilizing oil shale semicoke or oil shale ash classification as claimed in claim 1, wherein the method comprises the following steps of: the silica precipitation is carried out at 40-90 ℃.
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US20020144928A1 (en) * 2001-01-29 2002-10-10 Bronshtein Alexander P. Energy efficient process for converting refinery and petroleum-based waste to standard fuels
CN100484873C (en) * 2007-04-29 2009-05-06 东北大学 Method for preparing white carbon black by using oil shale ash
CN100560499C (en) * 2008-03-18 2009-11-18 抚顺矿业集团有限责任公司 A kind of method of from bituminous shale waste slag, extracting aluminum oxide and white carbon black
CN101254922A (en) * 2008-04-01 2008-09-03 大连理工大学 Method for preparing modified white carbon black by using oil shale oil-making residual
CN101693538B (en) * 2009-09-30 2011-05-11 渤海大学 Method for preparing white carbon black by using waste bauxite, diatomite and oil shale residue
CN103395793B (en) * 2013-07-22 2015-04-22 沈阳鑫博工业技术股份有限公司 Method for preparing aluminum oxide and white carbon black by utilizing oil shale ash

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