CN113457577B - Raw material mixing and melting device for producing p-tert-butyl catechol and application method thereof - Google Patents
Raw material mixing and melting device for producing p-tert-butyl catechol and application method thereof Download PDFInfo
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- CN113457577B CN113457577B CN202110761889.5A CN202110761889A CN113457577B CN 113457577 B CN113457577 B CN 113457577B CN 202110761889 A CN202110761889 A CN 202110761889A CN 113457577 B CN113457577 B CN 113457577B
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- 238000002156 mixing Methods 0.000 title claims abstract description 140
- 238000002844 melting Methods 0.000 title claims abstract description 28
- 230000008018 melting Effects 0.000 title claims abstract description 28
- 239000002994 raw material Substances 0.000 title claims abstract description 21
- XESZUVZBAMCAEJ-UHFFFAOYSA-N 4-tert-butylcatechol Chemical compound CC(C)(C)C1=CC=C(O)C(O)=C1 XESZUVZBAMCAEJ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims abstract description 118
- 238000005273 aeration Methods 0.000 claims abstract description 105
- 238000010438 heat treatment Methods 0.000 claims abstract description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 153
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- 238000002347 injection Methods 0.000 claims description 5
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- 238000004519 manufacturing process Methods 0.000 abstract description 6
- JIGUICYYOYEXFS-UHFFFAOYSA-N 3-tert-butylbenzene-1,2-diol Chemical compound CC(C)(C)C1=CC=CC(O)=C1O JIGUICYYOYEXFS-UHFFFAOYSA-N 0.000 abstract description 5
- BJEMXPVDXFSROA-UHFFFAOYSA-N 3-butylbenzene-1,2-diol Chemical group CCCCC1=CC=CC(O)=C1O BJEMXPVDXFSROA-UHFFFAOYSA-N 0.000 abstract description 2
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- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/005—Fusing
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/11—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms
- C07C37/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms by addition reactions, i.e. reactions involving at least one carbon-to-carbon unsaturated bond
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Raw material mixing and melting device for producing p-tert-butyl catechol and a using method thereof belong to the technical field of tert-butyl catechol production equipment. The downside of mixing barrel (1) is provided with heating storehouse (9), is provided with aeration board (24) in mixing barrel (1), and aeration board (24) set up with the bottom interval of mixing barrel (1) to form aeration storehouse (7) in the bottom of mixing barrel (1), the top of mixing barrel (1) is closed through the apron, and air feeder's air inlet communicates with the top of mixing barrel (1) through the apron. The raw material mixing and melting device for producing the para-tertiary butyl catechol greatly increases the heating area of the para-catechol, so that the catechol is melted quickly, the melting speed of the catechol is greatly improved, the temperature uniformity in the mixing barrel can be ensured, and the temperature of the mixing barrel is controlled conveniently and accurately; the use method can ensure the rapid melting of the catechol, avoid the vaporization of the catechol and avoid the pollution to the environment.
Description
Technical Field
Raw material mixing and melting device for producing p-tert-butyl catechol and a using method thereof belong to the technical field of tert-butyl catechol production equipment.
Background
At present, the main production method of the p-tert-butyl catechol mostly adopts a catechol isobutylene method, and the catechol is an important fine chemical raw material and chemical intermediate, has wide application, can be used as a rubber hardening agent, an electroplating additive, a skin antiseptic bactericide, a hair dye, a photographic developer, a color illumination antioxidant, a fur dyeing color developing agent, paint and varnish anti-skinning agent, and is an important raw material of synthetic resin, tannic acid, pesticide carbosulfan, propoxur, medical berberine, epinephrine, spice vanillin, safrole, piperonal and the like.
The catechol has a melting point of 105℃and, in order to increase the reaction rate, it is usually necessary to melt the catechol and then to carry out the reaction. However, since it is solid, it is usually required to be placed in a container when the para-catechol is melted, but there are the following technical problems when melted in this way: 1) When catechol is heated by the container, only the part contacted with the container is melted fast, the catechol melting speed is very slow, and the energy consumption is very high; 2) Since catechol is melted at a very low rate, the temperature distribution in the container is very uneven before catechol is completely melted, resulting in difficulty in controlling the temperature in the container.
Disclosure of Invention
The invention aims to solve the technical problems that: the raw material mixing and melting device for producing the p-tert-butyl catechol, which can melt the p-catechol by hot gas sprayed into the mixing barrel, fully utilizes the heating heat and greatly improves the catechol melting speed, and the use method thereof are provided.
The technical scheme adopted for solving the technical problems is as follows: the raw material mixing and melting device for producing the p-tert-butyl catechol is characterized in that: including mixing drum, electric heat dish and air feeder, the downside of mixing drum is provided with the heating storehouse, is provided with the electric heat dish that is used for heating the mixing drum in the heating storehouse, is provided with the aeration board in the mixing drum, and the bottom interval setting of aeration board and mixing drum to form the aeration storehouse in the bottom of mixing drum, the top of mixing drum is closed through the apron, and air feeder's air inlet passes through the apron and communicates with the top of mixing drum, air feeder's gas outlet and aeration storehouse intercommunication.
Preferably, the aeration plate on be provided with a plurality of spouts gas cap, be provided with the mounting hole on the aeration plate, the top diameter of spouting gas cap is greater than the diameter of bottom to form sealing portion at spouting the top of gas cap, set up the aeration passageway on the gas cap, the air inlet and the aeration storehouse intercommunication of aeration passageway, the gas outlet setting of aeration passageway is at spouting gas cap lateral part, and when spouting gas cap upward movement, the aeration passageway communicates aeration storehouse and blending tank, is provided with the spring that promotes spouting gas cap downward movement between spouting gas cap and the aeration plate. The spring promotes the jet cap to move downwards to seal the mounting hole through the sealing part, avoid the molten catechol to flow into in the aeration storehouse through the mounting hole, can also promote the jet cap upward movement when reaching certain pressure in the aeration storehouse, avoid in the aeration process liquid catechol to flow into in the aeration storehouse through the mounting hole.
Preferably, the diameter of the upper end of the mounting hole is larger than the diameter of the lower end, an air guide part is formed at the upper end of the mounting hole, the diameter of the upper part of the air spraying cap is larger than the diameter of the lower part, an exhaust part matched with the air guide part is formed at the upper part of the air spraying cap, the air spraying cap is a cylinder with a closed upper end, an exhaust hole is formed in the exhaust part, the exhaust hole and an inner hole of the air spraying cap are spliced into an aeration channel, the exhaust hole is in an inclined shape gradually upwards along the direction close to the middle part of the air spraying cap, and an exhaust groove communicated with the exhaust hole is formed in the inner wall of the air guide part. The vent hole is inclined, so that when tiny leakage occurs between the sealing part and the aeration plate, a small amount of melted catechol can be prevented from entering the aeration bin through the vent hole.
Preferably, a labyrinth seal is arranged between the air-spraying cap and the aeration plate. The labyrinth seals between the aeration plate and the jet cap, further avoiding the entry of molten catechol into the aeration bin.
Preferably, the air supply device comprises a nitrogen tank and an air inlet pump, wherein the input port of the air inlet pump is communicated with the lower part of the nitrogen tank, the input port of the air inlet pump is communicated with the aeration bin, the top of the nitrogen tank is communicated with the mixing barrel through a cover plate, and an air return check valve is arranged between the nitrogen tank and the mixing barrel. The nitrogen in the nitrogen tank is pressurized through the air supply pump, so that the pressure in the aeration bin is enough, the nitrogen is guaranteed to be fully circulated, and further the heating of the nitrogen to catechol is guaranteed to be more sufficient.
Preferably, the device further comprises a jacket arranged around the mixing barrel, the heating bin is arranged on the lower side of the jacket, and the jacket is connected with the buffer device. Heating oil is filled in the jacket, the mixing barrel is kept at a stable temperature through the heating oil, and the heating disc can assist nitrogen to heat catechol, and the heating disc can heat the mixing barrel and the aeration bin through the jacket, so that the temperature in the mixing barrel is kept stable.
Preferably, a coil is arranged in the jacket, an air inlet of the coil is communicated with an air outlet of the air supply device, and an air outlet of the coil is communicated with the aeration bin. The coil pipe is arranged in the jacket, so that nitrogen entering the aeration bin can reach specified stability rapidly.
Preferably, the coil comprises an inner coil and an outer coil, the inner coil is arranged in the outer coil, the air outlet of the air supply device is simultaneously communicated with the air inlet of the inner coil and the air inlet of the outer coil, the air outlet of the inner coil and the air outlet of the outer coil are simultaneously communicated with the aeration bin, an inner air inlet valve is arranged between the air outlet of the air supply device and the air inlet of the inner coil, an outer air inlet valve is arranged between the air outlet of the air supply device and the air inlet of the outer coil, and an electric heating tube is arranged between the air outlet of the air supply device and the air inlet of the inner coil. The inner coil pipe and the outer coil pipe can respectively supply air to the aeration bin, when the mixing drum starts to be heated, nitrogen passing through the air supply device enters the aeration bin through the inner coil pipe, and the electric heating pipe heats the nitrogen at the moment, so that heating oil in the jacket can quickly reach the designated temperature, and the temperature in the mixing drum can quickly reach the designated temperature due to the fact that the inner coil pipe is arranged close to the inner wall of the mixing drum; when normal circulation, the aeration bin is supplied with air through the outer coil pipe, nitrogen can quickly reach the designated temperature through heating oil in the jacket, and the temperature influence on the mixing barrel is small because the outer coil pipe is far away from the outer wall of the mixing barrel, so that the temperature in the mixing barrel is maintained uniformly.
Preferably, the buffer device comprises a buffer tank, and the bottom of the buffer tank is communicated with the bottom of the jacket. The buffer tank can play a role in buffering, and when the heating volume of heating oil in the jacket is increased, redundant heating oil enters the buffer tank, so that the danger caused by the increase of the pressure in the jacket is avoided.
A method for using the raw material mixing and melting device for producing p-tert-butylcatechol, which is characterized in that: the method comprises the following steps:
step) putting catechol to be melted into a mixing barrel, and sealing a cover plate;
step) the air supply device supplies nitrogen into the aeration bin, so that the nitrogen flows back into the air supply device after passing through the aeration bin and the mixing drum in sequence;
step) the aeration bin is heated by an electric heating disc until the temperature of the nitrogen in the air supply device is maintained at a specified temperature.
Compared with the prior art, the invention has the following beneficial effects:
this raw materials mix melting device for production of tert-butyl catechol send into the aeration storehouse with nitrogen gas in, make nitrogen gas flow back to in the air feeder after aeration storehouse and blending tank in proper order, make nitrogen gas form the circulation, the electric heat dish can be to aeration storehouse heating, spout into in the blending tank through overheated air, heat catechol in the blending tank, the heating area of para-catechol has been greatly increased, make catechol melt fast, the melting rate of catechol has been improved greatly, because the existence of aeration board, can guarantee that the temperature in the blending tank is even, the temperature of convenient accurate control blending tank.
According to the application method, the catechol is heated by the nitrogen, so that the catechol is prevented from being oxidized, the catechol can be guaranteed to be melted quickly, the catechol can be prevented from being vaporized, and the environmental pollution is avoided.
Drawings
FIG. 1 is a schematic diagram showing the front view of a raw material mixing and melting apparatus for producing p-tert-butylcatechol.
Fig. 2 is a schematic front sectional view of an aeration plate.
Fig. 3 is a partial enlarged view at a in fig. 2.
Fig. 4 is a schematic perspective view of the recovery device.
Fig. 5 is a schematic front cross-sectional view of a nitrogen tank.
Fig. 6 is a left side cross-sectional schematic view of a mixing drum.
In the figure: 1. mixing tub 2, mounting beam 3, preheating bin 4, jacket 5, outer coil 6, inner coil 7, aeration bin 8, electrothermal disk 9, heating bin 10, electrothermal pipe 11, nitrogen tank 12, gas outlet valve 13, outer gas inlet pipe 14, inner gas inlet pipe 15, inner gas inlet valve 16, outer gas inlet valve 17, gas return pipe 18, gas return check valve 19, gas discharge pump 20, gas discharge pipe 21, gas discharge valve 22, circulation pipe 23, circulation valve 24, aeration plate 2401, mounting hole 2402, gas guide portion 3, gas discharge tank 25, gas injection cap 2501, turnup 2502, gas discharge portion 2503, sealing portion 2504, gas discharge hole 26, spring 27, labyrinth seal 28, electric heater 29, storage tank 30, circulation pump 31, heat exchanger 32, output valve 33, input check valve 34, liquid inlet valve 35, liquid discharge valve 36, buffer tank 37, diaphragm 38, gas inlet nozzle 39, collection net 40, transparent pipe.
Detailed Description
FIGS. 1-6 illustrate preferred embodiments of the present invention, and the present invention will be further described with reference to FIGS. 1-6.
The utility model provides a raw materials mixing melting device is used in production of tert-butyl catechol, including mixing drum 1, electrothermal disk 8 and air feeder, the downside of mixing drum 1 is provided with heating storehouse 9, be provided with the electrothermal disk 8 that is used for heating mixing drum 1 in the heating storehouse 9, be provided with aeration board 24 in the mixing drum 1, aeration board 24 and mixing drum 1's bottom interval set up, and form aeration storehouse 7 in mixing drum 1's bottom, the top of mixing drum 1 is closed through the apron, air feeder's air inlet is through apron and mixing drum 1's top intercommunication, air feeder's gas outlet and aeration storehouse 7 intercommunication. This raw materials mix melting device for production of tert-butyl catechol send nitrogen gas into aeration storehouse 7 in, make nitrogen gas flow back to air feeder behind aeration storehouse 7 and mixing drum 1 in proper order, make nitrogen gas form the circulation, electric heat dish 8 can heat aeration storehouse 7, spout into mixing drum 1 through overheated air in, the catechol in the mixing drum 1 heats, the heating area of para-catechol has been greatly increased, make the catechol melt fast, the melting rate of catechol has been improved greatly, because aeration board 24's existence, can guarantee that the temperature in the mixing drum 1 is even, the temperature of convenient accurate control mixing drum 1.
The present invention will be further described with reference to specific embodiments, however, it will be appreciated by those skilled in the art that the detailed description herein with reference to the accompanying drawings is for better illustration, and that the invention is not necessarily limited to such embodiments, but rather is intended to cover various equivalent alternatives or modifications, as may be readily apparent to those skilled in the art.
Specific: as shown in fig. 1: the mixing drum 1 is a cylinder with an open upper end, the top of the mixing drum 1 is provided with a mounting beam 2, the mounting beam 2 is arranged in the middle of the mixing drum 1, the upper side of the mounting beam 2 is provided with a preheating bin 3, the two sides of the preheating bin 3 are provided with cover plates, and the top of the mixing drum 1 can be closed through the cover plates on the two sides. When the catechol in the mixing drum 1 is heated, the catechol to be hot melted can be placed in the preheating bin 3, and the catechol is preheated through the preheating bin 3, so that the hot melting speed of the catechol is improved.
The bottom of the mixing drum 1 is provided with an aeration plate 24, the aeration plate 24 is arranged at intervals with the bottom of the mixing drum 1, and the side part of the aeration plate 24 is connected with the side part of the mixing drum 1 in a sealing way, and an aeration bin 7 is formed at the bottom of the mixing drum 1. A jacket 4 is provided around the side and bottom of the mixing tub 1, and heating oil is provided in the jacket 4. The bottom of the mixing barrel 1 is provided with a heating bin 9, the heating bin 9 is arranged on the lower side of the jacket 4, a heating disc 8 is arranged in the heating bin 9, heating oil in the jacket 4 is heated through the heating disc 8, and catechol in the mixing barrel 1 is heated through the jacket 4.
The coil pipe that encircles mixing drum 1 and sets up is provided with in the clamp cover 4, and the coil pipe includes interior coil pipe 6 and outer coil pipe 5, and interior coil pipe 6 sets up the inboard at outer coil pipe 5, and interior coil pipe 6 is close to mixing drum 1 inner wall setting, and outer coil pipe 5 is close to the outer wall setting of clamp cover 4. The air outlets of the inner coil pipe 6 and the outer coil pipe 5 are arranged at the bottom of the jacket 4 and are communicated with the aeration bin 7.
The air supply device comprises a nitrogen tank 11, an air inlet pump and an exhaust pump 19, wherein an air inlet of the air inlet pump is communicated with the lower part of the nitrogen tank 11, an air outlet of the air inlet pump is communicated with an air inlet of the inner coil 6 through an inner air inlet pipe 14, an inner air inlet valve 15 is arranged on the inner air inlet pipe 14, an air outlet of the air inlet pump is communicated with an air inlet of the outer coil 5 through an outer air inlet pipe 13, and an outer air inlet valve 16 is arranged on the outer air inlet pipe 13. An electric heating tube 10 is arranged outside the inner air inlet tube 14. When the heating of the mixing drum 1 is started, the electric heating plate 8 heats heating oil in the jacket 4, the aeration bin 7 is supplied with air through the inner coil 6, the electric heating pipe 10 can heat nitrogen entering the inner coil 6, the nitrogen can heat the heating oil in the jacket 4, and the inner coil 6 is close to the inner wall of the mixing drum 1, so that the mixing drum 1 can reach the designated temperature quickly. When the mixing drum works normally, the aeration bin 7 is supplied with air through the outer coil 5, and at the moment, the nitrogen entering the aeration bin 7 is heated by heating oil in the jacket 4, and the temperature in the mixing drum 1 is ensured to be low in fluctuation due to the fact that the outer coil 5 is arranged far away from the outer wall of the mixing drum 1.
The top of nitrogen jar 11 is connected with muffler 17, the gas outlet of muffler 17 is linked together with nitrogen jar 11, the air inlet of muffler 17 is connected with circulating pipe 22 and blast pipe 20 simultaneously, the air inlet of blast pipe 20 is linked together with the top of mixing drum 1 through the apron, the gas outlet of blast pipe 20 is linked together with the air inlet of muffler 17, be provided with discharge valve 21 on the blast pipe 20, discharge pump 19 installs on blast pipe 20, the air inlet of circulating pipe 22 is linked together with the top of mixing drum 1 through the apron, the gas outlet of circulating pipe 22 is linked together with the air inlet of muffler 17, be provided with circulation valve 23 on the circulating pipe 22. During normal circulation, nitrogen gas is introduced into the return pipe 17 through the circulation pipe 22, and is introduced into the nitrogen tank 11 through the return pipe 17. When it is necessary to exhaust the nitrogen gas in the mixing tub 1, the nitrogen gas in the mixing tub 1 is fed into the nitrogen tank 11 through the exhaust pipe 20.
An air outlet valve 12 is arranged between the air inlet of the air inlet pump and the lower part of the nitrogen tank 11, so that the on-off of the exhaust of the nitrogen tank 11 can be conveniently controlled. The return air pipe 17 is provided with a return air check valve 18, so that the nitrogen in the nitrogen tank 11 can be prevented from flowing back. The heat of the heating oil in the jacket 4 can also be recovered by nitrogen.
As shown in fig. 2 to 3: the aeration plate 24 is provided with a plurality of mounting holes 2401, and each mounting hole 2401 is provided with a mounting cap 25.
The mounting hole 2401 is a vertically disposed through hole, the diameter of the upper end of the mounting hole 2401 is larger than the diameter of the lower end, and an air guide portion 2402 is formed at the upper end of the mounting hole 2401. The gas spraying cap 25 is a cylinder with a closed upper end, the diameter of the upper end of the gas spraying cap 25 is larger than the diameter of the lower part, a sealing part 2503 is formed at the upper end of the gas spraying cap 25, the diameter of the upper part of the gas spraying cap 25 is larger than the diameter of the lower part and smaller than the diameter of the sealing part 2503, and an exhaust part 2502 matched with the gas guiding part 2402 is formed at the upper part of the gas spraying cap 25. The exhaust portion 2502 is provided with a plurality of exhaust holes 2504, the exhaust holes 2504 are inclined gradually upwards along the diameter direction close to the middle of the air injection cap 25, so that a small amount of melted catechol can be prevented from entering the air injection cap 25, and each exhaust hole 2504 and the inner cavity of the air injection cap 25 are surrounded to form an aeration channel. The inner wall of the air guide portion 2402 is provided with air discharge grooves 2403, the air discharge grooves 2403 are in one-to-one correspondence with the air discharge holes 2504, and the outer ends of the air discharge holes 2504 are communicated with the air discharge grooves 2403.
An outward flanging 2501 is arranged around the lower end of the air spraying cap 25, a spring 26 is sleeved outside the air spraying cap 25, the spring 26 is arranged between the flanging 2501 and the aeration plate 24 and pushes the air spraying cap 25 to move downwards, the air spraying cap 25 is pushed to move upwards only when the air pressure in the aeration bin 7 reaches a specified pressure, and nitrogen in the aeration bin 7 is enabled to enter the mixing drum 1, so that molten catechol is prevented from entering the aeration bin 7.
A plurality of downward annular bosses are provided at intervals from inside to outside on the lower end face of the sealing portion 2503, grooves which are fitted with the bosses are provided at the top of the aeration plate 24, and a labyrinth seal 27 is formed between the sealing portion 2503 and the aeration plate 24. A plurality of downward annular bosses are arranged at intervals on the shoulder part of the exhaust part 2502, a plurality of grooves matched with the bosses are arranged at the bottom of the air guide part 2402, and a labyrinth seal 27 is formed between the air guide part 2402 and the exhaust part 2502, so that secondary seal is formed, and molten catechol is prevented from leaking and entering the aeration bin 7.
As shown in fig. 4 to 5: catechol in the mixing drum 1 always mixes catechol steam in nitrogen gas when melting, and nitrogen gas jar 11 still is connected with catechol recovery device, and catechol recovery device includes electric heater 28, storage tank 29, circulating pump 30 and heat exchanger 31, and storage tank 29 sets up under nitrogen gas jar 11, and the bottom of nitrogen gas jar 11 is linked together through the top of pipeline with storage tank 29, and electric heater 28 sets up outside the pipeline between storage tank 29 and nitrogen gas jar 11 to make nitrogen gas maintain the temperature above 105 ℃, avoid catechol to solidify. An output valve 32 is provided between the storage tank 29 and the nitrogen tank 11. The air inlet of the circulating pump 30 is communicated with the top of the storage tank 29, the air outlet of the circulating pump 30 is communicated with the tube side inlet of the heat exchanger 31, the tube side outlet of the heat exchanger 31 is communicated with the top of the nitrogen tank 11, and an input check valve 33 is arranged between the tube side outlet of the heat exchanger 31 and the nitrogen tank 11. The shell side inlet of the heat exchanger 31 is provided with the liquid inlet valve 34, the shell side outlet of the heat exchanger 31 is provided with the liquid discharge valve 35, heat in nitrogen can be recovered after the catechol is melted by heat through the heat exchanger, heat loss is avoided, catechol can be recovered before recovery, and the catechol is prevented from being solidified in a pipeline to block the pipeline.
The nitrogen tank 11 is internally provided with the trapping net 39, the trapping net 39 is tapered with gradually reduced diameter from top to bottom, and the trapping net can trap catechol steam entering the nitrogen tank 11 and condense the catechol steam into liquid, so that the catechol steam is convenient to recycle.
As shown in fig. 6: the jacket 4 is also connected with a buffer device, the buffer device comprises a buffer tank 36, the bottom of the buffer tank 36 is communicated with the bottom of the jacket 4, a diaphragm 37 is arranged in the buffer tank 36, the diaphragm 37 is an elastic membrane, the diaphragm 37 is arranged in the middle of the buffer tank 36 and divides the buffer tank 36 into an air pressure bin at the top and a hydraulic bin at the bottom, the top of the buffer tank 36 is provided with an air charging nozzle 38, the pressure in the air pressure bin can be regulated through the air charging nozzle 38, and then the liquid level of heating oil in the jacket 4 is controlled. A vertical transparent pipe 40 is arranged at the outer side of the jacket 4, the upper end of the transparent pipe 40 is communicated with the top of the jacket 4, and the lower end of the transparent pipe 40 is communicated with the bottom of the jacket 4, so that the liquid level of hydraulic oil in the jacket 4 is accurately controlled, and the liquid level of the jacket 4 is controlled according to the amount of hot-melted catechol.
The application method of the raw material mixing and melting device for producing the para-tertiary butyl catechol comprises the following steps:
step 1) catechol to be melted is put into a mixing tub 1 and a cover plate is closed.
Catechol to be melted was put into the mixing tub 1, and the top of the mixing tub 1 was closed by a cover plate. And simultaneously catechol is added into the preheating bin 3 for preheating.
Step 2) the air supply device supplies nitrogen into the aeration bin 7, so that the nitrogen flows back into the air supply device after passing through the aeration bin 7 and the mixing drum 1 in sequence.
The air inlet pump is started, the inner air inlet valve 15 is opened, at the moment, nitrogen enters the aeration bin 7 through the inner coil pipe 6, the electric heating pipe 10 heats the nitrogen entering the inner coil pipe 6, and heats heating oil in the jacket 4 through the nitrogen, the inner coil pipe 6 is arranged close to the mixing drum 1 and heats the mixing drum 1, the heated nitrogen enters the aeration bin 7, and enters the mixing drum 1 through the aeration plate 24 and heats the mixing drum 1.
And 3) heating the aeration bin 7 through the electric heating disc 8 until the temperature of the nitrogen in the air supply device is maintained at the specified temperature.
When the temperature in the mixing barrel 1 reaches 150-180 ℃, the inner air inlet valve 15 is closed, the outer air inlet valve 16 is opened, the electric heating tube 10 is powered off, nitrogen is fed into the aeration bin 7 through the outer coil 5, and the heating oil in the jacket 4 heats the nitrogen in the outer coil 5, so that the temperature fluctuation in the mixing barrel 1 can be avoided, and the temperature in the mixing barrel 1 is constant and uniform due to the fact that the outer coil 5 is far away from the mixing barrel 1.
After catechol is melted, tertiary butanol is added into a mixing drum 1, and inorganic acid and salt are added as catalysts to react.
The solvent can be directly added into the mixing tank 1, and at the moment, the temperature of the mixing tank 1 can be adjusted through the inner coil 6 and the outer coil 5 by the jacket 4 so as to maintain the reaction at a proper temperature, and the aeration plate 24 can also play a role in stirring the materials in the mixing tank 1.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (6)
1. Raw materials mixing and melting device for producing p-tert-butyl catechol is characterized in that: the device comprises a mixing barrel (1), an electric heating plate (8) and an air supply device, wherein the top of the mixing barrel (1) is provided with a mounting beam (2), the upper side of the mounting beam (2) is provided with a preheating bin (3), the lower side of the mixing barrel (1) is provided with a heating bin (9), the heating bin (9) is internally provided with the electric heating plate (8) for heating the mixing barrel (1), the mixing barrel (1) is internally provided with an aeration plate (24), the aeration plate (24) is arranged at intervals with the bottom of the mixing barrel (1), an aeration bin (7) is formed at the bottom of the mixing barrel (1), the top of the mixing barrel (1) is sealed by a cover plate, an air inlet of the air supply device is communicated with the top of the mixing barrel (1) by the cover plate, and an air outlet of the air supply device is communicated with the aeration bin (7);
the mixing device also comprises a jacket (4) arranged around the mixing barrel (1), a heating bin (9) is arranged at the lower side of the jacket (4), and the jacket (4) is connected with a buffer device; a coil pipe is arranged in the jacket (4), an air inlet of the coil pipe is communicated with an air outlet of the air supply device, and the air outlet of the coil pipe is communicated with the aeration bin (7);
the air supply device comprises a nitrogen tank (11) and an air inlet pump, wherein an input port of the air inlet pump is communicated with the lower part of the nitrogen tank (11), an input port of the air inlet pump is communicated with the aeration bin (7), the top of the nitrogen tank (11) is communicated with the mixing barrel (1) through a cover plate, and an air return check valve (18) is arranged between the nitrogen tank (11) and the mixing barrel (1);
the nitrogen tank (11) is also connected with a catechol recovery device, the catechol recovery device comprises an electric heater (28), a storage tank (29), a circulating pump (30) and a heat exchanger (31), the storage tank (29) is arranged right below the nitrogen tank (11), the bottom of the nitrogen tank (11) is communicated with the top of the storage tank (29) through a pipeline, the electric heater (28) is arranged outside a pipeline between the storage tank (29) and the nitrogen tank (11) and is used for keeping the temperature of nitrogen above 105 ℃, an air inlet of the circulating pump (30) is communicated with the top of the storage tank (29), an air outlet of the circulating pump (30) is communicated with a tube side inlet of the heat exchanger (31), and a tube side outlet of the heat exchanger (31) is communicated with the top of the nitrogen tank (11);
the coil pipe include interior coil pipe (6) and outer coil pipe (5), interior coil pipe (6) set up in outer coil pipe (5), air feeder's gas outlet is linked together with the air inlet of interior coil pipe (6) and the air inlet of outer coil pipe (5) simultaneously, the gas outlet of interior coil pipe (6) and the gas outlet of outer coil pipe (5) are linked together with aeration bin (7) simultaneously, and be provided with interior admission valve (15) between air feeder's gas outlet and the air inlet of interior coil pipe (6), be provided with outer admission valve (16) between air feeder's gas outlet and the air inlet of outer coil pipe (5), and be provided with electrothermal tube (10) between air feeder's gas outlet and the air inlet of interior coil pipe (6).
2. The raw material mixing and melting device for producing p-tert-butylcatechol according to claim 1, wherein: the utility model provides an aeration equipment, aeration board (24) on be provided with a plurality of spouts gas cap (25), be provided with mounting hole (2401) on aeration board (24), the top diameter of spouting gas cap (25) is greater than the diameter of bottom to form sealing (2503) at the top of spouting gas cap (25), set up the aeration passageway on spouting gas cap (25), aeration passageway's air inlet and aeration bin (7) intercommunication, aeration passageway's gas outlet sets up in spouting gas cap (25) lateral part, and when spouting gas cap (25) upward movement, aeration passageway communicates aeration bin (7) and mixing drum (1), be provided with between spouting gas cap (25) and aeration board (24) and promote spring (26) of spouting gas cap (25) downward movement.
3. The raw material mixing and melting device for producing p-tert-butylcatechol according to claim 2, wherein: the diameter of the upper end of the mounting hole (2401) is larger than that of the lower end, an air guide part (2402) is formed at the upper end of the mounting hole (2401), the diameter of the upper part of the air guide cap (25) is larger than that of the lower part, an exhaust part (2502) matched with the air guide part (2402) is formed at the upper part of the air guide cap (25), the air guide cap (25) is a cylinder with a closed upper end, an exhaust hole (2504) is formed in the exhaust part (2502), the exhaust hole (2504) and an inner hole of the air guide cap (25) are spliced to form an aeration channel, the exhaust hole (2504) is in an inclined shape gradually upwards along the direction close to the middle part of the air guide cap (25), and an exhaust groove (2403) communicated with the exhaust hole (2504) is formed in the inner wall of the air guide part (2402).
4. The raw material mixing and melting device for producing p-tert-butylcatechol according to claim 2 or 3, wherein: a labyrinth seal is arranged between the air injection cap (25) and the aeration plate (24).
5. The raw material mixing and melting device for producing p-tert-butylcatechol according to claim 1, wherein: the buffering device comprises a buffering tank (36), and the bottom of the buffering tank (36) is communicated with the bottom of the jacket (4).
6. A method for using the raw material mixing and melting device for producing p-tert-butylcatechol according to any one of claims 1 to 5, wherein: the method comprises the following steps:
step 1) putting catechol to be melted into a mixing barrel (1), and sealing a cover plate;
putting catechol to be melted into a mixing barrel (1), sealing the top of the mixing barrel (1) through a cover plate, and simultaneously adding catechol into a preheating bin (3) for preheating;
step 2), the air supply device supplies nitrogen into the aeration bin (7), so that the nitrogen flows back into the air supply device after passing through the aeration bin (7) and the mixing drum (1) in sequence;
starting an air inlet pump, opening an inner air inlet valve (15), enabling nitrogen to enter an aeration bin (7) through an inner coil pipe (6), heating the nitrogen entering the inner coil pipe (6) through an electric heating pipe (10), heating oil in a jacket (4) through the nitrogen, enabling the inner coil pipe (6) to be close to a mixing barrel (1) and heating the mixing barrel (1), enabling the heated nitrogen to enter the aeration bin (7), and enabling the heated nitrogen to enter the mixing barrel (1) through an aeration plate (24);
step 3) heating the aeration bin (7) through the electric heating disc (8) until the temperature of the nitrogen in the air supply device is maintained at a specified temperature;
when the temperature in the mixing barrel (1) reaches 150-180 ℃, the inner air inlet valve (15) is closed, the outer air inlet valve (16) is opened, the electric heating tube (10) is powered off, nitrogen is fed into the aeration bin (7) through the outer coil pipe (5), heating oil in the jacket (4) heats the nitrogen in the outer coil pipe (5), and the outer coil pipe (5) is far away from the mixing barrel (1), so that temperature fluctuation in the mixing barrel (1) can be avoided, and the temperature in the mixing barrel (1) is constant and uniform;
after catechol is melted, tertiary butanol is added into a mixing barrel (1), and inorganic acid and salt are added as catalysts to react;
the solvent is directly added into the mixing tank (1), and at the moment, the temperature of the mixing tank (1) is regulated by the inner coil (6) and the outer coil (5) through the jacket (4) so as to maintain the reaction at a proper temperature, and the stirring effect on the materials in the mixing tank (1) is achieved through the aeration plate (24).
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