A reaction device and method for preparing 9-bromoanthracene

Abstract

The present invention provides a kind of reaction device and method for preparing 9-bromoanthracene, including a pretreatment system, a solid hopper and a reaction system; the reaction system includes a reactor and an agitator arranged in the reactor, and the agitator is an anchor frame agitator; the pretreatment system includes a pulping kettle, a liquid feed port and a catalyst feed port are arranged on the pulping kettle, and a stirring pulping device is arranged inside, and a pulping outlet at the bottom of the pulping kettle is connected with a pulping inlet on the reactor; a feed port and a discharge port are arranged on the solid hopper, and the discharge port is connected with a solid feed port on the reactor. During use, Lewis acid and bromine source are added to the pulping kettle through the catalyst feed port, a solvent is added to the pulping kettle through the liquid feed port, a slurry is made in the pulping kettle, a reactor is fed, and anthracene is added to the reactor through a solid hopper; react in the reactor. Effectively solve the problems of heat transfer, mass transfer difficulties, and many by-products during the reaction process, and provide a new way for producing high-purity 9-bromoanthracene.

Description

Technical Field

[0001] The invention relates to the technical field of fine chemicals, and in particular to a reaction device and a method for preparing 9-bromoanthracene. Background Art

[0002] 9-Bromoanthracene is a fluorescent and phosphorescent material with excellent performance, which is widely used in optics, cosmetics, electronics, semiconductors and electroluminescent materials. At present, most of the synthesis methods of 9-bromoanthracene use highly corrosive substances such as liquid bromine (bromine), hydrogen bromide, dimethyl bromide and sulfur bromide as bromine sources, which have the disadvantages of poor reaction controllability, strong corrosiveness and serious environmental pollution.

[0003] In view of these shortcomings in the synthesis of 9-bromoanthracene, many different bromine sources and catalyst systems have been developed. In 2005, Rashid Badri et al. (Phosphorus, Sulfur, and Silicon, 180: 533–536, 2005) reported that the CuBr2 / K2Cr2O7 / HOAc system achieved a highly selective synthesis of anthracene under mild conditions. This method has the advantages of mild conditions, high yield and good selectivity, and provides a new route for the synthesis of 9-bromoanthracene. This study solves the problem of strong corrosiveness of liquid bromine and hydrogen bromide, but the use of toxic and carcinogenic strong oxidant K2Cr2O7 (potassium dichromate) as a catalyst still poses great hazards. At the same time, the price of the catalyst and bromine source is relatively expensive, which is not conducive to industrialization. Professor Li Feng (Journal of Materials Chemistry C, 2015, 3(38): 9942-9947) selected NBS as the bromine source to synthesize 9-bromoanthracene in chloroform. This not only overcomes the corrosiveness of the bromine source, but also makes the reaction conditions milder, effectively reducing the reaction cost. However, due to the symmetry of the bromine positions 9 and 10, the activity is comparable, and a large amount of 9,10-dibromoanthracene by-products appear during the reaction. The selectivity of the reaction system is low, only about 60%.

[0004] In addition, the current different synthesis methods of 9-bromoanthracene all use anthracene as the main raw material and are carried out in ordinary reactors. A large amount of heat is generated during the synthesis of 9-bromoanthracene, which causes the local temperature in the reactor to be too high, resulting in the production of 9,10-dibromoanthracene byproducts, resulting in a reduced yield of 9-bromoanthracene and low purity. Summary of the invention

[0005] In view of the problems existing in the prior art, the present invention provides a reaction device and method for preparing 9-bromoanthracene, which effectively solves the problems of heat transfer, mass transfer difficulties and large number of by-products in the reaction process, and provides a new way to produce high-purity 9-bromoanthracene.

[0006] The present invention is achieved through the following technical solutions:

[0007] A reaction device for preparing 9-bromoanthracene, comprising a pretreatment system, a solid hopper and a reaction system;

[0008] The reaction system comprises a reactor and a stirrer arranged in the reactor, the stirrer is an anchor frame stirrer, and a discharge port is arranged at the bottom of the reactor;

[0009] The pretreatment system includes a pulping kettle, which is provided with a liquid feeding port and a catalyst feeding port, and a stirring pulping device is arranged in the pulping kettle, and the pulp outlet at the bottom of the pulping kettle is connected to the pulp inlet on the reactor through a pump;

[0010] The solid hopper is provided with a feed inlet and a discharge port, and the discharge port is connected with the solid feed inlet on the reactor.

[0011] Preferably, a reflux system is also included, which includes a condenser, the gas outlet on the reactor is connected to the heat source inlet of the condenser through a gas pipeline, and the heat source outlet of the condenser is connected to the liquid return port of the reactor through a liquid reflux pipeline.

[0012] Furthermore, it also includes a solvent recovery tank, and the heat source outlet of the condenser is also connected to the solvent recovery tank.

[0013] Preferably, the stirrer is provided with blades.

[0014] Preferably, a solvent feed port is also reserved on the reaction kettle.

[0015] Preferably, the reactor is provided with a liquid level gauge, a pressure gauge and a thermometer.

[0016] The method for preparing 9-bromoanthracene by using the reaction device comprises the following steps: adding Lewis acid and bromine source into a pulping kettle through a catalyst feeding port, adding solvent into the pulping kettle through a liquid feeding port, rapidly stirring into slurry in the pulping kettle, sending the slurry into a reactor through a pump, turning on a stirrer in the reactor for stirring, and setting the initial speed of the stirrer to 80-120 r / min; adding anthracene into the reactor through a solid hopper in sequence; heating the reactor to maintain the temperature at 30-90°C, increasing the speed of the stirrer to 120-200 r / min, and maintaining the temperature for 2-6 hours after reaching a reaction reflux state;

[0017] The bromine source is NaBr, KBr, CuBr2, CuBr, MgBr2, FeBr3 or FeBr2. When the bromine source is NaBr, KBr, CuBr, MgBr2 or FeBr2, an oxidant needs to be added; when the bromine source is CuBr2 or FeBr3, no oxidant needs to be added; when it is necessary to add an oxidant, if the oxidant is liquid, it is added to the pulping kettle through the liquid feeding port; if the oxidant is solid, it is added to the reactor through the solid hopper.

[0018] Preferably, the Lewis acid is AlCl3, AlBr3, FeCl3, FeBr3 or BF3, and the oxidant is hydrogen peroxide, potassium persulfate or potassium persulfate.

[0019] Preferably, when an oxidant needs to be added, the molar ratio of anthracene to the oxidant is 1:(0.5-2); the molar ratio of the bromine source to anthracene is (0.2-4):1, and the molar ratio of the Lewis acid to anthracene is (0.02-0.1):1.

[0020] Preferably, the solvent is chloroform, methanol, acetonitrile or carbon tetrachloride.

[0021] Compared with the prior art, the present invention has the following beneficial technical effects:

[0022] The reactor of the device of the present invention adopts an anchor frame agitator, and the gap between the agitator and the reactor wall is small, which significantly enhances the stirring effect of the reactor and strengthens the mass transfer and heat transfer capacity of the reaction process; at the same time, the catalyst, bromine source and solvent are stirred and slurried in advance, and added to the reactor in the form of slurry, so as to avoid the catalyst and the like from being directly added to the reactor and agglomerating, thereby improving the reaction efficiency and avoiding the generation of by-products, effectively solving the problems of heat transfer and mass transfer difficulties and many by-products in the reaction process, and providing a new way to produce high-purity 9-bromoanthracene. The reaction device has a simple structure, a large operating range, and is conducive to scale-up production.

[0023] Furthermore, the reactor is equipped with a closed reflux system, which prevents the impact of material volatilization on the environment.

[0024] Furthermore, a solvent recovery tank is set up, which can be used for distillation and recovery of organic waste solvents when there is no reaction task, thereby reducing the organic waste liquid generated in the laboratory, improving the utilization rate of solvents, and being green and environmentally friendly.

[0025] The preparation method of the present invention adopts the above-mentioned reaction device to enhance the mass transfer and heat transfer capacity of the reaction process; at the same time, during the reaction process, the catalyst and the solvent are first slurried to make the catalyst evenly dispersed, and then slowly added to the reactor, effectively avoiding local overheating caused by heat generated by rapid feeding; the reaction temperature is controlled within 90°C, reducing the occurrence of side reactions, controlling the reaction time within 6 hours, avoiding the generation of by-products due to excessive reaction time, improving the reaction efficiency, and improving the yield and purity of the product 9-bromoanthracene. In addition, the raw material metal bromide of the present invention is mild in nature, has little corrosion to the reactor, and has high safety; the present invention adopts an oxidant plus a Lewis acid as a catalytic system, and the Lewis acid first forms a complex structure with a bromine atom with a relatively strong electronegativity, and reacts with anthracene activated by the oxidant to obtain the target product; the method not only avoids the strong corrosion of the reaction container when liquid bromine and hydrogen bromide are used as raw materials, but also improves the selectivity of the reaction, and obtains a target product with high yield and high purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic diagram of the device of the present invention.

[0027] In the figure: liquid feeding port 1, catalyst feeding port 2, solvent recovery tank 3, discharge port 4, exhaust pipe 5, pulping kettle 6, solid hopper 7, reaction kettle 8, condenser 9, solvent recovery tank 10, liquid level meter 11, pressure gauge 12, first thermometer 13, mass flowmeter 14, second thermometer 15, agitator 16. DETAILED DESCRIPTION

[0028] The present invention is further described in detail below in conjunction with specific embodiments, which are intended to explain the present invention rather than to limit it.

[0029] like Figure 1 As shown, the device of the present invention includes a pretreatment system, a solid hopper, a reaction system and a reflux system.

[0030] The reaction system comprises a reaction kettle 8 and an agitator 16 arranged in the reaction kettle. The agitator 16 is an anchor frame agitator with a certain number of blades.

[0031] The pretreatment system includes a pulping kettle 6, which is provided with a liquid feeding port 1 and a catalyst feeding port 2. A stirring pulping device is provided in the pulping kettle 6, and the pulping outlet at the bottom of the pulping kettle 6 is connected to the pulp inlet on the reaction kettle 8 through a pump.

[0032] The solid hopper 7 is provided with a feed port and a discharge port, and the discharge port is connected to the solid feed port on the reaction kettle 8 .

[0033] The reflux system includes a condenser 9, the gas outlet on the reactor 8 is connected to the heat source inlet of the condenser 9 through a gas pipeline, the heat source outlet of the condenser 9 is connected to the liquid return port of the reactor 8 through a liquid reflux pipeline, and the liquid reflux pipeline is also connected to the solvent recovery tank 10.

[0034] During the reaction process, the solvent distilled in the reflux system flows back into the reactor. When there is no reaction task, the device can be used alone to distill and recover the organic waste solvent, so the device of the present invention also has a distillation function. When the organic waste liquid generated in the reaction process or post-treatment process needs to be recovered, the organic waste liquid is transported to the reactor through the solvent feed port, stirring is turned on, the reactor is heated, and the distillation temperature is controlled according to the specific situation of the waste solvent, so that the light component evaporates and enters the condenser, and is collected in the recovery tank after condensation by the condenser. Therefore, the device can be used for distillation and recovery of organic waste solvents, reducing the amount of organic waste liquid in the laboratory, improving solvent utilization, and being green and environmentally friendly.

[0035] Method of using the device of the present invention:

[0036] Lewis acid and bromine source are added to the pulping kettle 6 through the catalyst feed port 2, and the solvent and oxidant (when the oxidant is liquid) or solvent (when the oxidant is solid) are added to the pulping kettle 6 through the liquid feed port 1. The pulping kettle 6 is quickly stirred into slurry, and the slurry is sent to the reactor 8 through a pump. The stirrer 16 in the reactor 8 is turned on for stirring, and the initial speed of the stirrer 16 is set to 80-120r / min; anthracene (when the oxidant is liquid) or anthracene and oxidant (when the oxidant is solid) are sequentially added to the reactor 8 through the solid hopper 7. Specifically, the bottom valve is opened during the reaction, and the reaction is observed. The mass flow meter 14 shows a number, and the valve is closed after reaching the specified amount; the electric heating is turned on to heat the reactor 8 to raise the temperature, and the temperature is maintained at 30-90°C, and the speed of the agitator 16 is increased to 120-200r / min. After the temperature reaches the reaction reflux state, it is maintained for 2-6h until the reaction is completed; during the reaction, the gas phase enters the condenser 9 through the gas pipeline at the top of the reactor 8, and after condensation, it returns to the reactor 8 from the liquid reflux pipeline; after the reaction is completed, the temperature and pressure of the reactor 8 are monitored at any time during the reflux process, and the second 15 parameter of the thermometer on the gas phase pipeline at the inlet of the condenser 9 is used.

[0037] The reactor 8 is also provided with a solvent feed port, through which solvent can be added when the solvent needs to be supplemented. A discharge port 4 is provided at the bottom of the reactor 8.

[0038] The reactor 8 is also provided with auxiliary equipment: a level meter 11, a pressure gauge 12, a first thermometer 13, and a valve and a mass flow meter 14 are provided on the connecting pipeline between the solid hopper 7 and the reactor 8. A second thermometer 15 is also provided on the gas pipeline. A gas extraction pipe 5 is provided on the top of the condenser 9.

[0039] The reaction equation is as follows:

[0040]

[0041] The bromine source (M(Br) n ) is NaBr, KBr, CuBr2, CuBr, MgBr2, FeBr3 or FeBr2. When the bromine source is NaBr, KBr, CuBr, MgBr2 or FeBr2, an oxidant needs to be added; when the bromine source is CuBr2 or FeBr3, no oxidant is needed; when it is necessary to add an oxidant, if the oxidant is liquid, it is added to the pulping kettle 6 through the liquid feeding port 1; if the oxidant is solid, it is added to the reaction kettle 8 through the solid hopper 7.

[0042] The oxidant is hydrogen peroxide, potassium persulfate Or potassium persulfate. The Lewis acid is AlCl3, AlBr3, FeCl3, FeBr3 or BF3.

[0043] The solvent is chloroform, methanol, acetonitrile or carbon tetrachloride; wherein carbon tetrachloride is a polar solvent.

[0044] The molar ratio of anthracene to the oxidant is 1:(0.5-2); the molar ratio of the bromine source to anthracene is (0.2-4):1, and the molar ratio of the added amount of Lewis acid to anthracene is (0.02-0.1):1.

[0045] Example 1

[0046] Ferric chloride (8.11 mg, 0.05 mmol) and potassium bromide (197.51 mg, 2.50 mmol) were added to the pulping kettle through the catalyst feed port, and acetonitrile was added to the pulping kettle through the liquid feed port, and the slurry was stirred; the prepared slurry was transported to the reactor by a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and solid raw materials anthracene (390 mg, 2.50 mmol) and potassium persulfate (210.20 mg, 1.25 mmol) were slowly added to the reactor in sequence through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 60°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser, and samples were taken for detection after 3 hours of reaction. After the detection was qualified, the reaction was stopped by cooling.

[0047] After the reaction, the solvent acetonitrile was evaporated in a rotary evaporator, and the obtained solid was added to a pre-packed silica gel column, and petroleum ether was used to pass through the column. The product was detected and collected by TLC plate, and the eluent was combined and concentrated to obtain 534.2 mg of the product 9-bromoanthracene: the product was a light yellow solid with a yield of 83.10%. The results of HPLC showed that its purity was 99.30% and the melting point was 103.7-107.8°C. The obtained product data: IR (KBr, cm-1): 3431, 3038, 2924, 2353, 1910, 1785, 1614, 1432, 1306, 1251, 1008, 885, 832, 723, 593, 525. HRMS (ESI) m / z: calcd for C14H9Br [M+H] + 257.9865, found 257.9869.

[0048] Example 2

[0049] Ferric bromide (36.94 mg, 0.125 mmol) and potassium bromide (595.01 mg, 5.00 mmol) were added to the pulping kettle through the catalyst feed port, and acetonitrile was added to the pulping kettle through the liquid feed port, and the slurry was stirred; the prepared slurry was transported to the reactor by a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and solid raw materials anthracene (390 mg, 2.50 mmol) and potassium persulfate (210.20 mg, 1.25 mmol) were slowly added to the reactor in sequence through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 60°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser, and samples were taken for detection after 3 hours of reaction. After the detection was qualified, the reaction was stopped by cooling. After the reaction is completed, the solvent acetonitrile is evaporated in a rotary evaporator, and the obtained solid is added to a pre-assembled silica gel column, and petroleum ether is passed through the column. The product is detected and collected by TLC plate, and the eluate is combined and concentrated to dryness to obtain 591.4 mg of the product 9-bromoanthracene: the product is a light yellow solid, the yield is 92.0%, the purity is 99.20%, and the melting point is 103.6-107.8°C.

[0050] Example 3

[0051] Ferric chloride (8.11 mg, 0.05 mmol) and potassium bromide (197.51 mg, 2.50 mmol) were added to the pulping kettle through the catalyst feed port, and acetonitrile and hydrogen peroxide (170.07 mg, 5.0 mmol) were added to the pulping kettle through the liquid feed port, and the slurry was stirred; the prepared slurry was transported to the reactor by a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and the solid raw material anthracene (390 mg, 2.50 mmol) was slowly added to the reactor through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 70°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser E, and samples were taken for detection after 2.0 h of reaction. After the detection was qualified, the reaction was stopped by cooling. After the reaction is completed, the solvent acetonitrile is evaporated in a rotary evaporator, and the obtained solid is added to a pre-assembled silica gel column, and petroleum ether is passed through the column. The product is detected and collected by TLC plate, and the eluate is combined and concentrated to dryness to obtain 561.19 mg of the product 9-bromoanthracene: the product is a light yellow solid, the yield is 87.30%, the purity is 99.26%, and the melting point is 103.1-107.4°C.

[0052] Example 4

[0053] Aluminum trichloride (16.67 mg, 0.125 mmol) and copper bromide (837.58 mg, 3.75 mmol) were added to the pulping kettle through the catalyst feed port, and chloroform was added to the pulping kettle through the liquid feed port, and the pulping was stirred; chloroform and solid raw materials were pre-stored in the solvent storage tank and the solid hopper, and 5 ml of chloroform was accurately added to the reactor through the metering flowmeter; the prepared slurry was transported to the reactor through a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and the solid raw material anthracene (390 mg, 2.50 mmol) was slowly added to the reactor through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 50°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser E, and samples were taken for detection after 6 hours of reaction. After the detection was qualified, the temperature was lowered to stop the reaction. After the reaction is completed, the solvent chloroform is evaporated in a rotary evaporator, and the obtained solid is added to a pre-assembled silica gel column, and petroleum ether is passed through the column. The product is detected and collected by TLC plate, and the eluate is combined and concentrated to dryness to obtain 544.60 mg of the product 9-bromoanthracene: the product is a light yellow solid, the yield is 84.72%, the purity is 99.41%, and the melting point is 103.2-107.5°C.

[0054] Example 5

[0055] Boron trifluoride (16.95 mg, 0.25 mmol) and copper bromide (837.58 mg, 3.75 mmol) were added to the pulping kettle through the catalyst feed port, and carbon tetrachloride was added to the pulping kettle through the liquid feed port, and the slurry was stirred; the prepared slurry was transported to the reactor by a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and the solid raw material anthracene (390 mg, 2.50 mmol) was slowly added to the reactor through the solid hopper in sequence, and the addition was completed within half an hour; the reaction temperature was controlled at 35°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser E, and samples were taken for detection after 4 hours of reaction. After the detection was qualified, the reaction was stopped by cooling. After the reaction is completed, the solvent carbon tetrachloride is evaporated in a rotary evaporator, and the obtained solid is added to a pre-assembled silica gel column, and petroleum ether is passed through the column. The product is detected and collected by TLC plate, and the eluate is combined and concentrated to dryness to obtain 550.2 mg of the product 9-bromoanthracene: the product is a light yellow solid, the yield is 85.60%, the purity is 99.35%, and the melting point is 103.4-107.8°C.

[0056] Example 6

[0057] Ferric bromide (36.94 mg, 0.125 mmol) and sodium bromide (514.45 mg, 5.00 mmol) were added to the pulping kettle through the catalyst feed port, and acetonitrile was added to the pulping kettle through the liquid feed port, and the slurry was stirred; the prepared slurry was transported to the reactor by a pump, the reactor agitator was turned on, the speed was set to 100 r / min, and solid raw materials anthracene (390 mg, 2.50 mmol) and potassium persulfate (210.20 mg, 1.25 mmol) were slowly added to the reactor in sequence through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 90°C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser, and samples were taken for detection after 3 hours of reaction. After the detection was qualified, the reaction was stopped by cooling. After the reaction is completed, the solvent acetonitrile is evaporated in a rotary evaporator, and the obtained solid is added to a pre-assembled silica gel column, and petroleum ether is passed through the column. The product is detected and collected by TLC plate, and the eluate is combined and concentrated to dryness to obtain 488.55 mg of the product 9-bromoanthracene: the product is a light yellow solid, the yield is 76.0%, the purity is 99.23%, and the melting point is 103.6-107.8°C.

[0058] Example 7

[0059] Iron tribromide (738.89 mg, 2.5 mmol) and acetonitrile were added to the slurry kettle through the catalyst feed port and the liquid feed port respectively, and stirred and slurried; the prepared slurry was transported to the reactor by a pump, the reactor stirrer was turned on, the speed was set to 100 r / min, and the solid raw material anthracene (390 mg, 2.50 mmol) was slowly added to the reactor through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 60 ° C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser, and the sample was tested after the reaction for 2 hours. After the test was qualified, the temperature was lowered to stop the reaction. After the reaction was completed, the solvent acetonitrile was evaporated in a rotary evaporator, and the obtained solid was added to the installed silica gel column, and petroleum ether was used to pass the column. The product was detected and collected by TLC plate, and the eluent was combined and concentrated and dried to obtain the product 9-bromoanthracene 584.97 mg: the product was a light yellow solid, with a yield of 91.0%, a purity of 99.46%, and a melting point of 103.6-107.8 ° C.

[0060] Example 8

[0061] Iron tribromide (147.78 mg, 0.5 mmol) and acetonitrile were added to the slurry kettle through the catalyst feed port and the liquid feed port respectively, and stirred and slurried; the prepared slurry was transported to the reactor by a pump, the reactor stirrer was turned on, the speed was set to 100 r / min, and the solid raw material anthracene (390 mg, 2.50 mmol) was slowly added to the reactor through the solid hopper, and the addition was completed within half an hour; the reaction temperature was controlled at 90 ° C, the reaction speed was increased to 150 r / min, the solvent was refluxed through the condenser, and the sample was tested after the reaction for 6 hours. After the test was qualified, the temperature was lowered to stop the reaction. After the reaction was completed, the solvent acetonitrile was evaporated in a rotary evaporator, and the obtained solid was added to the installed silica gel column, and petroleum ether was used to pass the column. The product was detected and collected by TLC plate, and the eluent was combined and concentrated and dried to obtain 469.26 mg of the product 9-bromoanthracene: the product was a light yellow solid with a yield of 73.0%, a purity of 99.37%, and a melting point of 103.6-107.8 ° C.

Claims

1. A method for preparing 9-bromoanthracene, characterized in that: The reaction device used in the method comprises a pretreatment system, a solid hopper and a reaction system; the reaction system comprises a reactor (8) and a stirrer (16) arranged in the reactor, the stirrer (16) is an anchor frame stirrer, and a discharge port (4) is arranged at the bottom of the reactor (8); the stirrer (16) is provided with blades; and a solvent feed port is also reserved on the reactor (8); the pretreatment system comprises a pulping reactor (6), the pulping reactor (6) is provided with a liquid feed port (1) and a catalyst feed port (2), a stirring pulping device is arranged in the pulping reactor (6), and a pulp outlet at the bottom of the pulping reactor (6) is connected to a pulp inlet on the reactor (8) through a pump; a solid hopper (7) is provided with a feed port and a discharge port, and the discharge port is connected to a solid feed port on the reactor (8); The method comprises: adding Lewis acid and bromine source into a pulping kettle (6) through a catalyst feeding port (2), adding solvent into the pulping kettle (6) through a liquid feeding port (1), rapidly stirring into a pulping kettle (6), sending the pulping kettle (6) into a reaction kettle (8) through a pump, turning on a stirrer (16) in the reaction kettle (8) for stirring, and setting the initial speed of the stirrer (16) to 80-120 r / min; adding anthracene into the reaction kettle (8) in sequence through a solid hopper (7); heating the reaction kettle (8) to maintain the temperature at 30-90° C., increasing the speed of the stirrer (16) to 120-200 r / min, and maintaining the temperature for 2-6 hours after reaching a reaction reflux state; The bromine source is NaBr, KBr, CuBr2, CuBr, MgBr 2、 FeBr3 or FeBr2, when the bromine source is NaBr, KBr, CuBr, MgBr2 or FeBr2, an oxidant needs to be added, and the oxidant is hydrogen peroxide, potassium persulfate or potassium persulfate; when the bromine source is CuBr2 or FeBr3, no oxidant needs to be added; when it is necessary to add an oxidant, if the oxidant is liquid, it is added to the pulping kettle (6) through the liquid feeding port (1); if the oxidant is solid, it is added to the reaction kettle (8) through the solid hopper (7); the Lewis acid is AlCl3, AlBr3, FeCl3, FeBr3 or BF3.

2. The method for preparing 9-bromoanthracene according to claim 1, characterized in that: When an oxidant needs to be added, the molar ratio of anthracene to the oxidant is 1:0.5-2; the molar ratio of the bromine source to anthracene is 0.2-4:1, and the molar ratio of the Lewis acid to anthracene is 0.02-0.1:

1.

3. The method for preparing 9-bromoanthracene according to claim 1, characterized in that: The solvent is chloroform, methanol, acetonitrile or carbon tetrachloride.

4. The method for preparing 9-bromoanthracene according to claim 1, characterized in that: The reaction device further comprises a reflux system, which comprises a condenser (9), wherein a gas outlet on the reaction kettle (8) is connected to a heat source inlet of the condenser (9) via a gas pipeline, and a heat source outlet of the condenser (9) is connected to a liquid return port of the reaction kettle (8) via a liquid reflux pipeline.

5. The method for preparing 9-bromoanthracene according to claim 1, characterized in that: The reaction device further comprises a solvent recovery tank (10), and the heat source outlet of the condenser (9) is also connected to the solvent recovery tank (10).

6. The method for preparing 9-bromoanthracene according to claim 1, characterized in that: The reaction kettle (8) is provided with a liquid level gauge (11), a pressure gauge (12) and a thermometer.

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