Rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar

Abstract

The utility model provides rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar, which adopts five solvent storage tanks to store and take recovered solvents (acetone, carbon disulfide, petroleum ether, methanol and acetonitrile) in each step so as to be recycled in cycles; carrying out deliming treatment on the medium-low temperature coal tar by using an acetone / carbon disulfide mixed solvent; petroleum ether and methanol, petroleum ether and acetonitrile, and methanol and carbon disulfide are used for carrying out step-by-step double-solvent layered extraction on the de-ashed tar. The device disclosed by the utility model realizes rapid enrichment of target components in medium and low temperature coal tar, provides extract oil which is simple in composition and easy to process for subsequent secondary upgrading, and solves the problems of high energy consumption, difficulty in large-scale commercialization and the like in the prior art.

Description

Technical Field

[0001] The utility model relates to the technical field of coal chemical industry, and particularly relates to a rapid enrichment device for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar. Background Art

[0002] Medium and low temperature coal tar is a by-product in the production process of coal semi-coke, mainly composed of aliphatic hydrocarbons, aromatic hydrocarbons, phenols and asphaltenes, and also contains a small amount of nitrogen / sulfur-containing species and C=O group compounds, such as aldehydes, ketones, carboxylic acids, esters, etc. The rich valuable group components endow medium and low temperature coal tar with unique advantages as an important chemical raw material for obtaining various fine chemicals. However, some undesirable characteristics, such as high moisture and ash content, high viscosity, and high compositional complexity, increase the difficulty and cost of extracting value-added downstream products. The limitation of the traditional distillation method that splits according to boiling point is that the composition of each fraction is still highly complex, and the interweaving or entrainment of group components makes it impossible to selectively choose a scientific and reasonable upgrading scheme. Currently, non-selective catalytic hydrorefining and other methods are mostly used to convert it into refined oil and then perform composition splitting and sales. The sales volume is greatly affected by the fluctuations in the fuel oil market, and the economic benefits need to be improved. Therefore, it is necessary to develop a reasonable rapid enrichment process technology to effectively split group components according to the composition distribution characteristics, and then select a suitable upgrading processing scheme according to the compositional differences of each enriched oil, so as to significantly improve the value-added utilization level of medium and low temperature coal tar and improve economic benefits.

[0003] In the current technology, medium and low temperature coal tar is mainly separated and processed by the following several methods:

[0004] The first method is the distillation process technology that splits fractions according to the boiling point difference, and the obtained are various tar fractions in different temperature ranges, and its intrinsic properties depend on the boiling point differences of each fraction. Therefore, the composition of the derived oil products obtained by this process technology still mainly contains the above-mentioned various group components. Due to the boiling point overlap area between various group components, the complexity of the composition is related to the entrainment between various species during the distillation process. In other words, the secondary upgrading processing of these tar fractions is still difficult. In addition, the boiling range of medium and low temperature coal tar is relatively wide, and the temperature range for full-component splitting is from room temperature to 500°C. The high energy consumption and the easy generation of coking and other adverse phenomena during the high-temperature operation make this strategy to be optimized. The current mode has certain drawbacks and is not conducive to the fine utilization of medium and low temperature coal tar.

[0005] The second method is an extraction process technology for component separation according to the solubility differences of different compounds. The obtained extraction oils have various component distributions of different groups, and their intrinsic properties depend on the extraction characteristics of the solvents used. This process technology often uses organic solvents with low boiling points and easy recovery, such as petroleum ether, n-heptane, methanol, ethanol, carbon disulfide, acetone, ethyl acetate, acetonitrile, dichloromethane, etc. Column chromatography under normal pressure / medium pressure / high pressure is carried out on the obtained extraction oils, and the enrichment and purification of various group components are achieved by modulating the mobile phase. On the one hand, this process usually uses single-solvent extraction (single-pass or step-by-step). The strong interaction between group components leads to a decrease in the proportion of target components and the loss of valuable compounds, and the extraction selectivity needs to be improved. On the other hand, the long processing flow results in low processing efficiency and a single product form that can be obtained, making large-scale production difficult.

[0006] Therefore, it is particularly urgent to develop a process technology and related equipment that can not only efficiently separate light hydrocarbon oil, medium hydrocarbon oil, and crude phenol from medium and low-temperature coal tar but also make full use of these group components. This new process technology not only needs to achieve the rapid enrichment of target components in medium and low-temperature coal tar to provide extraction oils with simple compositions and easy processing for subsequent secondary upgrading but also solve problems such as high energy consumption and difficulty in large-scale commercialization of existing technologies, enriching medium and low-temperature coal tar-derived products in a green, environmentally friendly, economical, and efficient manner and enhancing their value-added utilization space. Summary of the Utility Model

[0007] To solve the above defects, the present utility model provides a device for rapid enrichment of light hydrocarbon oil, medium hydrocarbon oil, and crude phenol in medium and low-temperature coal tar. The present utility model realizes the rapid enrichment of target components in medium and low-temperature coal tar, provides extraction oils with simple compositions and easy processing for subsequent secondary upgrading, and at the same time solves problems such as high energy consumption and difficulty in large-scale commercialization of existing technologies.

[0008] The utility model provides a rapid enrichment device for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar, which comprises: a first extraction kettle (1), a first rectification kettle (2), a second extraction kettle (3), a third extraction kettle (4), a fourth extraction kettle (5), a second rectification kettle (6), a third rectification kettle (7), a fourth rectification kettle (8), a fifth rectification kettle (9), a first storage tank (10), a second storage tank (11), a third storage tank (12), a fourth storage tank (13), a fifth storage tank (14), a buffer tank (15) and a horizontal tube heat exchanger (39). The top of the first extraction kettle (1) is respectively connected with the fourth storage tank (13) and the fifth storage tank (14) through pipelines, and the bottom of the first extraction kettle (1) is connected with the first rectification kettle (2) through a pipeline; the top of the first rectification kettle (2) is connected with the horizontal tube heat exchanger (39) through a pipeline, and the bottom of the first rectification kettle (2) is connected with the second extraction kettle (3) through a pipeline; the top of the second extraction kettle (3) is respectively connected with the second storage tank (11) and the third storage tank (12) through pipelines, and the bottom of the second extraction kettle (3) is respectively connected with the third extraction kettle (4) and the fourth extraction kettle (5) through pipelines; the top of the third extraction kettle (4) is connected with the first storage tank (10) through a pipeline, and the bottom of the third extraction kettle (4) is connected with the second rectification kettle (6) and the third rectification kettle (7) through pipelines; the top of the fourth extraction kettle (5) is connected with the fifth storage tank (14) through a pipeline, and the bottom of the fourth extraction kettle (5) is connected with the fourth rectification kettle (8) and the fifth rectification kettle (9) through pipelines; the tops of the second rectification kettle (6), the third rectification kettle (7), the fourth rectification kettle (8) and the fifth rectification kettle (9) are respectively connected with the horizontal tube heat exchanger (39), the horizontal tube heat exchanger (39) is connected with the buffer tank (15), and the buffer tank (15) is respectively connected with the first storage tank (10), the second storage tank (11), the third storage tank (12), the fourth storage tank (13) and the fifth storage tank (14).

[0009] Preferably, the first extraction kettle (1) is provided with a magnetic stirring device (19), a coarse filter plate (84) and a fine filter plate (85). The upper part of the first extraction kettle (1) is provided with a feeding tank (28) and a pressure gauge (30), and the lower part of the first extraction kettle (1) is provided with a discharging tank (29).

[0010] Preferably, the second extraction kettle (3), the third extraction kettle (4) and the fourth extraction kettle (5) are all provided with a magnetic stirring device and an observation window for observing the extraction liquid level.

[0011] Preferably, pressure gauges are arranged on the upper parts of the second extraction kettle (3), the third extraction kettle (4) and the fourth extraction kettle (5).

[0012] Preferably, the first rectification kettle (2), the second rectification kettle (6), the third rectification kettle (7), the fourth rectification kettle (8) and the fifth rectification kettle (9) are all provided with a supporting heating device and a magnetic stirring device.

[0013] Preferably, pressure gauges are provided on the tops of the No. 1 distillation kettle (2), the No. 2 distillation kettle (6), the No. 3 distillation kettle (7), the No. 4 distillation kettle (8) and the No. 5 distillation kettle (9).

[0014] Preferably, the valve pipeline of the horizontal shell-and-tube heat exchanger (39) is connected to the buffer tank (15) via an oil pump (17).

[0015] In summary, the utility model provides a process and equipment for rapidly enriching light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar. The beneficial effects of the utility model are:

[0016] Due to the adoption of the above scheme, acetone, carbon disulfide, petroleum ether, methanol and acetonitrile with boiling points below 100°C are used as extractants, which is conducive to the recycling of solvents after rapid enrichment. Compared with traditional high-boiling point single solvent extraction, the combination of low-boiling point dual solvents is more flexible and diverse, and has lower toxicity, and can adapt to a variety of substrates or a variety of complex extraction scenarios; the extraction operation is carried out at room temperature, which significantly reduces energy consumption, and no three wastes are generated, which can effectively avoid environmental pollution; 4 types of dual solvent systems are combined with 5 kinds of extractants and applied to the extraction of medium and low temperature coal tar. Only three steps are required to obtain three types of valuable secondary oil products, namely light hydrocarbon oil (aliphatic hydrocarbons), medium hydrocarbon oil (aromatic hydrocarbons) and crude phenol (phenols), with high extraction efficiency. While effectively separating out valuable family components, it enriches the types of secondary oil products and improves the complexity of oil product composition, thereby reducing the difficulty and cost of subsequent secondary quality improvement. Among them, light hydrocarbon oil is rich in aliphatic hydrocarbons, which can be distilled into downstream products such as naphtha, gasoline / diesel, paraffin, etc.; medium hydrocarbon oil is rich in aromatic hydrocarbons, and can be obtained by extraction / distillation / column chromatography / recrystallization to obtain the corresponding pure products, or by catalytic hydrogenation to obtain alkylcycloalkanes, which can then be used to prepare high-density liquid fuels; crude phenol is rich in various phenol monomers, which can be obtained by extraction / distillation / column chromatography / recrystallization to obtain the corresponding pure products, or by selective hydrogenation to obtain alkylcycloalkanols, which can then be used in medicine, agriculture, forestry, animal husbandry and other fields. Ash can be used in adsorption materials or combustion power generation. This process has the characteristics of being green and mild, no three wastes discharged, short production cycle, easy continuous production, and high product added value. The combination of extractants can be flexibly adjusted according to the distribution characteristics of oil components to obtain various value-added oil products in a targeted manner. It is an innovative process path for efficient utilization of medium and low temperature coal tar.

[0017] The utility model obtains three types of secondary oil products, including light hydrocarbon oil, medium hydrocarbon oil and crude phenol. Downstream products such as naphtha, gasoline / diesel oil, paraffin wax, etc. can be obtained from the light hydrocarbon oil; fine chemicals such as alkylbenzene, alkylnaphthalene, alkylanthracene / phenanthrene, etc. can be obtained from the medium hydrocarbon oil, and alkyl cycloalkanes can also be obtained through catalytic hydrorefining and then used to prepare high-density liquid fuels; fine chemicals such as phenol, alkylphenol, alkoxyphenol, etc. can be obtained from the crude phenol, and alkyl cycloalkanols can also be obtained through selective hydrogenation conversion. These downstream products can be widely used in the fields of energy, chemical industry, medicine, agriculture, forestry and animal husbandry. The flexible and variable oil product properties and diverse downstream conversion paths indicate that this process technology has good effects in treating medium and low temperature coal tar and potential for future promotion.

[0018] The process of the utility model is simple to operate and has mild conditions, and has the characteristics of being green, environmentally friendly, economical, efficient, low energy consumption and short production cycle. Through the intelligent control platform, different components can be separated directionally and reasonably according to the differences in the properties of different oil products, effectively improving the production efficiency and product diversity. Description of the Drawings

[0019] Figure 1 Schematic structural diagram of the rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar provided in Example 1;

[0020] Figure 2 Flow chart of the rapid enrichment process for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar provided in Example 1.

[0021] Description of the main element symbols:

[0022] 1. First extraction kettle; 2. First rectification kettle; 3. Second extraction kettle; 4. Third extraction kettle; 5. Fourth extraction kettle; 6. Second rectification kettle; 7. Third rectification kettle; 8. Fourth rectification kettle; 9. Fifth rectification kettle; 10. First storage tank; 11. Second storage tank; 12. Third storage tank; 13. Fourth storage tank; 14. Fifth storage tank; 15. Buffer tank; 16. First air compressor pump; 17. Buffer tank oil pump; 18. Second air compressor pump; 19. Magnetic stirring device of the first extraction kettle; 20. Magnetic stirring device of the first rectification kettle; 21. Magnetic stirring device of the second extraction kettle; 22. Magnetic stirring device of the third extraction kettle; 23. Magnetic stirring device of the fourth extraction kettle; 24. Magnetic stirring device of the second rectification kettle; 25. Magnetic stirring device of the third rectification kettle; 26. Magnetic stirring device of the fourth rectification kettle; 27. Magnetic stirring device of the fifth rectification kettle; 28. Feeding tank of the extraction kettle; 29. Discharge tank of the extraction kettle; 30. Pressure gauge of the first extraction kettle; 31. Pressure gauge of the first rectification kettle; 32. Pressure gauge of the second extraction kettle; 33. Pressure gauge of the third extraction kettle; 34. Pressure gauge of the fourth extraction kettle; 35. Pressure gauge of the second rectification kettle; 36. Pressure gauge of the third rectification kettle; 37. Pressure gauge of the fourth rectification kettle; 38. Pressure gauge of the fifth rectification kettle; 39. Horizontal shell-and-tube heat exchanger; 40. Control platform; 41. First valve; 42. Second valve; 43. Third valve; 44. Fourth valve; 45. Fifth valve; 46. Sixth valve; 47. Seventh valve; 48. Eighth valve; 49. Ninth valve; 50. Tenth valve; 51. Eleventh valve; 52. Twelfth valve; 53. Thirteenth valve; 54. Fourteenth valve; 55. Fifteenth valve; 56. Sixteenth valve; 57. Seventeenth valve; 58. Eighteenth valve; 59. Nineteenth valve; 60. Twentieth valve; 61. Twenty-first valve; 62. Twenty-second valve; 63. Twenty-third valve; 64. Twenty-fourth valve; 65. Twenty-fifth valve; 66. Twenty-sixth valve; 67. Twenty-seventh valve; 68. Twenty-eighth valve; 69. Twenty-ninth valve; 70. Thirtieth valve; 71. Thirty-first valve; 72. First three-way valve; 73. Second three-way valve; 74. Third three-way valve; 75. Fourth three-way valve; 76. Fifth three-way valve; 77. Sixth three-way valve; 78. Seventh three-way valve; 79. Eighth three-way valve; 80. Ninth three-way valve; 81. Tenth three-way valve; 82. Eleventh three-way valve; 83. Twelfth three-way valve; 84. Coarse filter sleeve; 85. Fine filter plate; 86. Observation window of the second extraction kettle; 87. Observation window of the third extraction kettle; 88. Observation window of the fourth extraction kettle. Detailed implementation manners

[0023] Combined with the process flow in the appendix Figure 1 and the schematic diagram of the equipment structure in the appendix Figure 2 the following embodiments are detailedly proposed to illustrate the present utility model in detail.

[0024] The separation process proposed by the present utility model is not limited to medium and low temperature coal tar. Those skilled in the art can easily understand the purpose of the present utility model and extend and apply the present utility model to the upgrading of other chemical raw materials, including petroleum, heavy oil, oil sludge, tar residue, organic waste liquid and other various chemical organic waste liquids, etc. However, as long as it does not depart from the spirit of the present utility model, it is within the protection scope of the present utility model.

[0025] Example 1

[0026] As Figure 1 shown, the rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar includes: a first extraction kettle 1, a first rectification kettle 2, a second extraction kettle 3, a third extraction kettle 4, a fourth extraction kettle 5, a second rectification kettle 6, a third rectification kettle 7, a fourth rectification kettle 8, a fifth rectification kettle 9, a first storage tank 10, a second storage tank 11, a third storage tank 12, a fourth storage tank 13, a fifth storage tank 14, a buffer tank 15 and a horizontal tube heat exchanger 39. The top of the first extraction kettle 1 is respectively connected to the fourth storage tank 13 and the fifth storage tank 14 through pipelines; the bottom of the first extraction kettle 1 is connected to the first rectification kettle 2 through a pipeline; the top of the first rectification kettle 2 is connected to the horizontal tube heat exchanger 39 through a pipeline, and the bottom of the first rectification kettle 2 is connected to the second extraction kettle 3 through a pipeline; the top of the second extraction kettle 3 is respectively connected to the second storage tank 11 and the third storage tank 12 through pipelines, and the bottom of the second extraction kettle 3 is respectively connected to the third extraction kettle 4 and the fourth extraction kettle 5 through pipelines; the top of the third extraction kettle 4 is connected to the first storage tank 10 through a pipeline, and the bottom of the third extraction kettle 4 is connected to the second rectification kettle 6 and the third rectification kettle 7 through pipelines; the top of the fourth extraction kettle 5 is connected to the fifth storage tank 14 through a pipeline, and the bottom of the fourth extraction kettle 5 is connected to the fourth rectification kettle 8 and the fifth rectification kettle 9 through pipelines; the tops of the second rectification kettle 6, the third rectification kettle 7, the fourth rectification kettle 8 and the fifth rectification kettle 9 are respectively connected to the horizontal tube heat exchanger 39, the horizontal tube heat exchanger 39 is connected to the buffer tank 15, and the buffer tank 15 is respectively connected to the first storage tank 10, the second storage tank 11, the third storage tank 12, the fourth storage tank 13 and the fifth storage tank 14.

[0027] The upper part of the first extraction kettle 1 is provided with an extraction kettle feeding tank 28 with six valves 46, a first extraction kettle pressure gauge 30 and a first extraction kettle magnetic stirring device 19. The upper part of the first extraction kettle 1 is connected to the fourth storage tank 13 and the fifth storage tank 14 through four valves 44, five valves 45, a sixth three-way valve 77 and related pipelines; the inner layer of the first extraction kettle 1 is provided with a coarse filter sleeve 84 and a fine filter plate 85. The side of the first extraction kettle 1 is connected to an external control platform 40, and the bottom is provided with an extraction kettle discharge tank 29 connected to a seven-valve 47, and is connected to the upper part of the first rectification kettle 2 through an eight-valve 48 and related pipelines;

[0028] On the upper part of the first rectification kettle 2, there is a magnetic stirring device 20 for the first rectification kettle, a pressure gauge 31 for the first rectification kettle, and a vent connected to nine valves 49; on the upper part of the first rectification kettle 2, it is connected to the left part of the horizontal tube heat exchanger 39 through ten valves 50, a seventh three-way valve 78 and relevant pipelines; the outer layer of the first rectification kettle 2 is a heating device for the rectification kettle and is connected to an external control platform 40 on the side; on the lower part of the first rectification kettle 2, it is connected to the upper part of the second extraction kettle 3 through eleven valves 51, an eighth three-way valve 79 and relevant pipelines;

[0029] On the upper part of the second extraction kettle 3, there is a magnetic stirring device 21 for the second extraction kettle, a pressure gauge 32 for the second extraction kettle, and a vent connected to twelve valves 52; on the upper part of the second extraction kettle 3, it is connected to the second storage tank 11 and the third storage tank 12 through two valves 42, three valves 43, an eighth three-way valve 79 and relevant pipelines; on the side of the second extraction kettle 3, there is an observation window 86 for the second extraction kettle and it is connected to an external control platform 40; on the lower part of the second extraction kettle 3, it is connected to the upper parts of the third extraction kettle 4 and the fourth extraction kettle 5 through fourteen valves 54, sixteen valves 56, and eighteen valves 58;

[0030] On the upper part of the third extraction kettle 4, there is a magnetic stirring device 22 for the third extraction kettle, a pressure gauge 33 for the third extraction kettle, and a vent connected to fifteen valves 55; on the upper part of the third extraction kettle 4, it is connected to the first storage tank 10 through one valve 41, thirteen valves 53 and relevant pipelines; on the side of the third extraction kettle 4, there is an observation window 87 for the third extraction kettle and it is connected to an external control platform 40; on the lower part of the third extraction kettle 4, it is connected to the relevant valve pipelines of the air compressor 16 through twenty valves 60;

[0031] On the upper part of the fourth extraction kettle 5, there is a magnetic stirring device 23 for the fourth extraction kettle, a pressure gauge 34 for the fourth extraction kettle, and a vent connected to seventeen valves 57; on the upper part of the fourth extraction kettle 5, it is connected to the fifth storage tank 14 through nineteen valves 59, a sixth three-way valve 77 and relevant pipelines; on the side of the fourth extraction kettle 5, there is an observation window 88 for the fourth extraction kettle and it is connected to an external control platform 40; on the lower part of the fourth extraction kettle 5, it is connected to the relevant valve pipelines of the first air compressor 16 through twenty - one valves 61;

[0032] On the upper part of the second rectification kettle 6, there is a magnetic stirring device 24 for the second rectification kettle and a pressure gauge 35 for the second rectification kettle; on the upper part of the second rectification kettle 6, it is connected to the left part of the horizontal tube heat exchanger 39 through twenty - two valves 62, a seventh three - way valve 78 and relevant pipelines, and the inlet pipeline at the upper part is connected to the relevant valve pipelines of the first air compressor 16 through a ninth three - way valve 80; the outer layer of the second rectification kettle 6 is a heating device for the rectification kettle and is connected to an external control platform 40 on the side; at the bottom of the second rectification kettle 6, there is a discharge port connected through twenty - six valves 66;

[0033] On the upper part of the third distillation kettle 7, there are a magnetic stirring device 25 for the third distillation kettle and a pressure gauge 36 for the third distillation kettle; the upper part of the third distillation kettle 7 is connected to the left part of the horizontal shell-and-tube heat exchanger 39 through a twenty-third valve 63, a seventh three-way valve 78 and relevant pipelines, and the inlet pipeline at the upper part is connected to the relevant valve pipelines of the first air compressor 16 through a tenth three-way valve 81; the outer layer of the third distillation kettle 7 is a heating device for the distillation kettle and is connected to an external control platform 40 on the side; the bottom is provided with a discharge port connected through a twenty-seventh valve 67;

[0034] On the upper part of the fourth distillation kettle 8, there are a magnetic stirring device 26 for the fourth distillation kettle and a pressure gauge 37 for the fourth distillation kettle; the upper part of the fourth distillation kettle 8 is connected to the left part of the horizontal shell-and-tube heat exchanger 39 through a twenty-fourth valve 64, a seventh three-way valve 78 and relevant pipelines, and the inlet pipeline at the upper part is connected to the relevant valve pipelines of the first air compressor 16 through an eleventh three-way valve 82; the outer layer of the fourth distillation kettle 8 is a heating device for the distillation kettle and is connected to an external control platform 40 on the side; the bottom of the fourth distillation kettle 8 is provided with a discharge port connected through a twenty-eighth valve 68;

[0035] On the upper part of the fifth distillation kettle 9, there are a magnetic stirring device 27 for the fifth distillation kettle and a pressure gauge 38 for the fifth distillation kettle; the upper part of the fifth distillation kettle 9 is connected to the left part of the horizontal shell-and-tube heat exchanger 39 through a twenty-fifth valve 65, a seventh three-way valve 78 and relevant pipelines, and the inlet pipeline at the upper part is connected to the relevant valve pipelines of the first air compressor 16 through a twelfth three-way valve 83; the outer layer of the fifth distillation kettle 9 is a heating device for the distillation kettle and is connected to an external control platform 40 on the side; the bottom of the fifth distillation kettle 9 is provided with a discharge port connected through a twenty-ninth valve 69;

[0036] The right side of the horizontal shell-and-tube heat exchanger 39 is connected to the top of the buffer tank 15 through a buffer tank oil pump 17; the bottom of the buffer tank 15 is connected to the relevant valve pipelines of the first air compressor 16 through a thirty-first valve 71 and relevant pipelines;

[0037] The upper part of the first storage tank 10 is connected to the second air compressor 18 through a valve pipeline with a first three-way valve 72; the upper part of the second storage tank 11 is connected to the second air compressor 18 through a valve pipeline with a second three-way valve 73; the upper part of the third storage tank 12 is connected to the second air compressor 18 through a valve pipeline with a third three-way valve 74; the upper part of the fourth storage tank 13 is connected to the second air compressor 18 through a valve pipeline with a fourth three-way valve 75; the upper part of the fifth storage tank 14 is connected to the second air compressor 18 through a valve pipeline with a fifth three-way valve 76.

[0038] Example 2

[0039] A rapid enrichment process for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in low-temperature coal tar, which uses five solvent storage tanks to store the recovered solvents (acetone, carbon disulfide, petroleum ether, methanol, acetonitrile) in each step for cyclic use; uses an acetone / carbon disulfide mixed solvent to deash the medium and low-temperature coal tar; and uses petroleum ether and methanol, petroleum ether and acetonitrile, and methanol and carbon disulfide to perform step-by-step double-solvent fractional extraction on the deashed tar. As Figure 2 shown, the specific steps are as follows:

[0040] Step 1: Place the raw medium and low-temperature coal tar into the first extraction kettle 1 through the extraction kettle feeding trough 28, and transport the acetone and carbon disulfide mixed solvent to the first extraction kettle 1 according to a volume ratio of 1:1 to deash the medium and low-temperature coal tar to obtain ash; evaporate the solvent in the first rectification kettle 2 to obtain deashed tar;

[0041] Step 2: Transport the deashed tar to the second extraction kettle 3, and perform fractional extraction with petroleum ether and methanol to obtain the upper phase (petroleum ether) and transport it to the third extraction kettle 4, and the lower phase (methanol) and transport it to the fourth extraction kettle 5; perform fractional extraction with petroleum ether and acetonitrile, and methanol and carbon disulfide in the third extraction kettle 4 and the fourth extraction kettle 5 respectively to obtain a petroleum ether phase, an acetonitrile phase, a methanol phase and a carbon disulfide phase;

[0042] Step 3: Transport the acetonitrile phase to the second rectification kettle 6, and evaporate the solvent in the second rectification kettle 6 to obtain medium hydrocarbon oil (acetonitrile-soluble matter); transport the petroleum ether phase to the third rectification kettle 7, and evaporate the solvent in the third rectification kettle 7 to obtain light hydrocarbon oil (petroleum ether-soluble matter); transport the carbon disulfide phase to the fourth rectification kettle 8, and evaporate the solvent in the fourth rectification kettle 8 to obtain medium hydrocarbon oil (carbon disulfide-soluble matter); transport the methanol phase to the fifth rectification kettle 9, and evaporate the solvent in the fifth rectification kettle 9 to obtain crude phenol (methanol-soluble matter).

[0043] In the said Step 1:

[0044] Step 1-1: Add the raw medium and low-temperature coal tar to the first extraction kettle 1 through the extraction kettle feeding trough 28, and close the six valves 46 of the extraction kettle feeding trough 28;

[0045] Step 1-2: Open the four-way valve 44, the five-way valve 45 and the upper and lower passages of the six-way three-way valve 77. Transport equal volumes of acetone stored in the fourth storage tank 13 and carbon disulfide stored in the fifth storage tank 14 to the first extraction kettle 1. Close the four-way valve 44, the five-way valve 45 and the upper and lower passages of the six-way three-way valve 77;

[0046] Step 1-3: Operate the control platform 40 of the first extraction kettle 1, start the magnetic stirring program, and stir for 10-30 minutes. Separate the solid-liquid two phases by using the coarse filter sleeve 84 and the fine filter plate 85. The solid phase is ash, and the liquid phase is a mixture of soluble matter and solvent;

[0047] Step 1-4: The liquid phase flows into the first distillation kettle 2 through the eight-way valve 48. When there is no liquid flowing through, close the eight-way valve 48. Open the seven-way valve 47, take out the ash residue (solid phase) from the extraction kettle discharge tank 29, and then close the seven-way valve 47;

[0048] Step 1-5: Operate the control platform 40 of the first distillation kettle 2, start the heating and magnetic stirring programs, and stir at the set temperature (boiling point of carbon disulfide). Open the ten-way valve 50 and the left and right passages of the seven-way three-way valve 78, and start the horizontal shell-and-tube heat exchanger 39. Use the buffer tank oil pump 17 to transport the condensed and recovered carbon disulfide solvent to the buffer tank 15;

[0049] Step 1-6: Observe the liquid level of the buffer tank 15, and open the thirty-first valve 71 and the lower right passage of the five-way three-way valve 76. Use the second air compression pump 18 to transport the condensed and recovered carbon disulfide solvent to the fifth storage tank 14 for storage and standby. When there is no recovered solvent flowing out, close the thirty-first valve 71 and the lower right passage of the five-way three-way valve 76;

[0050] Step 1-7: Operate the control platform 40 of the first distillation kettle 2 to raise the temperature to near the boiling point of acetone. Use the buffer tank oil pump 17 to transport the condensed and recovered acetone solvent to the buffer tank 15;

[0051] Step 1-8: Observe the liquid level of the buffer tank 15, open the thirty-first valve 71, the lower right passage of the four-way three-way valve 75 and the left and right passages of the five-way three-way valve 76. Use the second air compression pump 18 to transport the condensed and recovered acetone solvent to the fourth storage tank 13 for storage and standby. When there is no recovered solvent flowing out, close the thirty-first valve 71, the lower right passage of the four-way three-way valve 75 and the left and right passages of the five-way three-way valve 76;

[0052] Step 1-9: Operate the control platform 40 of the first distillation kettle 2 to turn off the heating and magnetic stirring programs, turn off the horizontal shell-and-tube heat exchanger 39, and close the ten-way valve 50 and the left and right passages of the seven-way three-way valve 78. At this time, the remaining substance in the first distillation kettle 2 is deashed tar.

[0053] In the second step:

[0054] Step 2-1: Open the eleven-way valve 51 and the upper and lower passages of the eight-way three-way valve 79, transport the deashed tar in the first distillation kettle 2 to the second extraction kettle 3, and then close the eleven-way valve 51 and the upper and lower passages of the eight-way three-way valve 79. Open the two-way valve 42, the three-way valve 43 and the lower left passage of the eight-way three-way valve 79, and transport the methanol stored in the second storage tank 11 and the petroleum ether stored in the third storage tank 12 to the second extraction kettle 3 according to a certain volume ratio (petroleum ether / methanol = 3 / 1, 2 / 1 or 1 / 1), and then close the two-way valve 42, the three-way valve 43 and the lower left passage of the eight-way three-way valve 79;

[0055] Step 2-2: Operate the control platform 40 of the second extraction kettle 3, start the magnetic stirring program, and stir at room temperature for 10 - 30 min. After completion, operate the control platform 40 of the second extraction kettle 3 to turn off the magnetic stirring program, and let it stand for 10 - 30 min until liquid phase separation occurs;

[0056] Step 2-3: Open the sixteenth valve 56 and the eighteenth valve 58, monitor the liquid level in the second extraction kettle 3 through the observation window 86 of the second extraction kettle, transfer the lower phase (methanol) in the second extraction kettle 3 to the fourth extraction kettle 5, and then close the sixteenth valve 56 and the eighteenth valve 58;

[0057] Step 2-4: Open the fourteenth valve 54 and the sixteenth valve 56, monitor the liquid level in the second extraction kettle 3 through the observation window 86 of the second extraction kettle, transfer the upper phase (petroleum ether) in the second extraction kettle 3 to the third extraction kettle 4, and finally close the fourteenth valve 54 and the sixteenth valve 56;

[0058] Step 2-5: Open the first valve 41 and the thirteenth valve 53, transfer the acetonitrile stored in the first storage tank 10 to the third extraction kettle 4 according to a certain volume ratio (petroleum ether / acetonitrile = 3 / 1, 2 / 1 or 1 / 1), and then close the first valve 41 and the thirteenth valve 53;

[0059] Step 2-6: Open the nineteenth valve 59 and the upper right passage of the sixth three-way valve 77, transfer the carbon disulfide stored in the fifth storage tank 14 to the extraction kettle 5 according to a certain volume ratio (methanol / carbon disulfide = 3 / 1, 2 / 1 or 1 / 1), and then close the nineteenth valve 59 and the upper right passage of the sixth three-way valve 77;

[0060] Step 2-7: Operate the control platforms 40 of the third extraction kettle 4 and the fourth extraction kettle 5, start the magnetic stirring program, and extract at room temperature for 10 - 30 min. After completion, operate the control platforms 40 of the third extraction kettle 4 and the fourth extraction kettle 5 to turn off the magnetic stirring program, and let it stand for 10 - 30 min until liquid phase separation occurs;

[0061] Step 2-8: Open the twentieth valve 60 and the upper left passage of the ninth three-way valve 80, monitor the liquid level in the third extraction kettle 4 through the observation window 87 of the third extraction kettle, and use the first air compressor pump 16 to transfer the lower phase (acetonitrile) in the third extraction kettle 4 to the second rectification kettle 6 for storage and standby;

[0062] Step 2-9: Close the upper left passage of the ninth three-way valve 80, open the left and right passages of the ninth three-way valve 80 and the upper left passage of the tenth three-way valve 81, and use the first air compressor pump 16 to transfer the upper phase (petroleum ether) in the third extraction kettle 4 to the third rectification kettle 7 for storage and standby;

[0063] Step 2-10: Close the twentieth valve 60 and the upper left passage of the tenth three-way valve 81, open the twenty-first valve 61, the left and right passages of the tenth three-way valve 81, and the upper left passage of the eleventh three-way valve 82. Monitor the liquid level in the fourth extraction kettle 5 through the observation window 88 of the fourth extraction kettle, and use the first air compressor pump 16 to transport the lower phase (carbon disulfide) in the fourth extraction kettle 5 to the fourth rectification kettle 8 for storage and standby;

[0064] Step 2-11: Close the upper left passage of the eleventh three-way valve 82, open the left and right passages of the eleventh three-way valve 82 and the upper left passage of the twelfth three-way valve 83. Use the first air compressor pump 16 to transport the upper phase (methanol) in the fourth extraction kettle 5 to the fifth rectification kettle 9 for storage and standby. Close the twenty-first valve 61 and the upper left passage of the twelfth three-way valve 83. Open the left and right passages of the twelfth three-way valve 83 to vent the pipeline, and then close the left and right passages of the ninth three-way valve 80, the tenth three-way valve 81, the eleventh three-way valve 82, and the twelfth three-way valve 83.

[0065] In the said step three:

[0066] Step 3-1: Operate the control platform 40 of the second rectification kettle 6, start the heating and magnetic stirring programs, stir at the set temperature (boiling point of acetonitrile), open the twenty-second valve 62 and the lower right passage of the seventh three-way valve 78, start the horizontal shell-and-tube heat exchanger 39, and use the buffer tank oil pump 17 to transport the condensed acetonitrile solvent to the buffer tank 15. Observe the liquid level of the buffer tank 15, open the thirty-first valve 71, the lower right passage of the first three-way valve 72, and the left and right passages of the second three-way valve 73, the third three-way valve 74, the fourth three-way valve 75, and the fifth three-way valve 76. Use the second air compressor pump 18 to transport the recycled acetonitrile solvent to the first storage tank 10 for storage and standby;

[0067] Step 3-2: When no recycled solvent flows out, close the horizontal shell-and-tube heat exchanger 39, close the twenty-second valve 62 and the thirty-first valve 71, close the lower right passage of the first three-way valve 72 and the seventh three-way valve 78, and close the left and right passages of the second three-way valve 73, the third three-way valve 74, the fourth three-way valve 75, and the fifth three-way valve 76. At this time, the remaining substance in the second rectification kettle 6 is medium hydrocarbon oil;

[0068] Step 3-3: Operate the control platform 40 of the third rectification kettle 7, start the heating and magnetic stirring programs, stir at the set temperature (boiling point of petroleum ether), open the twenty-third valve 63 and the lower right passage of the seventh three-way valve 78, start the horizontal shell-and-tube heat exchanger 39, and use the buffer tank oil pump 17 to transport the condensed petroleum ether solvent to the buffer tank 15. Observe the liquid level of the buffer tank 15, open the thirty-first valve 71, the lower right passage of the third three-way valve 74, and the left and right passages of the fourth three-way valve 75 and the fifth three-way valve 76. Use the second air compressor pump 18 to transport the recycled petroleum ether solvent to the third storage tank 12 for storage and standby;

[0069] Step 3-4: When no recycled solvent flows out, close the horizontal shell-and-tube heat exchanger 39, close the twenty-third valve 63 and the thirty-first valve 71, close the lower right passages of the third three-way valve 74 and the seventh three-way valve 78, and close the left and right passages of the fourth three-way valve 75 and the fifth three-way valve 76. At this time, the remaining substance in the third distillation kettle 7 is light hydrocarbon oil;

[0070] Step 3-5: Operate the control platform 40 of the fourth distillation kettle 8, start the heating and magnetic stirring programs, stir at the set temperature (the boiling point of carbon disulfide), open the twenty-fourth valve 64 and the lower right passage of the seventh three-way valve 78, start the horizontal shell-and-tube heat exchanger 39, use the buffer tank oil pump 17 to transport the condensed carbon disulfide solvent to the buffer tank 15, observe the liquid level of the buffer tank 15, open the thirty-first valve 71 and the lower right passage of the fifth three-way valve 76, and use the second air compressor pump 18 to transport the recycled carbon disulfide solvent to the fifth storage tank 14 for storage and standby;

[0071] Step 3-6: When no recycled solvent flows out, close the horizontal shell-and-tube heat exchanger 39, close the twenty-fourth valve 64 and the thirty-first valve 71, close the lower right passages of the fifth three-way valve 76 and the seventh three-way valve 78. At this time, the remaining substance in the fourth distillation kettle 8 is medium hydrocarbon oil;

[0072] Step 3-7: Operate the control platform 40 of the fifth distillation kettle 9, start the heating and magnetic stirring programs, stir at the set temperature (the boiling point of methanol), open the twenty-fifth valve 65 and the lower right passage of the seventh three-way valve 78, start the horizontal shell-and-tube heat exchanger 39, use the buffer tank oil pump 17 to transport the condensed methanol solvent to the buffer tank 15, observe the liquid level of the buffer tank 15, open the thirty-first valve 71, the lower right passage of the second three-way valve 73, and the left and right passages of the third three-way valve 74, the fourth three-way valve 75, and the fifth three-way valve 76, and use the second air compressor pump 18 to transport the recycled methanol solvent to the second storage tank 11 for storage and standby;

[0073] Step 3-8: When no recycled solvent flows out, close the horizontal shell-and-tube heat exchanger 39, close the twenty-fifth valve 65 and the thirty-first valve 71, close the lower right passages of the second three-way valve 73 and the seventh three-way valve 78, and close the left and right passages of the third three-way valve 74, the fourth three-way valve 75, and the fifth three-way valve 76. At this time, the remaining substance in the fifth distillation kettle 9 is crude phenol;

[0074] Step 3-9: Open the twenty-seventh valve 67 to obtain light hydrocarbon oil, open the twenty-sixth valve 66 and the twenty-eighth valve 68 to obtain medium hydrocarbon oil, and open the twenty-ninth valve 69 to obtain crude phenol. Finally, close the twenty-sixth valve 66, the twenty-seventh valve 67, the twenty-eighth valve 68, and the twenty-ninth valve 69.

[0075] The compositions of light hydrocarbon oil, medium hydrocarbon oil and crude phenol obtained by gas chromatography / mass spectrometry analysis are shown in Table 1 for light hydrocarbon oil, medium hydrocarbon oil and crude phenol.

[0076] Table 1

[0077]

[0078] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, various changes and modifications can be made to the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. Rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar, characterized in that: It includes: No. An extraction kettle (1), a first distillation kettle (2), a second extraction kettle (3), a third extraction kettle (4), a fourth extraction kettle (5), a second distillation kettle (6), a third distillation kettle (7), a fourth distillation kettle (8), a fifth distillation kettle (9), a first storage tank (10), a second storage tank (11), a third storage tank (12), a fourth storage tank (13), a fifth storage tank (14), a buffer tank (15) and a horizontal shell-and-tube heat exchanger (39); the top of the first extraction kettle (1) is connected to the fourth storage tank (13) and the fifth storage tank (14) respectively through pipelines, and the bottom of the first extraction kettle (1) is connected to the first distillation kettle (2) through a pipeline; The top of the No. 1 distillation kettle (2) is connected to the horizontal shell-and-tube heat exchanger (39) through a pipeline, and the bottom of the No. 1 distillation kettle (2) is connected to the No. 2 extraction kettle (3) through a pipeline; The top of the second extraction kettle (3) is connected to the second storage tank (11) and the third storage tank (12) through pipelines, and the bottom of the second extraction kettle (3) is connected to the third extraction kettle (4) and the fourth extraction kettle (5) through pipelines; The top of the No. 3 extraction kettle (4) is connected to the No. 1 storage tank (10) through a pipeline, and the bottom of the No. 3 extraction kettle (4) is connected to the No. 2 distillation kettle (6) and the No. 3 distillation kettle (7) through a pipeline; The top of the No. 4 extraction kettle (5) is connected to the No. 5 storage tank (14) through a pipeline, and the bottom of the No. 4 extraction kettle (5) is connected to the No. 4 distillation kettle (8) and the No. 5 distillation kettle (9) through pipelines; The tops of the No. 2 distillation kettle (6), the No. 3 distillation kettle (7), the No. 4 distillation kettle (8), and the No. 5 distillation kettle (9) are respectively connected to the horizontal shell and tube heat exchanger (39), the horizontal shell and tube heat exchanger (39) is connected to the buffer tank (15), and the buffer tank (15) is respectively connected to the No. 1 storage tank (10), the No. 2 storage tank (11), the No. 3 storage tank (12), the No. 4 storage tank (13), and the No. 5 storage tank (14).

2. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: The first extraction kettle (1) is provided with a magnetic stirring device (19), a coarse filter plate (84) and a fine filter plate (85), the upper part of the first extraction kettle (1) is provided with a feeding trough (28) and a pressure gauge (30), and the lower part of the first extraction kettle (1) is provided with a discharge trough (29).

3. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: The second extraction kettle (3), the third extraction kettle (4) and the fourth extraction kettle (5) are all provided with a magnetic stirring device and an observation window for observing the extraction liquid level.

4. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: Pressure gauges are provided on the tops of the No. 2 extraction kettle (3), the No. 3 extraction kettle (4) and the No. 4 extraction kettle (5).

5. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: The first distillation kettle (2), the second distillation kettle (6), the third distillation kettle (7), the fourth distillation kettle (8) and the fifth distillation kettle (9) are all provided with matching heating devices and magnetic stirring devices.

6. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: Pressure gauges are provided on the tops of the No. 1 distillation kettle (2), the No. 2 distillation kettle (6), the No. 3 distillation kettle (7), the No. 4 distillation kettle (8) and the No. 5 distillation kettle (9).

7. The rapid enrichment equipment for light hydrocarbon oil, medium hydrocarbon oil and crude phenol in medium and low temperature coal tar according to claim 1, characterized in that: The valve pipeline of the horizontal shell-and-tube heat exchanger (39) is connected to the buffer tank (15) through an oil pump (17).

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