Method and device for producing sealing oil

文档序号:1211098 发布日期:2020-09-04 浏览:23次 中文

阅读说明:本技术 密封油的生产方法和装置 (Method and device for producing sealing oil ) 是由 逯波 刘付升 乔元 王喜武 温俊刚 杨东 牛刚 马翔 吕大伟 于 2020-05-14 设计创作,主要内容包括:本发明涉及煤液化领域,公开了一种密封油的生产方法,该方法包括:1)将油煤浆与氢气进行第一反应,得到煤液化反应产物;2)将所述煤液化反应产物进行第一分馏,得到第一轻组分和第一重组分;3)将所述第一重组分进行第二分馏,得到第二轻组分和第二重组分;4)将所述第一轻组分、第二轻组分和部分第二重组分混合得到液化油,将所述液化油与氢气进行第二反应,得到加氢反应产物;5)将所述加氢反应产物进行第三分馏,得到第一溶剂油和第二溶剂油;6)将第一溶剂油、第二溶剂油与剩余的第二重组分进行混合,得到密封油。该方法不需要调整装置工况即可在线生产符合标准的密封油,保证了装置运行安全稳定,降低了生产成本。(The invention relates to the field of coal liquefaction, and discloses a production method of sealing oil, which comprises the following steps: 1) carrying out a first reaction on the oil coal slurry and hydrogen to obtain a coal liquefaction reaction product; 2) performing first fractionation on the coal liquefaction reaction product to obtain a first light component and a first heavy component; 3) subjecting the first heavy component to a second fractionation to obtain a second light component and a second heavy component; 4) mixing the first light component, the second light component and part of the second heavy component to obtain liquefied oil, and carrying out a second reaction on the liquefied oil and hydrogen to obtain a hydrogenation reaction product; 5) performing third fractionation on the hydrogenation reaction product to obtain first solvent oil and second solvent oil; 6) and mixing the first solvent oil, the second solvent oil and the rest second heavy component to obtain the sealing oil. The method can produce the sealing oil meeting the standard on line without adjusting the working condition of the device, ensures the safe and stable operation of the device and reduces the production cost.)

1. A method of producing a sealing oil, the method comprising:

(1) carrying out a first reaction on the oil coal slurry and hydrogen to obtain a coal liquefaction reaction product;

(2) performing first fractionation on the coal liquefaction reaction product to obtain a first light component and a first heavy component;

(3) subjecting the first heavy component to a second fractionation to obtain a second light component and a second heavy component;

(4) mixing the first light component, the second light component and part of the second heavy component to obtain liquefied oil, and carrying out a second reaction on the liquefied oil and hydrogen to obtain a hydrogenation reaction product;

(5) performing third fractionation on the hydrogenation reaction product to obtain first solvent oil and second solvent oil;

(6) and mixing the first solvent oil, the second solvent oil and the rest second heavy component to obtain the sealing oil.

2. The method according to claim 1, wherein in the step (6), the weight ratio of the first solvent oil, the second solvent oil and the rest of the second heavy components in the mixing process is (0.5-3): (0.5-3): 1, preferably (1-1.5): (1-1.5): 1;

preferably, the sealing oil has a flash point of 150 ℃ to 220 ℃, preferably 170 ℃ to 210 ℃.

3. The process according to claim 1 or 2, wherein in step (1), the conditions of the first reaction comprise: the temperature is 420-470 ℃, preferably 430-465 ℃; the pressure is 13-22MPa, preferably 15-19 MPa.

4. The process of any one of claims 1-3, wherein in step (2), the conditions of the first fractionation comprise: the temperature is 300-400 ℃, and the optimal temperature is 340-360 ℃; the pressure is 0-1.0MPa, preferably 0.1-0.3 MPa;

preferably, the distillation range of the first light component is 75-380 ℃, preferably 130-350 ℃;

preferably, the distillation conditions of the first light component comprise: the temperature is 120-365 ℃, and the temperature is preferably 130-350 ℃; the pressure is 0 to 1.0MPa, preferably 0.1 to 0.3 MPa.

5. The process of any one of claims 1-4, wherein in step (3), the conditions of the second fractionation comprise: the temperature is 330-420 ℃, preferably 350-410 ℃; the pressure is 0 to 30kPa, preferably 0 to 15 kPa.

6. The process as claimed in any one of claims 1 to 5, wherein the second light fraction has a distillation range of 230-380 ℃, preferably 250-370 ℃;

preferably, the distillation range of the second heavy component is 260-420 ℃, preferably 280-370 ℃;

preferably, the distillation conditions of the second heavy component comprise: the temperature is 200-300 ℃, preferably 230-280 ℃, and the pressure is 0-30kPa, preferably 0-15 kPa.

7. The method according to any one of claims 1 to 6, wherein in step (4), the conditions of the second reaction comprise: the temperature is 300-420 ℃, and the optimal temperature is 330-380 ℃; the pressure is 12-19MPa, preferably 15-18 MPa.

8. The process of any one of claims 1-7, wherein in step (5), the conditions of the third fractionation comprise: the temperature is 230-360 ℃, and the preferred temperature is 250-340 ℃; the pressure is 0 to 0.6MPa, preferably 0.1 to 0.3 MPa.

9. The process according to any one of claims 1 to 8, wherein the first solvent oil has a distillation range of 220-310 ℃, preferably 230-290 ℃;

preferably, the distillation range of the second solvent oil is 250-410 ℃, preferably 260-400 ℃;

preferably, the distillation conditions of the first solvent oil comprise: the temperature is 240-280 ℃, preferably 250-270 ℃, and the pressure is 0-0.6MPa, preferably 0.1-0.3 MPa;

preferably, the distillation conditions of the second solvent oil comprise: the temperature is 260-390 ℃, preferably 270-360 ℃, and the pressure is 0-0.6MPa, preferably 0.1-0.3 MPa.

10. An apparatus for producing sealing oil, the apparatus comprising: a coal liquefaction reactor (103), a first fractionating tower (106), a second fractionating tower (107), a hydrogenation reactor (501) and a third fractionating tower (505);

the top outlet of the coal liquefaction reactor (103) is communicated with the middle inlet of the first fractionating tower (106);

the bottom outlet of the first fractionating tower (106) is communicated with the lower inlet of the second fractionating tower (107), and the upper and middle outlets of the first fractionating tower (106) are communicated with the bottom inlet of the hydrogenation reactor (501);

the upper and middle outlets of the second fractionating tower (107) are communicated with the bottom inlet of the hydrogenation reactor (501);

the top outlet of the hydrogenation reactor (501) is communicated with the middle inlet of the third fractionating tower (505);

the middle outlet of the second fractionating tower (107) and the middle and bottom outlets of the third fractionating tower (505) are also communicated with a sealing oil mixing system through pipelines.

Technical Field

The invention relates to the field of coal liquefaction, in particular to a method and a device for producing sealing oil.

Background

In the direct coal liquefaction process, a circulating pump at the bottom of a reactor belongs to important core equipment, sealing oil of the circulating pump plays a role in lubricating a motor bearing and cooling a motor, and meanwhile, abrasion products are prevented from entering the motor by the sealing oil in a mode of flowing outwards from an internal part of a pressurizing motor, so that the requirement of the circulating pump on the sealing oil is quite strict.

The circulating pump sealing oil is generally purchased from professional manufacturers, but the price of the purchased sealing oil is relatively high, and the circulating pump sealing oil cannot be recycled after entering a process medium, so that the production cost is high under the condition of long-period operation. Therefore, enterprises urgently need to adopt the existing device to research and develop and produce the circulating pump sealing oil to replace outsourcing sealing oil, so that the production cost is reduced, and the economic benefit is improved.

There are two ways to produce the circulating pump seal oil. One is that a professional manufacturer adopts special lubricating oil to process and produce sealing oil, and the special lubricating oil needs special production, and has high energy consumption and high production cost. And for a client manufacturer, the purchase period is longer, the transportation cost is increased, and the price of the sealing oil is higher, so that the operation cost is additionally increased for the user manufacturer.

At present, if a client manufacturer produces the sealing oil by itself, the working condition of part of the device needs to be adjusted, and the current product is suspended to produce the sealing oil, and under the special working condition, potential safety hazards exist in the operation of the device, and meanwhile, the resource waste can be caused in the production process. The production cost of the sealing oil is high, and the industrial economic benefit is not high.

In summary, there is a need to develop a process capable of safely producing a substitute for purchased sealing oil without adjusting the working conditions of the existing devices.

Disclosure of Invention

The invention aims to solve the problems of complex process for producing sealing oil by adopting special lubricating oil and high production cost of the sealing oil and unsafe device operation caused by adjusting the working condition of the device in the prior art, and provides a method and a device for producing the sealing oil.

In order to achieve the above object, a first aspect of the present invention provides a method for producing a sealing oil, the method comprising:

(1) carrying out a first reaction on the oil coal slurry and hydrogen to obtain a coal liquefaction reaction product;

(2) performing first fractionation on the coal liquefaction reaction product to obtain a first light component and a first heavy component;

(3) subjecting the first heavy component to a second fractionation to obtain a second light component and a second heavy component;

(4) mixing the first light component, the second light component and part of the second heavy component to obtain liquefied oil, and carrying out a second reaction on the liquefied oil and hydrogen to obtain a hydrogenation reaction product;

(5) performing third fractionation on the hydrogenation reaction product to obtain first solvent oil and second solvent oil;

(6) and mixing the first solvent oil, the second solvent oil and the rest second heavy component to obtain the sealing oil.

A second aspect of the present invention provides a seal oil production apparatus, comprising: a coal liquefaction reactor 103, a first fractionating tower 106, a second fractionating tower 107, a hydrogenation reactor 501, and a third fractionating tower 505;

the top outlet of the coal liquefaction reactor 103 is communicated with the middle inlet of the first fractionating tower 106;

the bottom outlet of the first fractionating tower 106 is communicated with the lower inlet of the second fractionating tower 107, and the upper and middle outlets of the first fractionating tower 106 are communicated with the bottom inlet of the hydrogenation reactor 501;

the upper and middle outlets of the second fractionating tower 107 are communicated with the bottom inlet of the hydrogenation reactor 501;

the top outlet of the hydrogenation reactor 501 is communicated with the middle inlet of the third fractionating tower 505;

the middle outlet of the second fractionating tower 107 and the middle and bottom outlets of the third fractionating tower 505 are also connected to a seal oil mixing system via lines.

The inventor of the invention finds that the sealing oil is produced by taking Heavy Vacuum Gas Oil (HVGO) obtained by further fractionating after direct coal liquefaction reaction as base oil, can realize online production of the sealing oil, has simple flow, does not influence the working condition of the existing device, avoids adjusting the working condition and reduces the production cost.

Through the technical scheme, the qualified sealing oil can be directly produced on line by using the existing equipment under the condition that the working condition of the device is not required to be adjusted, the device is safe and stable to operate, and the produced sealing oil is excellent in quality, so that the operation cost of an enterprise is saved, and the economic benefit is improved. The method has the advantages of simple process, low production cost of the sealing oil, wide industrial application prospect and large-scale popularization.

Drawings

FIG. 1 is a flow chart of a sealing oil production process according to a preferred embodiment of the present invention;

fig. 2 is a schematic view of a sealing oil mixing process according to a preferred embodiment of the present invention.

Description of the reference numerals

101. Oil coal slurry 103, coal liquefaction reactor 105 and first separation system

106. First fractionating tower 107, second fractionating tower 403, and second heavy component

501. A hydrogenation reactor 504, a second separation system 505 and a third fractionating tower

401. First solvent oil 402, second solvent oil 201 and raw material tank

202. First filter 204, second filter 205, sealed oil tank

206. Oil filter

102. 502 are all hydrogen

104. 203, 503 are both pumps

301. 302, 303, 304, 305, 306 are all pipelines

Detailed Description

The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.

In the present invention, the pressure refers to the absolute pressure unless otherwise specified.

In the present invention, the distillation range refers to the temperature range from the initial distillation point to the final distillation point obtained by distilling the oil under standard conditions.

Unless otherwise specified, the average boiling point in the following text refers to the mass average boiling point, in particular to the sum of the products of the mass fractions of the individual components and the respective distillation temperatures.

In the invention, the coal oil slurry refers to a coal liquefaction raw material obtained by mixing coal powder and a solvent.

In the present invention, unless otherwise specified, the coal liquefaction refers to a process of directly liquefying coal, that is, a process of directly producing gas, liquid, solid fuel and chemical products from coal as a raw material under the conditions of high temperature, high pressure and hydrogen presence and under the action of a catalyst.

In the present invention, the survey line refers to the middle part of the fractionating column. The line material refers to the material led out from the middle part of the fractionating tower.

In the present invention, the terms of orientation such as "upper", "middle" and "lower" are used to refer to the upper, middle and lower parts of a reactor or a fractionation column, respectively, unless otherwise specified. The upper part, the middle part and the lower part of the reactor or the fractionating tower can be three sections which are uniformly divided from top to bottom, or can be three sections which are not uniformly divided by taking an internal member as a segmentation standard, so long as the reactor or the fractionating tower can be distinguished by a person skilled in the art.

The present invention provides, in a first aspect, a method for producing a sealing oil, the method comprising:

(1) carrying out a first reaction on the oil coal slurry and hydrogen to obtain a coal liquefaction reaction product;

(2) performing first fractionation on the coal liquefaction reaction product to obtain a first light component and a first heavy component;

(3) subjecting the first heavy component to a second fractionation to obtain a second light component and a second heavy component;

(4) mixing the first light component, the second light component and part of the second heavy component to obtain liquefied oil, and carrying out a second reaction on the liquefied oil and hydrogen to obtain a hydrogenation reaction product;

(5) performing third fractionation on the hydrogenation reaction product to obtain first solvent oil and second solvent oil;

(6) and mixing the first solvent oil, the second solvent oil and the rest second heavy component to obtain the sealing oil.

According to a preferred embodiment of the present invention, in step (6), the weight ratio of the first solvent oil, the second solvent oil and the rest of the second heavy component in the mixing process is (0.5-3): (0.5-3): 1, more preferably (1-1.5): (1-1.5): 1. in this preferred case, it is advantageous to improve the quality of the sealing oil product.

According to the invention, the flash point of the sealing oil is preferably 150-.

According to a preferred embodiment of the present invention, the second heavy component obtained after the second fractionation after the coal liquefaction reaction is Heavy Vacuum Gas Oil (HVGO), and the distillation range of the second heavy component is 260-420 ℃. In this preferred embodiment, it is more advantageous to improve the quality of the sealing oil. The inventor of the invention finds that the sealing oil is produced by taking Heavy Vacuum Gas Oil (HVGO) obtained by further fractionating after direct coal liquefaction reaction as base oil, can realize online production of the sealing oil, has simple flow, does not need to adjust the working condition of the existing device, not only obtains the sealing oil with the quality meeting the standard, but also ensures the safe and stable operation of the device.

Preferably, the seal oil has an API gravity of 20 to 40, preferably 22 to 38, further preferably 24 to 36, more preferably 25 to 35.

Preferably, the sealing oil has a pour point of less than 28 ℃, preferably less than 26 ℃, further preferably less than 23 ℃, more preferably less than 21 ℃.

Preferably, the sealing oil has an insulation strength (according to ASTM) of more than 15000V, preferably more than 18000V, further preferably more than 20000V, more preferably more than 25000V.

Preferably, the seal oil has a Saybolt viscosity at 37.8 deg.C (100F) of 135-165s, preferably 145-165s, more preferably 150-165s, and even more preferably 155-60 s.

Preferably, the sealing oil has a viscosity at 93.3 ℃ (200 ° f) of 38 to 50s, preferably 38 to 45s, further preferably 38 to 42s, more preferably 40 to 42 s.

Preferably, the sealing oil has a sulphur content of less than 0.4 wt.%, preferably less than 0.35 wt.%, more preferably less than 0.3 wt.%, more preferably less than 0.2 wt.%.

Preferably, the copper strip test of the sealing oil reaches the 1a standard of GB/T5096.

According to the present invention, preferably, in step (1), the conditions of the first reaction include: the temperature is 420-470 ℃, preferably 430-465 ℃; the pressure is 13-22MPa, preferably 15-19 MPa.

The present invention has a wide range of options for the equipment for carrying out the first reaction, and preferably, the first reaction of the present invention is a direct coal liquefaction reaction, and specifically, the direct coal liquefaction reaction is carried out, for example, using a suspension bed. In the invention, the process of the reaction in the suspension bed comprises the steps of premixing the catalyst and the raw materials, then feeding the premixed catalyst and hydrogen into the reactor together for flowing from bottom to top, and carrying out hydrocracking reaction, wherein the catalyst is suspended in a liquid phase and flows out from the top of the reactor along with reaction products. In the present invention, the structure of the suspended bed reactor is not particularly limited, and may be conventionally selected in the art, for example, a hollow cylindrical structure.

According to the present invention, the catalyst in the first reaction is selected from a wide range, and preferably, in the step (1), the catalyst comprises a carrier and an active component supported on the carrier.

In the present invention, the element in the active component is selected from a wide range, for example, a metal element, preferably, the metal element in the active component is a group VIII element and/or a group IIB element, and more preferably, at least one of iron, nickel and zinc.

The present invention has a wide range of selection of the carrier for the catalyst in the first reaction, and preferably, the carrier is at least one selected from the group consisting of pulverized coal, furnace dust, and powdery minerals.

According to the present invention, preferably, step (1) further comprises, after the first reaction, performing a first separation on the product of the first reaction. Preferably, the first separation process comprises removing hydrogen from the product after the first reaction to obtain a coal liquefaction reaction product. The first separation apparatus is not particularly limited in the present invention, as long as the purpose of separating hydrogen from the coal liquefaction reaction product can be achieved, and those skilled in the art can select the first separation apparatus as needed according to actual circumstances.

According to the present invention, preferably, the hydrogen in the obtained product of the first reaction is reused in the first reaction process. Under the optimal condition, the method is favorable for improving the utilization rate of raw materials and reducing the production cost.

The conditions for the first fractionation are selected from a wide range according to the present invention, and preferably, in the step (2), the conditions for the first fractionation include: the temperature is 300-400 ℃, and the optimal temperature is 340-360 ℃; the pressure is 0 to 1.0MPa, preferably 0.1 to 0.3 MPa. In this preferred case, it is more advantageous to improve the product quality of the sealing oil. The method of the invention adopts the existing equipment in the device, and can realize the production of the sealing oil without adjusting the current working condition, thereby not only ensuring the operation safety of the device, but also greatly reducing the production cost of enterprises.

In the present invention, the apparatus of the first fractionation is not particularly limited, and specifically, for example, it may be carried out using a fractionation column, which may be a tray column and/or a packed column. In the present invention, the number of theoretical plates of the fractionating tower is not particularly limited, and those skilled in the art can select the number as needed according to actual needs, as long as the purpose of fractionating the coal liquefaction reaction product to obtain substances with different boiling points can be achieved.

According to one embodiment of the invention, the first fractionation is an atmospheric fractionation. By atmospheric fractionation is meant fractionation at atmospheric pressure (or slightly above atmospheric pressure).

In the present invention, the manner of obtaining the first light component is not particularly limited. One strand of material or two or more strands of material can be used for the measuring line of the fractionating tower.

In one embodiment, the first fractionation results in three inline streams, and the first light fraction is at least one of the three inline streams.

The distillation range of the first light component is selected to be wider, and the distillation range of the first light component is preferably 75-380 ℃, and more preferably 130-350 ℃. In this preferred case, it is more advantageous to improve the product quality of the sealing oil.

The present invention has a wide selection range of the distillation conditions of the first light component, and preferably, the distillation conditions of the first light component include: the temperature is 120-365 ℃, and the temperature is preferably 130-350 ℃; the pressure is 0 to 1.0MPa, preferably 0.1 to 0.3 MPa.

In one embodiment, the first fractionation produces the first heavy component at the bottom of a fractionation column. Preferably, the distillation range of the first heavy component is not less than 300 ℃, further preferably not less than 330 ℃.

According to a preferred embodiment of the present invention, in the step (3), the conditions of the second fractionation include: the temperature is 330-420 ℃, preferably 350-410 ℃; the pressure is 0 to 30kPa, preferably 0 to 15 kPa. Under the preferred embodiment, the product quality of the sealing oil is improved more favorably under the condition that the current working condition of the device is not adjusted. The method of the invention adopts the existing equipment in the device, and can realize the production of the sealing oil without adjusting the current working condition, thereby ensuring the safe operation of the device and greatly reducing the production cost of enterprises.

In one embodiment, the second fractionation is a vacuum fractionation. The equipment for carrying out the vacuum fractionation is not particularly limited in the present invention, and those skilled in the art can select the equipment as needed according to actual circumstances. Preferably, the vacuum fractionation is achieved by communicating the equipment of the second fractionation with a vacuum device. The selection of the vacuum device in the present invention may be conventional in the art, and the present invention will not be described herein.

The equipment for the second fractionation according to the present invention is widely selected, and the second fractionation is preferably carried out using a fractionation column. The choice of the fractionating tower for the first fractionation is not particularly limited in the present invention, and specifically, the fractionating tower as described above may be used, and the present invention will not be described herein again.

In one embodiment, the second fractionation produces two inline streams and the second light fraction is at least one of the two inline streams.

The distillation range of the second light component is selected to be wider, and the distillation range of the second light component is preferably 230-380 ℃, and is preferably 250-370 ℃. In this preferred case, it is advantageous to improve the product quality of the sealing oil.

According to the present invention, preferably, the distillation range of the second heavy component is 260-420 ℃, preferably 280-370 ℃.

According to a preferred embodiment of the present invention, the distillation conditions of the second heavy component include: the temperature is 200-300 ℃, preferably 230-280 ℃, and the pressure is 0-30kPa, preferably 0-15 kPa. Under the preferred embodiment, the product quality of the sealing oil is improved under the condition that the current working condition of the device is not adjusted. The inventor of the invention finds that the second heavy component obtained by performing the second fractionation on the coal liquefaction reaction product is used as the base oil, the online production can be realized by using the normal production working condition under the condition that the existing device does not adjust the working condition, the process flow is simple, the production cost is reduced, and the obtained sealing oil has excellent product quality and meets the standard.

According to a specific embodiment of the present invention, the side streams of the atmospheric fractionation and the vacuum fractionation are mixed to obtain the liquefied oil.

In the present invention, the mixing ratio of the side line is selected in a wide range. According to one embodiment of the invention, at least three side streams of the atmospheric fractionation and the vacuum fractionation are combined, preferably at least four, more preferably five.

According to the present invention, preferably, in step (4), the conditions of the second reaction include: the temperature is 300-420 ℃, and the optimal temperature is 330-380 ℃; the pressure is 12-19MPa, preferably 15-18 MPa.

In the present invention, the catalyst in the second reaction is selected from a wide range, and preferably, in the step (4), the catalyst comprises a carrier and an active component supported on the carrier. The elements in the active component are selected from a wide range, such as metal elements, preferably, the metal elements in the active component are group VIB elements and/or group VIII elements, and further preferably at least one of cobalt, nickel and tungsten. The invention is more widely applicable to the selection of the carrier, in particular, the carrier is alumina and/or silica.

In the present invention, the second reaction reduces the aromatic carbon rate of the liquefied oil. The apparatus for the second reaction in the present invention is not particularly limited, and specifically, for example, an ebullated bed reactor and/or a fixed bed reactor can be used. The ebullated bed reactor and the fixed bed reactor described in the present invention may be conventional in the art and will not be described in detail herein.

According to the present invention, the step (4) further comprises, after the second reaction, performing a second separation on the product of the second reaction. Preferably, the second separation process comprises removing hydrogen from the product after the second reaction to obtain a hydrogenation reaction product. The second separation apparatus is not particularly limited in the present invention, as long as the purpose of separating hydrogen from the coal liquefaction reaction product can be achieved, and those skilled in the art can select the second separation apparatus as needed according to actual circumstances.

According to the present invention, preferably, in step (5), the conditions of the third fractionation include: the temperature is 230-360 ℃, and the preferred temperature is 250-340 ℃; the pressure is 0 to 0.6MPa, preferably 0.1 to 0.3 MPa. Under the optimal condition, the product quality of the sealing oil is improved under the condition that the current working condition of the device is not adjusted.

The third fractionation apparatus of the present invention is not particularly limited, and specifically, for example, it may be carried out using a fractionation column, which may be a tray column and/or a packed column. In the present invention, the number of theoretical plates of the fractionating tower is not particularly limited, and those skilled in the art can select the number as needed according to actual needs, as long as the purpose of fractionating the hydrogenation reaction product to obtain substances with different boiling points can be achieved.

According to the invention, the distillation range of the first solvent oil is preferably 220-310 ℃, and preferably 230-290 ℃.

According to the invention, the distillation range of the second solvent oil is preferably 250-410 ℃, and preferably 260-400 ℃.

According to a preferred embodiment of the present invention, the distillation conditions of the first solvent oil include: the temperature is 240-280 ℃, preferably 250-270 ℃, and the pressure is 0-0.6MPa, preferably 0.1-0.3 MPa.

Preferably, the distillation conditions of the second solvent oil comprise: the temperature is 260-390 ℃, preferably 270-360 ℃, and the pressure is 0-0.6MPa, preferably 0.1-0.3 MPa.

According to the invention, the average boiling point of the second solvent oil is preferably 20 to 90 ℃ higher than the average boiling point of the first solvent oil at the same distillation pressure.

According to an embodiment of the present invention, during the third fractionation, the first solvent oil is extracted from a middle portion of the fractionation tower, and the second solvent oil is extracted from a bottom portion of the fractionation tower.

According to the present invention, preferably, the step (6) further comprises performing a purification treatment on the mixed product after the first solvent oil, the second solvent oil and the remaining second heavy component are mixed. In this preferred case, it is advantageous to improve the product quality of the sealing oil.

In the present invention, the purification treatment process comprises mechanical impurity removal and/or dehydration. In the present invention, the mechanical impurity removal process is not particularly limited, and specifically, for example, the mechanical impurity removal process may be performed by using a filtration device. The filtration means may be conventional in the art and the present invention will not be described in detail herein. In the invention, the impurity content analysis method after mechanical impurity removal refers to GB/T511.

In the present invention, the dewatering process is not particularly limited, and specifically, for example, an oil filter may be used, and those skilled in the art may select the dewatering process according to actual needs. The analysis method of the water content after dehydration refers to GB/T1113.

According to a preferred embodiment of the present invention, the primary sealing oil is obtained by mixing the Heavy Vacuum Gas Oil (HVGO) directly liquefied from coal, the medium temperature solvent oil and the high temperature solvent oil, and the sealing oil is obtained by purifying (mechanical impurity and dehydration) the primary sealing oil.

A second aspect of the present invention provides an apparatus for producing sealing oil, as shown in fig. 2, comprising: a coal liquefaction reactor 103, a first fractionating tower 106, a second fractionating tower 107, a hydrogenation reactor 501, and a third fractionating tower 505;

the top outlet of the coal liquefaction reactor 103 is communicated with the middle inlet of the first fractionating tower 106;

the bottom outlet of the first fractionating tower 106 is communicated with the lower inlet of the second fractionating tower 107, and the upper and middle outlets of the first fractionating tower 106 are communicated with the bottom inlet of the hydrogenation reactor 501;

the upper and middle outlets of the second fractionating tower 107 are communicated with the bottom inlet of the hydrogenation reactor 501;

the top outlet of the hydrogenation reactor 501 is communicated with the middle inlet of the third fractionating tower 505;

the middle outlet of the second fractionating tower 107 and the middle and bottom outlets of the third fractionating tower 505 are also connected to a seal oil mixing system via lines.

According to the present invention, the apparatus preferably further comprises a seal oil mixing system, a first separation system 105 and a second separation system 504.

According to a preferred embodiment of the present invention, the seal oil mixing system includes a mixing tank 201, a first filter 202, a second filter 204, a seal oil tank 205, and an oil filter 206; the mixing tank 201 is communicated with the outlet of the first filter 202; the outlet of the second filter 204 communicates with the inlet of the seal oil tank 205, and the oil filter 206 communicates with the seal oil tank 205.

According to the present invention, the first separation system 105 is in communication with the outlet of the coal liquefaction reactor 103 for separating hydrogen from the coal liquefaction reaction product.

According to the present invention, the second separation system 504 is communicated with the outlet of the hydrogenation reactor 501 for separating hydrogen from the hydrogenation reaction product.

According to a preferred embodiment of the present invention, the method for producing the sealing oil provided by the present invention is performed according to the process flow diagram shown in fig. 1, specifically:

(1) the method comprises the steps that oil coal slurry 101 and hydrogen 102 enter from the bottom of a coal liquefaction reactor 103 to carry out a first reaction, an obtained coal liquefaction reaction product is subjected to first separation through a first separation system 105, and obtained hydrogen returns to the coal liquefaction reactor 103; the conditions of the first reaction include: the temperature is 430-465 ℃ and the pressure is 15-19 MPa;

(2) feeding the coal liquefaction reaction product obtained in the step (1) into a first fractionating tower 106 for first fractionating to obtain three strands of a first fractionating tower measuring line as a first light component, and obtaining a first heavy component at the bottom of the first fractionating tower; the conditions of the first fractionation include: the temperature is 340 ℃ and 360 ℃, and the pressure is 0.1-0.3 MPa; the distillation range of the first light component is 130-350 ℃; the distillation conditions of the first light component comprise: the temperature is 130-350 ℃, and the pressure is 0.1-0.3 MPa;

(3) the first heavy component enters a second fractionating tower 107 to be subjected to second fractionation, a second light component is obtained at the upper part of the second fractionating tower 107, and a second heavy component is obtained at the middle part of the second fractionating tower 107; the conditions of the second fractionation include: the temperature is 350-410 ℃, and the pressure is 0-15 kPa; the distillation range of the second light component is 250-370 ℃; the distillation range of the second heavy component is 280-370 ℃; the distillation conditions of the second heavy component comprise: the temperature is 230 ℃ and 280 ℃, and the pressure is 0-15 kPa;

(4) after the first light component, the second light component and part of the second heavy component are mixed, the mixture and hydrogen 205 enter a hydrogenation reactor 501 for a second reaction, a product of the second reaction is subjected to second separation by a second separation system 504, and the obtained hydrogen returns to the hydrogenation reactor 501; the conditions of the second reaction include: the temperature is 300-420 ℃, and the pressure is 10-19 MPa;

(5) feeding the hydrogenation reaction product obtained in the step (4) into a third fractionating tower 505 for third fractionating, obtaining a first solvent oil 401 at the middle part of the third fractionating tower 505, and obtaining a second solvent oil 402 at the bottom part of the third fractionating tower 505; the conditions of the third fractionation include: the temperature is 250 ℃ and 340 ℃, and the pressure is 0.1-0.3 MPa; the distillation range of the first solvent oil is 230-290 ℃; the distillation range of the second solvent oil is 260-400 ℃; the distillation conditions of the first solvent oil comprise: the temperature is 250 ℃ and 270 ℃, and the pressure is 0.1-0.3 MPa; the distillation conditions of the second solvent oil comprise: the temperature is 270-360 ℃, and the pressure is 0.1-0.3 MPa;

(6) the weight ratio of the first solvent oil 401, the second solvent oil 402 and the rest of the second heavy components 403 is (1-1.5): (1-1.5): 1 to obtain the sealing oil.

According to a preferred embodiment of the present invention, in step (6), the mixing is performed according to a schematic sealing oil mixing flow shown in fig. 2, specifically:

the first solvent oil 401, the second solvent oil 402 and the second heavy component 403 enter the raw material tank 201 through a pipeline 301 to obtain primary seal oil, and the primary seal oil enters the first filter 202 through a pipeline 302 to be subjected to first filtration and then returns to the raw material tank 201 through a pipeline 303; the primary seal oil enters the second filter 204 through the line 304 for second filtration to remove mechanical impurities and then enters the seal oil tank 205; the primary seal oil enters the oil filter 206 through a pipeline 305 for dehydration and then returns to the seal oil tank 205 through a pipeline 306 to obtain the seal oil, and the flash point of the seal oil is 170-210 ℃.

The present invention will be described in detail below by way of examples.

In the following examples, the coal oil slurry concentration by weight was 50% by weight, the feed rate was 476t/h, and the hydrogen consumption of the coal liquefaction reactor was 180000m3H, hydrogen consumption of the hydrogenation reactor is 60000m3/h。

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