Production device of beta-acetylnaphthalene

Abstract

A beta-acetylnaphthalene production device belongs to the technical field of chemical equipment and comprises a dissolving kettle, a tubular reactor, a hydrolysis liquid separation kettle and an external evaporation crystallization kettle, a dissolving kettle solid feed inlet and a dissolving kettle liquid inlet are formed in the top of the dissolving kettle, a dissolving kettle liquid outlet is formed in the bottom of the dissolving kettle, and a first constant-temperature heat exchanger is arranged on the outer wall of the dissolving kettle; a solid feeding port of the dissolving kettle is connected with a solid feeding machine through a pipeline and connected with a valve in series, a liquid inlet of the dissolving kettle is connected with a solvent storage tank through a pipeline and connected with a valve, an electronic flowmeter and a transmission pump in series, and a liquid outlet of the dissolving kettle is connected with a tubular reactor and an acetyl chloride storage tank through a first tee joint. According to the utility model, beta-acetylnaphthalene can be continuously produced in a continuous feeding and intermittent discharging manner, so that the production efficiency is improved, and the production cost is reduced; meanwhile, through the design, multiple treatment procedures are simplified in one device for treatment, the device utilization rate is increased while the device is simplified, the occupied space of production equipment is saved, and industrial popularization is facilitated.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of chemical equipment, especially relates to a beta-acetylnaphthalene production device. BACKGROUND

[0002] Beta-acetylnaphthalene, also known as beta-naphthyl ketone, methyl-beta-naphthyl ketone, etc., is a commonly used intermediate, which can be used as a raw material for the synthesis of cosmetics, dyes or medicines, and is a very basic chemical raw material.

[0003] At present, for the production of beta-acetylnaphthalene, Friedel-Crafts acylation reaction is generally used: naphthalene and acetyl chloride are used as raw materials, and under the action of Lewis acid and nitroalkane / nitrobenzene, alpha-acetylnaphthalene and beta-acetylnaphthalene are generated, and then beta-acetylnaphthalene is obtained by hydrolysis, separation, and distillation. The production mode is generally intermittent production, which has low production capacity and high cost. SUMMARY

[0004] In view of the problems existing in the prior art, the present application provides a beta-acetylnaphthalene production device, which uses continuous feeding and intermittent discharging to realize continuous production of beta-acetylnaphthalene, reduces the purification temperature, saves production energy, and improves the intrinsic safety of production.

[0005] To achieve the above-mentioned purpose, the utility model adopts the following technical scheme: a beta-acetylnaphthalene production device, characterized by comprising: a dissolving kettle, a tubular reactor, a hydrolysis separation kettle and an external steam crystallization kettle, the top of the dissolving kettle is provided with a dissolving kettle solid feeding port and a dissolving kettle liquid inlet, the bottom is provided with a dissolving kettle liquid outlet, and the outer wall is provided with a first constant temperature heat exchanger, the dissolving kettle solid feeding port is connected with a solid feeding machine through a pipeline and is connected with a valve in series, the dissolving kettle liquid inlet is connected with a solvent storage tank through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series, and the dissolving kettle liquid outlet is connected with the tubular reactor and an acetyl chloride storage tank through a first three-way joint;

[0006] One end of the tubular reactor is provided with a tubular reactor liquid inlet, the other end is provided with a tubular reactor liquid outlet, the outer wall is sleeved with a tubular constant temperature heat exchanger, the tubular constant temperature heat exchanger water inlet of the tubular constant temperature heat exchanger is connected with a circulating water inlet pipeline through a pipeline and is connected with an electromagnetic valve, an electronic flowmeter and an electromagnetic pump in series, and the tubular constant temperature heat exchanger water outlet is connected with a circulating water return pipeline through a pipeline and is connected with a valve in series;

[0007] The hydrolysis separation tank is provided with a hydrolysis separation tank liquid inlet and a hydrolysis separation tank acid inlet at the top, a hydrolysis separation tank liquid outlet at the bottom, and a second constant temperature heat exchanger on the outer wall.

[0008] The outer steam crystallization tank is provided with an outer steam crystallization tank liquid inlet and an outer steam crystallization tank gas outlet at the top, an outer steam crystallization tank discharge port at the bottom, and a third constant temperature heat exchanger on the outer wall.

[0009] Preferably, the pipe reactor is provided with a spiral propelling baffle in the pipe.

[0010] Preferably, the pipe reactor has an inner diameter of 5-10 cm and a length of 50-200 m.

[0011] Preferably, the pipe reactor has an inner diameter of 7 cm and a length of 100 m.

[0012] Preferably, the hydrolysis separation tank has a column diameter ratio of (3-5):1.

[0013] Preferably, the left end of the first three-way joint is connected to the dissolution tank liquid outlet through a pipeline and is connected in series with an electromagnetic valve, an electronic flow meter and an electromagnetic pump, the upper end is connected to the acetyl chloride storage tank through a pipeline and is connected in series with an electromagnetic valve, an electronic flow meter and an electromagnetic pump, and the right end is connected to the pipe reactor liquid inlet through a pipeline.

[0014] Preferably, the left side of the first three-way joint is designed with a first PLC and a second PLC, the first PLC is connected to the electronic flow meter at the left end of the first three-way joint and the electromagnetic valve, the electronic flow meter and the electromagnetic pump connected in series at the upper end of the first three-way joint through data lines, forming interlocking; the second PLC is connected to the electronic flow meter at the left end of the first three-way joint and the electromagnetic valve, the electronic flow meter and the electromagnetic pump connected in series with the water inlet of the constant temperature heat exchanger through data lines, forming interlocking.

[0015] Preferably, the left end of the second three-way joint is connected to the outer steam crystallization tank liquid inlet through a pipeline and is connected in series with a valve, an electronic flow meter and a transfer pump, the upper end is connected to the hydrolysis separation tank liquid outlet through a pipeline and is connected in series with a valve, and the right end is connected to the brine storage tank through a pipeline and is connected in series with a valve and a transfer pump.

[0016] Preferably, the upper end of the third three-way joint is connected to the outer steam liquid collection tank through a pipeline and is connected in series with a valve and a vacuum pump, the lower end is connected to the gas outlet of the outer steam crystallization tank through a pipeline, and the right end is connected to the ethanol storage tank through a pipeline and is connected in series with a valve, an electronic flow meter and a transfer pump.

[0017] Preferably, the dissolving kettle, hydrolysis kettle or external steam crystallization kettle is parallelly connected according to actual needs, N≥2.

[0018] The present application has the following advantages:

[0019] The production device of beta-acetylnaphthalene provided by the utility model continuously produces beta-acetylnaphthalene through the mode of continuous feeding and intermittent discharging, improves production efficiency and reduces production cost; meanwhile, through design, multiple processing procedures are simplified in one equipment for processing, equipment utilization is improved while equipment is simplified, production equipment occupied space is saved, and industrialization popularization is beneficial. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 It is a whole structure schematic view of the utility model.

[0021] In the figure: 1, dissolving kettle, 101, dissolving kettle solid feeding port, 102, dissolving kettle liquid inlet, 103, dissolving kettle liquid outlet, 104, first constant temperature heat exchanger, 2, tubular reactor, 201, tubular reactor liquid inlet, 202, tubular reactor liquid outlet, 203, tubular constant temperature heat exchanger, 2031, tubular constant temperature heat exchanger water inlet, 2032, tubular constant temperature heat exchanger water outlet, 3, hydrolysis kettle, 301, hydrolysis kettle liquid inlet, 302, hydrolysis kettle acid inlet, 303, hydrolysis kettle liquid outlet, 304, second constant temperature heat exchanger, 4, external steam crystallization kettle, 401, external steam crystallization kettle liquid inlet, 402 external steam crystallization kettle gas outlet, 403, external steam crystallization kettle discharge port, 404, third constant temperature heat exchanger, 5, first PLC, 6, second PLC, 7, first three-way, 8, second three-way, 9, third three-way. DETAILED DESCRIPTION

[0022] The utility model will be further described in detail in connection with the drawings and specific embodiments. A kind of production device of beta-acetylnaphthalene, it is characterized in that, including: dissolving kettle 1, tubular reactor 2, hydrolysis kettle 3 and external steam crystallization kettle 4, the top of the dissolving kettle 1 is equipped with dissolving kettle solid feeding port 101 and dissolving kettle liquid inlet 102, bottom is equipped with dissolving kettle liquid outlet 103, outer wall is equipped with first constant temperature heat exchanger 104, the dissolving kettle solid feeding port 101 is connected solid feeding machine by pipeline and is connected valve in series, the dissolving kettle liquid inlet 102 is connected solvent storage tank by pipeline and is connected valve in series, electronic flowmeter and transmission pump, the dissolving kettle liquid outlet 103 is connected tubular reactor 2 and acetyl chloride storage tank respectively by first three-way 7;

[0023] The tubular reactor 2 is provided with a tubular reactor liquid inlet 201 at one end and a tubular reactor liquid outlet 202 at the other end, and is provided with a shell-and-tube constant-temperature heat exchanger 203 on the outer wall, wherein a shell-and-tube constant-temperature heat exchanger water inlet 2031 of the shell-and-tube constant-temperature heat exchanger 203 is connected to a circulating water inlet pipeline through a pipeline and is connected in series with a solenoid valve, an electronic flow meter and a solenoid pump, and a shell-and-tube constant-temperature heat exchanger water outlet 2032 is connected to a circulating water return pipeline through a pipeline and is connected in series with a valve.

[0024] The hydrolysis separation kettle 3 is provided with a hydrolysis separation kettle liquid inlet 301 and a hydrolysis separation kettle acid inlet 302 at the top and a hydrolysis separation kettle liquid outlet 303 at the bottom, and is provided with a second constant-temperature heat exchanger 304 on the outer wall, wherein the hydrolysis separation kettle liquid inlet 301 is connected to the tubular reactor liquid outlet 202 through a pipeline and is connected in series with a valve, an electronic flow meter and a transfer pump, the hydrolysis separation kettle acid inlet 302 is connected to a hydrochloric acid storage tank through a pipeline and is connected in series with a valve, an electronic flow meter and a transfer pump, and the hydrolysis separation kettle liquid outlet 303 is connected to the outer steam crystallization kettle 4 and the brine storage tank through the second three-way valve 8 respectively.

[0025] The outer steam crystallization kettle 4 is provided with an outer steam crystallization kettle liquid inlet 401 and an outer steam crystallization kettle gas outlet 402 at the top and an outer steam crystallization kettle discharge port 403 at the bottom, and is provided with a third constant-temperature heat exchanger 404 on the outer wall, wherein the outer steam crystallization kettle gas outlet 402 is connected to the outer steam liquid collection tank and the ethanol storage tank through the third three-way valve 9 respectively.

[0026] In the embodiment, the tubular reactor 2 is provided with a spiral propelling baffle in the tube.

[0027] In the embodiment, the tubular reactor 2 has an inner diameter of 5-10 cm and a length of 50-200 m.

[0028] In the embodiment, the tubular reactor 2 has an inner diameter of 7 cm and a length of 100 m.

[0029] In the embodiment, the hydrolysis separation kettle 3 has a column diameter ratio of (3-5):1.

[0030] In the embodiment, the left end of the first three-way valve 7 is connected to the dissolution kettle liquid outlet 103 through a pipeline and is connected in series with a solenoid valve, an electronic flow meter and a solenoid pump, the upper end is connected to an acetyl chloride storage tank through a pipeline and is connected in series with a solenoid valve, an electronic flow meter and a solenoid pump, and the right end is connected to the tubular reactor liquid inlet 201 through a pipeline.

[0031] In the embodiment, the first three-way 7 is designed with a first PLC 5 and a second PLC 6 on the left side. The first PLC 5 is connected by data lines to the electronic flow meter at the left end of the first three-way, and to the electromagnetic valve, electronic flow meter and electromagnetic pump in series at the upper end of the first three-way, forming interlocking.

[0032] In the embodiment, the left end of the second three-way 8 is connected by a pipeline to the liquid inlet 401 of the outer steam crystallization kettle and is connected in series with a valve, an electronic flow meter and a transfer pump. The upper end is connected by a pipeline to the liquid outlet 303 of the hydrolysis separation kettle and is connected in series with a valve. The right end is connected by a pipeline to the brine storage tank and is connected in series with a valve and a transfer pump.

[0033] In the embodiment, the upper end of the third three-way 9 is connected by a pipeline to the outer steam liquid collection tank and is connected in series with a valve and a vacuum pump. The lower end is connected by a pipeline to the gas outlet 402 of the outer steam crystallization kettle. The right end is connected by a pipeline to the ethanol storage tank and is connected in series with a valve, an electronic flow meter and a transfer pump.

[0034] In the embodiment, the dissolution kettle 1, the hydrolysis separation kettle 3 or the outer steam crystallization kettle 4 is connected in parallel according to actual needs, and N≥2.

[0035] Main raw material equipment specifications:

[0036] The dissolution kettle and the outer steam crystallization kettle are both 5000L enamel kettles, and 2 are connected in parallel.

[0037] The hydrolysis separation kettle is a 3000L enamel kettle, and the column diameter ratio is 3:1, and 4 are connected in parallel.

[0038] The inner diameter of the tubular reactor is 10cm, and the length is 150m.

[0039] Naphthalene, nitrobenzene and aluminum chloride are industrial grade; acetyl chloride is self-produced by the company, and the purity is >99.5%.

[0040] PLC parameter setting:

[0041] According to the content of naphthalene in the dissolution kettle and the real-time flow rate of the electronic flow meter at the left end of the first three-way, the flow rate of acetyl chloride with the same molar amount of naphthalene is calculated, the electromagnetic valve and the electromagnetic pump at the upper end of the first three-way are operated by the first PLC interlocking control, and the real-time monitoring is performed by the electronic flow meter at the upper end of the first three-way.

[0042] According to the real-time flow rate of the electronic flow meter at the left end of the first three-way, the water inlet flow rate of the constant temperature heat exchanger 203 is controlled, and the flow rate ratio is 1:1. The electromagnetic valve and the electromagnetic pump connected in series with the water inlet 2031 of the constant temperature heat exchanger are operated by the second PLC interlocking control, and the real-time monitoring is performed by the electronic flow meter connected in series with the water inlet 2031 of the constant temperature heat exchanger. Embodiment

[0043] Step 1: open the corresponding valve, pump 3000 kg of nitrobenzene into the dissolving kettle 1 through the liquid inlet 102 of the dissolving kettle, start stirring, and sequentially add 1000 kg of naphthalene and 1300 kg of aluminum chloride from the solid inlet 101 of the dissolving kettle, control the temperature in the kettle to 30-50℃ through the first constant temperature heat exchanger 104, and stir until the solids are completely dissolved. The same operation is performed on the parallel dissolving kettle.

[0044] Step 2: the tube-shell constant temperature heat exchanger 203 of the tubular reactor 2 is filled with cooling water of a certain temperature in advance. Open the valve, and the material in the dissolving kettle 1 is pumped out from the outlet 103 through the first three-way valve 7 and into the tubular reactor 2 through the liquid inlet 201 of the tubular reactor; at the same time, the first PLC 5 controls the corresponding electromagnetic valve and electromagnetic pump according to the set parameters to mix the acetyl chloride with the material at a certain flow rate through the first three-way valve 7 and into the tubular reactor 2 through the liquid inlet 201 of the tubular reactor; the second PLC 6 controls the corresponding electromagnetic valve and electromagnetic pump according to the set parameters to pump the cooling water at a certain flow rate into the tube-shell constant temperature heat exchanger 203 through the water inlet 2031 of the tube-shell constant temperature heat exchanger.

[0045] Step 3: after a certain period of time, the material starts to flow out from the liquid outlet 202 of the tubular reactor, the corresponding valves and transfer pumps are opened and closed, and the material is pumped into the hydrolysis separation kettle 3 through the liquid inlet 301 of the hydrolysis separation kettle. After enrichment to a certain amount, the material is pumped into other parallel hydrolysis separation kettles by controlling the valve. Start stirring, pump a certain amount of dilute hydrochloric acid into the hydrolysis separation kettle through the acid inlet 302, control the temperature in the hydrolysis separation kettle 3 to 20-50℃ through the second constant temperature heat exchanger 304, and after hydrolysis is completed, stop stirring and let it stand to separate.

[0046] Step 4: by controlling the valve connected with the second three-way 8, the lower organic phase in the hydrolysis separation kettle 3 is transferred into the external steam crystallization kettle 4 through the liquid inlet 401 of the external steam crystallization kettle, and the upper aqueous phase is transferred into the brine storage tank for treatment and reuse. The corresponding valves and vacuum pumps connected with the third three-way 9 are opened, the heat source is provided by the third constant temperature heat exchanger 404, the negative pressure external steam nitrobenzene enters the external steam collection tank through the gas outlet 402 of the external steam crystallization kettle, and is recycled; the third constant temperature heat exchanger 404 is cooled, and when the temperature in the external steam crystallization kettle 4 is lower than 40℃, the corresponding valves connected with the third three-way 9 are opened and the transfer pump is started, a certain amount of anhydrous ethanol is pumped into the external steam crystallization kettle 4 through the gas outlet 402, the stirring is started, and after the material in the kettle is completely dissolved, the third constant temperature heat exchanger 404 is continuously cooled to-10~10℃, the product is precipitated in large amount, the liquid in the kettle is filtered and recovered through the discharge port 403 of the external steam crystallization kettle, the remaining solid in the kettle is washed and filtered at low temperature by adding a small amount of anhydrous ethanol through the gas outlet 402, the corresponding valves connected with the third three-way 9 are opened again, and the vacuum pump is started, the heat source is provided by the third constant temperature heat exchanger 404, the remaining solid in the kettle is dried under negative pressure, and is discharged from the discharge port 403, so that the purity of β-acetylnaphthalene is more than 99%.

[0047] The above describes the preferred embodiments of the present application, and for those skilled in the art, according to the teaching of the present application, the changes, modifications, replacements and variations of the embodiments without departing from the principles and spirits of the present application still fall within the protection scope of the present application.

Claims

1. A production apparatus for β-acetylnaphthalene, characterized in that, include: The dissolving vessel (1), tubular reactor (2), hydrolysis separation vessel (3), and external evaporation crystallization vessel (4) are provided. The top of the dissolving vessel (1) is provided with a solid feed inlet (101) and a liquid inlet (102), and the bottom is provided with a liquid outlet (103). The outer wall is provided with a first constant temperature heat exchanger (104). The solid feed inlet (101) of the dissolving vessel is connected to a solid feeder and a valve in series through a pipeline. The liquid inlet (102) of the dissolving vessel is connected to a solvent storage tank and a valve, an electronic flow meter, and a transfer pump in series through a pipeline. The liquid outlet (103) of the dissolving vessel is connected to the tubular reactor (2) and the acetyl chloride storage tank respectively through a first tee (7). The tubular reactor (2) has a tubular reactor inlet (201) at one end and a tubular reactor outlet (202) at the other end. The outer wall is fitted with a shell-and-tube constant temperature heat exchanger (203). The shell-and-tube constant temperature heat exchanger (2031) is connected to the circulating water inlet pipe and connected in series with a solenoid valve, an electronic flow meter and a solenoid pump. The shell-and-tube constant temperature heat exchanger outlet (2032) is connected to the circulating water return pipe and connected in series with a valve. The hydrolysis separator (3) is provided with a hydrolysis separator inlet (301) and a hydrolysis separator acid inlet (302) at the top and a hydrolysis separator outlet (303) at the bottom. The outer wall is provided with a second constant temperature heat exchanger (304). The hydrolysis separator inlet (301) is connected to the tubular reactor outlet (202) through a pipeline and connected in series with a valve, an electronic flow meter and a transfer pump. The hydrolysis separator acid inlet (302) is connected to the hydrochloric acid storage tank through a pipeline and connected in series with a valve, an electronic flow meter and a transfer pump. The hydrolysis separator outlet (303) is connected to the external evaporation crystallization vessel (4) and the brine storage tank through a second tee (8). The external evaporation crystallization vessel (4) is provided with an external evaporation crystallization vessel liquid inlet (401) and an external evaporation crystallization vessel gas outlet (402) at the top, an external evaporation crystallization vessel material outlet (403) at the bottom, and a third constant temperature heat exchanger (404) on the outer wall. The external evaporation crystallization vessel gas outlet (402) is connected to the external evaporation liquid collection tank and the ethanol storage tank respectively through the third tee (9).

2. The apparatus for producing β-acetylnaphthalene according to claim 1, characterized in that, The tubular reactor (2) is equipped with a spiral propulsion baffle inside the tube.

3. The apparatus for producing β-acetylnaphthalene according to claim 2, characterized in that, The tubular reactor (2) has an inner diameter of 5~10cm and a length of 50~200m.

4. The apparatus for producing β-acetylnaphthalene according to claim 3, characterized in that, The tubular reactor (2) has an inner diameter of 7 cm and a length of 100 m.

5. The apparatus for producing β-acetylnaphthalene according to claim 4, characterized in that, The diameter ratio of the hydrolysis separator (3) is (3~5):

1.

6. A production apparatus for β-acetylnaphthalene according to claim 1, 2, 3, 4, or 5, characterized in that, The left end of the first three-way valve (7) is connected to the outlet (103) of the dissolving vessel via a pipeline and is connected in series with a solenoid valve, an electronic flow meter and a solenoid pump. The upper end is connected to the acetyl chloride storage tank via a pipeline and is connected in series with a solenoid valve, an electronic flow meter and a solenoid pump. The right end is connected to the inlet (201) of the tubular reactor via a pipeline.

7. The apparatus for producing β-acetylnaphthalene according to claim 6, characterized in that, The left side of the first tee (7) is equipped with a first PLC (5) and a second PLC (6). The first PLC (5) is connected to the electronic flow meter at the left end of the first tee and the solenoid valve, electronic flow meter and solenoid pump connected in series at the upper end of the first tee via data lines to form an interlock. The second PLC (6) is connected to the electronic flow meter at the left end of the first tee and the solenoid valve, electronic flow meter and solenoid pump connected in series with the inlet (2031) of the constant temperature heat exchanger via data lines to form an interlock.

8. The apparatus for producing β-acetylnaphthalene according to claim 7, characterized in that, The left end of the second three-way valve (8) is connected to the inlet (401) of the external evaporation crystallizer via a pipeline and connected in series with a valve, an electronic flow meter and a transfer pump. The upper end is connected to the outlet (303) of the hydrolysis separator via a pipeline and connected in series with a valve. The right end is connected to the brine storage tank via a pipeline and connected in series with a valve and a transfer pump.

9. The apparatus for producing β-acetylnaphthalene according to claim 8, characterized in that, The upper end of the third tee (9) is connected to the external evaporation liquid collection tank via a pipeline and connected in series with a valve and a vacuum pump. The lower end is connected to the outlet (402) of the external evaporation crystallization vessel via a pipeline. The right end is connected to the ethanol storage tank via a pipeline and connected in series with a valve, an electronic flow meter and a transfer pump.

10. The apparatus for producing β-acetylnaphthalene according to claim 9, characterized in that, The dissolving vessel (1), hydrolysis separator (3), or external evaporation crystallization vessel (4) are connected in parallel in N units as needed, where N≥2.

Images