Continuous production system and method for co-producing alkyl naphthalene base oil and liquid wax

By adopting a continuous production system of co-producing alkylnaphthalene base oil and liquid wax in the field of coal chemical industry, and using micro reactors and multi-channel distillation separation devices, the existing technology has been solved with low reaction efficiency, many side reactions and low added value. The problem has achieved efficient and low-cost co-production.

CN119455841APending Publication Date: 2025-02-18CHINA ENERGY GRP NINGXIA COAL IND CO LTD +1
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Patent Information

Application Number
CN202411594081.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-08
Publication Date
2025-02-18

AI Technical Summary

Technical Problem

In the prior art, the reactor has low reaction efficiency and many side reactions, resulting in low product yield, low recycling rate of solvents and excess raw materials leads to high cost, and the cogeneration of alkyl naphthalene base oil and liquid wax leads to additional value. Low.

Method used

Provided is a continuous production system for co-producing alkylnaphthalene base oil and liquid wax, including a continuous alkylation reaction device, a first continuous separation device, a first continuous distillation device, a second continuous distillation device and a third continuous distillation device, The micro reactor is used to carry out continuous alkylation reaction, and the catalyst, solvent and raw materials are recovered through multiple distillation and separation devices.

Benefits of technology

The yield and added value of alkylnaphthalene base oil and liquid wax is improved, and the efficient recycling and utilization of catalysts, solvents and raw materials is achieved, production costs are reduced, and production efficiency is improved.

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Abstract

The invention provides a continuous production system and method for co-producing alkyl naphthalene base oil and liquid wax. The continuous production system comprises a continuous alkylation reaction device, a first continuous separation device, a first continuous distillation device, a second continuous distillation device and a third continuous distillation device. The continuous alkylation reaction device is used for carrying out continuous alkylation reaction on Fischer-Tropsch synthetic oil and naphthalene in a solvent under the catalysis of an ionic liquid catalyst to obtain a product system; the continuous alkylation reaction device is a microreactor; the first continuous separation device is used for separating and recovering a catalyst; the first continuous distillation device is used for separating and recovering a solvent; the second continuous distillation device is used for separating and recovering the unreacted raw material naphthalene; the third continuous distillation device is used for separating to obtain alkyl naphthalene base oil and liquid wax. By adopting the continuous production system, the alkyl naphthalene base oil and the liquid wax can be obtained at the same time, the solvent, the raw materials and the catalyst can be recycled, the utilization rate of the raw materials is increased, and the cost is reduced.
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Description

Technical Field

[0001] The invention relates to the field of coal chemical industry, and in particular to a continuous production system and method for co-producing alkyl naphthalene base oil and liquid wax. Background Art

[0002] With the development of social economy, lubricants based on mineral oil can no longer meet the requirements, and the research and application of synthetic base oils have gradually become a hot spot. Alkyl naphthalene, as a Class V synthetic base oil, has excellent thermal oxidation stability, hydrolysis stability, additive solubility and anti-emulsification properties due to the 10-electron large π conjugated structure of the naphthalene ring and the structure of the connected alkyl group. It is widely used in hydraulic oil, gear oil, heat transfer oil, compressor oil and other fields.

[0003] The existing document (publication number CN114790407A) discloses a method for preparing alkylnaphthalene lubricating oil base oil from coal-based α-olefins, and the specific preparation method is: using coal-based α-olefins, naphthalene and / or methylnaphthalene as raw materials, mixing in a solvent, adding a solid acid catalyst, reacting under normal pressure conditions, and filtering and distilling to obtain alkylnaphthalene after the reaction is completed. The catalyst in this process method is easy to coke, has a limited service life, and the process cannot achieve continuous production.

[0004] Existing document (publication number CN1676207A) discloses a continuous reactor suitable for ionic liquid catalyst, including a reaction section and a settling section, the reaction section includes 1 to 8 reaction tanks connected in series, the settling section includes 1 settling tank, wherein the reaction tank includes a raw material inlet, a new catalyst inlet, a circulating catalyst inlet and a material outlet, the settling tank includes a material inlet, a material outlet and a catalyst collector, the catalyst collector is located at the bottom of the settling tank, the outlet of the collector is connected to the circulating catalyst inlet of the reaction tank through a pipeline, and a valve is provided on the pipeline to control the circulation amount of the catalyst. The continuous reactor cannot realize the separation and reuse of the solvent and the unreacted raw materials, and its cost is high and the added value is low.

[0005] In summary, it is necessary to research and develop a continuous production system and method for the co-production of alkyl naphthalene base oil and liquid wax with simple process flow, safety and efficiency, low cost, high reaction efficiency, few side reactions and high added value. Summary of the invention

[0006] The main purpose of the present invention is to provide a continuous production system and method for the co-production of alkyl naphthalene base oil and liquid wax, so as to solve the problems in the prior art that the reaction efficiency of the reactor is low and the side reactions are many, resulting in low product yield, the recovery rate of the solvent and excess raw materials is low, resulting in high cost, and the existing production process cannot achieve the co-production of alkyl naphthalene base oil and liquid wax, resulting in low added value.

[0007] In order to achieve the above objectives, the present invention provides a continuous production system for co-producing alkyl naphthalene base oil and liquid wax, the continuous production system comprising: a continuous alkylation reaction unit, a first continuous separation unit, a first continuous distillation unit, a second continuous distillation unit and a third continuous distillation unit. The invention discloses a continuous alkylation reaction device, which is used for making Fischer-Tropsch synthetic oil and naphthalene undergo continuous alkylation reaction in a solvent under the catalysis of a catalyst to obtain a product system; the continuous alkylation reaction device is provided with a first Fischer-Tropsch synthetic oil inlet, a first naphthalene inlet, a first catalyst inlet, a first solvent inlet and a product system outlet; the continuous alkylation reaction device is a microreactor; the Fischer-Tropsch synthetic oil comprises a mixture of alkanes and olefins having a carbon number of 9 to 24; the catalyst is an ionic liquid catalyst; the first continuous separation device is provided with a product system inlet, a catalyst recovery outlet and an oil phase outlet; the product system inlet is connected to the product system outlet; the catalyst recovery outlet is connected to the first catalyst inlet; the first continuous distillation device is provided with a first oil phase inlet, a first distillation product outlet and a solvent recovery outlet; the first oil phase inlet is connected to the oil phase outlet; the solvent recovery outlet is connected to the first solvent inlet; the second continuous distillation device is provided with a first distillation product inlet, a second distillation product outlet and a naphthalene recovery outlet; the first distillation product inlet is connected to the first distillation product outlet; the naphthalene recovery outlet is connected to the first naphthalene inlet; the third continuous distillation device is provided with a second distillation product inlet, a liquid wax outlet and a first alkyl naphthalene base oil outlet; the second distillation product inlet is connected to the second distillation product outlet.

[0008] On the other hand, the present invention also provides a continuous production method for co-producing alkylnaphthalene base oil and liquid wax. The continuous production method is carried out using the above-mentioned continuous production system provided by the present application, and the continuous production method comprises: step S1, passing Fischer-Tropsch synthesis oil, naphthalene, catalyst and solvent into a continuous alkylation reaction device for continuous alkylation reaction to obtain a product system; step S2, passing the product system into a first continuous separation device for separation to obtain a recovered catalyst and an oil phase; returning at least a portion of the recovered catalyst to step S1; step S3, passing the oil phase into a first continuous distillation device for a first continuous distillation to obtain a first distillation product and a recovered solvent; returning at least a portion of the recovered solvent to step S1; step S4, passing the first distillation product into a second continuous distillation device for a second continuous distillation to obtain a second distillation product and recovered naphthalene; returning at least a portion of the recovered naphthalene to step S1; step S5, passing the second distillation product into a third continuous distillation device for a third continuous distillation to obtain an alkylnaphthalene base oil and liquid wax.

[0009] Applying the technical solution of the present invention, the above-mentioned continuous production system for co-producing alkyl naphthalene base oil and liquid wax provided in the present application includes a continuous alkylation reaction device, a first continuous separation device, a first continuous distillation device, a second continuous distillation device and a third continuous distillation device. The continuous alkylation reaction device can cause the Fischer-Tropsch synthetic oil and naphthalene to undergo continuous alkylation reaction in a solvent under the catalysis of a catalyst to obtain a product system; the microreactor can achieve precise control of the reaction temperature and reaction time due to its smaller channel size (equivalent diameter ≤ 700 μm), shorter mass transfer distance and larger specific surface area, and can also export heat in a strong exothermic reaction in time to maintain the stability of the reaction; compared with the traditional kettle reactor, the continuous alkylation reaction device in the present application adopts a microreactor, which can improve the reaction efficiency of the continuous alkylation reaction, inhibit the occurrence of side reactions caused by local overheating or excessive reaction time, thereby improving the production efficiency of continuous production. The first continuous separation device is used to separate the recovered catalyst from the oil phase in the product system, thereby realizing the recovery of the catalyst; the first continuous distillation device is used to separate and recover the solvent; the second continuous distillation device is used to separate and recover the unreacted raw material naphthalene; the third continuous distillation device is used to separate and obtain alkyl naphthalene base oil and liquid wax.

[0010] The above-mentioned continuous production system can pass the separated and recovered catalyst, solvent and raw material naphthalene into a continuous alkylation reaction device to participate in a continuous alkylation reaction. The above-mentioned continuous production system of the present application can not only simultaneously obtain alkyl naphthalene base oil and liquid wax, thereby increasing the added value of production, but also realize the recycling of catalyst, solvent and excess raw material naphthalene, thereby increasing the utilization rate of raw materials and reducing costs.

[0011] Compared with traditional liquid acid catalysts, the use of ionic liquid catalysts can improve the catalytic efficiency of continuous alkylation reactions, thereby improving the reaction efficiency of continuous alkylation reactions, and ionic liquid catalysts are non-volatile and easy to recycle. Compared with single carbon number olefins used in traditional alkyl naphthalene production processes, this application uses Fischer-Tropsch synthetic oil as a starting material, which can reduce costs and achieve efficient use of Fischer-Tropsch synthetic oil.

[0012] In summary, the above-mentioned continuous production system provided in the present application has a simple structure and low energy consumption, and can improve the utilization rate of raw materials and the yield of products. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0014] Figure 1A schematic diagram of the structure of a continuous production system for co-producing alkyl naphthalene base oil and liquid wax in one embodiment of the present application is shown;

[0015] Figure 2 A schematic structural diagram of a continuous production system for co-producing alkyl naphthalene base oil and liquid wax in another embodiment of the present application is shown.

[0016] The above drawings include the following reference numerals:

[0017] 100, continuous alkylation reaction unit; 101, first Fischer-Tropsch synthesis oil inlet; 102, first naphthalene inlet; 103, first catalyst inlet; 104, first solvent inlet; 105, product system outlet; 200, first continuous separation unit; 201, product system inlet; 202, catalyst recovery outlet; 203, oil phase outlet; 300, first continuous distillation unit; 301, first oil phase inlet; 302, first distillation product outlet; 303, solvent recovery outlet; 400, second continuous distillation unit; 401, first distillation product inlet; 402, second distillation product outlet; 403, naphthalene recovery outlet; 500, third continuous distillation unit; 501, second distillation product inlet; 502, liquid wax outlet; 503, first alkyl naphthalene base oil outlet; 600, continuous washing unit; 60 1. Second oil phase inlet; 602. Detergent inlet; 603. Washing product outlet; 700. Second continuous separation device; 701. Washing product inlet; 702. Waste detergent outlet; 703. Separation product outlet; 800. Continuous adsorption device; 801. Alkyl naphthalene base oil inlet; 802. Second alkyl naphthalene base oil outlet; 900. First continuous mixing device; 901. Second naphthalene inlet; 902. Second solvent inlet; 903. First mixture outlet; 1000. Fischer-Tropsch synthesis oil storage device; 1100. Catalyst storage device; 1200. First continuous feed pump; 1300. Second continuous mixing device; 1400. Second continuous feed pump; 1500. Third continuous feed pump; 1600. Third continuous mixing device; 1700. Fourth continuous feed pump; 1800. Preheating device. DETAILED DESCRIPTION

[0018] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present invention will be described in detail below in conjunction with the embodiments.

[0019] As described in the background technology, the existing devices for producing alkyl naphthalene base oils have problems such as low reaction efficiency of the reactor and many side reactions leading to low product yield, low raw material utilization leading to high production cost, and the existing production process cannot achieve the co-production of alkyl naphthalene base oil and liquid wax, resulting in low added value. In order to solve the above technical problems, the present application provides a continuous production system for co-producing alkyl naphthalene base oil and liquid wax, such as Figure 1 As shown, the continuous production system includes a continuous alkylation reaction device 100, a first continuous separation device 200, a first continuous distillation device 300, a second continuous distillation device 400 and a third continuous distillation device 500. The continuous alkylation reaction device 100 is used to cause the Fischer-Tropsch synthesis oil and naphthalene to undergo a continuous alkylation reaction in a solvent under the catalysis of a catalyst to obtain a product system; the continuous alkylation reaction device 100 is provided with a first Fischer-Tropsch synthesis oil inlet 101, a first naphthalene inlet 102, a first catalyst inlet 103, a first solvent inlet 104 and a product system outlet 105; the continuous alkylation reaction device 100 is a microreactor; the Fischer-Tropsch synthesis oil includes a mixture of alkanes and olefins with a carbon number of 9 to 24; the catalyst is an ionic liquid catalyst; the first continuous separation device 200 is provided with a product system inlet 201, a recovery catalyst outlet 202 and an oil phase outlet 203; the product system inlet 201 is connected to the product system outlet 105; the recovery catalyst outlet 202 is connected to the first catalyst inlet 103 The first continuous distillation apparatus 300 is provided with a first oil phase inlet 301, a first distillation product outlet 302 and a recovery solvent outlet 303; the first oil phase inlet 301 is communicated with the oil phase outlet 203; the recovery solvent outlet 303 is communicated with the first solvent inlet 104; the second continuous distillation apparatus 400 is provided with a first distillation product inlet 401, a second distillation product outlet 402 and a recovery naphthalene outlet 403; the first distillation product inlet 401 is communicated with the first distillation product outlet 302; the recovery naphthalene outlet 403 is communicated with the first naphthalene inlet 102; the third continuous distillation apparatus 500 is provided with a second distillation product inlet 501, a liquid wax outlet 502 and a first alkyl naphthalene base oil outlet 503; the second distillation product inlet 501 is communicated with the second distillation product outlet 402.

[0020] The above-mentioned continuous production system for co-producing alkyl naphthalene base oil and liquid wax provided in the present application includes a continuous alkylation reaction device 100, a first continuous separation device 200, a first continuous distillation device 300, a second continuous distillation device 400 and a third continuous distillation device 500. The continuous alkylation reaction device 100 can cause the Fischer-Tropsch synthetic oil and naphthalene to undergo continuous alkylation reaction in a solvent under the catalysis of a catalyst to obtain a product system; the microreactor can achieve precise control of the reaction temperature and reaction time due to its smaller channel size (equivalent diameter ≤ 700 μm), shorter mass transfer distance and larger specific surface area, and can also export heat in a strong exothermic reaction in time to maintain the stability of the reaction; compared with the traditional kettle reactor, the continuous alkylation reaction device 100 in the present application adopts a microreactor, which can improve the reaction efficiency of the continuous alkylation reaction, inhibit the occurrence of side reactions caused by local overheating or excessive reaction time, thereby improving the production efficiency of continuous production. The first continuous separation device 200 is used to separate the recovered catalyst from the oil phase in the product system, thereby realizing the recycling of the catalyst; the first continuous distillation device 300 is used to separate and recover the solvent; the second continuous distillation device 400 is used to separate and recover the unreacted raw material naphthalene; the third continuous distillation device 500 is used to separate and obtain alkyl naphthalene base oil and liquid wax. The above-mentioned continuous production system can pass the separated and recovered catalyst, solvent and raw material naphthalene into the continuous alkylation reaction device 100 to participate in the continuous alkylation reaction. The above-mentioned continuous production system of the present application can not only obtain alkyl naphthalene base oil and liquid wax at the same time, thereby improving the added value of production, but also can realize the recycling of catalyst, solvent and excess raw material naphthalene, which can improve the utilization rate of raw materials and reduce costs. Compared with traditional liquid acid catalysts, the use of ionic liquid catalysts can improve the catalytic efficiency of continuous alkylation reactions, thereby improving the reaction efficiency of continuous alkylation reactions, and ionic liquid catalysts are not volatile and are easy to recover. Compared with single carbon number olefins used in traditional alkyl naphthalene base oil production processes, the present application uses Fischer-Tropsch synthetic oil as a starting raw material, which can reduce costs and realize efficient utilization of Fischer-Tropsch synthetic oil.

[0021] In summary, the above-mentioned continuous production system provided in the present application has a simple structure and low energy consumption, and can improve the utilization rate of raw materials and the yield of products.

[0022] In a preferred embodiment, the first continuous distillation device 300 is an atmospheric distillation tower. Compared with other types of distillation towers, the first continuous distillation device 300 is an atmospheric distillation tower, which is simple to operate and has high separation efficiency, is conducive to improving the recovery rate of the solvent, and thus is conducive to improving the utilization rate of raw materials in continuous production, and is suitable for continuous production.

[0023] In a preferred embodiment, the second continuous distillation device 400 is a first vacuum distillation tower. Compared with other types of distillation towers, the second continuous distillation device 400 is a first vacuum distillation tower, which can reduce the boiling point of the first distillation product by reducing the pressure, which is beneficial to reduce the occurrence of thermal decomposition, and is beneficial to improve the separation efficiency of naphthalene, thereby facilitating the improvement of the recovery rate of naphthalene, and further facilitating the improvement of the utilization rate of raw materials in continuous production.

[0024] In a preferred embodiment, the third continuous distillation device 500 is a second vacuum distillation tower. Compared with other types of distillation towers, the third continuous distillation device 500 is a second vacuum distillation tower, which can reduce the boiling point of the second distillation product by reducing the pressure, which is beneficial to reduce the occurrence of thermal decomposition, and is beneficial to improve the separation efficiency of alkyl naphthalene base oil and liquid wax, thereby facilitating the improvement of the yield of alkyl naphthalene base oil and liquid wax, and further facilitating the co-production of alkyl naphthalene base oil and liquid wax, and improving the added value of production.

[0025] The tubular reactor has the characteristics of uniform heating and fast mass transfer, and it has a large heat exchange area, which is particularly suitable for large-scale continuous chemical production. In a preferred embodiment, the continuous alkylation reaction device 100 is a tubular reactor. Compared with other types of reactors, the use of the above-mentioned type of reactor is conducive to improving the reaction efficiency of the continuous alkylation reaction, and is conducive to suppressing the occurrence of side reactions caused by local overheating or excessive reaction time, thereby helping to improve the production efficiency of continuous production and is suitable for continuous production.

[0026] In order to further improve the reaction efficiency of the continuous alkylation reaction and further suppress the occurrence of side reactions caused by local overheating or excessive reaction time, preferably, the diameter of the tubular reactor is 0.2 to 0.7 mm.

[0027] The enamel material is fired at high temperature, and has a smooth and hard surface. It can remain unchanged under extreme temperature, humidity and chemical corrosion. In a preferred embodiment, the material of the first continuous separation device 200 is enamel. Compared with other materials, the use of enamel material is conducive to inhibiting equipment corrosion, extending the service life of the equipment, thereby reducing equipment maintenance, and further reducing costs.

[0028] In a preferred embodiment, the continuous production system further comprises a continuous washing device 600, which is provided with a second oil phase inlet 601, a detergent inlet 602 and a washing product outlet 603, and the second oil phase inlet 601 is connected to the oil phase outlet 203. The continuous washing device 600 is used to wash the oil phase obtained in the first continuous separation process to obtain a washing product, which is beneficial to remove the catalyst remaining in the oil phase, thereby facilitating the separation effect of the subsequent separation step, and further facilitating the improvement of the purity of the alkyl naphthalene base oil and the liquid wax.

[0029] In a preferred embodiment, the continuous production system further comprises a second continuous separation device 700, which is provided with a washing product inlet 701, a waste detergent outlet 702 and a separation product outlet 703; the separation product outlet 703 is connected to the first oil phase inlet 301. The second continuous separation device 700 is used to separate the washing product to remove the waste detergent in the washing product, thereby facilitating the separation effect of the subsequent separation step, and further facilitating the improvement of the purity of the alkyl naphthalene base oil and the liquid wax.

[0030] In a preferred embodiment, the continuous production system further comprises a continuous adsorption device 800, which is provided with an alkylnaphthalene base oil inlet 801 and a second alkylnaphthalene base oil outlet 802; the alkylnaphthalene base oil inlet 801 is connected to the first alkylnaphthalene base oil outlet 503. When the above-mentioned continuous production system further comprises a continuous adsorption device 800, the first alkylnaphthalene base oil outlet 503 in the third continuous adsorption device 800 is used to discharge the alkylnaphthalene base oil crude product, so that the third continuous distillation process obtains the alkylnaphthalene base oil crude product and liquid wax. The continuous adsorption device 800 is used to perform adsorption refining on the alkylnaphthalene base oil crude product, which is beneficial to improve the purity of the alkylnaphthalene base oil, and is beneficial to obtain an alkylnaphthalene base oil with a smaller chroma, thereby improving the product quality of the alkylnaphthalene base oil.

[0031] In a preferred embodiment, a distributor is provided at the top of the inner cavity of the continuous adsorption device 800. The distributor is conducive to improving the distribution uniformity of the crude alkyl naphthalene base oil product in the continuous adsorption device 800, thereby improving the adsorption efficiency of the continuous adsorption, and further improving the product quality of the alkyl naphthalene base oil.

[0032] In order to further improve the distribution uniformity of the crude alkylnaphthalene base oil product in the continuous adsorption device 800, thereby further improving the adsorption efficiency of the continuous adsorption, which is beneficial to further improve the purity of the alkylnaphthalene base oil, preferably, the distributor includes but is not limited to a trough type liquid distributor and / or a disc type hole flow type liquid distributor.

[0033] In a preferred embodiment, a demister is provided at the bottom of the inner cavity of the continuous adsorption device 800. The demister is helpful in removing the foam generated during the continuous adsorption process, thereby helping to improve the purity of the alkyl naphthalene base oil and the product quality.

[0034] In order to further remove the foam generated during the continuous adsorption process, thereby further improving the purity and product quality of the alkyl naphthalene base oil, preferably, the demister includes but is not limited to a baffle demister and / or a swirl plate demister. Compared with other types of demisters, the use of the above-mentioned type of demister is also beneficial to reducing material loss, thereby facilitating improving the yield of the alkyl naphthalene base oil.

[0035] The grid layer has the characteristics of cooling and heat dissipation, the wire mesh layer has the function of filtering, the porcelain ball layer facilitates the distribution of the crude product of alkyl naphthalene base oil to be more uniform, and plays a supporting role, the adsorption layer can play the role of adsorption, and the magnetic ball layer can play the role of material distribution at the same time. In a preferred embodiment, the inner cavity of the continuous adsorption device 800 is sequentially provided with a grid layer, a wire mesh layer, a porcelain ball layer, an adsorption layer and a magnetic ball layer from bottom to top, and the grid layer is located above the demister, and the magnetic ball layer is located below the distributor. The above-mentioned continuous adsorption device 800 is used to improve the adsorption efficiency of the continuous adsorption process, thereby helping to improve the purity and product quality of the alkyl naphthalene base oil.

[0036] In order to further improve the adsorption efficiency of the continuous adsorption device 800, thereby further improving the purity and quality of the alkyl naphthalene base oil, preferably, the material of the adsorption layer includes but is not limited to activated carbon and / or clay.

[0037] In order to further improve the adsorption efficiency of the adsorption layer in the continuous adsorption device 800, thereby further improving the purity and quality of the alkyl naphthalene base oil, preferably, the porosity of the activated carbon is 40-50%, and the specific surface area is 800-1000m 2 / g, specific surface area is 180~200m 2 / g.

[0038] In a preferred embodiment, the continuous production system further comprises a first continuous mixing device 900 for mixing naphthalene with a solvent to obtain a first mixture; the first continuous mixing device 900 is provided with a second naphthalene inlet 901, a second solvent inlet 902 and a first mixture outlet 903; the first mixture outlet 903 is connected to the first Fischer-Tropsch synthetic oil inlet 101, or the first naphthalene inlet 102, or the first catalyst inlet 103, or the first solvent inlet 104. The use of the first continuous mixing device 900 is conducive to mixing naphthalene with the solvent, which is conducive to improving the compatibility of naphthalene with the solvent, thereby improving the reaction efficiency of the continuous alkylation reaction; the first mixture outlet 903 is connected to the first Fischer-Tropsch synthetic oil inlet 101, or the first naphthalene inlet 102, or the first catalyst inlet 103, or the first solvent inlet 104, which is conducive to passing the first mixture into the continuous alkylation reaction device 100 for continuous alkylation reaction, which is conducive to saving the mixing time during the continuous alkylation reaction, thereby improving the continuous production efficiency.

[0039] In a preferred embodiment, the second solvent inlet 902 is connected to the recovery solvent outlet 303; the second naphthalene inlet 901 is connected to the recovery naphthalene outlet 403. The above connection method is convenient for returning the recovery solvent and the recovery naphthalene to the first continuous mixing device 900, which is beneficial to improve the recovery rate of raw materials and reduce costs.

[0040] In a preferred embodiment, the first continuous mixing device 900 is equipped with a stirring member and a heating member, and the heating member is arranged at the periphery of the first continuous mixing device 900. The stirring member is used to stir naphthalene and the solvent, which is conducive to fully mixing naphthalene and the solvent; the heating member is used to heat the first continuous mixing device 900, which is conducive to improving the compatibility of naphthalene and the solvent.

[0041] In a preferred embodiment, the continuous production system further includes a Fischer-Tropsch synthesis oil storage device 1000 for storing and supplying Fischer-Tropsch synthesis oil, and the Fischer-Tropsch synthesis oil storage device 1000 is connected to the continuous alkylation reaction device 100. The Fischer-Tropsch synthesis oil storage device 1000 can store Fischer-Tropsch synthesis oil on the one hand, and can continuously provide raw materials to the continuous alkylation reaction on the other hand, thereby facilitating improving the production efficiency of continuous production.

[0042] In a preferred embodiment, the continuous production system further includes a catalyst storage device 1100 for storing and supplying catalysts, and the catalyst storage device 1100 is connected to the continuous alkylation reaction device 100 and / or the first continuous separation device 200. The catalyst storage device 1100 can store additional added catalysts on the one hand, and can also store recovered catalysts separated by the first continuous separation device 200 on the other hand. At the same time, the setting of the catalyst storage device 1100 is conducive to continuously providing catalysts to the continuous alkylation reaction, thereby facilitating the improvement of the production efficiency of the continuous production.

[0043] In a preferred embodiment, the catalyst storage device 1100 is connected to the first continuous separation device 200 via a recovered catalyst delivery pipeline. The above connection method facilitates returning the recovered catalyst to the catalyst storage device 1100, thereby facilitating the improvement of the catalyst recovery rate.

[0044] In order to facilitate the control of the feed amount and feed rate of the recovered catalyst into the catalyst storage device 1100, thereby facilitating the improvement of the stability and safety of continuous production, preferably, a first continuous feed pump 1200 is provided on the recovered catalyst delivery pipeline.

[0045] In a preferred embodiment, the continuous production system further includes a second continuous mixing device 1300 for mixing the first mixture with the Fischer-Tropsch synthetic oil to obtain a second mixture; the second continuous mixing device 1300 is connected to the first continuous mixing device 900, the Fischer-Tropsch synthetic oil storage device 1000 and the continuous alkylation reaction device 100. The use of the second continuous mixing device 1300 is conducive to mixing the first mixture with the Fischer-Tropsch synthetic oil, which is conducive to improving the compatibility of the two, thereby improving the reaction efficiency of the continuous alkylation reaction; the second continuous mixing device 1300 is connected to the continuous alkylation reaction device 100, which is conducive to passing the second mixture into the continuous alkylation reaction device 100 for continuous alkylation reaction, which is conducive to saving the mixing time during the continuous alkylation reaction, thereby helping to improve the continuous production efficiency.

[0046] In order to facilitate the control of the feed amount and feed rate of the first mixture into the second continuous mixing device 1300, thereby improving the stability and safety of continuous production, preferably, the second continuous mixing device 1300 is connected to the first continuous mixing device 900 through a first mixture conveying pipeline, and a second continuous feed pump 1400 is provided on the first mixture conveying pipeline.

[0047] In order to facilitate the control of the feed amount and feed rate of Fischer-Tropsch oil into the second continuous mixing device 1300, thereby improving the stability and safety of continuous production, preferably, the second continuous mixing device 1300 is connected to the Fischer-Tropsch oil storage device 1000 through a Fischer-Tropsch oil delivery pipeline, and a third continuous feed pump 1500 is arranged on the Fischer-Tropsch oil delivery pipeline.

[0048] In a preferred embodiment, the continuous production system further includes a third continuous mixing device 1600, which is used to mix the second mixture with the catalyst and / or the recovered catalyst to obtain a third mixture; the third continuous mixing device 1600 is connected to the second continuous mixing device 1300, the catalyst storage device 1100 and the continuous alkylation reaction device 100. The use of the third continuous mixing device 1600 is conducive to mixing the second mixture with the catalyst, which is conducive to improving the compatibility of each material, thereby improving the reaction efficiency of the continuous alkylation reaction; the third continuous mixing device 1600 is connected to the continuous alkylation reaction device 100, which is conducive to passing the third mixture into the continuous alkylation reaction device 100 for continuous alkylation reaction, which is conducive to saving the mixing time during the continuous alkylation reaction, thereby helping to improve the continuous production efficiency.

[0049] In order to facilitate the control of the feed amount and feed rate of the catalyst into the third continuous mixing device 1600, thereby improving the stability and safety of continuous production, preferably, the third continuous mixing device 1600 is connected to the catalyst storage device 1100 through a catalyst delivery pipeline, and a fourth continuous feed pump 1700 is arranged on the catalyst delivery pipeline.

[0050] In a preferred embodiment, the third continuous mixing device 1600 is connected to the continuous alkylation reaction device 100 through a third mixture delivery pipeline, and the third mixture delivery pipeline is provided with a preheating device 1800. The preheating device 1800 is used to preheat the third mixture to facilitate the subsequent continuous alkylation reaction, thereby improving the reaction efficiency of the continuous alkylation reaction.

[0051] In order to improve the preheating efficiency of the second mixture and reduce equipment cost, preferably, the preheating device 1800 is a tubular heat exchanger.

[0052] Microchannel reactors have the characteristics of efficient and rapid mixing of materials; membrane dispersion microreactors can achieve rapid and uniform mixing at the millisecond level; microsieve reactors have the characteristics of simple operation, rapid and efficient, and large processing capacity per unit volume. In a preferred embodiment, the second continuous mixing device 1300 and the third continuous mixing device 1600 each independently include but are not limited to a microchannel reactor, a membrane dispersion microreactor or a microsieve reactor. Compared with other types of reactors, the use of the above-mentioned types of reactors is conducive to increasing the mixing rate, thereby helping to improve the continuous production efficiency.

[0053] The second aspect of the present application also provides a continuous production method for co-producing alkylnaphthalene base oil and liquid wax using the above-mentioned continuous production system, and the continuous production method comprises: step S1, passing Fischer-Tropsch synthetic oil, naphthalene, catalyst and solvent into a continuous alkylation reaction device 100 for continuous alkylation reaction to obtain a product system; wherein the Fischer-Tropsch synthetic oil comprises a mixture of alkanes and olefins having a carbon number of 9 to 24, and the catalyst is an ionic liquid catalyst; step S2, passing the product system into a first continuous separation device 200 for separation to obtain a recovered catalyst and an oil phase; returning at least part of the recovered catalyst to step S1; step S3, passing the oil phase into a first continuous distillation device 300 for a first continuous distillation to obtain a first distillation product and a recovered solvent; returning at least part of the recovered solvent to step S1; step S4, passing the first distillation product into a second continuous distillation device 400 for a second continuous distillation to obtain a second distillation product and recovered naphthalene; returning at least part of the recovered naphthalene to step S1; step S5, passing the second distillation product into a third continuous distillation device 500 for a third continuous distillation to obtain an alkylnaphthalene base oil and liquid wax.

[0054] Compared with the use of traditional kettle reactors for alkylation reactions, the use of microreactors for continuous alkylation reactions in the present application can improve the reaction efficiency of the continuous alkylation reaction and inhibit the occurrence of side reactions caused by local overheating or excessive reaction time, thereby improving the production efficiency of continuous production.

[0055] Compared with the single carbon number olefins used in the traditional alkyl naphthalene base oil production process, the present application uses Fischer-Tropsch synthetic oil as the starting raw material, which can reduce costs and achieve efficient utilization of Fischer-Tropsch synthetic oil. At the same time, compared with other carbon numbers, the use of the above-mentioned specific carbon number Fischer-Tropsch synthetic oil in the present application can improve the product quality of alkyl naphthalene base oil and liquid wax.

[0056] Ionic liquid catalysts have high catalytic activity and good stability. Compared with other types, the use of ionic liquid catalysts as catalysts in continuous alkylation reactions can improve the catalytic efficiency of the continuous alkylation reaction, thereby helping to improve the reaction efficiency of the continuous alkylation reaction. At the same time, ionic liquid catalysts are non-volatile and easy to recycle, which can improve the recovery rate of the catalyst, thereby realizing the reuse of the catalyst in continuous production.

[0057] Fischer-Tropsch synthetic oil and naphthalene can undergo continuous alkylation reaction in a solvent under the catalysis of a catalyst to obtain a product system; after separating the recovered catalyst and the oil phase in the product system, the recovered catalyst is returned to step S1, so that the catalyst can be recycled; the obtained oil phase is subjected to a first continuous distillation to obtain a first distillation product and a recovered solvent, and the recovered solvent is returned to step S1, so that the solvent can be recycled; the obtained first distillation product is subjected to a second continuous distillation to obtain a second distillation product and recovered naphthalene, and the recovered naphthalene is returned to step S1, so that naphthalene can be recycled; the obtained second distillation product is subjected to a third continuous distillation to obtain an alkyl naphthalene base oil and liquid wax, so as to realize the co-production of the two. The above-mentioned continuous production method of the present application can not only obtain alkyl naphthalene base oil and liquid wax at the same time, thereby improving the added value of production, but also realize the recycling of catalysts, solvents and raw materials, and can improve the utilization rate of raw materials, thereby reducing costs.

[0058] In summary, the above-mentioned continuous production method provided in the present application is simple and efficient to operate, can improve the utilization rate of raw materials and the yield of products, and can realize continuous production.

[0059] In a preferred embodiment, the first continuous distillation is a continuous atmospheric distillation. The first continuous distillation is carried out by atmospheric distillation, which has low cost and is easy to operate. Only simple heating and cooling are required to separate the solvent in the oil phase from the first distillation product, which is beneficial to improving the recovery rate of the solvent, thereby improving the utilization rate of raw materials in continuous production.

[0060] In order to further improve the recovery rate of the solvent and thus further improve the utilization rate of raw materials in continuous production, preferably, a first continuous distillation is performed on the oil phase in step S2 using an atmospheric distillation tower to obtain a first distillation product and a recovered solvent.

[0061] In a preferred embodiment, the number of theoretical plates of the atmospheric distillation tower is 30 to 60, the tower top temperature is 78 to 82°C, the tower top pressure is 10 to 50 kPa, the tower bottom temperature is 220 to 240°C, the reflux ratio is 1 to 5, and the feed position of the oil phase is the 15th to 30th plate. The number of theoretical plates, tower top temperature, tower top pressure, tower bottom temperature, reflux ratio and feed position of the oil phase of the atmospheric distillation tower include but are not limited to the above ranges, and limiting them within the above ranges is conducive to improving the separation efficiency of the first continuous distillation, and is conducive to improving the recovery and utilization rate of the solvent, thereby helping to reduce production costs.

[0062] In order to further improve the separation efficiency of the first continuous distillation, and thus further improve the recovery rate of the solvent, preferably, the content of the solvent in the bottom of the atmospheric distillation tower is ≤0.05% by weight of the bottom material of the atmospheric distillation tower.

[0063] In a preferred embodiment, the second continuous distillation is a continuous vacuum distillation. Compared with atmospheric distillation, vacuum distillation can reduce the boiling point of the separated substance by reducing the pressure, which is beneficial to reduce the occurrence of thermal decomposition, and is beneficial to improve the separation efficiency of the second continuous distillation, thereby helping to improve the recovery rate of naphthalene, and further helping to reduce production costs.

[0064] In order to further improve the recovery rate of naphthalene, and thus further improve the utilization rate of raw materials in continuous production, it is preferred to use a first vacuum distillation tower to perform a second continuous distillation on the first distillation product in step S3 to obtain a second distillation product and recovered naphthalene.

[0065] In a preferred embodiment, the number of theoretical plates of the first vacuum distillation tower is 40 to 80, the tower top temperature is 215 to 220° C., the tower top pressure is 10 to 20 kPa, the tower bottom temperature is 305 to 315° C., the reflux ratio is 2 to 10, and the feeding position of the first distillation product is the 20th to 40th plate. The number of theoretical plates, tower top temperature, tower top pressure, tower bottom temperature, reflux ratio and the feeding position of the first distillation product of the first vacuum distillation tower include but are not limited to the above ranges, and limiting them within the above ranges is conducive to improving the separation efficiency of the second continuous distillation, and is conducive to improving the recovery and utilization rate of naphthalene, thereby helping to reduce production costs.

[0066] In order to further improve the separation efficiency of the second continuous distillation, and thus further improve the recovery rate of naphthalene, preferably, the content of naphthalene in the bottom of the first vacuum distillation tower is ≤0.05% by weight of the bottom material of the first vacuum distillation tower.

[0067] In a preferred embodiment, the third continuous distillation is a continuous vacuum distillation. Compared with atmospheric distillation, vacuum distillation can reduce the boiling point of the separated substances by reducing the pressure, which is beneficial to reduce the occurrence of thermal decomposition, and is beneficial to improve the separation efficiency of alkyl naphthalene base oil and liquid wax, thereby helping to improve the yield of alkyl naphthalene base oil and liquid wax, and further to achieve the co-production of alkyl naphthalene base oil and liquid wax, which is beneficial to improve the added value of production.

[0068] In order to further improve the separation efficiency of alkylnaphthalene base oil and liquid wax, thereby further improving the yield of alkylnaphthalene base oil and liquid wax, preferably, a second vacuum distillation tower is used to perform a third continuous distillation on the second distillation product in step S4 to obtain alkylnaphthalene base oil and liquid wax.

[0069] In a preferred embodiment, the second vacuum distillation tower has a theoretical plate number of 40 to 80, a tower top temperature of 140 to 145° C., a tower top pressure of 1 to 10 kPa, a tower bottom temperature of 170 to 180° C., a reflux ratio of 2 to 8, and the feeding position of the second distillation product is the 20th to 40th plate. The theoretical plate number, tower top temperature, tower top pressure, tower bottom temperature, reflux ratio and the feeding position of the second distillation product of the second vacuum distillation tower include but are not limited to the above ranges, and limiting them within the above ranges is conducive to improving the separation efficiency of the third continuous distillation, and is conducive to improving the yield of alkyl naphthalene base oil and liquid wax, thereby facilitating the co-production of alkyl naphthalene base oil and liquid wax.

[0070] In order to further improve the separation efficiency of the third continuous distillation, thereby further improving the yield of alkylnaphthalene base oil and liquid wax, preferably, the content of liquid wax in the bottom of the second vacuum distillation tower is ≤25ppm, measured by weight percentage of the bottom material of the second vacuum distillation tower.

[0071] In a preferred embodiment, the reaction temperature of the continuous alkylation reaction is 30-90° C., the reaction pressure is 0.5-1.5 MPa, and the material residence time is 0.1-10 min. Compared with other ranges, limiting the reaction temperature, reaction pressure and material residence time of the continuous alkylation reaction within the above range is conducive to improving the reaction rate of the continuous alkylation reaction, inhibiting side reactions, thereby facilitating the increase of the yield of alkyl naphthalene base oil and liquid wax, and also facilitating the improvement of the efficiency of continuous production.

[0072] In a preferred embodiment, in step S1, the feed rate of Fischer-Tropsch synthesis oil is 1.1-2.3 kg / h, the feed rate of naphthalene is 7.0-14.2 kg / h, the feed rate of solvent is 28.2-56.5 kg / h, and the feed rate of catalyst is 0.50-0.92 kg / h. The feed rates of Fischer-Tropsch synthesis oil, naphthalene, solvent and catalyst include but are not limited to the above ranges, and limiting them within the above ranges is conducive to improving the utilization rate of the above raw materials, improving the reaction efficiency of the continuous alkylation reaction, inhibiting side reactions, and thus helping to improve the yield of alkyl naphthalene base oil and liquid wax.

[0073] In a preferred embodiment, the Fischer-Tropsch oil comprises a mixture of alkanes and olefins having a carbon number of 14 to 16. The carbon number of the Fischer-Tropsch oil includes but is not limited to the above range, and limiting it to the above range is conducive to improving the product quality of alkyl naphthalene base oil and liquid wax.

[0074] In order to improve the solubility of naphthalene, thereby facilitating the improvement of the reaction rate of the continuous alkylation reaction, in a preferred embodiment, the solvent includes but is not limited to one or more of the group consisting of cyclohexane, cycloheptane and cyclooctane.

[0075] In a preferred embodiment, the ionic liquid catalyst includes but is not limited to 1-alkyl-3-methylimidazolium naphthylacetate ionic liquid catalyst and / or chloroaluminate ionic liquid catalyst. Compared with other types, the use of the above-mentioned types of ionic liquid catalysts is conducive to improving the catalytic efficiency of the catalyst, thereby facilitating the improvement of the rate of the continuous alkylation reaction. At the same time, the above-mentioned types of ionic liquid catalysts are more convenient to recycle, which is conducive to improving the recovery rate of the catalyst and facilitating the reuse of the catalyst in continuous production.

[0076] In order to further improve the catalytic efficiency of the catalyst and further improve the recovery rate of the catalyst, preferably, the 1-alkyl-3-methylimidazolium naphthylacetate ionic liquid catalyst includes but is not limited to one or more of the group consisting of 1-butyl-3-methylimidazolium naphthylacetate ionic liquid catalyst, 1-hexyl-3-methylimidazolium naphthylacetate ionic liquid catalyst and 1-octyl-3-methylimidazolium naphthylacetate ionic liquid catalyst; the chloroaluminate ionic liquid catalyst includes but is not limited to Me 3 HNCl-xAlCl 3 and / or Et 3 HNCl-xAlCl 3 More preferably, Me 3 HNCl-xAlCl 3 Compared with other types, the use of Me 3 HNCl-xAlCl 3Ionic liquid catalysts are beneficial to further improving the catalytic efficiency of the catalyst and improving the recovery rate of the catalyst. At the same time, the preparation method thereof is simple, which is beneficial to reducing the production cost.

[0077] In a preferred embodiment, the following steps are further included between step S2 and step S3: step S2-A: passing the oil phase and the detergent into the continuous washing device 600 for continuous washing to obtain a washing product. Washing the oil phase obtained in step S2 is beneficial to removing the catalyst remaining in the oil phase, thereby improving the separation effect of the subsequent separation step, and further improving the purity of the alkyl naphthalene and the liquid wax.

[0078] In order to further remove the residual catalyst in the oil phase, preferably, the washing agent is water.

[0079] In a preferred embodiment, between step S2 and step S3, there is also a step S2-B: passing the washed product into the second continuous separation device 700 for separation to obtain a separated product. The washed product is subjected to a second continuous separation to remove the waste detergent in the washed product, thereby facilitating the separation effect of the subsequent first distillation product and the recovered solvent, and further facilitating the improvement of the yield of the alkyl naphthalene base oil and the liquid wax. Preferably, the second continuous separation process is a static separation process.

[0080] In a preferred embodiment, step S5 includes: passing the second distillation product into a third continuous distillation device 500 for a third continuous distillation to obtain a crude alkylnaphthalene base oil product, and continuously adsorbing and refining the crude alkylnaphthalene base oil product using a continuous adsorption device 800 to obtain an alkylnaphthalene base oil. Continuously adsorbing the crude alkylnaphthalene base oil product obtained by the third continuous distillation is beneficial to improving the purity of the alkylnaphthalene base oil, and is beneficial to obtaining an alkylnaphthalene base oil with a smaller chroma, thereby improving the product quality of the alkylnaphthalene base oil.

[0081] Compared with other ranges, limiting the rate at which the crude alkylnaphthalene base oil product is introduced into the continuous adsorption device 800 and the material residence time within the above range is beneficial to improving the adsorption efficiency, thereby improving the purity and product quality of the alkylnaphthalene base oil, and also improving the efficiency of continuous production.

[0082] In order to improve the adsorption efficiency of continuous adsorption, thereby further improving the purity and product quality of alkyl naphthalene base oil, preferably, the temperature of continuous adsorption is 30-60°C, and the adsorption space velocity is 1-5h -1 .

[0083] In a preferred embodiment, before step S1, the process further includes: performing a first continuous mixing on naphthalene and the solvent by using a first continuous mixing device 900 to obtain a first mixture. Premixing naphthalene and the solvent to obtain the first mixture is beneficial to improving the compatibility of the two, facilitating improving the reaction efficiency of the continuous alkylation reaction, and shortening the mixing time of the continuous alkylation reaction.

[0084] In a preferred embodiment, stirring is performed during the first continuous mixing process; preferably, the stirring rate is 100 to 500 rpm. Stirring is performed during the mixing of naphthalene and the solvent, and limiting the stirring rate to the above range is conducive to fully mixing naphthalene and the solvent, thereby facilitating improving the compatibility of naphthalene and the solvent.

[0085] In a preferred embodiment, heating is performed during the first continuous mixing process; preferably, the temperature of the first continuous mixing is 30 to 70° C., and the material residence time is 30 to 50 min. Heating during the mixing of naphthalene and the solvent, and limiting the temperature of the first continuous mixing and the material residence time to the above range is conducive to improving the mixing efficiency of naphthalene and the solvent, thereby helping to improve the compatibility of naphthalene and the solvent, and helping to inhibit the precipitation of naphthalene from the solvent.

[0086] In a preferred embodiment, the content of naphthalene is 10-30wt% in terms of weight percentage of the first mixture. Compared with other ranges, limiting the content of naphthalene within the above range is conducive to improving the reaction efficiency of the subsequent continuous alkylation reaction, thereby facilitating the increase in the yield of alkyl naphthalene base oil and liquid wax.

[0087] In a preferred embodiment, between step S1 and the first continuous mixing, the step further includes: performing a second continuous mixing of the first mixture and the Fischer-Tropsch synthetic oil by a second continuous mixing device 1300 to obtain a second mixture. Premixing the first mixture and the Fischer-Tropsch synthetic oil to obtain the second mixture is beneficial to improving the compatibility of the two, facilitating the improvement of the reaction efficiency of the continuous alkylation reaction, and at the same time, is beneficial to improving the efficiency of continuous production.

[0088] In a preferred embodiment, heating is performed during the second continuous mixing process; preferably, the temperature of the second continuous mixing is 30-70°C, and the material residence time is 0.1-1s. Heating during the second continuous mixing process and limiting the temperature and material residence time of the process within the above range is conducive to improving the mixing efficiency of the first mixture and the Fischer-Tropsch synthetic oil, and is conducive to improving the compatibility of the two, and is convenient for subsequent continuous alkylation reaction.

[0089] In order to further improve the mixing efficiency of the first mixture and the Fischer-Tropsch synthetic oil, thereby further improving the reaction efficiency of the subsequent continuous alkylation reaction, preferably, in the second continuous mixing, the feed rate of the first mixture is 7.0-14.2 kg / h, and the feed rate of the Fischer-Tropsch synthetic oil is 1.1-2.3 kg / h.

[0090] In a preferred embodiment, the continuous production method further comprises: using a Fischer-Tropsch synthesis oil storage device 1000 to store the Fischer-Tropsch synthesis oil, and passing the Fischer-Tropsch synthesis oil into the continuous alkylation reaction device 100 for continuous alkylation reaction; preferably, using an inert gas to seal the Fischer-Tropsch synthesis oil storage device 1000, and the inert gas includes but is not limited to nitrogen. The above method is convenient for the storage of the Fischer-Tropsch synthesis oil and is conducive to suppressing the volatilization of the Fischer-Tropsch synthesis oil.

[0091] In a preferred embodiment, between step S1 and the second continuous mixing, the step further includes: performing a third continuous mixing of the second mixture and the catalyst to obtain a third mixture by using a third continuous mixing device 1600. Premixing the second mixture and the catalyst to obtain the third mixture is beneficial to improving the compatibility of the materials, facilitating the improvement of the reaction efficiency of the continuous alkylation reaction, and thus facilitating the shortening of the mixing time of the continuous alkylation reaction.

[0092] In a preferred embodiment, heating is performed during the third continuous mixing process; preferably, the temperature of the third continuous mixing is 30-70°C, and the material residence time is 0.1-1s. Heating during the third continuous mixing process and limiting the temperature and material residence time of the process within the above range is beneficial to improving the mixing efficiency of the second mixture and the catalyst, improving the compatibility of each material, and shortening the mixing time of the continuous alkylation reaction. In order to further improve the mixing efficiency of the second mixture and the catalyst, thereby further improving the reaction efficiency of the continuous alkylation reaction, preferably, in the third continuous mixing, the feed rate of the second mixture is 8.1-16.4kg / h, and the feed rate of the catalyst is 0.50-0.92kg / h.

[0093] In a preferred embodiment, the continuous production method further comprises: using a catalyst storage device 1100 to store the catalyst, and passing the catalyst into the continuous alkylation reaction device 100 for continuous alkylation reaction; preferably, using an inert gas to seal the catalyst storage device 1100, the inert gas includes but is not limited to nitrogen. The above method is conducive to maintaining the activity of the catalyst in the catalyst storage device 1100, and inhibiting the decrease in activity or even deactivation.

[0094] The present application is further described in detail below in conjunction with specific embodiments. These embodiments should not be construed as limiting the scope of protection claimed in the present application.

[0095] It should be noted that the ionic liquid catalysts used in all the examples and comparative examples of this application are Me 3 HNCl-xAlCl 3 The preparation method is as follows: (1) at 60°C, high-purity nitrogen is introduced into a dry three-necked flask at a flow rate of 20 mL / min for 30 minutes to replace the air retained in the flask, ensuring that the entire reaction system is carried out under anhydrous and oxygen-free conditions; (2) after the internal and external air pressures are balanced, the nitrogen flow rate is adjusted to 10 mL / min, and then trimethylamine hydrochloride and anhydrous aluminum chloride are added to the three-necked flask in sequence according to a weight ratio of 1:3, and after stirring at 60°C and a rotation speed of 500 rpm for 1 hour, the stirring is stopped and the mixture is allowed to stand for 5 minutes to obtain a yellow-brown ionic liquid catalyst.

[0096] The compositions of the Fischer-Tropsch synthetic oil used in all the examples and comparative examples 2 to 4 in the present application are shown in Table 1.

[0097] Table 1

[0098] Element <![CDATA[C 9 ~C 16 Olefins]]> <![CDATA[C 9 ~C 16 Alkanes]]> Oxygenated compounds Water (ppm) Content (wt%) 40~60 36~57 3~4 <50

[0099] Example 1

[0100] A continuous production method for co-producing alkyl naphthalene base oil and liquid wax, using Figure 2 The continuous production system for co-producing alkyl naphthalene base oil and liquid wax shown in the figure is prepared, comprising the following steps:

[0101] (1) introducing naphthalene and cyclohexane into a stirred tank, stirring at 50° C. and 300 rpm for 40 min to dissolve naphthalene in the cyclohexane, to obtain a first mixture having a naphthalene content of 20 wt %;

[0102] At 70° C., introducing the Fischer-Tropsch synthetic oil and the first mixture into a first microchannel reactor for mixing, wherein the feed rate of the Fischer-Tropsch synthetic oil is 1.9 kg / h, the feed rate of the first mixture is 11.76 kg / h, and the material residence time is 0.5 s, to obtain a second mixture;

[0103] At 60°C, Me 3 HNCl-xAlCl 3 The ionic liquid catalyst and the second mixture are introduced into a second microchannel reactor for mixing, wherein the feed rate of the ionic liquid catalyst is 0.8 kg / h, the feed rate of the second mixture is 12.3 kg / h, and the material residence time is 0.5 s, to obtain a third mixture;

[0104] (2) preheating the third mixture to 70° C. via a tubular heat exchanger, and then passing the third mixture into a tubular reactor (with a tube diameter of 0.5 mm), and continuously performing an alkylation reaction under reaction conditions of 70° C. and 1.0 MPa to obtain a product system, wherein the feed rate of the third mixture is 13.1 kg / h, and the material residence time is 0.5 s;

[0105] (3) The product system is passed into the first enamel separation tank and allowed to stand for 10 min to separate the oil phase and the recovered catalyst. The recovered catalyst is transported to the catalyst storage tank through a feed pump and then returned to the second microchannel reactor for reuse as needed;

[0106] The oil phase is passed into a water washing tank and washed with water at 35° C. to remove the residual ionic liquid catalyst in the oil phase, thereby obtaining a water-washed product;

[0107] The washed product is passed into the second enamel separation tank and allowed to stand for 30 minutes to remove waste water from the washed product to obtain a separated product;

[0108] (4) passing the separated product into an atmospheric distillation tower for atmospheric distillation to obtain a first distillation product and recovered cyclohexane; returning all the recovered cyclohexane to the stirred tank of step (1); wherein the atmospheric distillation tower has 40 theoretical plates, a tower top temperature of 80° C., a tower top pressure of 30 kPa, a tower bottom temperature of 230° C., a reflux ratio of 3, and the feeding position of the separated product is the 20th plate;

[0109] The first distillation product is passed into a first vacuum distillation tower for vacuum distillation to obtain a second distillation product and recovered naphthalene; and all the recovered naphthalene is returned to the stirred tank of step (1); wherein the first vacuum distillation tower has 60 theoretical plates, a tower top temperature of 217° C., a tower top pressure of 15 kPa, a tower bottom temperature of 310° C., a reflux ratio of 4, and the feeding position of the first distillation product is the 30th plate;

[0110] The second distillation product is passed into a second vacuum distillation tower for vacuum distillation, wherein the second vacuum distillation tower has 60 theoretical plates, a tower top temperature of 143° C., a tower top pressure of 2 kPa, a tower bottom temperature of 175° C., a reflux ratio of 4, and a feeding position of the second distillation product is the 30th plate. The obtained alkylnaphthalene base oil crude product is discharged from the first alkylnaphthalene base oil outlet 503 at a rate of 1.25 kg / h, and liquid wax is discharged from the liquid wax outlet 502 at a rate of 1.12 kg / h;

[0111] (5) The crude alkyl naphthalene base oil product is introduced into a continuous adsorption device 800, wherein the kaolin (specific surface area: 900 m 2 / g) as adsorbent at 40℃ for 2h -1Adsorption refining is carried out under the condition of adsorption space velocity to obtain alkyl naphthalene base oil.

[0112] Example 2

[0113] The difference from Example 1 is that: in step (1), the content of naphthalene is 10wt% in terms of weight percentage of the first mixture; during the mixing process of the Fischer-Tropsch oil and the first mixture, the feed rate of the Fischer-Tropsch oil is 1.1kg / h, the feed rate of the first mixture is 7.0kg / h, and the material residence time is 0.1s; in Me 3 HNCl-xAlCl 3 During the mixing process of the ionic liquid catalyst and the second mixture, the feed rate of the ionic liquid catalyst was 0.50 kg / h, the feed rate of the second mixture was 8.1 kg / h, and the material residence time was 0.1 s; the remaining steps were the same as in Example 1.

[0114] Example 3

[0115] The difference from Example 1 is that: in step (1), the content of naphthalene is 30wt% in terms of weight percentage of the first mixture; during the mixing process of the Fischer-Tropsch oil and the first mixture, the feed rate of the Fischer-Tropsch oil is 2.3kg / h, the feed rate of the first mixture is 14.2kg / h, and the material residence time is 1s; in Me 3 HNCl-xAlCl 3 During the mixing process of the ionic liquid catalyst and the second mixture, the feed rate of the ionic liquid catalyst was 0.92 kg / h, the feed rate of the second mixture was 16.4 kg / h, and the material residence time was 1 s; the remaining steps were the same as in Example 1.

[0116] Example 4

[0117] The difference from Example 1 is that: in step (1), the content of naphthalene is 5wt% in terms of weight percentage of the first mixture; during the mixing process of the Fischer-Tropsch oil and the first mixture, the feed rate of the Fischer-Tropsch oil is 3.2kg / h, the feed rate of the first mixture is 6.4kg / h, and the material residence time is 0.05s; in Me 3 HNCl-xAlCl 3 During the mixing process of the ionic liquid catalyst and the second mixture, the feed rate of the ionic liquid catalyst was 0.47 kg / h, the feed rate of the second mixture was 7.9 kg / h, and the material residence time was 0.05 s; the remaining steps were the same as in Example 1.

[0118] Example 5

[0119] The difference from Example 1 is that in step (2), the reaction conditions of the continuous alkylation reaction are: reaction temperature is 30° C., reaction pressure is 0.5 MPa, and material residence time is 10 min; the remaining steps are the same as Example 1.

[0120] Example 6

[0121] The difference from Example 1 is that in step (2), the reaction conditions of the continuous alkylation reaction are: reaction temperature is 90° C., reaction pressure is 1.5 MPa, and material residence time is 0.1 min; the remaining steps are the same as Example 1.

[0122] Example 7

[0123] The difference from Example 1 is that in step (2), the reaction conditions of the continuous alkylation reaction are: reaction temperature is 150° C., reaction pressure is 2 MPa, and material residence time is 15 min; the remaining steps are the same as Example 1.

[0124] Example 8

[0125] The difference from Example 1 is that: in step (4), the number of theoretical plates of the atmospheric distillation tower is 60, the tower top temperature is 82°C, the tower top pressure is 50 kPa, the tower bottom temperature is 240°C, the reflux ratio is 5, and the feed position of the separated product is the 30th plate; the number of theoretical plates of the first vacuum distillation tower is 80, the tower top temperature is 220°C, the tower top pressure is 20 kPa, the tower bottom temperature is 315°C, the reflux ratio is 10, and the feed position of the first distillation product is the 40th plate; the number of theoretical plates of the second vacuum distillation tower is 80, the tower top temperature is 145°C, the tower top pressure is 10 kPa, the tower bottom temperature is 180°C, the reflux ratio is 8, and the feed position of the second distillation product is the 40th plate; the remaining steps are the same as in Example 1.

[0126] Example 9

[0127] The difference from Example 1 is that: in step (4), the number of theoretical plates of the atmospheric distillation tower is 30, the tower top temperature is 78°C, the tower top pressure is 10 kPa, the tower bottom temperature is 220°C, the reflux ratio is 1, and the feed position of the separated product is the 15th plate; the number of theoretical plates of the first vacuum distillation tower is 40, the tower top temperature is 215°C, the tower top pressure is 10 kPa, the tower bottom temperature is 305°C, the reflux ratio is 2, and the feed position of the first distillation product is the 20th plate; the number of theoretical plates of the second vacuum distillation tower is 40, the tower top temperature is 140°C, the tower top pressure is 1 kPa, the tower bottom temperature is 170°C, the reflux ratio is 2, and the feed position of the second distillation product is the 20th plate; the remaining steps are the same as in Example 1.

[0128] Example 10

[0129] The difference from Example 1 is that: in step (4), the number of theoretical plates of the atmospheric distillation tower is 20, the tower top temperature is 60°C, the tower top pressure is 5 kPa, the tower bottom temperature is 200°C, the reflux ratio is 8, and the feed position of the separated product is the 12th plate; the number of theoretical plates of the first vacuum distillation tower is 30, the tower top temperature is 200°C, the tower top pressure is 5 kPa, the tower bottom temperature is 280°C, the reflux ratio is 1, and the feed position of the first distillation product is the 15th plate; the remaining steps are the same as in Example 1.

[0130] Embodiment 11

[0131] The difference from Example 1 is that in step (4), the theoretical number of plates of the second vacuum distillation tower is 30, the top temperature is 120° C., the top pressure is 15 kPa, the bottom temperature is 150° C., the reflux ratio is 1, and the feeding position of the second distillation product is the 15th plate; the remaining steps are the same as in Example 1.

[0132] Example 12

[0133] The difference from Example 1 is that the adsorption refining in step (5) is carried out at 60°C for 5 h. -1 The adsorption was carried out under the conditions of adsorption space velocity, and the remaining steps were the same as those in Example 1.

[0134] Embodiment 13

[0135] The difference from Example 1 is that the adsorption refining in step (5) is carried out at 100°C for 10 h. -1 The adsorption was carried out under the conditions of adsorption space velocity, and the remaining steps were the same as those in Example 1.

[0136] Embodiment 14

[0137] The difference from Example 1 is that the adsorption refining process in step (5) is omitted, the crude alkyl naphthalene base oil product obtained in step (4) is used as the final product, and the remaining steps are the same as in Example 1.

[0138] Comparative Example 1

[0139] The difference from Example 1 is that the continuous alkylation reaction in step (2) is carried out in a tank reactor, and the remaining steps are the same as in Example 1.

[0140] Comparative Example 2

[0141] The difference from Example 1 is that the reaction and each step are batch reactions.

[0142] Comparative Example 3

[0143] The difference from Example 1 is that 1-octene (CAS No.: 111-66-0) is used as the raw material in step (1), and the remaining steps are the same as those in Example 1.

[0144] Comparative Example 4

[0145] The difference from Example 1 is that the recovered cyclohexane obtained in step (4) is not returned to step (1), and the remaining steps are the same as in Example 1.

[0146] Comparative Example 5

[0147] The difference from Example 1 is that the recovered naphthalene obtained in step (4) is not returned to step (1), and the remaining steps are the same as in Example 1.

[0148] The alkyl naphthalene base oils prepared in all the examples and comparative examples of the present application were subjected to viscosity test, pour point test, flash point test, color test, acid value test and water content test. (1) The viscosity at 40°C was measured according to the method in GB / T265; (2) The viscosity at 100°C was measured according to the method in GB / T265; (3) The viscosity index was measured according to the method in GB / T265; (4) The pour point was measured according to the method in GB / T3535; (5) The flash point was measured according to the method in GB / T3536; (6) The color was measured according to the method in GB / T6540; (7) The acid value was measured according to the method in GB / T264; (8) The water content was measured according to the method in GB / T260.

[0149] The test results are shown in Table 2.

[0150] Table 2

[0151]

[0152] The yields of alkyl naphthalene base oil and liquid wax obtained in all the examples and comparative examples of the present application are shown in Table 3.

[0153] Table 3

[0154]

[0155]

[0156] From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:

[0157] By comparing Example 1 and Comparative Example 1, it can be seen that compared with the traditional kettle reactor, the present application adopts a microreactor for continuous alkylation reaction. Due to its smaller channel size, shorter mass transfer distance and larger specific surface area, the microreactor can achieve precise control of reaction temperature and reaction time, and can also timely export heat in a strong exothermic reaction to maintain the stability of the reaction, thereby improving the reaction efficiency of the continuous alkylation reaction and inhibiting the occurrence of side reactions caused by local overheating or excessive reaction time, thereby improving the yield of alkyl naphthalene base oil and liquid wax and the production efficiency of continuous production.

[0158] By comparing Example 1 and Comparative Example 2, it can be seen that compared with traditional intermittent production, the continuous production system of the present application can be used for continuous production, which can more accurately control the reaction conditions, thereby reducing the occurrence of side reactions and improving the reaction efficiency of the continuous alkylation reaction, thereby increasing the yield of alkyl naphthalene base oil and liquid wax, and at the same time reducing material losses in the production process, thereby reducing energy consumption, reducing production costs, and improving production efficiency.

[0159] By comparing Example 1 and Comparative Example 3, it can be seen that compared with the single carbon number olefins used in the traditional alkyl naphthalene production process, the present application uses Fischer-Tropsch synthetic oil as the starting raw material, which can reduce costs and achieve efficient utilization of Fischer-Tropsch synthetic oil.

[0160] By comparing Example 1 with Comparative Examples 4 and 5, it can be seen that the continuous production system of the present application can be used for continuous production, and the raw material naphthalene and the solvent can be separated and recovered, thereby realizing the recycling of the raw materials and the solvent, thereby improving the utilization rate of the raw materials and reducing the production cost.

[0161] Comparing Examples 1 to 4, it can be seen that, compared with other ranges, limiting the feed rate and material residence time of each material in the first continuous mixing, the second continuous mixing and the third continuous mixing processes within the above-mentioned range of the present application is beneficial to improving the utilization rate of the above-mentioned materials, improving the reaction efficiency of the continuous alkylation reaction, inhibiting side reactions, and thus helping to increase the yield of alkyl naphthalene base oil and liquid wax.

[0162] By comparing Examples 1 and 5 to 7, it can be seen that, compared with other ranges, limiting the reaction temperature, reaction pressure and material residence time of the continuous alkylation reaction within the above ranges is beneficial to increasing the reaction rate of the continuous alkylation reaction and inhibiting side reactions, thereby facilitating an increase in the yield of alkyl naphthalene base oil and liquid wax, and also beneficial to improving the efficiency of continuous production.

[0163] By comparing Examples 1 and 8 to 11, it can be seen that the theoretical number of plates, the top temperature, the top pressure, the bottom temperature, the reflux ratio and the feed position of the separated product of the atmospheric distillation tower, the first vacuum distillation tower and the second vacuum distillation tower include but are not limited to the above-mentioned ranges of the present application. Limiting them within the above-mentioned ranges is beneficial to improving the separation efficiency of the first continuous distillation, the second continuous distillation and the third continuous distillation, to improving the recovery rate of the solvent and the raw material naphthalene, to improving the yield of alkyl naphthalene base oil and liquid wax, and further to achieving the co-production of alkyl naphthalene base oil and liquid wax, to increasing the added value of production, and thus to reducing production costs.

[0164] Comparing Examples 1 and 12 to 14, it can be seen that, compared with other ranges, limiting the temperature and space velocity of adsorption refining within the above ranges of the present application is beneficial to improving the adsorption efficiency of continuous adsorption, thereby further improving the purity and product quality of alkyl naphthalene base oil.

[0165] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the terms used in this way can be interchangeable where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than those described herein, for example.

[0166] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A continuous production system for co-producing alkyl naphthalene base oil and liquid wax, characterized in that: The continuous production system comprises: A continuous alkylation reaction device (100) is used for causing a continuous alkylation reaction between Fischer-Tropsch synthesis oil and naphthalene in a solvent under the catalysis of a catalyst to obtain a product system; the continuous alkylation reaction device (100) is provided with a first Fischer-Tropsch synthesis oil inlet (101), a first naphthalene inlet (102), a first catalyst inlet (103), a first solvent inlet (104) and a product system outlet (105); the continuous alkylation reaction device (100) is a microreactor; the Fischer-Tropsch synthesis oil comprises a mixture of alkanes and olefins having a carbon number of 9 to 24; the catalyst is an ionic liquid catalyst; A first continuous separation device (200), wherein the first continuous separation device (200) is provided with a product system inlet (201), a catalyst recovery outlet (202) and an oil phase outlet (203); the product system inlet (201) is connected to the product system outlet (105); the catalyst recovery outlet (202) is connected to the first catalyst inlet (103); A first continuous distillation device (300), wherein the first continuous distillation device (300) is provided with a first oil phase inlet (301), a first distillation product outlet (302) and a recovery solvent outlet (303); the first oil phase inlet (301) is connected to the oil phase outlet (203); the recovery solvent outlet (303) is connected to the first solvent inlet (104); A second continuous distillation device (400), wherein the second continuous distillation device (400) is provided with a first distillation product inlet (401), a second distillation product outlet (402) and a recovered naphthalene outlet (403); the first distillation product inlet (401) is connected to the first distillation product outlet (302); the recovered naphthalene outlet (403) is connected to the first naphthalene inlet (102); A third continuous distillation device (500), wherein the third continuous distillation device (500) is provided with a second distillation product inlet (501), a liquid wax outlet (502) and a first alkyl naphthalene base oil outlet (503); the second distillation product inlet (501) is connected to the second distillation product outlet (402).

2. The continuous production system for co-producing alkyl naphthalene base oil and liquid wax according to claim 1, characterized in that: The first continuous distillation device (300) is an atmospheric distillation tower; and / or, The second continuous distillation device (400) is a first vacuum distillation tower; and / or, The third continuous distillation device (500) is a second vacuum distillation tower; and / or, The continuous alkylation reaction device (100) is a tubular reactor, and preferably the diameter of the tubular reactor is 0.2 to 0.7 mm; and / or, The material of the first continuous separation device (200) is enamel.

3. The continuous production system for co-producing alkyl naphthalene base oil and liquid wax according to claim 1, characterized in that: The continuous production system further comprises a continuous washing device (600), wherein the continuous washing device (600) is provided with a second oil phase inlet (601), a detergent inlet (602) and a washing product outlet (603), wherein the second oil phase inlet (601) is connected to the oil phase outlet (203); Preferably, the continuous production system further comprises a second continuous separation device (700), wherein the second continuous separation device (700) is provided with a washing product inlet (701), a waste washing agent outlet (702) and a separation product outlet (703); The separated product outlet (703) is connected to the first oil phase inlet (301).

4. The continuous production system for co-producing alkyl naphthalene base oil and liquid wax according to any one of claims 1 to 3, characterized in that: The continuous production system further comprises a continuous adsorption device (800), wherein the continuous adsorption device (800) is provided with an alkyl naphthalene base oil inlet (801) and a second alkyl naphthalene base oil outlet (802); the alkyl naphthalene base oil inlet (801) is in communication with the first alkyl naphthalene base oil outlet (503); Preferably, a distributor is provided at the top of the inner cavity of the continuous adsorption device (800), and the distributor is preferably selected from a trough-type liquid distributor and / or a disc-type hole-flow type liquid distributor; Preferably, a demister is provided at the bottom of the inner cavity of the continuous adsorption device (800), and the demister is preferably selected from a baffle demister and / or a swirl plate demister; More preferably, the inner cavity of the continuous adsorption device (800) is provided with a grid layer, a wire mesh layer, a porcelain ball layer, an adsorption layer and a magnetic ball layer in order from bottom to top, and the grid layer is located above the demister, and the magnetic ball layer is located below the distributor; More preferably, the material of the adsorption layer is selected from activated carbon and / or clay, and further preferably, the activated carbon has a porosity of 40-50% and a specific surface area of ​​800-1000m 2 / g, the specific surface area of ​​the clay is 180-200m 2 / g.

5. The continuous production system for co-producing alkyl naphthalene base oil and liquid wax according to any one of claims 1 to 3, characterized in that: The continuous production system further comprises a first continuous mixing device (900) for mixing the naphthalene with the solvent to obtain a first mixture; the first continuous mixing device (900) is provided with a second naphthalene inlet (901), a second solvent inlet (902) and a first mixture outlet (903); the first mixture outlet (903) is communicated with the first Fischer-Tropsch synthetic oil inlet (101), or the first naphthalene inlet (102), or the first catalyst inlet (103), or the first solvent inlet (104); preferably, the second solvent inlet (902) is communicated with the recovered solvent outlet (303); preferably, the second naphthalene inlet (901) is communicated with the recovered naphthalene outlet (403); Preferably, the first continuous mixing device (900) is equipped with a stirring component and a heating component, and the heating component is arranged on the periphery of the first continuous mixing device (900); Preferably, the continuous production system further comprises a Fischer-Tropsch synthetic oil storage device (1000) for storing and supplying the Fischer-Tropsch synthetic oil, and the Fischer-Tropsch synthetic oil storage device (1000) is connected to the continuous alkylation reaction device (100); Preferably, the continuous production system further comprises a catalyst storage device (1100) for storing and supplying the catalyst, wherein the catalyst storage device (1100) is connected to the continuous alkylation reaction device (100) and / or the first continuous separation device (200); preferably, the catalyst storage device (1100) is connected to the first continuous separation device (200) via a recovered catalyst delivery pipeline, and a first continuous feed pump (1200) is provided on the recovered catalyst delivery pipeline; More preferably, the continuous production system further comprises a second continuous mixing device (1300) for mixing the first mixture with the Fischer-Tropsch synthetic oil to obtain a second mixture; the second continuous mixing device (1300) is connected to the first continuous mixing device (900), the Fischer-Tropsch synthetic oil storage device (1000) and the continuous alkylation reaction device (100); preferably, the second continuous mixing device (1300) is connected to the first continuous mixing device (900) via a first mixture delivery pipeline, and a second continuous feed pump (1400) is provided on the first mixture delivery pipeline; preferably, the second continuous mixing device (1300) is connected to the Fischer-Tropsch synthetic oil storage device (1000) via a Fischer-Tropsch synthetic oil delivery pipeline, and a third continuous feed pump (1500) is provided on the Fischer-Tropsch synthetic oil delivery pipeline; More preferably, the continuous production system further comprises a third continuous mixing device (1600) for mixing the second mixture with the catalyst and / or the recovered catalyst to obtain a third mixture; the third continuous mixing device (1600) is connected to the second continuous mixing device (1300), the catalyst storage device (1100) and the continuous alkylation reaction device (100); preferably, the third continuous mixing device (1600) is connected to the catalyst storage device (1100) via a catalyst delivery pipeline, and a fourth continuous feed pump (1700) is provided on the catalyst delivery pipeline; preferably, the third continuous mixing device (1600) is connected to the continuous alkylation reaction device (100) via a third mixture delivery pipeline, and a preheating device (1800) is provided on the third mixture delivery pipeline, and more preferably, the preheating device (1800) is a tubular heat exchanger; Preferably, the second continuous mixing device (1300) and the third continuous mixing device (1600) are each independently a microchannel reactor, or a membrane dispersion microreactor, or a microsieve reactor.

6. A continuous production method for co-producing alkyl naphthalene base oil and liquid wax, characterized in that: The continuous production method is carried out using the continuous production system according to any one of claims 1 to 5, and the continuous production method comprises: Step S1, introducing Fischer-Tropsch synthesis oil, naphthalene, a catalyst and a solvent into a continuous alkylation reaction device (100) for continuous alkylation reaction to obtain a product system; Step S2, passing the product system into a first continuous separation device (200) for separation to obtain a recovered catalyst and an oil phase; returning at least a portion of the recovered catalyst to the step S1; Step S3, passing the oil phase into a first continuous distillation device (300) for a first continuous distillation to obtain a first distillation product and a recovered solvent; returning at least a portion of the recovered solvent to the step S1; Step S4, passing the first distillation product into a second continuous distillation device (400) for second continuous distillation to obtain a second distillation product and recovered naphthalene; returning at least part of the recovered naphthalene to the step S1; Step S5, passing the second distillation product into a third continuous distillation apparatus (500) for a third continuous distillation to obtain the alkyl naphthalene base oil and the liquid wax.

7. The continuous production method for co-producing alkyl naphthalene base oil and liquid wax according to claim 6, characterized in that: The first continuous distillation is a continuous atmospheric distillation; preferably, an atmospheric distillation tower is used to perform the first continuous distillation on the oil phase in step S2 to obtain the first distillation product and the recovered solvent; preferably, the atmospheric distillation tower has 30 to 60 theoretical plates, a tower top temperature of 78 to 82°C, a tower top pressure of 10 to 50 kPa, a tower bottom temperature of 220 to 240°C, and a reflux ratio of 1 to 5; the feed position of the oil phase is the 15th to 30th plate; preferably, the content of the solvent in the bottom of the atmospheric distillation tower is ≤0.05% in terms of weight percentage of the material in the bottom of the atmospheric distillation tower; and / or, The second continuous distillation is a continuous vacuum distillation; preferably, the first vacuum distillation tower is used to perform the second continuous distillation on the first distillation product in the step S3 to obtain the second distillation product and the recovered naphthalene; preferably, the first vacuum distillation tower has a theoretical plate number of 40 to 80, a tower top temperature of 215 to 220° C., a tower top pressure of 10 to 20 kPa, a tower bottom temperature of 305 to 315° C., a reflux ratio of 2 to 10, and the feeding position of the first distillation product is the 20th to 40th plate; preferably, the content of the naphthalene in the bottom of the first vacuum distillation tower is ≤0.05% in terms of the weight percentage of the bottom material of the first vacuum distillation tower; and / or, The third continuous distillation is a continuous vacuum distillation; preferably, a second vacuum distillation tower is used to perform a third continuous distillation on the second distillation product in the step S4 to obtain the alkyl naphthalene base oil and the liquid wax; preferably, the second vacuum distillation tower has a theoretical plate number of 40 to 80, a tower top temperature of 140 to 145°C, a tower top pressure of 1 to 10 kPa, a tower bottom temperature of 170 to 180°C, a reflux ratio of 2 to 8, and the feeding position of the second distillation product is the 20th to 40th plate; preferably, the content of the liquid wax in the bottom of the second vacuum distillation tower is ≤25ppm, based on the weight percentage of the bottom material of the second vacuum distillation tower.

8. The continuous production method for co-producing alkyl naphthalene base oil and liquid wax according to claim 6, characterized in that: The reaction temperature of the continuous alkylation reaction is 30-90°C, the reaction pressure is 0.5-1.5MPa, and the material residence time is 0.1-10min; Preferably, in step S1, the feed rate of the Fischer-Tropsch synthetic oil is 1.1-2.3 kg / h, the feed rate of the naphthalene is 7.0-14.2 kg / h, the feed rate of the solvent is 28.2-56.5 kg / h, and the feed rate of the catalyst is 0.50-0.92 kg / h; Preferably, the Fischer-Tropsch synthetic oil comprises a mixture of alkanes and olefins having a carbon number of 14 to 16; Preferably, the solvent is selected from one or more of the group consisting of cyclohexane, cycloheptane and cyclooctane; Preferably, the ionic liquid catalyst is selected from 1-alkyl-3-methylimidazolium naphthylacetate ionic liquid catalyst and / or chloroaluminate ionic liquid catalyst; preferably, the 1-alkyl-3-methylimidazolium naphthylacetate ionic liquid catalyst is selected from one or more of the group consisting of 1-butyl-3-methylimidazolium naphthylacetate ionic liquid catalyst, 1-hexyl-3-methylimidazolium naphthylacetate ionic liquid catalyst and 1-octyl-3-methylimidazolium naphthylacetate ionic liquid catalyst; preferably, the chloroaluminate ionic liquid catalyst is selected from Me3HNCl-xAlCl3 and / or Et3HNCl-xAlCl3; More preferably, the ionic liquid catalyst is Me3HNCl-xAlCl3.

9. The continuous production method for co-producing alkyl naphthalene base oil and liquid wax according to any one of claims 6 to 8, characterized in that: The step S2 and the step S3 also include: Step S2-A: passing the oil phase and detergent into a continuous washing device (600) for continuous washing to obtain a washed product; preferably, the detergent is water; Step S2-B: passing the washed product into a second continuous separation device (700) for separation to obtain a separated product; Preferably, the step S5 comprises: passing the second distillation product into a third continuous distillation device (500) for third continuous distillation to obtain a crude alkylnaphthalene base oil product, and continuously adsorbing the crude alkylnaphthalene base oil product using a continuous adsorption device (800) to obtain the alkylnaphthalene base oil; Preferably, the temperature of the continuous adsorption is 30-60°C, and the adsorption space velocity is 1-5h -1 .

10. The continuous production method for co-producing alkyl naphthalene base oil and liquid wax according to any one of claims 6 to 8, characterized in that: Prior to step S1, the method further comprises: performing a first continuous mixing process on the naphthalene and the solvent by using a first continuous mixing device (900) to obtain a first mixture; preferably, stirring is performed during the first continuous mixing process, and more preferably, the stirring rate is 100 to 500 rpm; preferably, heating is performed during the first continuous mixing process, and more preferably, the temperature of the first continuous mixing process is 30 to 70° C., and the material residence time is 30 to 50 min; preferably, the content of the naphthalene is 10 to 30 wt % in terms of weight percentage of the first mixture; Preferably, the step S1 and the first continuous mixing further include: using a second continuous mixing device (1300) to perform a second continuous mixing on the first mixture and the Fischer-Tropsch synthetic oil to obtain a second mixture; preferably, heating is performed during the second continuous mixing; more preferably, the temperature of the second continuous mixing is 30-70° C., and the material residence time is 0.1-1 s; preferably, during the second continuous mixing, the feed rate of the first mixture is 7.0-14.2 kg / h, and the feed rate of the Fischer-Tropsch synthetic oil is 1.1-2.3 kg / h; Preferably, the continuous production method further comprises: using a Fischer-Tropsch synthetic oil storage device (1000) to store the Fischer-Tropsch synthetic oil, and passing the Fischer-Tropsch synthetic oil into the continuous alkylation reaction device (100) to carry out the continuous alkylation reaction, more preferably using an inert gas to seal the Fischer-Tropsch synthetic oil storage device (1000), and further preferably the inert gas is nitrogen; Preferably, between step S1 and the second continuous mixing, the method further comprises: using a third continuous mixing device (1600) to perform a third continuous mixing of the second mixture and the catalyst to obtain a third mixture; preferably, heating is performed during the third continuous mixing; more preferably, the temperature of the third continuous mixing is 30 to 70° C., and the material residence time is 0.1 to 1 s; preferably, during the third continuous mixing, the feed rate of the second mixture is 8.1 to 16.4 kg / h, and the feed rate of the catalyst is 0.50 to 0.92 kg / h; Preferably, the continuous production method further comprises: using a catalyst storage device (1100) to store the catalyst, and introducing the catalyst into the continuous alkylation reaction device (100) to carry out the continuous alkylation reaction, more preferably using an inert gas to seal the catalyst storage device (1100), and further preferably the inert gas is nitrogen.

Citation Information

Patent Citations

  • Method for preparing alkyl naphthalene lubricant base oil from coal alpha-olefin

    CN114790407A

  • Continuous reactor suitable for ion liquid catalyst and its use

    CN1676207A