Continuous production system and continuous production method of artificial beeswax
Through continuous Fischer-Tropsch wax melting and oxidation reaction technology, combined with catalyst and microchannel reactor, the problem of low ester acid ratio and high impurities of artificial beeswax oxidation is solved, achieving efficient and low-cost beeswax production and improving product purity and yield.
Patent Information
- Application Number
- CN202411327577.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-23
- Publication Date
- 2024-12-20
AI Technical Summary
In the existing artificial beeswax production technology, the oxidized wax ester acid ratio is low, the yield is low and the impurity content is high. Especially when paraffin is used as raw material, impurities such as sulfur, nitrogen, aromatic hydrocarbons, etc. are present, which affects the use range of products and environmental protection.
The continuous Fischer-Tropsch wax melting device and continuous oxidation reaction device are used to carry out the heating and melting and oxidation reaction of Fischer-Tropsch wax, and the esterification reaction is carried out in combination with the catalyst to improve the ester-acid ratio of oxidized wax, and the reaction conditions are optimized through the microchannel reactor and the gas distributor. , improve reaction efficiency and product purity.
It improves the ester acid ratio and product yield of artificial beeswax, reduces impurity content, meets the requirements of acid value and saponification value, reduces production costs and waste emissions, and improves production efficiency and raw material utilization.
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Figure CN119161905A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of coal chemical and fine chemical industry, and in particular to a continuous production system and a continuous production method of artificial beeswax. Background Art
[0002] At present, natural beeswax is mainly used in cosmetics, leather polish, food packaging, ink, printing and dyeing, etc., but natural beeswax is scarce and expensive. Although a large amount of beeswax is imported every year, it still cannot meet the market demand. At present, most of my country's artificial beeswax is made of paraffin as the main raw material, but paraffin usually contains impurities such as sulfur, nitrogen, and aromatics, which seriously affects the scope of use of its products. In addition, the paraffin production process is usually accompanied by high energy consumption and high pollution, which is not conducive to environmental protection.
[0003] Fischer-Tropsch wax uses CO and H2 as raw materials. Compared with natural beeswax and paraffin-based beeswax, it has the advantages of wide sources and stable prices, which is in line with the sustainable development strategy. With the construction of Fischer-Tropsch synthesis industrial plants of Ningmei, Yitai, Lu'an, Future Energy and other companies, and the realization of long-term and full-load operation, the production capacity has been continuously expanded. Fischer-Tropsch wax has changed from a scarce resource to a mass product, and has become an important part of the domestic and foreign wax market. Compared with paraffin, Fischer-Tropsch wax contains almost no impurities such as sulfur, nitrogen, and aromatics. It is more advantageous to use it as a raw material for the preparation of oxidized wax and artificial beeswax, and has broad development prospects.
[0004] The existing document (publication number CN1613841A) discloses a method for preparing artificial beeswax, which uses mineral paraffin and other substances through a catalytic oxidation method to synthesize an artificial beeswax whose various indicators meet the requirements of natural beeswax, wherein the white powder of cobalt carbonate obtained by the reaction of cobalt salt and carbonate is used as a catalyst for synthesizing artificial beeswax; the catalyst is then melted with solid paraffin, alum, and white carbon black, and then air or oxygen is introduced for heating to perform a catalytic oxidation reaction to obtain artificial beeswax. The ester acid of the oxidized wax prepared by the one-step oxidation method is relatively low, and it is difficult to obtain an artificial beeswax whose acid value and saponification value meet the requirements by direct oxidation in one step.
[0005] In summary, it is necessary to research and develop a continuous production system and method for artificial beeswax that can improve the oxidized wax ester acid ratio and product yield and reduce the impurity content of the product. Summary of the invention
[0006] The main purpose of the present invention is to provide a continuous production system and a continuous production method of artificial beeswax to solve the problems of low ester acid ratio of oxidized wax in the prior art, low yield and high impurity content of the oxidized wax obtained by the existing production system.
[0007] In order to achieve the above-mentioned object, the present invention provides a continuous production system of artificial beeswax on one hand, comprising at least one continuous Fischer-Tropsch wax melting device, a continuous oxidation reaction device and a continuous esterification reaction unit. Wherein, each continuous Fischer-Tropsch wax melting device is provided with a Fischer-Tropsch wax raw material inlet and a liquid wax outlet; the continuous Fischer-Tropsch wax melting device is also provided with a heating component; the continuous oxidation reaction device is provided with a liquid wax inlet, an oxidizing gas inlet and an oxidation reaction product outlet; the liquid wax inlet is connected to the liquid wax outlet; the continuous esterification reaction unit comprises a continuous esterification reaction device, and the continuous esterification reaction device is provided with a first oxidation reaction product inlet, a first catalyst inlet and an artificial beeswax outlet; the first oxidation reaction product inlet is connected to the oxidation reaction product outlet.
[0008] Furthermore, the continuous oxidation reaction device is selected from a microchannel reactor or a vertical tube reactor; preferably, the liquid wax inlet is arranged at the upper part of the continuous oxidation reaction device, and the oxidizing gas inlet is arranged at the lower part of the continuous oxidation reaction device, and the total height of the continuous oxidation reaction device is H1, and more preferably, the liquid wax inlet is arranged at the position of 0.9H1~H1, and the oxidizing gas inlet is arranged at the position of 0~0.05H1.
[0009] Furthermore, the continuous oxidation reaction device also includes a first gas distributor, which is arranged on the inner side of the continuous oxidation reaction device near the oxidation gas inlet; preferably, the first gas distributor is selected from a membrane gas distributor or a coil distributor; more preferably, the membrane gas distributor is selected from a metal membrane and / or a ceramic membrane; further preferably, the membrane gas distributor has a pore size of 5 to 50 μm, a porosity of 10 to 40%, and a thickness of 1 to 5 mm.
[0010] Further, the continuous esterification reaction device is also provided with an inert gas inlet for introducing inert gas to stir the oxidation reaction product and the catalyst; and / or, a first stirring component is provided in the continuous esterification reaction device; preferably, the first oxidation reaction product inlet is arranged at the upper part of the continuous esterification reaction device, and the inert gas inlet is arranged at the lower part of the continuous esterification reaction device, and the total height of the continuous esterification reaction device is H2, and more preferably, the first oxidation reaction product inlet is arranged at the position of 0.9H2~H2, and the inert gas inlet is arranged at the position of 0~0.05H2; preferably, when the continuous esterification reaction device includes an inert gas inlet, the continuous esterification reaction device also includes a second gas distributor, and the second gas distributor is arranged on the inner side of the continuous esterification reaction device near the inert gas inlet; more preferably, the second gas distributor is selected from a membrane gas distributor or a coil distributor; more preferably, the membrane gas distributor is selected from a metal membrane and / or a ceramic membrane; further preferably, the membrane gas distributor has a pore size of 5~50μm, a porosity of 10~40%, and a thickness of 1~5mm.
[0011] Furthermore, the continuous esterification reaction unit also includes a first continuous mixing device, a second continuous mixing device and a third continuous mixing device; the first continuous mixing device is used to mix the oxidation reaction product with the catalyst to obtain a first mixture; the first continuous mixing device is provided with a second oxidation reaction product inlet, a second catalyst inlet and a first mixture outlet; the second oxidation reaction product inlet is connected to the oxidation reaction product outlet; the continuous esterification reaction device also includes a first mixture inlet, and the first mixture outlet is connected to the first mixture inlet; preferably, the first mixture inlet is arranged at the upper part of the continuous esterification reaction device, and more preferably, the first mixture inlet is arranged at the position of 0.9H2~H2; preferably, the second continuous mixing device is used to mix the esterifying agent with the catalyst to obtain a second mixture; the second continuous mixing device is provided There are an esterification agent inlet, a third catalyst inlet and a second mixture outlet, the first continuous mixing device also includes a second mixture inlet, and the second mixture outlet is connected to the second mixture inlet; preferably, the continuous esterification reaction device is selected from a microchannel reactor or a vertical tube reactor; more preferably, the third continuous mixing device is used to mix the second mixture with the oxidation reaction product; the third continuous mixing device is provided with a first inlet, a second inlet and a third mixture outlet; the first inlet is connected to the second mixture outlet, and the second inlet is connected to the oxidation reaction product outlet; the continuous esterification reaction device also includes a third mixture inlet, and the third mixture outlet is connected to the third mixture inlet; preferably, the third mixture inlet is arranged at the upper part of the continuous esterification reaction device, and more preferably, the third mixture inlet is arranged at the position of 0.9H2~H2.
[0012] Furthermore, a second stirring component is provided in the continuous Fischer-Tropsch wax melting device; and / or, when the continuous production system comprises two continuous Fischer-Tropsch wax melting devices, one of them is in working state and the other is on standby.
[0013] Furthermore, the liquid wax inlet and the liquid wax outlet are connected through a liquid wax delivery pipeline, and a continuous feed pump is arranged on the liquid wax delivery pipeline.
[0014] In order to achieve the above-mentioned object, the second aspect of the present invention further provides a continuous production method of artificial beeswax, which is carried out using the above-mentioned continuous production system of artificial beeswax. The continuous production method comprises: step S1, using a continuous Fischer-Tropsch wax melting device to heat and melt the Fischer-Tropsch wax raw material to obtain liquid wax; step S2, allowing the liquid wax to undergo continuous oxidation reaction with oxidizing gas in a continuous oxidation reaction device to obtain an oxidation reaction product; step S3, under the catalysis of a catalyst, allowing the oxidation reaction product to undergo continuous esterification reaction in a continuous esterification reaction device to obtain artificial beeswax.
[0015] Furthermore, the oxidizing gas is selected from one or more of the group consisting of air, oxygen and a mixture of nitrogen and oxygen; preferably, when the oxidizing gas is a mixture of nitrogen and oxygen, the volume concentration of oxygen in the mixture is 15 to 30 vol%; preferably, the rate at which the oxidizing gas is introduced into the continuous oxidation reaction device is 0.3 to 0.8 standard cubic meters per hour; more preferably, when the oxidizing gas is air, the rate at which air is introduced into the continuous oxidation reaction device is 0.4 to 0.6 standard cubic meters per hour; more preferably, when the oxidizing gas is oxygen, the rate at which oxygen is introduced into the continuous oxidation reaction device is 0.3 to 0.4 standard cubic meters per hour; more preferably, when the oxidizing gas is a mixture of nitrogen and oxygen, the rate at which the mixture is introduced into the continuous oxidation reaction device is 0.4 to 0.6 standard cubic meters per hour.
[0016] Furthermore, the catalyst is fed into the continuous esterification reaction device at a rate of 10 to 100 g / h; preferably, the catalyst is selected from C8 to C 12 Alkylbenzene sulfonic acid and / or ester compound with 15 to 20 carbon atoms.
[0017] Furthermore, during the continuous esterification reaction, an inert gas is continuously introduced into the continuous esterification reaction device; and / or, stirring is performed during the continuous esterification reaction; preferably, the introduction rate of the inert gas is 0.2 to 0.5 standard cubic meters / h; preferably, the stirring rate is 100 to 500 rpm; more preferably, the inert gas is selected from nitrogen and / or argon.
[0018] Further, the rate at which the oxidation reaction product is continuously introduced into the continuous esterification reaction device is 1 to 10 kg / h; preferably, between step S2 and step S3, a process of mixing the oxidation reaction product with the catalyst by using a first continuous mixing device is included to obtain a first mixture; more preferably, the rate at which the oxidation reaction product is introduced into the first continuous mixing device is 1 to 10 kg / h, the rate at which the catalyst is introduced into the first continuous mixing device is 10 to 100 g / h, and the rate at which the first mixture is introduced into the continuous esterification reaction device is 1 to 10 kg / h; preferably, between step S2 and step S3, a process of mixing the esterifying agent with the catalyst by using a second continuous mixing device is included to obtain a second mixture; more preferably, the rate at which the esterifying agent is introduced into the second continuous mixing device is 100 to 100 g / h. 0g / h, the rate at which the catalyst is introduced into the second continuous mixing device is 10-100g / h, and the rate at which the second mixture is introduced into the continuous esterification reaction device is 100-1000g / h; more preferably, the continuous production method also includes passing the second mixture into a third continuous mixing device to mix the second mixture with the oxidation reaction product to obtain a third mixture; further preferably, the rate at which the second mixture is introduced into the third continuous mixing device is 100-1000g / h, the rate at which the oxidation reaction product is introduced into the third continuous mixing device is 1-10kg / h, and the rate at which the third mixture is introduced into the continuous esterification reaction device is 1-10kg / h; more preferably, the esterifying agent is selected from alcohols having a carbon number of 16 to 20; further preferably, the esterifying agent is selected from octadecyl alcohol and / or hexadecanol.
[0019] Furthermore, the reaction temperature of the continuous oxidation reaction is 150-180°C, and the material residence time is 1-4h; preferably, the reaction temperature of the continuous oxidation reaction is 160-175°C; and / or, the reaction temperature of the continuous esterification reaction is 140-170°C, and the material residence time is 1-3h; preferably, the reaction temperature of the continuous esterification reaction is 150-165°C.
[0020] Furthermore, the Fischer-Tropsch wax raw material is selected from one or more of the group consisting of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, 65# Fischer-Tropsch wax, 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, 90# Fischer-Tropsch wax, 100# Fischer-Tropsch wax, 105# Fischer-Tropsch wax and 110# Fischer-Tropsch wax; preferably, the heating and melting temperature is 80-120°C, and the material residence time is 1-10h; preferably, stirring is performed during the heating and melting process; more preferably, the stirring rate is 50-200rpm.
[0021] Furthermore, the rate at which the liquid wax is passed into the continuous oxidation reaction device is 1 to 12 kg / h; preferably, when the Fischer-Tropsch wax raw material is selected from one or more of 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, and 90# Fischer-Tropsch wax, the rate at which the liquid wax is passed into the continuous oxidation reaction device is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 165 to 175°C, and the material residence time is 2 to 3 hours; preferably, when the Fischer-Tropsch wax raw material is selected from one or more of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, and 65# Fischer-Tropsch wax, the rate at which the liquid wax is passed into the continuous oxidation reaction device is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 160 to 175°C, and the material residence time is 1 to 2 hours.
[0022] Applying the technical solution of the present invention, the present application provides a continuous production system of artificial beeswax, including a continuous Fischer-Tropsch wax melting device, a continuous oxidation reaction device and a continuous esterification reaction unit. The continuous Fischer-Tropsch wax melting device is used to heat and melt the Fischer-Tropsch wax raw material to obtain liquid wax, and the heating component is used to provide heat to heat and melt the Fischer-Tropsch wax raw material, so as to facilitate subsequent reactions; the continuous oxidation reaction device is provided with a liquid wax inlet, an oxidizing gas inlet and an oxidation reaction product outlet, and the continuous oxidation reaction device can make the liquid wax contact with the oxidizing gas and undergo an oxidation reaction to obtain an oxidation reaction product containing carboxylic acid and alcohol compounds; the setting of the continuous esterification reaction unit can make the oxidation reaction product undergo an esterification reaction under the action of a catalyst, thereby increasing the ester-acid ratio of the artificial beeswax, and then obtaining an artificial beeswax with an acid value and a saponification value that meet the requirements; and the setting of the first catalyst inlet is convenient for adding a catalyst, which can catalyze the esterification reaction of the byproduct carboxylic acid produced in the continuous oxidation reaction with the alcohol, can reduce the reaction activation energy of the continuous esterification reaction, and can increase its reaction rate.
[0023] Compared with the prior art using paraffin as the main raw material, the present application uses Fischer-Tropsch wax as the starting raw material, which is beneficial to reduce the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby improving the yield and purity of the product. At the same time, using Fischer-Tropsch wax as a raw material can reduce costs and reduce waste emissions. Compared with the prior art using a one-step oxidation method to prepare oxidized wax, the artificial beeswax produced by the continuous production system of artificial beeswax mentioned above in the present application has a high ester-acid ratio, and the obtained artificial beeswax can meet the requirements of acid value and saponification value at the same time. Compared with an intermittent reaction device, the continuous production system provided by the present application can realize continuous production, thereby improving production efficiency and reducing production costs, while also being able to improve the utilization rate of raw materials and the purity and yield of products. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] 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:
[0025] Figure 1 A schematic structural diagram of a continuous production system of artificial beeswax in one embodiment of the present application is shown;
[0026] Figure 2 A schematic structural diagram of a continuous production system of artificial beeswax in another embodiment of the present application is shown.
[0027] The above drawings include the following reference numerals:
[0028] 100. Continuous Fischer-Tropsch wax melting device; 101. Fischer-Tropsch wax raw material inlet;
[0029] 200. Continuous oxidation reaction device; 201. Oxidation gas inlet;
[0030] 300, continuous esterification reaction unit; 301, continuous esterification reaction device; 302, artificial beeswax outlet; 303, inert gas inlet; 304, first continuous mixing device; 305, second catalyst inlet; 306, second continuous mixing device; 307, esterification agent inlet; 308, third catalyst inlet; 309, third continuous mixing device;
[0031] 400. Continuous feed pump. DETAILED DESCRIPTION
[0032] 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.
[0033] As described in the background technology, the existing artificial beeswax has the problems of low oxidized wax ester acid ratio, low product yield and high content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons. In order to solve the above technical problems, the first aspect of the present application provides a continuous production system for artificial beeswax, such as Figure 1 or Figure 2 As shown, the device includes at least one continuous Fischer-Tropsch wax melting device 100, a continuous oxidation reaction device 200 and a continuous esterification reaction unit 300. Each continuous Fischer-Tropsch wax melting device 100 is provided with a Fischer-Tropsch wax raw material inlet 101 and a liquid wax outlet; the continuous Fischer-Tropsch wax melting device 100 is also equipped with a heating component; the continuous oxidation reaction device 200 is provided with a liquid wax inlet, an oxidation gas inlet 201 and an oxidation reaction product outlet; the liquid wax inlet is connected to the liquid wax outlet; the continuous esterification reaction unit 300 includes a continuous esterification reaction device 301, and the continuous esterification reaction device 301 is provided with a first oxidation reaction product inlet, a first catalyst inlet and an artificial beeswax outlet 302; the first oxidation reaction product inlet is connected to the oxidation reaction product outlet.
[0034] The continuous production system of artificial beeswax provided in the present application includes a continuous Fischer-Tropsch wax melting device 100, a continuous oxidation reaction device 200 and a continuous esterification reaction unit 300. The continuous Fischer-Tropsch wax melting device 100 is used to heat and melt the Fischer-Tropsch wax raw material to obtain liquid wax, and the heating component is used to provide heat to heat and melt the Fischer-Tropsch wax raw material, so as to facilitate subsequent reactions; the continuous oxidation reaction device 200 is provided with a liquid wax inlet, an oxidation gas inlet 201 and an oxidation reaction product outlet, and the continuous oxidation reaction device 200 can make the liquid wax and the oxidation gas contact and undergo an oxidation reaction to obtain an oxidation reaction product containing carboxylic acid and alcohol compounds; the setting of the continuous esterification reaction unit 300 can make the oxidation reaction product undergo an esterification reaction under the action of a catalyst, thereby increasing the ester-acid ratio of artificial beeswax, and then obtaining an artificial beeswax with an acid value and a saponification value that meet the requirements. Moreover, the setting of the catalyst inlet is convenient for adding a catalyst, which can catalyze the esterification reaction of the byproduct carboxylic acid produced in the continuous oxidation reaction with the alcohols, can reduce the reaction activation energy of the continuous esterification reaction, and can increase its reaction rate.
[0035] Compared with the prior art using paraffin as the main raw material, the present application uses Fischer-Tropsch wax as the starting raw material, which is beneficial to reduce the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby improving the yield and purity of the product. At the same time, using Fischer-Tropsch wax as a raw material can reduce costs and reduce waste emissions. Compared with the prior art using a one-step oxidation method to prepare oxidized wax, the artificial beeswax produced by the continuous production system of artificial beeswax mentioned above in the present application has a high ester-acid ratio, and the obtained artificial beeswax can meet the requirements of acid value and saponification value at the same time. Compared with an intermittent reaction device, the continuous production system provided by the present application can realize continuous production, thereby improving production efficiency and reducing production costs, while also being able to improve the utilization rate of raw materials and the purity and yield of products.
[0036] The microchannel reactor can mix the reactants quickly, thereby increasing the reaction rate. The vertical tube reactor has the characteristics of fast, high efficiency and low energy consumption. In a preferred embodiment, the continuous oxidation reaction device 200 includes but is not limited to a microchannel reactor or a vertical tube reactor. The use of the above-mentioned type of reactor is conducive to increasing the reaction rate of the continuous oxidation reaction, is conducive to increasing the production efficiency of the continuous reaction, and is conducive to improving the utilization rate of the raw materials and the purity and yield of the artificial beeswax.
[0037] In a preferred embodiment, the liquid wax inlet is arranged at the upper part of the continuous oxidation reaction device 200, and the oxidizing gas inlet 201 is arranged at the lower part of the continuous oxidation reaction device 200. The liquid wax inlet and the oxidizing gas inlet 201 are arranged at the above positions respectively, which is conducive to the countercurrent contact between the liquid wax flowing from top to bottom and the oxidizing gas introduced from bottom to top, and is conducive to making the two contact more fully, thereby facilitating the reaction efficiency of the continuous oxidation reaction, and further improving the yield of artificial beeswax.
[0038] In order to make the liquid wax react with the oxidizing gas more fully, thereby further improving the reaction efficiency of the continuous oxidation reaction, preferably, the total height of the continuous oxidation reaction device 200 is H1, the liquid wax inlet is set at the position of 0.9H1~H1, and the oxidizing gas inlet 201 is set at the position of 0~0.05H1.
[0039] In a preferred embodiment, the continuous oxidation reaction device 200 further includes a first gas distributor, which is disposed on the inner side of the continuous oxidation reaction device 200 near the oxidation gas inlet 201. The provision of the first gas distributor is conducive to making the oxidation gas more evenly distributed in the inner cavity of the continuous oxidation reaction device 200, thereby facilitating the improvement of the reaction efficiency of the continuous oxidation reaction, and further facilitating the improvement of the yield of artificial beeswax.
[0040] In a preferred embodiment, the first gas distributor includes but is not limited to a membrane gas distributor or a coil-type distributor. The use of the above-mentioned type of gas distributor is conducive to more uniform distribution of the oxidizing gas in the inner cavity of the continuous oxidation reaction device 200.
[0041] In order to further distribute the oxidizing gas more evenly in the inner cavity of the continuous oxidation reaction device 200, preferably, the membrane gas distributor includes but is not limited to a metal membrane and / or a ceramic membrane.
[0042] In order to improve the distribution uniformity of the oxidizing gas in the inner cavity of the continuous oxidation reaction device 200, improve the raw material utilization rate of the oxidizing gas, and thus improve the reaction efficiency of the continuous oxidation reaction, preferably, the pore size of the membrane gas distributor is 5 to 50 μm, the porosity is 10 to 40%, and the thickness is 1 to 5 mm.
[0043] In a preferred embodiment, the continuous esterification reaction device 301 is further provided with an inert gas inlet 303 for introducing inert gas to stir the oxidation reaction product and the catalyst. The inert gas is introduced into the continuous esterification reaction device 301, and the fluidity of the inert gas is utilized to disperse the reaction heat generated in the continuous esterification reaction, and to provide a dynamic equilibrium environment for the reaction, thereby facilitating the reaction rate of the continuous esterification reaction, and further facilitating the improvement of the ester-acid ratio of the oxidized wax, and facilitating the acquisition of artificial beeswax having an acid value and a saponification value that meet the requirements.
[0044] In a preferred embodiment, the first oxidation reaction product inlet is arranged at the upper part of the continuous esterification reaction device 301, and the inert gas inlet 303 is arranged at the lower part of the continuous esterification reaction device 301. The first oxidation reaction product inlet and the inert gas inlet 303 are arranged at the above positions respectively, which is conducive to the countercurrent contact between the first oxidation product flowing from top to bottom and the inert gas introduced from bottom to top, and is conducive to the reaction heat generated in the inert gas dispersion reaction, thereby facilitating the dynamic balance of the reaction, facilitating the reaction rate of the continuous esterification reaction, and further facilitating the improvement of the ester-acid ratio of the artificial beeswax, and facilitating the acquisition of the artificial beeswax with the acid value and saponification value meeting the requirements.
[0045] In order to make the first oxidation product contact with the inert gas more fully, further improve the efficiency of the inert gas in dispersing the reaction heat, and thus further improve the reaction rate of the continuous esterification reaction, preferably, the total height of the continuous esterification reaction device 301 is H2, the first oxidation reaction product inlet is set at the position of 0.9H2~H2, and the inert gas inlet 303 is set at the position of 0~0.05H2.
[0046] In a preferred embodiment, a first stirring member is provided in the continuous esterification reaction device 301. The first stirring member is used to stir the oxidation reaction product and the catalyst, which is beneficial to disperse the reaction heat generated in the continuous esterification reaction, and to provide a dynamic equilibrium environment for the reaction, thereby facilitating the reaction rate of the continuous esterification reaction, and further facilitating the improvement of the ester-acid ratio of the artificial beeswax, and facilitating the acquisition of an artificial beeswax having an acid value and a saponification value that meet the requirements.
[0047] In a preferred embodiment, when the continuous esterification reaction device 301 includes the inert gas inlet 303, the continuous esterification reaction device 301 also includes a second gas distributor, which is arranged on the inner side of the continuous esterification reaction device 301 near the inert gas inlet 303. The arrangement of the second gas distributor is conducive to uniformly distributing the inert gas in the inner cavity of the continuous esterification reaction device 301, and is conducive to fully contacting the inert gas with the reactants to disperse the reaction heat generated in the reaction, thereby facilitating the provision of a dynamic equilibrium environment for the continuous esterification reaction, thereby facilitating the improvement of the reaction rate of the continuous esterification reaction, and facilitating the acquisition of artificial beeswax having an acid value and a saponification value that meet the requirements.
[0048] In a preferred embodiment, the second gas distributor includes but is not limited to a membrane gas distributor or a coil distributor. The use of the above-mentioned type of gas distributor is conducive to more uniform distribution of the inert gas in the inner cavity of the continuous esterification reaction device 301.
[0049] In order to further distribute the inert gas more evenly in the inner cavity of the continuous esterification reaction device 301, preferably, the membrane gas distributor includes but is not limited to a membrane gas distributor and / or a coil distributor.
[0050] In order to further improve the distribution uniformity of the inert gas in the inner cavity of the continuous esterification reaction device 301, preferably, the membrane gas distributor has a pore size of 5 to 50 μm, a porosity of 10 to 40%, and a thickness of 1 to 5 mm.
[0051] In a preferred embodiment, Figure 2 As shown, the continuous esterification reaction unit 300 also includes a first continuous mixing device 304, which is used to mix the oxidation reaction product with the catalyst to obtain a first mixture; the first continuous mixing device 304 is provided with a second oxidation reaction product inlet, a second catalyst inlet 305 and a first mixture outlet; the second oxidation reaction product inlet is connected to the oxidation reaction product outlet, and the continuous esterification reaction device 301 also includes a first mixture inlet, and the first mixture outlet is connected to the first mixture inlet. The setting of the first continuous mixing device 304 is conducive to pre-mixing the oxidation reaction product with the catalyst before sending it into the continuous esterification reaction device 301 for continuous esterification reaction, which is conducive to saving the mixing time during the subsequent continuous esterification reaction, thereby helping to improve the continuous production efficiency.
[0052] In a preferred embodiment, the first mixture inlet is arranged at the upper part of the continuous esterification reaction device 301. The first mixture inlet is arranged at the above position, which is conducive to the countercurrent contact between the first mixture flowing from top to bottom and the inert gas introduced from bottom to top, so that the inert gas can take away the reaction heat generated in the continuous esterification reaction, provide a dynamic balance for the reaction, and improve the reaction rate of the continuous esterification, thereby facilitating the improvement of the ester-acid ratio of the artificial beeswax, and facilitating the acquisition of the artificial beeswax with the acid value and saponification value meeting the requirements.
[0053] In order to make the first mixture contact with the inert gas more fully, further improve the efficiency of the inert gas in taking away the reaction heat, and thus further improve the reaction efficiency of the continuous esterification reaction, preferably, the first mixture inlet is set at the position of 0.9H2~H2.
[0054] In a preferred embodiment, the continuous esterification reaction unit 300 further includes a second continuous mixing device 306 for mixing the esterifying agent with the catalyst to obtain a second mixture; the second continuous mixing device 306 is provided with an esterifying agent inlet 307, a third catalyst inlet 308 and a second mixture outlet, and the first continuous mixing device 304 further includes a second mixture inlet, and the second mixture outlet is connected to the second mixture inlet. The esterifying agent inlet 307 is used to add the esterifying agent, and the addition of the esterifying agent is conducive to the esterification reaction with the by-product carboxylic acid produced in the continuous oxidation reaction, thereby facilitating the improvement of the ester-acid ratio of the artificial beeswax, and further facilitating the acquisition of the artificial beeswax with the acid value and saponification value meeting the requirements. The third catalyst inlet 308 is used to add the catalyst, and pre-mixing the esterifying agent with the catalyst in the second continuous mixing device 306 is conducive to improving the dispersibility of the two, and at the same time, the second mixture obtained after mixing is passed into the third continuous mixing device 309, which is conducive to saving the subsequent mixing time, thereby facilitating the improvement of the continuous production efficiency.
[0055] In a preferred embodiment, Figure 1 As shown, the continuous esterification reaction unit 300 also includes a third continuous mixing device 309 for mixing the second mixture with the oxidation reaction product; the third continuous mixing device 309 is provided with a first inlet, a second inlet and a third mixture outlet; the first inlet is connected to the second mixture outlet, and is used to pass the mixture of the esterifying agent and the catalyst into the third continuous mixing device 309, and the second inlet is connected to the oxidation reaction product outlet, and is used to pass the oxidation reaction product into the third continuous mixing device 309; the continuous esterification reaction device 301 also includes a third mixture inlet, and the third mixture outlet is connected to the third mixture inlet. The setting of the third continuous mixing device 309 is conducive to pre-mixing the oxidation reaction product with the second mixture before the continuous esterification reaction occurs, which is conducive to improving the dispersibility of each material, and the third mixture obtained after mixing is sent to the continuous esterification reaction device 301 for continuous esterification reaction, which is conducive to saving the mixing time during the subsequent continuous esterification reaction, thereby facilitating the improvement of continuous production efficiency.
[0056] In a preferred embodiment, the third mixture inlet is arranged at the upper part of the continuous esterification reaction device 301. The third mixture inlet is arranged at the above position, which is conducive to the countercurrent contact between the third mixture flowing from top to bottom and the inert gas introduced from bottom to top, so that the inert gas can take away the reaction heat generated in the continuous esterification reaction, provide a dynamic balance for the reaction, and improve the reaction rate of the continuous esterification, thereby facilitating the improvement of the ester-acid ratio of the oxidized wax, and facilitating the acquisition of artificial beeswax with acid value and saponification value meeting the requirements.
[0057] In order to make the third mixture contact with the inert gas more fully, further improve the efficiency of the inert gas in taking away the reaction heat, and thus further improve the reaction efficiency of the continuous esterification reaction, preferably, the inlet of the third mixture is set at the position of 0.9H2~H2.
[0058] In a preferred embodiment, the continuous esterification reaction device 301 includes but is not limited to a microchannel reactor or a vertical tube reactor. The use of the above-mentioned type of reactor is conducive to improving the reaction rate of the continuous esterification reaction, thereby helping to improve the ester-acid ratio of the artificial beeswax, and further to obtain the artificial beeswax with acid value and saponification value that meet the requirements, in addition, it is also conducive to improving the production efficiency of the continuous reaction, and is conducive to improving the raw material utilization rate and the purity and yield of the artificial beeswax.
[0059] In a preferred embodiment, a second stirring member is provided in the continuous Fischer-Tropsch wax melting device 100. The second stirring member is used to stir the Fischer-Tropsch wax raw material when it is heated and melted, which is beneficial to make the Fischer-Tropsch wax raw material heated more evenly, thereby improving the heating and melting efficiency.
[0060] In a preferred embodiment, when the continuous production system includes two continuous Fischer-Tropsch wax melting devices 100, one of them is in working state and the other is in standby state. When one of the continuous Fischer-Tropsch wax melting devices 100 is in working state, the other continuous Fischer-Tropsch wax melting device 100 can store raw materials, which is convenient for timely allocation of raw materials, thereby facilitating the improvement of the production efficiency of continuous production.
[0061] The feed pump can provide pressure and flow, and can lift the material from a low place to a high place. In a preferred embodiment, the liquid wax inlet and the liquid wax outlet are connected through a liquid wax delivery pipeline, and a continuous feed pump 400 is provided on the liquid wax delivery pipeline. When the liquid wax inlet is arranged at the upper part of the continuous oxidation reaction device 200, it is convenient for the continuous feed pump 400 to continuously lift the liquid wax from a low place to a high place, thereby facilitating the continuous oxidation reaction.
[0062] The second aspect of the present application also provides a method for continuously producing artificial beeswax using the above-mentioned continuous production system provided by the present application, the method comprising: step S1, using a continuous Fischer-Tropsch wax melting device 100 to heat and melt the Fischer-Tropsch wax raw material to obtain liquid wax; step S2, allowing the liquid wax to undergo a continuous oxidation reaction with an oxidizing gas in a continuous oxidation reaction device 200 to obtain an oxidation reaction product; step S3, under the catalysis of a catalyst, allowing the oxidation reaction product to undergo a continuous esterification reaction in a continuous esterification reaction device 301 to obtain artificial beeswax.
[0063] Heating and melting the Fischer-Tropsch wax raw material can obtain liquid wax, which is convenient for subsequent reactions; the liquid wax is subjected to continuous oxidation reaction with oxidizing gas to obtain an oxidation reaction product containing carboxylic acid and alcohol compounds; under the catalysis of the catalyst, the oxidation reaction product obtained in step S2 is subjected to continuous esterification reaction to obtain artificial beeswax. The addition of the catalyst can catalyze the esterification reaction between the byproduct carboxylic acid produced in the continuous oxidation reaction and the alcohol, which can reduce the reaction activation energy of the continuous esterification reaction, thereby increasing the reaction rate. The above-mentioned continuous production method of the present application can increase the ester-acid ratio of artificial beeswax, thereby obtaining artificial beeswax with an acid value and a saponification value that meet the requirements.
[0064] Compared with the prior art using paraffin as the main raw material, the present application uses Fischer-Tropsch wax as the starting raw material, which is beneficial to reduce the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby improving its yield and purity. At the same time, using Fischer-Tropsch wax as a raw material can reduce costs and reduce waste emissions. Compared with the preparation of oxidized wax by a one-step oxidation method, the artificial beeswax produced by the continuous production method of artificial beeswax mentioned above in the present application has a high ester-acid ratio, and the obtained artificial beeswax can meet the requirements of acid value and saponification value at the same time. Compared with the intermittent production process, the continuous production method provided by the present application is used for continuous production, which can improve production efficiency, reduce production costs, and at the same time improve the utilization rate of raw materials and the yield of artificial beeswax.
[0065] The oxidizing gas is used to provide an oxidant source for the continuous oxidation reaction. In a preferred embodiment, the oxidizing gas includes, but is not limited to, one or more of the group consisting of air, oxygen, and a mixture of nitrogen and oxygen. The use of the above-mentioned types of oxidizing gases for the oxidation reaction has a simple process flow, and the chemical properties of the above-mentioned types of gases are stable, which is conducive to improving the safety of the production process.
[0066] In order to further provide a source of oxidant with stable properties and high oxidation efficiency for the continuous oxidation reaction, preferably, when the oxidizing gas is a mixture of nitrogen and oxygen, the volume concentration of oxygen in the mixture is 15 to 30 vol%.
[0067] In a preferred embodiment, the rate at which the oxidizing gas is introduced into the continuous oxidation reaction device 200 is 0.3 to 0.8 standard cubic meters per hour. Compared with other ranges, limiting the introduction rate of the oxidizing gas within the above range is conducive to controlling the volume concentration of the oxidizing gas in the continuous oxidation reaction process within an appropriate range, and is conducive to improving the contact efficiency between the oxidizing gas and the liquid wax, thereby facilitating the reaction rate of the continuous oxidation reaction and improving the yield of the oxidation reaction product.
[0068] In order to further improve the contact efficiency between the oxidizing gas and the liquid wax, thereby further improving the reaction rate of the continuous oxidation reaction, preferably, when the oxidizing gas is air, the rate at which air is passed into the continuous oxidation reaction device 200 is 0.4 to 0.6 standard cubic meters per hour; when the oxidizing gas is oxygen, the rate at which oxygen is passed into the continuous oxidation reaction device 200 is 0.3 to 0.4 standard cubic meters per hour; when the oxidizing gas is a mixture of nitrogen and oxygen, the rate at which the mixture is passed into the continuous oxidation reaction device 200 is 0.4 to 0.6 standard cubic meters per hour.
[0069] In a preferred embodiment, the feed rate of the catalyst into the continuous esterification reaction device 301 is 10 to 100 g / h. Compared with other ranges, limiting the catalyst feed rate within the above range is conducive to increasing the concentration of the catalyst during the continuous esterification reaction, and is conducive to reducing the reaction activation energy of the continuous esterification reaction, thereby facilitating increasing its reaction rate.
[0070] In order to further reduce the reaction activation energy of the continuous esterification reaction and further increase its reaction rate, preferably, the catalyst includes but is not limited to C8~C 12 Alkylbenzene sulfonic acid and / or ester compound with 15 to 20 carbon atoms.
[0071] In a preferred embodiment, during the continuous esterification reaction, an inert gas is continuously introduced into the continuous esterification reaction device 301. The introduction of the inert gas into the continuous esterification reaction device 301 facilitates the use of the fluidity of the inert gas, is conducive to taking away the reaction heat generated in the continuous esterification reaction, is conducive to providing a dynamic equilibrium environment for the reaction, and is conducive to improving the reaction efficiency of the continuous esterification reaction, and is further conducive to improving the ester-acid ratio of the artificial beeswax, and is conducive to obtaining an artificial beeswax whose acid value and saponification value meet the requirements.
[0072] In order to further improve the fluidity of the inert gas, preferably, the introduction rate of the inert gas is 0.2 to 0.5 standard cubic meters per hour.
[0073] In a preferred embodiment, the inert gas includes but is not limited to nitrogen and / or argon. Compared with other types, the use of the above types of inert gas is conducive to improving the reaction efficiency of the continuous esterification reaction.
[0074] In a preferred embodiment, stirring is performed during the continuous esterification reaction. The above method can stir the reaction system, which is beneficial to dispersing the reaction heat generated in the continuous esterification reaction, thereby providing a dynamic equilibrium environment for the reaction, thereby facilitating the reaction efficiency of the continuous esterification reaction, and further facilitating the improvement of the ester-acid ratio of the artificial beeswax, and facilitating the acquisition of an artificial beeswax having an acid value and a saponification value that meet the requirements.
[0075] In order to further provide a dynamic equilibrium environment for the continuous esterification reaction, thereby further improving its reaction efficiency, preferably, the stirring rate is 100-500 rpm.
[0076] In a preferred embodiment, the rate at which the oxidation reaction product is continuously introduced into the continuous esterification reaction device 301 is 1 to 10 kg / h. Compared with other ranges, limiting the introduction rate of the oxidation reaction product within the above range is beneficial to controlling the concentration of the oxidation reaction product in the continuous esterification reaction process within a suitable range, which is beneficial to providing a dynamic equilibrium environment for the reaction, thereby facilitating the improvement of the reaction rate of the continuous esterification reaction and the yield of artificial beeswax.
[0077] In a preferred embodiment, between step S2 and step S3, a process of mixing the oxidation reaction product with the catalyst by using the first continuous mixing device 304 is also included to obtain the first mixture. The oxidation reaction product and the catalyst are pre-mixed in the first continuous mixing device 304 to obtain the first mixture, which is beneficial to improving the dispersibility of the two, facilitating the subsequent continuous esterification reaction, thereby helping to improve the production efficiency of the continuous reaction.
[0078] In order to further improve the mixing efficiency of the oxidation reaction product and the catalyst, preferably, the rate at which the oxidation reaction product is introduced into the first continuous mixing device 304 is 1 to 10 kg / h, and the rate at which the catalyst is introduced into the first continuous mixing device 304 is 10 to 100 g / h.
[0079] In a preferred embodiment, the rate at which the first mixture is introduced into the continuous esterification reaction device 301 is 1 to 10 kg / h. Compared with other ranges, limiting the introduction rate of the first mixture within the above range is conducive to controlling the concentration of the first mixture in the continuous esterification reaction process within a suitable range, which is conducive to providing a dynamic equilibrium environment for the reaction, thereby facilitating the improvement of the reaction rate of the continuous esterification reaction and the yield of artificial beeswax.
[0080] In a preferred embodiment, between step S2 and step S3, there is also included a process of mixing the esterifying agent with the catalyst using the second continuous mixing device 306 to obtain a second mixture. The addition of the esterifying agent is conducive to an esterification reaction between the esterifying agent and the by-product carboxylic acid produced in the continuous oxidation reaction, thereby facilitating an increase in the ester-acid ratio of the artificial beeswax, and further facilitating the acquisition of an artificial beeswax having an acid value and a saponification value that meet the requirements. Premixing the esterifying agent with the catalyst in the second continuous mixing device 306 is conducive to a more complete mixing of the two, and at the same time, the second mixture obtained after mixing is passed into the third mixing device, which is conducive to saving subsequent mixing time, thereby facilitating an increase in the production efficiency of the continuous reaction.
[0081] In order to further improve the mixing efficiency of the esterification agent and the catalyst, preferably, the rate at which the esterification agent is introduced into the second continuous mixing device 306 is 100-1000 g / h, and the rate at which the catalyst is introduced into the second continuous mixing device 306 is 10-100 g / h.
[0082] In a preferred embodiment, the rate at which the second mixture is introduced into the continuous esterification reaction device 301 is 100 to 1000 g / h. Compared with other ranges, limiting the introduction rate of the second mixture within the above range is conducive to controlling the concentration of the second mixture in the continuous esterification reaction process within a suitable range, which is conducive to providing a dynamic equilibrium environment for the reaction, thereby facilitating the improvement of the reaction rate of the continuous esterification reaction and the yield of artificial beeswax.
[0083] In a preferred embodiment, the continuous production method further comprises passing the second mixture into a third continuous mixing device 309, mixing the second mixture with the oxidation reaction product to obtain a third mixture. Pre-mixing the second mixture with the oxidation reaction product in the third continuous mixing device 309 to obtain the third mixture is beneficial to improving the dispersibility of the two, facilitating the subsequent continuous esterification reaction, thereby helping to improve the production efficiency of the continuous reaction.
[0084] In order to further improve the mixing efficiency of the second mixture and the oxidation reaction product, preferably, the rate at which the second mixture is introduced into the third continuous mixing device 309 is 100 to 1000 g / h, and the rate at which the oxidation reaction product is introduced into the third continuous mixing device 309 is 1 to 10 kg / h.
[0085] In a preferred embodiment, the rate at which the third mixture is introduced into the continuous esterification reaction device 301 is 1 to 10 kg / h. Compared with other ranges, limiting the introduction rate of the third mixture within the above range is conducive to controlling the concentration of the third mixture in the continuous esterification reaction process within an appropriate range, which is conducive to providing a dynamic equilibrium environment for the reaction, thereby facilitating the improvement of the reaction rate of the continuous esterification reaction and the yield of artificial beeswax.
[0086] In a preferred embodiment, the esterifying agent includes but is not limited to alcohols with carbon numbers of 16 to 20. Compared with other types, the use of the above-mentioned types of esterifying agents is conducive to esterification with the by-product carboxylic acid produced in the continuous oxidation reaction, thereby facilitating the improvement of the ester-acid ratio of the artificial beeswax, and further facilitating the acquisition of artificial beeswax with acid value and saponification value meeting the requirements.
[0087] In order to further allow the esterifying agent to undergo an esterification reaction with the byproduct carboxylic acid produced in the continuous oxidation reaction, thereby facilitating further increasing the ester-acid ratio of the artificial beeswax, preferably, the esterifying agent includes but is not limited to octadecyl alcohol and / or hexadecanol.
[0088] In a preferred embodiment, the reaction temperature of the continuous oxidation reaction is 150-180° C., and the material residence time is 1-4 hours. Compared with other ranges, limiting the reaction temperature and material residence time of the continuous oxidation reaction within the above range is conducive to improving the reaction rate of the continuous oxidation reaction, thereby improving the efficiency of continuous production.
[0089] In order to further increase the reaction rate of the continuous oxidation reaction, preferably, the reaction temperature of the continuous oxidation reaction is 160-175°C.
[0090] In a preferred embodiment, the reaction temperature of the continuous esterification reaction is 140-170° C., and the material residence time is 1-3 hours. Compared with other ranges, limiting the reaction temperature and material residence time of the continuous esterification reaction within the above range is conducive to increasing the reaction rate of the continuous esterification reaction, thereby improving the efficiency of continuous production, and is also conducive to increasing the ester-acid ratio of artificial beeswax.
[0091] In order to further increase the reaction rate of the continuous esterification reaction, preferably, the reaction temperature of the continuous esterification reaction is 150-165°C.
[0092] In a preferred embodiment, the Fischer-Tropsch wax raw material includes but is not limited to one or more of the group consisting of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, 65# Fischer-Tropsch wax, 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, 90# Fischer-Tropsch wax, 100# Fischer-Tropsch wax, 105# Fischer-Tropsch wax and 110# Fischer-Tropsch wax. The use of the above-mentioned types of Fischer-Tropsch wax is beneficial to reducing the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby helping to improve the yield and purity of the product. At the same time, using Fischer-Tropsch wax as a raw material is beneficial to reducing costs and reducing the discharge of waste.
[0093] In a preferred embodiment, the heating and melting temperature is 80-120°C, and the material residence time is 1-10 hours. Compared with other ranges, limiting the heating and melting temperature and material residence time within the above range is conducive to increasing the heating and melting rate of the Fischer-Tropsch wax raw material and facilitating subsequent reactions.
[0094] In a preferred embodiment, stirring is performed during the heating and melting process. Stirring the Fischer-Tropsch wax raw material during heating and melting is beneficial for making the Fischer-Tropsch wax raw material heated more evenly, thereby improving the heating and melting efficiency and facilitating subsequent reactions.
[0095] In order to further improve the heating and melting efficiency of the Fischer-Tropsch wax raw material and facilitate subsequent reactions, preferably, the stirring rate is 50 to 200 rpm.
[0096] In a preferred embodiment, the rate at which the liquid wax is introduced into the continuous oxidation reaction device 200 is 1 to 12 kg / h. Compared with other ranges, limiting the introduction rate of the liquid wax within the above range is conducive to improving the raw material utilization rate of the liquid wax, thereby facilitating the reaction rate of the continuous oxidation reaction and improving the yield of the oxidation reaction product.
[0097] In order to further improve the raw material utilization rate of liquid wax, thereby further improving the reaction rate of the continuous oxidation reaction and the yield of the oxidation reaction product, preferably, when the Fischer-Tropsch wax raw material includes but is not limited to one or more of 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, and 90# Fischer-Tropsch wax, the rate at which the liquid wax is passed into the continuous oxidation reaction device 200 is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 165 to 175°C, and the material residence time is 2 to 3 hours; when the Fischer-Tropsch wax raw material includes but is not limited to one or more of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, and 65# Fischer-Tropsch wax, the rate at which the liquid wax is passed into the continuous oxidation reaction device 200 is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 160 to 175°C, and the material residence time is 1 to 2 hours.
[0098] 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.
[0099] It should be noted that the products produced in all the examples and comparative examples of the present application were tested, and the specific test methods are as follows:
[0100] The acid value of the product is tested according to ASTM D1386-15 "Standard Test Method for Acid Number (Empirical) of Synthetic and Natural Waxes"; the saponification value of the product is tested according to ASTM D1387-89 "Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes"; the melting point of the product is tested according to GB / T 617-2006 "General Method for Determination of Melting Point Range of Chemical Reagents"; the relative refractive index of the product is tested according to GB / T 6488-2008 "Determination of Refractive Index of Liquid Chemical Products (20°C)"; the drop melting point of the product is tested according to GB / T 8026-2023 "Determination of Drop Melting Point of Petroleum Wax and Petroleum Fat"; the dynamic viscosity of the product at 140°C is tested according to SH / T 0018 "Determination of Apparent Viscosity of Petroleum Wax (Hot Melt Adhesive) Containing Additives"; the color of the product is tested according to SH / T 0168-1992 "Determination of Chroma of Petroleum Products".
[0101] All embodiments of this application adopt Figure 1 The continuous production system shown carries out the continuous production of artificial beeswax. The continuous Fischer-Tropsch wax melting device 100 adopts two heating tanks arranged in series to melt the Fischer-Tropsch wax, one of which is in working state and the other is in standby state; the continuous oxidation reaction device 200 adopts a microchannel reactor (Nanjing Kemik Equipment Co., Ltd., WTDFRQ-001); the continuous esterification reaction device 301 adopts a microchannel reactor (Nanjing Kemik Equipment Co., Ltd., model WTDFRQ-002).
[0102] The raw materials used in the examples of the present application are 70# Fischer-Tropsch wax and 90# Fischer-Tropsch wax, which are wax phase raw materials obtained by Fischer-Tropsch synthesis and oil-wax separation, wherein the initial distillation point of 70# Fischer-Tropsch wax is 467°C, the final distillation point is 687.5°C, and the carbon number of the fraction is 28-48; the initial distillation point of 90# Fischer-Tropsch wax is 496°C, the final distillation point is 719°C, and the carbon number of the fraction is 31-51. The raw material used in Comparative Example 1 of the present application is paraffin wax, which has an initial distillation point of 396°C, a final distillation point of 700°C, and a carbon number of the fraction is 21-42. The distillation range properties of 70# Fischer-Tropsch wax, 90# Fischer-Tropsch wax and paraffin wax are shown in Table 1.
[0103] Table 1
[0104]
[0105] Example 1
[0106] A continuous production method for artificial beeswax, comprising:
[0107] (1) Under stirring conditions of 50 rpm, 70# Fischer-Tropsch wax was continuously introduced into two heating tanks arranged in series for heating and melting to obtain liquid wax, wherein the heating and melting temperature was 80° C. and the material residence time was 1 h;
[0108] (2) The liquid wax obtained in step (1) is delivered to the liquid wax inlet through a continuous feed pump 400 with a feed rate of 6 kg / h and introduced into a microchannel reactor, wherein the total height H1 of the microchannel reactor is 2 m, the liquid wax inlet is arranged at the top thereof, the oxidizing gas inlet 201 is arranged at the bottom thereof, air is introduced into the microchannel reactor through the oxidizing gas inlet 201, the temperature in the microchannel reactor is set to 175° C., and the air and the liquid wax are continuously oxidized to obtain an oxidation reaction product; wherein the material residence time is 2 h, the liquid wax introduction rate is 6 kg / h, and the air introduction rate is 0.4 standard cubic meters / h;
[0109] (3) introducing octadecyl alcohol as an esterifying agent and dodecylbenzenesulfonic acid as a catalyst into a stirred tank for mixing to obtain a mixture containing the esterifying agent and the catalyst; wherein the introduction rate of octadecyl alcohol is 600 g / h, and the introduction rate of the catalyst is 60 g / h;
[0110] (4) introducing the oxidation reaction product obtained in step (2) and the mixture containing the esterifying agent and the catalyst obtained in step (3) into a mixer for mixing to obtain a mixture; wherein the introduction rate of the oxidation reaction product is 6 kg / h, and the introduction rate of the mixture containing the esterifying agent and the catalyst is 600 g / h;
[0111] (5) The mixture obtained in step (4) is introduced into a microchannel reactor, the total height H2 of the microchannel reactor is 2m, the first mixture inlet is arranged at the top, the inert gas inlet 303 is arranged at the bottom, N2 is introduced into the microchannel reactor through the inert gas inlet 303, the temperature in the microchannel reactor is set to 150°C, and a continuous esterification reaction is carried out to obtain artificial beeswax; wherein the material residence time is 2h, the introduction rate of the mixture obtained in step (4) is 6kg / h, and the introduction rate of N2 is 0.5 standard cubic meters / h.
[0112] Example 2
[0113] The difference from Example 1 is that in step (2), the liquid wax inlet is set at the 0.9H1 position of the microchannel reactor, the oxidizing gas inlet 201 is set at the 0.05H1 position, and the remaining steps are the same as Example 1.
[0114] Example 3
[0115] The difference from Example 1 is that in step (2), the liquid wax inlet is set at the 0.7H1 position of the microchannel reactor, the oxidizing gas inlet 201 is set at the 0.2H1 position, and the remaining steps are the same as Example 1.
[0116] Example 4
[0117] The difference from Example 1 is that in step (5), the first mixture inlet is set at the 0.9H2 position of the microchannel reactor, the inert gas inlet 303 is set at the 0.05H2 position, and the remaining steps are the same as Example 1.
[0118] Example 5
[0119] The difference from Example 1 is that in step (5), the first mixture inlet is set at the 0.7H2 position of the microchannel reactor, the inert gas inlet 303 is set at the 0.2H2 position, and the remaining steps are the same as Example 1.
[0120] Example 6
[0121] The difference from Example 1 is that a ceramic membrane gas distributor is arranged at the oxidizing gas inlet 201 of the microchannel reactor in step (2) near the inner side of the microchannel reactor, and its pore size is 15 μm, the porosity is 25%, and the thickness is 3 mm; a metal membrane gas distributor is arranged at the inert gas inlet 303 of the microchannel reactor in step (5) near the inner side of the microchannel reactor, and its pore size is 50 μm, the porosity is 40%, and the thickness is 5 mm. The remaining steps are the same as Example 1.
[0122] Example 7
[0123] The difference from Example 1 is that: a ceramic membrane gas distributor is arranged at the oxidation gas inlet 201 of the microchannel reactor in step (2) near the inner side of the microchannel reactor, and its pore size is 60 μm, the porosity is 5%, and the thickness is 6 mm; a metal membrane gas distributor is arranged at the oxidation gas inlet 201 of the microchannel reactor in step (5) near the inner side of the microchannel reactor, and its pore size is 70 μm, the porosity is 45%, and the thickness is 7 mm. The remaining steps are the same as Example 1.
[0124] Example 8
[0125] The difference from Example 1 is that stirring is performed during the continuous esterification reaction in step (5), and N2 is not introduced into the microchannel reactor. The stirring rate is 500 rpm, and the remaining steps are the same as in Example 1.
[0126] Example 9
[0127] The difference from Example 1 is that N2 is not introduced during the continuous esterification reaction in step (5), and the remaining steps are the same as Example 1.
[0128] Example 10
[0129] The difference from Example 1 is that no esterifying agent is added in step (5), and the catalyst dodecylbenzenesulfonic acid and the oxidation reaction product obtained in step (2) are directly introduced into a microchannel reactor for continuous esterification reaction; wherein the rate at which the catalyst is introduced into the microchannel reactor is 10 g / h, and the rate at which the oxidation reaction product is introduced into the microchannel reactor is 1 kg / h, and the remaining steps are the same as in Example 1.
[0130] Embodiment 11
[0131] The difference from Example 1 is that no esterifying agent is added in step (5), and the catalyst dodecylbenzenesulfonic acid and the oxidation reaction product obtained in step (2) are directly introduced into a microchannel reactor for continuous esterification reaction; wherein the rate at which the catalyst is introduced into the microchannel reactor is 120 g / h, and the rate at which the oxidation reaction product is introduced into the microchannel reactor is 0.5 kg / h, and the remaining steps are the same as in Example 1.
[0132] Example 12
[0133] The difference from Example 1 is that: no esterifying agent is added in step (5), the catalyst dodecylbenzenesulfonic acid and the oxidation reaction product obtained in step (2) are directly introduced into a mixer for mixing to obtain a first mixture, and the first mixture is introduced into a microchannel reactor for continuous esterification reaction; wherein the rate at which the catalyst is introduced into the mixer is 100 g / h, the rate at which the oxidation reaction product is introduced into the mixer is 10 kg / h, and the remaining steps are the same as in Example 1.
[0134] Embodiment 13
[0135] The difference from Example 1 is that: no esterifying agent is added in step (5), the catalyst dodecylbenzenesulfonic acid and the oxidation reaction product obtained in step (2) are directly introduced into a mixer for mixing to obtain a first mixture, and the first mixture is introduced into a microchannel reactor for continuous esterification reaction; wherein the rate at which the catalyst is introduced into the mixer is 8 g / h, and the rate at which the oxidation reaction product is introduced into the mixer is 15 kg / h, and the remaining steps are the same as in Example 1.
[0136] Embodiment 14
[0137] The difference from Example 1 is that the reaction temperature of the continuous oxidation reaction is 160° C., the material residence time is 1 h, and the remaining steps are the same as in Example 1.
[0138] Embodiment 15
[0139] The difference from Example 1 is that the reaction temperature of the continuous oxidation reaction is 195° C., the material residence time is 8 h, and the remaining steps are the same as in Example 1.
[0140] Example 16
[0141] The difference from Example 1 is that the reaction temperature of the continuous esterification reaction is 165° C., the material residence time is 3 h, and the remaining steps are the same as in Example 1.
[0142] Embodiment 17
[0143] The difference from Example 1 is that the reaction temperature of the continuous esterification reaction is 120° C., the material residence time is 6 h, and the remaining steps are the same as in Example 1.
[0144] Embodiment 18
[0145] The difference from Example 1 is that in step (1), 90# Fischer-Tropsch wax is used as raw material, the heating melting temperature is 120°C, and the material residence time is 8 hours. In step (2), the rate at which the liquid wax is introduced into the microchannel reactor is 10 kg / h, the reaction temperature of continuous oxidation is 175°C, and the material residence time is 3 hours. The remaining steps are the same as in Example 1.
[0146] Embodiment 19
[0147] The difference from Example 1 is that the heating and melting temperature in step (1) is 140° C., the material residence time is 0.5 h, and the remaining steps are the same as in Example 1.
[0148] Comparative Example 1
[0149] The difference from Example 1 is that at a stirring rate of 200 rpm, paraffin is passed into two heating tanks arranged in series for heating and melting to obtain liquid paraffin. The heating and melting temperature is 140° C., the material residence time is 4 hours, and the remaining steps are the same as in Example 1.
[0150] Comparative Example 2
[0151] The difference from Example 1 is that the product is directly obtained after the continuous oxidation reaction is completed without subsequent continuous esterification reaction, and the remaining steps are the same as Example 1.
[0152] The index requirements of Western beeswax are shown in Table 2; the test results of the artificial beeswax products prepared in the examples and comparative examples of this application are shown in Table 3.
[0153] Table 2
[0154] Acid value (mgKOH / g) Saponification value (mgKOH / g) Melting point(℃) Relative refractive index Western Beeswax 16.00~23.00 75.00~110.0 62~67 1.4410~1.4430
[0155] Table 3
[0156]
[0157] From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:
[0158] By comparing Example 1 and Comparative Example 1, it can be seen that compared with using paraffin as the main raw material, the present application uses Fischer-Tropsch wax as the starting raw material, which is beneficial to reducing the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby improving the yield and purity of the product. The prepared artificial beeswax can meet the requirements of acid ester and saponification value at the same time. At the same time, using Fischer-Tropsch wax as raw material can reduce costs and reduce waste emissions.
[0159] By comparing Example 1 and Comparative Example 2, it can be seen that compared with the one-step oxidation method for preparing oxidized wax, the artificial beeswax produced by the continuous production system and continuous production method of artificial beeswax in the present application can meet the requirements for acid value and saponification value at the same time.
[0160] By comparing Examples 1 to 3, it can be seen that the positions of the liquid wax inlet and the oxidizing gas inlet 201 in the present application include but are not limited to the above-mentioned range. Limiting them within the above-mentioned range is beneficial to the countercurrent contact between the liquid wax flowing from top to bottom and the oxidizing gas introduced from bottom to top, which is beneficial to making the contact between the two more complete, thereby facilitating the improvement of the reaction efficiency of the continuous oxidation reaction, and further facilitating the improvement of the acid value and saponification value of the obtained artificial beeswax.
[0161] By comparing Examples 1, 4 and 5, it can be seen that the positions of the first mixture inlet and the inert gas inlet 303 in the present application include but are not limited to the above-mentioned range. Limiting them within the above-mentioned range is beneficial to the countercurrent contact between the first oxidation product flowing from top to bottom and the inert gas introduced from bottom to top, which is beneficial for the inert gas to disperse the reaction heat generated in the reaction, thereby facilitating the provision of a dynamic equilibrium environment for the reaction, and improving the reaction rate of the continuous esterification reaction, thereby facilitating the improvement of the acid value and saponification value of the obtained artificial beeswax.
[0162] By comparing Examples 1, 6 and 7, it can be seen that a gas distributor is arranged inside the continuous oxidation microchannel reactor and the continuous esterification microchannel reactor, and its pore size, porosity and thickness include but are not limited to the above-mentioned ranges. Limiting it within the above-mentioned range is beneficial to more evenly distribute the oxidizing gas and the inert gas in the inner cavity of the continuous oxidation reaction device 200 and the inner cavity of the continuous esterification reaction device 301, respectively, thereby helping to improve the reaction efficiency of the continuous oxidation reaction and the continuous esterification reaction, and further helping to improve the acid value and saponification value of the obtained artificial beeswax.
[0163] By comparing Examples 1, 8 and 9, it can be seen that introducing N2 into the continuous esterification reaction or stirring during the continuous esterification reaction is beneficial to dispersing the reaction heat generated in the continuous esterification reaction, and is beneficial to providing a dynamic equilibrium environment for the reaction, thereby helping to increase the reaction rate of the continuous esterification reaction, and further helping to increase the acid value and saponification value of the obtained artificial beeswax.
[0164] By comparing Examples 1 and 10 to 13, it can be seen that the rate at which the catalyst and the oxidation reaction product are introduced into the continuous esterification reaction device 301 or the first continuous mixing device 304 includes but is not limited to the above range. Limiting it within the above range is beneficial to improving the reaction efficiency of the continuous esterification reaction, thereby helping to improve the acid value and saponification value of the obtained artificial beeswax; using the first continuous mixing device 304 to pre-mix the oxidation reaction product with the catalyst to obtain a first mixture is beneficial to improving the dispersibility of the two and facilitating the subsequent continuous esterification reaction. The addition of the esterifying agent is beneficial to causing an esterification reaction between it and the by-product carboxylic acid produced in the continuous oxidation reaction, thereby helping to improve the reaction efficiency of the continuous esterification reaction, and further helping to improve the acid value and saponification value of the obtained artificial beeswax.
[0165] By comparing Examples 1, 14 and 15, it can be seen that the reaction temperature and material residence time of the continuous oxidation reaction include but are not limited to the above ranges. Limiting them within the above ranges is beneficial to increasing the reaction rate of the continuous oxidation reaction, thereby improving the efficiency of continuous production, and is also beneficial to increasing the acid value and saponification value of the obtained artificial beeswax.
[0166] By comparing Examples 1, 16 and 17, it can be seen that the reaction temperature and material residence time of the continuous esterification reaction include but are not limited to the above ranges. Limiting them within the above ranges is beneficial to increasing the reaction rate of the continuous esterification reaction, thereby improving the efficiency of continuous production, and is also beneficial to increasing the acid value and saponification value of the obtained artificial beeswax.
[0167] By comparing Examples 1, 18 and 19, it can be seen that the use of different types of Fischer-Tropsch wax raw materials is beneficial to reducing the content of impurities such as sulfur, nitrogen, and aromatic hydrocarbons in artificial beeswax products, thereby helping to improve the yield and purity of the product; at the same time, the heating and melting temperature and material residence time include but are not limited to the above ranges. Limiting them within the above ranges is beneficial to improving the heating and melting efficiency and facilitating subsequent reactions, thereby helping to improve the acid value and saponification value of the obtained artificial beeswax.
[0168] 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.
[0169] 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 artificial beeswax, characterized in that: The continuous production system of the artificial beeswax comprises: At least one continuous Fischer-Tropsch wax melting device (100), each of the continuous Fischer-Tropsch wax melting devices (100) being provided with a Fischer-Tropsch wax raw material inlet (101) and a liquid wax outlet; the continuous Fischer-Tropsch wax melting device (100) being further provided with a heating component; A continuous oxidation reaction device (200), wherein the continuous oxidation reaction device (200) is provided with a liquid wax inlet, an oxidation gas inlet (201) and an oxidation reaction product outlet; the liquid wax inlet is connected to the liquid wax outlet; A continuous esterification reaction unit (300), the continuous esterification reaction unit (300) comprises a continuous esterification reaction device (301), the continuous esterification reaction device (301) is provided with a first oxidation reaction product inlet, a first catalyst inlet and an artificial beeswax outlet (302); the first oxidation reaction product inlet is connected to the oxidation reaction product outlet.
2. The continuous production system of artificial beeswax according to claim 1, characterized in that: The continuous oxidation reaction device (200) is selected from a microchannel reactor or a vertical tube reactor; Preferably, the liquid wax inlet is arranged at the upper part of the continuous oxidation reaction device (200), and the oxidizing gas inlet (201) is arranged at the lower part of the continuous oxidation reaction device (200), and the total height of the continuous oxidation reaction device (200) is H1. More preferably, the liquid wax inlet is arranged at a position of 0.9H1~H1, and the oxidizing gas inlet (201) is arranged at a position of 0~0.05H1.
3. The continuous production system of artificial beeswax according to claim 1 or 2, characterized in that: The continuous oxidation reaction device (200) also includes a first gas distributor, which is arranged on the inner side of the continuous oxidation reaction device (200) near the oxidation gas inlet (201); preferably, the first gas distributor is selected from a membrane gas distributor or a coil distributor; more preferably, the membrane gas distributor is selected from a metal membrane and / or a ceramic membrane; further preferably, the membrane gas distributor has a pore size of 5 to 50 μm, a porosity of 10 to 40%, and a thickness of 1 to 5 mm.
4. The continuous production system of artificial beeswax according to any one of claims 1 to 3, characterized in that: The continuous esterification reaction device (301) is further provided with an inert gas inlet (303) for introducing an inert gas to stir the oxidation reaction product and the catalyst; and / or, a first stirring component is provided in the continuous esterification reaction device (301); Preferably, the first oxidation reaction product inlet is arranged at the upper part of the continuous esterification reaction device (301), and the inert gas inlet (303) is arranged at the lower part of the continuous esterification reaction device (301), and the total height of the continuous esterification reaction device (301) is H2, more preferably, the first oxidation reaction product inlet is arranged at a position of 0.9H2-H2, and the inert gas inlet (303) is arranged at a position of 0-0.05H2; Preferably, when the continuous esterification reaction device (301) comprises an inert gas inlet (303), the continuous esterification reaction device (301) further comprises a second gas distributor, and the second gas distributor is arranged inside the continuous esterification reaction device (301) near the inert gas inlet (303); more preferably, the second gas distributor is selected from a membrane gas distributor or a coil distributor; More preferably, the membrane gas distributor is selected from metal membrane and / or ceramic membrane; further preferably, the membrane gas distributor has a pore size of 5 to 50 μm, a porosity of 10 to 40%, and a thickness of 1 to 5 mm.
5. The continuous production system of artificial beeswax according to claim 4, characterized in that: The continuous esterification reaction unit (300) further comprises a first continuous mixing device (304) for mixing the oxidation reaction product with the catalyst to obtain a first mixture; the first continuous mixing device (304) is provided with a second oxidation reaction product inlet, a second catalyst inlet (305) and a first mixture outlet; the second oxidation reaction product inlet is connected to the oxidation reaction product outlet; the continuous esterification reaction device (301) further comprises a first mixture inlet, and the first mixture outlet is connected to the first mixture inlet; Preferably, the first mixture inlet is arranged at the upper part of the continuous esterification reaction device (301), and more preferably, the first mixture inlet is arranged at the position of 0.9H2-H2; Preferably, the continuous esterification reaction unit (300) further comprises a second continuous mixing device (306) for mixing the esterifying agent with the catalyst to obtain a second mixture; the second continuous mixing device (306) is provided with an esterifying agent inlet (307), a third catalyst inlet (308) and a second mixture outlet, the first continuous mixing device (304) further comprises a second mixture inlet, and the second mixture outlet is connected to the second mixture inlet; Preferably, the continuous esterification reaction device (301) is selected from a microchannel reactor or a vertical tube reactor; More preferably, the continuous esterification reaction unit (300) further includes a third continuous mixing device (309) for mixing the second mixture with the oxidation reaction product; the third continuous mixing device (309) is provided with a first inlet, a second inlet and a third mixture outlet; the first inlet is connected to the second mixture outlet, and the second inlet is connected to the oxidation reaction product outlet; the continuous esterification reaction device (301) further includes a third mixture inlet, and the third mixture outlet is connected to the third mixture inlet; preferably, the third mixture inlet is arranged at the upper part of the continuous esterification reaction device (301), and more preferably, the third mixture inlet is arranged at the position of 0.9H2~H2.
6. The continuous production system of artificial beeswax according to claim 1, characterized in that: A second stirring component is provided in the continuous Fischer-Tropsch wax melting device (100); and / or when the continuous production system comprises two continuous Fischer-Tropsch wax melting devices (100), one of them is in working state and the other is in standby state.
7. The continuous production system of artificial beeswax according to claim 1, characterized in that: The liquid wax inlet is connected to the liquid wax outlet via a liquid wax delivery pipeline, and a continuous feed pump (400) is provided on the liquid wax delivery pipeline.
8. A continuous production method for artificial beeswax, characterized in that: The continuous production method is carried out using the continuous production system of artificial beeswax according to any one of claims 1 to 7, and the continuous production method comprises: Step S1, using a continuous Fischer-Tropsch wax melting device (100) to heat and melt the Fischer-Tropsch wax raw material to obtain liquid wax; Step S2, subjecting the liquid wax and the oxidizing gas to a continuous oxidation reaction in a continuous oxidation reaction device (200) to obtain an oxidation reaction product; Step S3, subjecting the oxidation reaction product to a continuous esterification reaction in a continuous esterification reaction device (301) under the catalysis of a catalyst to obtain the artificial beeswax.
9. The continuous production method of artificial beeswax according to claim 8, characterized in that: The oxidizing gas is selected from one or more of the group consisting of air, oxygen, and a mixture of nitrogen and oxygen; Preferably, when the oxidizing gas is a mixed gas of nitrogen and oxygen, the volume concentration of the oxygen in the mixed gas is 15 to 30 vol%; Preferably, the rate at which the oxidizing gas is introduced into the continuous oxidation reaction device (200) is 0.3 to 0.8 standard cubic meters per hour; More preferably, when the oxidizing gas is the air, the rate at which the air is introduced into the continuous oxidation reaction device (200) is 0.4 to 0.6 standard cubic meters per hour; More preferably, when the oxidizing gas is oxygen, the rate at which the oxygen is introduced into the continuous oxidation reaction device (200) is 0.3 to 0.4 standard cubic meters per hour; More preferably, when the oxidizing gas is a mixed gas of nitrogen and oxygen, the rate at which the mixed gas is introduced into the continuous oxidation reaction device (200) is 0.4 to 0.6 standard cubic meters per hour.
10. The continuous production method of artificial beeswax according to claim 8, characterized in that: The catalyst is fed into the continuous esterification reaction device (301) at a rate of 10 to 100 g / h; Preferably, the catalyst is selected from C8 to C 12 Alkylbenzene sulfonic acid and / or ester compound with 15 to 20 carbon atoms.
11. The continuous production method of artificial beeswax according to claim 8, characterized in that: During the continuous esterification reaction, an inert gas is continuously introduced into the continuous esterification reaction device (301); and / or, stirring is performed during the continuous esterification reaction; Preferably, the inert gas introduction rate is 0.2 to 0.5 standard cubic meters per hour; Preferably, the stirring rate is 100 to 500 rpm; More preferably, the inert gas is selected from nitrogen and / or argon.
12. The continuous production method of artificial beeswax according to claim 8, characterized in that: The oxidation reaction product is continuously introduced into the continuous esterification reaction device (301) at a rate of 1 to 10 kg / h; Preferably, between step S2 and step S3, a process of mixing the oxidation reaction product with the catalyst by a first continuous mixing device (304) is further included to obtain a first mixture; more preferably, the rate at which the oxidation reaction product is introduced into the first continuous mixing device (304) is 1 to 10 kg / h, the rate at which the catalyst is introduced into the first continuous mixing device (304) is 10 to 100 g / h, and the rate at which the first mixture is introduced into the continuous esterification reaction device (301) is 1 to 10 kg / h; Preferably, between step S2 and step S3, a process of mixing the esterifying agent and the catalyst by a second continuous mixing device (306) is further included to obtain a second mixture; more preferably, the rate at which the esterifying agent is introduced into the second continuous mixing device (306) is 100 to 1000 g / h, the rate at which the catalyst is introduced into the second continuous mixing device (306) is 10 to 100 g / h, and the rate at which the second mixture is introduced into the continuous esterification reaction device (301) is 100 to 1000 g / h; More preferably, the continuous production method further comprises passing the second mixture into a third continuous mixing device (309) to mix the second mixture with the oxidation reaction product to obtain a third mixture; further preferably, the rate at which the second mixture is passed into the third continuous mixing device (309) is 100 to 1000 g / h, the rate at which the oxidation reaction product is passed into the third continuous mixing device (309) is 1 to 10 kg / h, and the rate at which the third mixture is passed into the continuous esterification reaction device (301) is 1 to 10 kg / h; More preferably, the esterifying agent is selected from alcohols having 16 to 20 carbon atoms; further preferably, the esterifying agent is selected from octadecyl alcohol and / or hexadecanol.
13. The continuous production method of artificial beeswax according to claim 8, characterized in that: The reaction temperature of the continuous oxidation reaction is 150-180°C, and the material residence time is 1-4h; preferably, the reaction temperature of the continuous oxidation reaction is 160-175°C; and / or, The reaction temperature of the continuous esterification reaction is 140-170°C, and the material residence time is 1-3h; preferably, the reaction temperature of the continuous esterification reaction is 150-165°C.
14. The continuous production method of artificial beeswax according to any one of claims 8 to 13, characterized in that: The Fischer-Tropsch wax raw material is selected from one or more of the group consisting of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, 65# Fischer-Tropsch wax, 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, 90# Fischer-Tropsch wax, 100# Fischer-Tropsch wax, 105# Fischer-Tropsch wax and 110# Fischer-Tropsch wax; Preferably, the heating and melting temperature is 80-120°C, and the material residence time is 1-10h; Preferably, stirring is performed during the heating and melting process; more preferably, the stirring rate is 50 to 200 rpm.
15. The method for continuous production of artificial beeswax according to claim 14, characterized in that: The rate at which the liquid wax is introduced into the continuous oxidation reaction device (200) is 1 to 12 kg / h; Preferably, when the Fischer-Tropsch wax raw material is selected from one or more of 70# Fischer-Tropsch wax, 80# Fischer-Tropsch wax, and 90# Fischer-Tropsch wax, the rate at which the liquid wax is introduced into the continuous oxidation reaction device (200) is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 165 to 175° C., and the material residence time is 2 to 3 hours; Preferably, when the Fischer-Tropsch wax raw material is selected from one or more of 52# Fischer-Tropsch wax, 60# Fischer-Tropsch wax, and 65# Fischer-Tropsch wax, the rate at which the liquid wax is introduced into the continuous oxidation reaction device (200) is 1 to 10 kg / h, the reaction temperature of the continuous oxidation reaction is 160 to 175°C, and the material residence time is 1 to 2 hours.
Citation Information
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