CN210022090U - Device for producing pinacolone by continuous method - Google Patents

Device for producing pinacolone by continuous method Download PDF

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CN210022090U
CN210022090U CN201920423038.8U CN201920423038U CN210022090U CN 210022090 U CN210022090 U CN 210022090U CN 201920423038 U CN201920423038 U CN 201920423038U CN 210022090 U CN210022090 U CN 210022090U
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condensation
reactor
differential
separator
addition
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邱振中
汪美贞
***
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Hangzhou Zhongli Chemical Technology Co Ltd
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Hangzhou Zhongli Chemical Technology Co Ltd
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Abstract

The utility model discloses a device for producing pinacolone by a continuous method, which comprises an addition reactor, an addition circulating pump, a first differential reaction of condensation, a second differential reaction of condensation, a separator, a discharge pump, a pipeline and a self-control instrument, wherein the addition reactor is a reaction rectification device, and is sequentially a first liquid distributor, a cooler, a packing tower section, a gas-liquid separator and a reboiler from top to bottom, the second differential reactor of condensation is a tubular microchannel reaction heat exchanger which is provided with a plurality of transverse second differential reactor tube passes and a plurality of longitudinal second differential reactor shell passes, the utility model discloses a coupling technology of the addition reactor (tower reaction rectification) and the condensation reactor (tubular differential circulation reaction) and utilizes the hydrogen chloride of the byproduct of the condensation reaction as the raw material of the addition reaction, and the added hydrochloric acid is only used as the catalyst of the condensation reaction, the usage amount of the hydrochloric acid can be reduced by 50%, meanwhile, the reaction speed is accelerated, the product yield is improved, the original intermittent operation is converted into continuous automatic operation, the efficiency is improved, and the cost is saved.

Description

Device for producing pinacolone by continuous method
Technical Field
The utility model relates to a fine chemistry industry field, concretely relates to continuous process produces pinacolone's device.
Background
The pinacolone is methyl tert-butyl ketone with a molecular formula of C6H12O, is colorless liquid, has mint or camphor-like smell, can volatilize with water vapor, is dissolved in ethanol, diethyl ether and acetone, has the water solubility of 2.44% at 15 ℃, the relative density of 0.8012, the melting point of-49.8 ℃, the boiling point of 106 ℃, the refractive index of 1.3952 and the flash point of 12 ℃, and is inflammable and toxic.
Pinacolone is mainly used for producing triazole pesticides and plant growth regulators, such as triadimefon, paclobutrazol, uniconazole, metribuzin, benzyl chloride triadimenol, bitertadone, octoxazone, imazalil, paclobutrazol and the like, and is also used for herbicides and medical products.
The pinacolone is synthesized by a plurality of methods, and the rearrangement method takes pinacol as a raw material and is generated by dehydration rearrangement in an acidic environment, which has the defects that the source of the pinacol is difficult and the reaction conditions are harsh; the oxidation method takes 2, 3-dimethyl-2-butylene as a raw material, takes organic peroxy acid or hydrogen peroxide as an oxidant for oxidation, and then obtains pinacolone by rearrangement, and has the defects of limited source of the raw material 2, 3-dimethyl-2-butylene, harsh process conditions, long process flow and the like; the isoamylene method takes isoamylene as a raw material, firstly reacts with hydrochloric acid or sulfuric acid to generate tertiary amyl chloride, and then reacts with hydrated formaldehyde to generate pina.
The Chinese utility model patent application No. 99114409.0 discloses a new method for preparing pinacolone, which uses industrial isoamylene as raw material and adds phosphorus trichloride and isoamylene dropwise in acid medium to obtain an intermediate. And dripping formaldehyde solution into the intermediate under the reflux condition to perform condensation reaction to obtain pinacolone [ CN1286242A ]. The method has the defects that the problem of waste acid is still not solved, and the yield is low.
Plum brightening, yellow navy and the like in the patent of an adlay clean production process firstly drop sulfuric acid or phosphoric acid into hydrochloric acid to prepare mixed acid, then industrial isoamylene is taken as a raw material, isoamylene is dropped into the prepared mixed acid medium to prepare an intermediate, and the intermediate is added with paraformaldehyde in batches under the reflux condition to react to prepare pinacolone [ CN102557905A ], wherein the method has the defects that a large amount of inorganic acid is still used and a large amount of waste acid containing various impurities is generated.
The equipment using isoamylene as the raw material is intermittent production, generates a large amount of waste acid, causes pressure on the environment, and has low conversion rate of the raw material, large consumption of public works and high cost.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a device and technology of continuous method production pinacolone to solve the problem that proposes among the above-mentioned background art.
In order to achieve the above object, the utility model provides a following technical scheme:
a device for producing pinacolone by a continuous method comprises an addition reactor, an addition circulating pump, a first condensation differential reactor, a second condensation differential reactor, a separator, a discharge pump, a pipeline and a self-control instrument;
the addition reactor is a reaction rectifying device and sequentially comprises a first liquid distributor, a cooler, a packing tower section, a gas-liquid separator and a reboiler from top to bottom, wherein a gas outlet is formed in the top of the addition reactor and connected with hydrogen chloride absorption acid making equipment, a hydrochloric acid adding port is formed in the first liquid distributor, a cooling pipe is arranged in the cooler, two ends of the cooling pipe are respectively connected with a cooler water inlet and a cooler water outlet which are formed in a cooler shell, packing is arranged in the packing tower section, a second liquid distributor is arranged in the middle of the packing tower section, an isoamylene adding port is formed in the second liquid distributor, a gas inlet, a circulating liquid inlet and a material outlet are formed in the gas-liquid separator, a circulating liquid pipeline is arranged in the reboiler, and two ends of the circulating liquid pipeline are respectively connected with the circulating liquid inlet and the circulating liquid outlet formed in the bottom of the addition reactor;
the condensation second differential reactor is a tubular microchannel reaction heat exchanger and is provided with a plurality of transverse condensation second differential reactor tube passes and a plurality of longitudinal condensation second differential reactor shell passes, two ends of the condensation second differential reactor shell pass are respectively connected with a condensation second differential reactor cooling water inlet and a condensation second differential reactor cooling water outlet on two sides of the condensation second differential reactor, and two ends of the condensation second differential reactor tube pass are respectively connected with a condensation second differential reactor discharge port and a condensation second differential reactor feed port;
the top of the separator is provided with a separator feeding port, a separator gas outlet and a separator return port, and the bottom of the separator is provided with a separator discharging port;
the inlet of the addition circulating pump is connected with a circulating liquid outlet, and the outlet of the addition circulating pump is connected with a circulating liquid inlet; an inlet of the first condensation differential reactor is connected with a material outlet of the addition reactor, and an outlet of the first condensation differential reactor is connected with a material inlet of the second differential reactor; the discharge hole of the condensation second differential reactor is connected with the feed hole of the separator; the gas outlet of the separator is connected with the gas inlet of the addition reactor, the discharge port of the separator is connected with the inlet of the condensation first differential reactor and the inlet of the discharge pump, and the reflux port of the separator is connected with the outlet of the discharge pump; the outlet of the discharge pump is connected with the phase separator; the first condensation differential reactor and the discharge pump are both provided with a formaldehyde feeding port.
Preferably, the diameter of the tube side of the condensation second differential reactor is 9-110 mm, and the micro-channel ceramic filler is filled in the tube side of the condensation second differential reactor and has a diameter of 8-80 mm.
Preferably, the addition reactor and the condensation second differential reactor can be vertically or horizontally installed, the main bodies of the addition reactor and the condensation second differential reactor are made of one or more of titanium alloy, impregnated graphite, carbon steel and silicon carbide, and the shells of the addition reactor and the condensation second differential reactor are made of carbon steel.
Preferably, the top of the addition reactor is provided with a thermometer and a pressure gauge, the second liquid distributor is provided with a second liquid distributor temperature measuring port, and the gas-liquid separator is provided with a gas-liquid separator temperature measuring port.
Compared with the prior art, the utility model has the advantages of it is following:
(1) the production cost is low: the addition reaction temperature is high, so that hydrogen chloride gas released by the condensation reaction is fully utilized to react with isoamylene in a reaction rectifying device (an addition reactor), and the consumption of hydrochloric acid is reduced; because the continuous reaction saves the heating up by steam in the condensation reaction, the temperature of the addition reaction is high, the introduction of chilled water is avoided, the electric energy is saved, the reaction speed is accelerated, the material retention time is short, and the amount of side reaction products, namely tar, is reduced, so the operation cost is low;
(2) the production efficiency is high: the reaction rectification and circulation coupling continuous production are integrally formed, and a microchannel mechanism is adopted in a first differential reactor for condensation to achieve micron-grade material mixing and a second differential reactor for condensation, so that the reaction efficiency is greatly improved, and the conversion rate of raw materials isoamylene and formaldehyde is further improved;
(3) green and environment-friendly: as the closed cycle system that the byproduct hydrogen chloride generated by the condensation reaction is taken as the raw material of the addition reaction is fully utilized, the adding amount of the hydrochloric acid is reduced, and the hydrochloric acid is added only to prevent the unreacted isoamylene from escaping from the top of the addition reaction and to be taken as the catalyst of the condensation reaction; after the hydrochloric acid phase of the reaction product is recycled, dilute hydrochloric acid (the concentration is 18%) can be subjected to tar removal (microfiltration, hydrogen peroxide decolorization and activated carbon decolorization), and then is subjected to pressure-differential pressure analysis, dehydration and concentration to obtain 31% hydrochloric acid, so that the hydrochloric acid can be recycled.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic diagram of a structure of a middle addition reactor according to the present invention;
FIG. 3 is a schematic diagram of a second differential reactor for condensation according to the present invention;
fig. 4 is a schematic structural diagram of the separator of the present invention.
In the figure: 1-addition reactor, 2-addition circulating pump, 3-condensation first differential reactor, 4-condensation second differential reactor, 5-separator, 6-discharge pump, 101-gas outlet, 102-packing tower section, 103-isoamylene inlet, 104-cooler water inlet, 105-cooler, 106-hydrochloric acid inlet, 107-thermometer, 108-gas outlet, 109-pressure gauge, 110-first liquid distributor, 111-cooler water outlet, 112-cooling pipe, 113-second liquid distributor, 114-second liquid distributor temperature measuring port, 115-gas inlet, 116-material outlet, 117-gas-liquid separator, 118-circulating liquid pipeline, 119-circulating liquid outlet, 120-reboiler, 121-a circulating liquid inlet, 122-a gas-liquid separator temperature measuring port, 401-a condensation second differential reactor discharge port, 402-a condensation second differential reactor feed port, 403-a condensation second differential reactor shell pass, 404-a condensation second differential reactor tube pass, 405-a condensation second differential reactor cooling water inlet, 406-a condensation second differential reactor cooling water outlet, 501-a separator gas outlet, 502-a separator feed port, 503-a separator return port, and 504-a separator discharge port.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to fig. 1-4, a continuous method for producing pinacolone comprises an addition reactor 1, an addition circulation pump 2, a first differential condensation reactor 3, a second differential condensation reactor 4, a separator 5, a discharge pump 6, a pipeline and a self-control instrument;
the addition reactor 1 is a reaction rectifying device and sequentially comprises a first liquid distributor 110, a cooler 105, a packing tower section 102, a gas-liquid separator 117 and a reboiler 120 from top to bottom, the top of the addition reactor 1 is provided with a gas outlet 108, the gas outlet 108 is connected with hydrogen chloride absorption acid making equipment, a hydrochloric acid adding port 106 is arranged on a first liquid distributor 110, a cooling pipe 112 is arranged in a cooler 105, two ends of the cooling pipe 112 are respectively connected with a cooler water inlet 104 and a cooler water outlet 111 which are arranged on a shell of the cooler 105, a filler is arranged in a filler tower section 102, a second liquid distributor 113 is arranged in the middle of the reaction kettle, an isoamylene adding port 103 is arranged on the second liquid distributor 113, a gas-liquid separator 115 is arranged on the gas-liquid separator 117, a circulating liquid inlet 121 and a material outlet 116 are arranged on the gas-liquid separator, a circulating liquid pipeline 118 is arranged in the reboiler 120, and two ends of the circulating liquid pipeline 118 are respectively connected with the circulating liquid inlet 121 and the circulating liquid outlet 119 arranged at the bottom of the addition reactor 1;
the condensation second differential reactor 4 is a tubular microchannel reaction heat exchanger and is provided with a plurality of transverse condensation second differential reactor tube passes 403 and a plurality of longitudinal condensation second differential reactor shell passes 404, two ends of the condensation second differential reactor shell passes 404 are respectively connected with a condensation second differential reactor cooling water inlet 405 and a condensation second differential reactor cooling water outlet 406 on two sides of the condensation second differential reactor, and two ends of the condensation second differential reactor tube passes 405 are respectively connected with a condensation second differential reactor discharge port 401 and a condensation second differential reactor feed port 402;
the top of the separator 5 is provided with a separator feeding port 502, a separator air outlet 501 and a separator return port 503, and the bottom is provided with a separator discharging port 504;
the inlet of the addition circulation pump 2 is connected with a circulation liquid outlet 119, and the outlet of the addition circulation pump 2 is connected with a circulation liquid inlet 121; the inlet of the first condensation differential reactor 3 is connected with the material outlet 116 of the addition reactor 1, and the outlet of the first condensation differential reactor 3 is connected with the material inlet 402 of the second differential reactor; the discharge port 401 of the condensation second differential reactor is connected with the feed port 502 of the separator; the gas outlet 501 of the separator is connected with the gas inlet 115 of the addition reactor 1, the discharge outlet 504 of the separator is connected with the inlet of the condensation first differential reactor 3 and the inlet of the discharge pump 6, and the reflux inlet 503 of the separator is connected with the outlet of the discharge pump 6; the outlet of the discharge pump 6 is connected with a phase splitter; the first condensation differential reactor 3 and the discharge pump 6 are both provided with a formaldehyde feeding port.
The diameter of the tube pass 404 of the condensation second differential reactor is 9-110 mm, and a micro-channel ceramic filler is filled in the tube pass, wherein the diameter of the micro-channel ceramic filler is 8-80 mm.
The addition reactor 1 and the condensation second differential reactor 4 can be vertically or horizontally installed, the main bodies of the addition reactor and the condensation second differential reactor are made of one or more of titanium alloy, impregnated graphite, carbon steel and silicon carbide, and the shells of the addition reactor 1 and the condensation second differential reactor 4 are made of carbon steel.
Wherein, the top of the addition reactor 1 is provided with a thermometer 107 and a pressure gauge 107, the second liquid distributor 113 is provided with a second liquid distributor temperature measurement port 114, and the gas-liquid separator 117 is provided with a gas-liquid separator temperature measurement port 122.
The first embodiment is as follows:
step 1: adding 31% of hydrochloric acid into a first liquid distributor 110 arranged in the addition reactor 1 from a hydrochloric acid adding port 106 at the top of the addition reactor 1, enabling the hydrochloric acid to enter a packing tower section 102 of the addition reactor 1 from top to bottom through a cooler 105, enabling isoamylene serving as a raw material to enter a second liquid distributor 113 from a middle isoamylene adding port 103, enabling the 31% of hydrochloric acid to be added in an amount which is 2 times of the mass ratio of the added isoamylene, enabling the hydrochloric acid to be in countercurrent contact with hydrogen chloride (discharged by condensation reaction) gas entering from a gas inlet 115 of a gas-liquid separator 117 at the lower part of the addition reactor 1 to generate chemical reaction (the reaction temperature is 0 ℃ and the reaction pressure is 80KPa), enabling the raw material and products after the chemical reaction to enter a reboiler 120 at the bottom of the addition reactor 1 to be heated by circulating water, controlling the temperature of the gas-liquid separator 117 to be 50 ℃ and mixing the gas-liquid separator 2 to prevent the organic phase and the hydrochloric acid solution from being layered, and enabling the hydrochloric acid aqueous solution 3, part of the mixture enters a discharge port pipeline of the separator;
step 2: 36% formaldehyde solution enters an inlet of a first condensation differential reactor 3 to perform condensation reaction with materials from an addition reactor 1 in the first condensation differential reactor 3 (the addition amount of 36% formaldehyde is 1.152 times of the addition amount of isoamylene), and a part of materials in a separator 5 also enter the first condensation differential reactor 3;
and step 3: the material out of the first condensation differential reactor 3 enters a second condensation differential reactor 4 for chemical reaction (the reaction temperature is 50 ℃, and the reaction pressure is 10KPa), the material out of the second condensation differential reactor 4 enters a separator 5, and the heat of the chemical reaction during the reaction of the second condensation differential reactor 4 is cooled by cooling water in a shell pass 404 of the second differential reactor;
and 4, step 4: the material from the condensation second differential reactor 4 is subjected to gas-liquid separation in a separator 5, the separated hydrogen chloride gas is discharged from a gas outlet 501 of the separator and then enters a gas inlet 115 of an addition reactor 1, a part of the feed liquid in the separator 5 is discharged through a material outlet 504 of the separator and then enters a condensation first differential reactor 3 to continuously react with new formaldehyde and addition reaction materials, the other part of the feed liquid is partially circulated and partially discharged through a discharge pump 6, the discharge pump 6 pumps out the material under the condition that the density of the material in the separator 5 reaches 0.95, the material pumped out through the discharge pump 6 is cooled and then enters a phase separator, an organic phase is rectified, a hydrochloric acid phase is removed from waste hydrochloric acid, and pinacolone is recovered through distillation;
and 5: adding hydrogen chloride gas and isoamylene in an addition reactor 1 to perform addition reaction, cooling part of the hydrogen chloride gas in a cooler 105 at the top of the addition reactor 1, absorbing 31 percent hydrochloric acid to prepare 34 percent hydrochloric acid, and controlling the temperature of hydrochloric acid solution in the cooler 105 to be-10 ℃;
example two:
step 1: adding 31% of hydrochloric acid into a first liquid distributor 110 arranged in the addition reactor 1 from a hydrochloric acid adding port 106 at the top of the addition reactor 1, enabling the hydrochloric acid to enter a packing tower section 102 of the addition reactor 1 from top to bottom through a cooler 105, enabling isoamylene serving as a raw material to enter a second liquid distributor 113 from a middle isoamylene adding port 103, enabling the 31% of hydrochloric acid to be 5 times of the adding amount of the isoamylene, enabling the hydrochloric acid to be in countercurrent contact with hydrogen chloride (discharged by condensation reaction) gas entering from a gas inlet 115 of a gas-liquid separator 117 at the lower part of the addition reactor 1 to generate chemical reaction (the reaction temperature is 80 ℃ and the reaction pressure is 250KPa), enabling the raw material and products after the chemical reaction to enter a reboiler 120 at the bottom of the addition reactor 1 to be heated by circulating water, controlling the temperature of the gas-liquid separator 117 to be 50 ℃ and mixing the gas-liquid separator 2 to prevent the organic phase and the hydrochloric acid solution from being layered, and enabling the hydrochloric acid aqueous solution and the reaction products to enter a 3, part of the mixture enters a discharge port pipeline of the separator;
step 2: 36% formaldehyde solution enters an inlet of a first condensation differential reactor 3 to perform condensation reaction with materials from an addition reactor 1 in the first condensation differential reactor 3 (the addition amount of 36% formaldehyde is 1.5 times of the addition amount of isoamylene), and a part of the materials in a separator 5 also enter the first condensation differential reactor 3;
and step 3: the material out of the first condensation differential reactor 3 enters a second condensation differential reactor 4 for chemical reaction (the reaction temperature is 95 ℃ and the reaction pressure is 250KPa), the material out of the second condensation differential reactor 4 enters a separator 5, and the heat of the chemical reaction during the reaction of the second condensation differential reactor 4 is cooled by cooling water in a shell pass 404 of the second differential reactor;
and 4, step 4: the material from the condensation second differential reactor 4 is subjected to gas-liquid separation in a separator 5, the separated hydrogen chloride gas is discharged from a gas outlet 501 of the separator and then enters a gas inlet 115 of an addition reactor 1, a part of the feed liquid in the separator 5 is discharged through a material outlet 504 of the separator and then enters a condensation first differential reactor 3 to continuously react with new formaldehyde and addition reaction materials, the other part of the feed liquid is partially circulated and partially discharged through a discharge pump 6, the discharge pump 6 pumps out the material under the condition that the density of the material in the separator 5 reaches 1.15, the material pumped out through the discharge pump 6 is cooled and then enters a phase separator, an organic phase is rectified, a hydrochloric acid phase is removed of waste hydrochloric acid, and pinacolone is recovered through distillation;
and 5: adding hydrogen chloride gas and isoamylene in an addition reactor 1, cooling part of hydrogen chloride in a cooler 105 at the top of the addition reactor 1, absorbing 31% hydrochloric acid to prepare 36% hydrochloric acid, and controlling the temperature of hydrochloric acid solution in the cooler 105 to be 30 ℃;
example three:
step 1: adding 31% of hydrochloric acid into a first liquid distributor 110 arranged in the addition reactor 1 from a hydrochloric acid adding port 106 at the top of the addition reactor 1, enabling the raw material isoamylene to enter a packing tower section 102 of the addition reactor 1 from a middle isoamylene adding port 103, enabling the raw material isoamylene to enter a second liquid distributor 113 from a middle isoamylene adding port 103, enabling the adding amount of the 31% of hydrochloric acid to be 2.25 times of the adding amount mass ratio of the isoamylene, enabling the raw material to be in countercurrent contact with hydrogen chloride (discharged by condensation reaction) entering from a gas inlet 115 of a gas-liquid separator 117 at the lower part of the addition reactor 1 to generate chemical reaction (the reaction temperature is 50 ℃ and the reaction pressure is 170KPa), enabling the raw material and a product after the chemical reaction to enter a reboiler 120 at the bottom of the addition reactor 1 to be heated by circulating water, controlling the temperature of the gas-liquid separator 117 to be 50 ℃ and mixing the raw material and the gas-liquid separator 2 to prevent the organic phase and the hydrochloric acid solution from being layered, enabling the hydrochloric acid 3, part of the mixture enters a discharge port pipeline of the separator;
step 2: 36% formaldehyde solution enters an inlet of a first condensation differential reactor 3 to perform condensation reaction with materials from an addition reactor 1 in the first condensation differential reactor 3 (the addition amount of 36% formaldehyde is 1.3 times of the addition amount of isoamylene), and a part of the materials in a separator 5 also enter the first condensation differential reactor 3;
and step 3: the material out of the first condensation differential reactor 3 enters a second condensation differential reactor 4 for chemical reaction (the reaction temperature is 70 ℃, and the reaction pressure is 130KPa), the material out of the second condensation differential reactor 4 enters a separator 5, and the heat of the chemical reaction during the reaction of the second condensation differential reactor 4 is cooled by cooling water in a shell pass 404 of the second differential reactor;
and 4, step 4: the material from the condensation second differential reactor 4 is subjected to gas-liquid separation in a separator 5, the separated hydrogen chloride gas is discharged from a gas outlet 501 of the separator and then enters a gas inlet 115 of an addition reactor 1, a part of the feed liquid in the separator 5 is discharged through a material outlet 504 of the separator and then enters a condensation first differential reactor 3 to continuously react with new formaldehyde and addition reaction materials, the other part of the feed liquid is partially circulated and partially discharged through a discharge pump 6, the discharge pump 6 pumps out the material under the condition that the density of the material in the separator 5 reaches 1.05, the material pumped out through the discharge pump 6 is cooled and then enters a phase separator, an organic phase is rectified, a hydrochloric acid phase is removed of waste hydrochloric acid, and pinacolone is recovered through distillation;
and 5: adding hydrogen chloride gas and isoamylene in an addition reactor 1, cooling part of the hydrogen chloride gas in a cooler 105 at the top of the addition reactor 1, absorbing 31% hydrochloric acid to prepare 35% hydrochloric acid, and controlling the temperature of hydrochloric acid solution in the cooler 105 to be 10 ℃;
it is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (4)

1. The utility model provides a device of continuous method production pinacolone, includes addition reaction ware, addition circulating pump, the first differential reactor of condensation, condensation second differential reactor, separator, discharge pump and pipeline and automatic control instrument, its characterized in that:
the addition reactor is a reaction rectifying device and sequentially comprises a first liquid distributor, a cooler, a packing tower section, a gas-liquid separator and a reboiler from top to bottom, wherein a gas outlet is formed in the top of the addition reactor and connected with hydrogen chloride absorption acid making equipment, a hydrochloric acid adding port is formed in the first liquid distributor, a cooling pipe is arranged in the cooler, two ends of the cooling pipe are respectively connected with a cooler water inlet and a cooler water outlet which are formed in a cooler shell, packing is arranged in the packing tower section, a second liquid distributor is arranged in the middle of the packing tower section, an isoamylene adding port is formed in the second liquid distributor, a gas inlet, a circulating liquid inlet and a material outlet are formed in the gas-liquid separator, a circulating liquid pipeline is arranged in the reboiler, and two ends of the circulating liquid pipeline are respectively connected with the circulating liquid inlet and the circulating liquid outlet formed in the bottom of the addition reactor;
the condensation second differential reactor is a tubular microchannel reaction heat exchanger and is provided with a plurality of transverse condensation second differential reactor tube passes and a plurality of longitudinal condensation second differential reactor shell passes, two ends of the condensation second differential reactor shell pass are respectively connected with a condensation second differential reactor cooling water inlet and a condensation second differential reactor cooling water outlet on two sides of the condensation second differential reactor, and two ends of the condensation second differential reactor tube pass are respectively connected with a condensation second differential reactor discharge port and a condensation second differential reactor feed port;
the top of the separator is provided with a separator feeding port, a separator gas outlet and a separator return port, and the bottom of the separator is provided with a separator discharging port;
the inlet of the addition circulating pump is connected with a circulating liquid outlet, and the outlet of the addition circulating pump is connected with a circulating liquid inlet; an inlet of the first condensation differential reactor is connected with a material outlet of the addition reactor, and an outlet of the first condensation differential reactor is connected with a material inlet of the second differential reactor; the discharge hole of the condensation second differential reactor is connected with the feed hole of the separator; the gas outlet of the separator is connected with the gas inlet of the addition reactor, the discharge port of the separator is connected with the inlet of the condensation first differential reactor and the inlet of the discharge pump, and the reflux port of the separator is connected with the outlet of the discharge pump; the outlet of the discharge pump is connected with the phase separator; the first condensation differential reactor and the discharge pump are both provided with a formaldehyde feeding port.
2. The device for producing pinacolone by the continuous method according to claim 1 is characterized in that: the diameter of the tube pass of the condensation second differential reactor is 9-110 mm, and the micro-channel ceramic filler is filled in the condensation second differential reactor and has a diameter of 8-80 mm.
3. The device for producing pinacolone by the continuous method according to claim 1 is characterized in that: the addition reactor and the condensation second differential reactor can be vertically or horizontally arranged, the main bodies of the addition reactor and the condensation second differential reactor are made of one or more of titanium alloy, impregnated graphite, carbon steel and silicon carbide, and the shells of the addition reactor and the condensation second differential reactor are made of carbon steel.
4. The device for producing pinacolone by the continuous method according to claim 1 is characterized in that: the top of the addition reactor is provided with a thermometer and a pressure gauge, the second liquid distributor is provided with a second liquid distributor temperature measuring port, and the gas-liquid separator is provided with a gas-liquid separator temperature measuring port.
CN201920423038.8U 2019-04-01 2019-04-01 Device for producing pinacolone by continuous method Active CN210022090U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002977A (en) * 2019-04-01 2019-07-12 杭州众立化工科技有限公司 A kind of device and process of continuity method production pinacolone

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002977A (en) * 2019-04-01 2019-07-12 杭州众立化工科技有限公司 A kind of device and process of continuity method production pinacolone

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