CN211546371U - Continuous hydrolysis device for 2,4,6 trimethyl benzoic acid acylation liquid - Google Patents
Continuous hydrolysis device for 2,4,6 trimethyl benzoic acid acylation liquid Download PDFInfo
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- CN211546371U CN211546371U CN202020128934.4U CN202020128934U CN211546371U CN 211546371 U CN211546371 U CN 211546371U CN 202020128934 U CN202020128934 U CN 202020128934U CN 211546371 U CN211546371 U CN 211546371U
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 158
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 145
- 239000007788 liquid Substances 0.000 title claims abstract description 48
- 238000005917 acylation reaction Methods 0.000 title claims abstract description 39
- FFFIRKXTFQCCKJ-UHFFFAOYSA-N 2,4,6-trimethylbenzoic acid Chemical compound CC1=CC(C)=C(C(O)=O)C(C)=C1 FFFIRKXTFQCCKJ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 230000010933 acylation Effects 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000005406 washing Methods 0.000 claims abstract description 64
- 238000000926 separation method Methods 0.000 claims abstract description 28
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 20
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 abstract description 32
- 230000000694 effects Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 29
- 239000000463 material Substances 0.000 description 20
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 16
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 16
- 239000012295 chemical reaction liquid Substances 0.000 description 15
- 239000011259 mixed solution Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 239000012074 organic phase Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 239000012071 phase Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- UKRQMDIFLKHCRO-UHFFFAOYSA-N 2,4,6-trimethylbenzoyl chloride Chemical compound CC1=CC(C)=C(C(Cl)=O)C(C)=C1 UKRQMDIFLKHCRO-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 125000002252 acyl group Chemical group 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229940093503 ethyl maltol Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000000066 reactive distillation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a continuous hydrolysis device for producing acylation liquid of 2,4,6 trimethyl benzoic acid by acylation reaction, which comprises a mixer, a first hydrolysis kettle, a second hydrolysis kettle, a hydrolysis separation tank, a water washing tank and a separator; the lower end of the mixer is connected with the first hydrolysis kettle through a pipeline, and the outlet of the first hydrolysis kettle is connected with the feed liquid inlet of the second hydrolysis kettle through a pipeline; the feed liquid outlet of the second hydrolysis kettle is connected with the feed liquid inlet of the hydrolysis separation tank through a pipeline; a feed liquid outlet of the hydrolysis separation tank is respectively connected with a feed liquid inlet of the aluminum trichloride solution storage tank and a feed liquid inlet of the washing tank through pipelines; the outlet of the washing tank is connected with the feed liquid inlet of the separator through a pipeline; the outlet of the separator is respectively connected with a crude product collecting tank and a washing water collecting tank through pipelines. The device can carry out continuous hydrolysis, continuous feeding and continuous discharging; the separation effect is good; the efficiency is high, and the yield is high; stable product quality, high quality product rate and the like.
Description
Technical Field
The utility model belongs to the chemical products field relates to the apparatus for producing of 2,4,6 trimethyl benzoyl chloride, concretely relates to continuous hydrolysis unit of acylation reaction production 2,4,6 trimethyl benzoic acid's acylation liquid.
Background
The production of 2,4,6 trimethyl benzoyl chloride is carried out by two steps of acylation and acyl chlorination, the acylation is a chemical reaction carried out under the catalysis of anhydrous aluminum trichloride, and the reaction liquid after the acylation is hydrolyzed under the acidic condition to prepare 2,4,6 trimethyl benzoic acid which is used as the raw material of the acyl chlorination or sold as a product.
The acylation reaction liquid hydrolysis process usually adopts single-kettle intermittent operation, hydrochloric acid and water are added into a hydrolysis kettle, reaction materials are slowly added under stirring, the materials are added after being cooled, and then the temperature is raised after the materials are added to carry out hydrolysis reaction.
Chinese patent document CN 209778707U (201920242060.2) is a system for producing ethyl maltol by continuous hydrolysis of a chloride solution, which comprises a storage kettle, a feed pump, a preheater, a reactive distillation tower, a tower top condenser, a tower bottom reboiler, a tower bottom circulating pump, a liquid seal tank, a reflux pump, an alkaline washing tower, a first condenser, an alkaline washing pump, an alcoholic washing tower, a second condenser and an alcoholic washing pump. However, the above device is a rectification device, the hydrolysis reaction conditions of which are completely different from the hydrolysis reaction of 2,4,6 trimethylbenzoyl chloride, and the device is not suitable for the hydrolysis reaction of 2,4,6 trimethylbenzoyl chloride, and has high requirements on equipment and increased cost.
Therefore, in order to solve the problems of low efficiency of discontinuous operation process, complicated temperature reduction and temperature rise and difficult stability of product quality in the hydrolysis reaction of the 2,4,6 trimethyl benzoyl chloride acylation liquid, a continuous hydrolysis device and a continuous hydrolysis method suitable for the hydrolysis reaction of the 2,4,6 trimethyl benzoyl chloride acylation liquid are urgently needed.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a continuous hydrolysis unit of acylation reaction production 2,4,6 trimethyl benzoic acid's acylation liquid has solved prior art intermediate sex operation process inefficiency, and the cooling intensifies loaded down with trivial details, and product quality is difficult to stable problem. The utility model adopts the mixer to feed, so that feeding and hydrolysis are separately carried out, the mixer is adopted to control low-temperature feeding, the hydrolysis kettle is used to control higher hydrolysis temperature, low-temperature feeding and high-temperature hydrolysis are respectively controlled, the single kettle is not needed to be cooled and heated for repeated operation, and the cooling and feeding time of the hydrolysis kettle is saved; adopt the two-stage cauldron of hydrolysising, after preheating through first cauldron of hydrolysising, the rate of hydrolysising of second cauldron obtains improving, hydrolysises more fully, makes single cauldron operation become two cauldron continuous simultaneous operation, and the continuous hydrolysis time has shortened more than 1 times than the single cauldron operation of intermittent type formula, and production efficiency obtains improving, because continuous feeding and continuous ejection of compact, produces more steadily, makes product quality more stable, and product 2,4, 6-trimethyl benzoic acid quality obtains improving.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a continuous hydrolysis device for producing acylation liquid of 2,4,6 trimethyl benzoic acid by acylation reaction comprises a mixer 3, a first hydrolysis kettle, a second hydrolysis kettle, a hydrolysis separation tank, a water washing tank and a separator;
the lower end of the mixer is connected with the first hydrolysis kettle through a pipeline, and the outlet of the first hydrolysis kettle is connected with the feed liquid inlet of the second hydrolysis kettle through a pipeline; the feed liquid outlet of the second hydrolysis kettle is connected with the feed liquid inlet of the hydrolysis separation tank through a pipeline; a feed liquid outlet of the hydrolysis separation tank is respectively connected with a feed liquid inlet of the aluminum trichloride solution storage tank and a feed liquid inlet of the washing tank through pipelines; the outlet of the washing tank is connected with the feed liquid inlet of the separator through a pipeline; the outlet of the separator is respectively connected with a crude product collecting tank and a washing water collecting tank through pipelines.
Preferably, stirrers are arranged in the mixer, the first hydrolysis kettle and the second hydrolysis kettle; the side wall is provided with a jacket. Circulating water is introduced into the jacket, and the circulating water is used for heating.
Preferably, the washing tank is provided with a washing water inlet which is connected with a water inlet pipeline. The washing tank is internally provided with a stirring device.
Preferably, the feed liquid inlet of the separator is located at the top of the separator.
Preferably, the wash water outlet of the wash water collection tank is connected to the inlet of the wash water delivery pump through a pipeline.
Preferably, the upper end of the mixer is connected with a buffer tank and a diluted hydrochloric acid preparation tank. The buffer tank is filled with acylation reaction liquid and is connected with an acylation reaction liquid pipeline.
Preferably, the tail gas discharge ports of the first hydrolysis kettle, the second hydrolysis kettle, the hydrolysis separation tank, the washing tank and the washing collection tank are connected with a tail gas discharge system through pipelines.
The device is applied to a method for continuously hydrolyzing an acylation liquid for producing 2,4,6 trimethyl benzoic acid by acylation reaction, and comprises the following steps:
(1) adding the reaction liquid after the dilute hydrochloric acid and the acylation reaction in the buffer tank into a mixer, and fully stirring and mixing the reaction liquid by the mixer, wherein the temperature in the mixer is controlled to be below 50 ℃;
(2) continuously feeding the mixed solution into a first hydrolysis kettle and a second hydrolysis kettle, and keeping a certain temperature and retention time to fully hydrolyze the solution; the mixed solution is preheated and hydrolyzed in a first hydrolysis kettle, and is further hydrolyzed in a second hydrolysis kettle;
(3) the hydrolyzed material liquid enters a hydrolysis separation tank for standing, the organic phase and the water phase are separated, and the water phase aluminum trichloride solution enters an aluminum trichloride solution tank; the organic phase enters a water washing tank, water is added for stirring, and further washing is carried out;
(4) the mixed solution of the washed organic phase and water enters a separator, the water phase is continuously separated, the organic phase out of the separator enters a crude product collecting tank, and the mesitylene solution of 2,4, 6-trimethyl benzoic acid is obtained;
(5) sending the mesitylene solution of 2,4, 6-trimethyl benzoic acid to a crystallizing device, cooling, crystallizing, and centrifugally separating to obtain crystals of 2,4, 6-trimethyl benzoic acid.
Preferably, the reaction solution after the acylation reaction in the step (1) is obtained by performing acylation reaction on raw materials such as mesitylene and the like under the condition of taking anhydrous aluminum trichloride as a catalyst.
Preferably, the first hydrolysis kettle and the second hydrolysis kettle in the step (2) are heated by circulating water in a jacket; the first hydrolysis kettle and the second hydrolysis kettle keep the temperature in the kettles at 80-90 ℃, and the residence time of the two-stage hydrolysis kettle is 2 hours in total.
The material flow rate is suitable for maintaining the hydrolysis reaction for 1-3 h.
Preferably, the standing time in the step (3) is 0.5-2 h. And (4) the organic phase in the step (3) is a mesitylene solution of 2,4, 6-trimethyl benzoic acid.
Preferably, the mixed solution obtained in the step (4) enters a separator and stands for 0.5-2 h, and washing water and a mesitylene solution of 2,4, 6-trimethylbenzoic acid are separated.
Preferably, the water separated by the separator enters a washing water collecting tank, is pumped into a dilute hydrochloric acid preparation tank by a pump to prepare dilute hydrochloric acid, and is then sent into a mixer for hydrolysis.
The embodiment of the utility model provides an one or more embodiment has following technological effect at least:
(1) continuous hydrolysis, continuous feeding and continuous discharging;
(2) a novel oil-water separator is adopted, so that the separation effect is good;
(3) the efficiency is high, and the yield is high;
(4) the product quality is stable, and the high-quality product rate is high.
The process for preparing 2,4, 6-trimethyl benzoic acid by hydrolyzing acylation reaction liquid of 2,4, 6-trimethyl benzoic acid produced by an acylation method mostly adopts single-kettle intermittent operation, hydrochloric acid and water are added into a hydrolysis kettle, reaction materials are slowly added at low temperature and in a stirring state, cooling water is firstly used for cooling to below 50 ℃, the temperature is increased to 50-60 ℃ after the materials are added, hydrolysis reaction is carried out for 1.5-2 h, and due to intermittent operation, the working procedure efficiency is low, the temperature reduction and the temperature increase are tedious, and the product quality is difficult to stabilize.
The utility model adopts the feeding in the mixer to separately carry out the feeding and the hydrolysis, adopts the mixer to control the low-temperature feeding, controls the hydrolysis kettle to control higher hydrolysis temperature, controls the low-temperature feeding and the high-temperature hydrolysis respectively, does not need the single kettle to cool and heat, and saves the cooling and feeding time of the hydrolysis kettle; adopt the two-stage cauldron of hydrolysising, after preheating through first cauldron of hydrolysising, the rate of hydrolysising of second cauldron obtains improving, hydrolysises more fully, makes single cauldron operation become two cauldron continuous simultaneous operation, and the continuous hydrolysis time has shortened more than 1 times than the single cauldron operation of intermittent type formula, and production efficiency obtains improving, because continuous feeding and continuous ejection of compact, produces more steadily, makes product quality more stable, and product 2,4, 6-trimethyl benzoic acid quality obtains improving.
The utility model discloses equipment adopts glass-lined, pipeline to adopt the lining tetrafluoro material, and is more corrosion-resistant, and impurity still less, and product quality is higher. By adopting the novel glass lining high-efficiency oil-water separator, the separation efficiency is higher, the obtained mesitylene solution of 2,4, 6-trimethylbenzoic acid has lower water content and high product purity.
Drawings
FIG. 1 is a flow chart of the continuous hydrolysis apparatus of the present invention;
FIG. 2 is a spectrum of 2,4, 6-trimethylbenzoic acid obtained by crystallization separation after continuous hydrolysis at about 80 ℃ for 2 hours;
FIG. 3 is a spectrum of 2,4, 6-trimethylbenzoic acid obtained by crystallization separation after continuous hydrolysis at about 85 ℃ for 2 hours;
FIG. 4 shows the spectrum of 2,4, 6-trimethylbenzoic acid obtained by batch hydrolysis crystallization.
Reference numerals: 1-a buffer tank; 2-dilute hydrochloric acid preparation tank; 3-a mixer; 4-a first hydrolysis kettle; 5-a second hydrolysis kettle; 6-hydrolysis separating tank; 7-aluminum trichloride solution storage tank; 8-water washing tank; 9-a separator; 10-a crude product collection tank; 11-a wash water collection tank; 12-pump.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and specific embodiments:
example 1
Fig. 1 shows a continuous hydrolysis device for producing an acylation liquid of 2,4,6 trimethyl benzoic acid by acylation reaction of the present invention, which comprises a mixer 3, a first hydrolysis kettle 4, a second hydrolysis kettle 5, a hydrolysis separation tank 6, a water washing tank 8 and a separator 9;
the lower end of the mixer 3 is connected with a first hydrolysis kettle 4 through a pipeline, and the outlet of the first hydrolysis kettle 4 is connected with the feed liquid inlet of a second hydrolysis kettle 5 through a pipeline; a feed liquid outlet of the second hydrolysis kettle 5 is connected with a feed liquid inlet of the hydrolysis separation tank 6 through a pipeline; a feed liquid outlet of the hydrolysis separation tank 6 is respectively connected with a feed liquid inlet of the aluminum trichloride solution storage tank 7 and a feed liquid inlet of the washing tank 8 through pipelines; an outlet of the washing tank 8 is connected with a feed liquid inlet of the separator 9 through a pipeline, and an outlet of the washing tank 8 is arranged at the upper part of the washing tank and is 40-50 cm away from the top of the washing tank; the outlet of the separator 9 is respectively connected with the feed liquid inlet of the crude product collecting tank 10 and the washing water inlet of the washing water collecting tank 11 through pipelines; the inlet of the separator 9 is arranged at the top of the separator, the outlet at the upper part of the separator 9 is arranged at the position 40-50 cm away from the upper part of the separator and is arranged at the opposite side of the inlet and at 2/3 of the height of the tank body, and the outlet at the bottom is an acid water outlet. Stirrers are arranged in the mixer 3, the first hydrolysis kettle 4 and the second hydrolysis kettle 5; the side wall is provided with a jacket, and circulating water is introduced into the jacket for heating. A washing water inlet of the washing tank 8 is arranged on a feed inlet pipeline of the washing tank 8 and is the same as the material, and the washing water inlet is connected with a water inlet pipeline; the inside of the washing tank 8 is provided with a baffle plate, and the materials and the washing water are mixed, stirred and washed. The water washing tank 8 is internally provided with a stirring device. The feed liquid inlet of the separator 9 is located at the top of the separator 9. The washing water outlet of the washing water collecting tank 11 is connected to the inlet of the washing water delivery pump 12 through a pipeline. The upper end of the mixer 3 is connected with the buffer tank 1 and the dilute hydrochloric acid preparation tank. The buffer tank 1 is filled with acylation reaction liquid, and the buffer tank 1 is connected with an acylation reaction liquid pipeline. The tail gas discharge ports of the first hydrolysis kettle 4, the second hydrolysis kettle 5, the hydrolysis separation tank 6, the washing tank 8 and the washing collection tank 11 are connected with a tail gas discharge system through pipelines.
The separator 9 is a standard tank body, a visual cup is mounted at an upper outlet of the separator 9, and the separated two-phase liquid level is observed through a sight glass, so that the liquid level is prevented from being too high or too low and is adjusted. The hydrolysis separation tank 6 also has the same sight glass or sight cup structure as the separator 9.
Test example 1
Raw materials such as mesitylene and the like are subjected to acylation reaction under the condition that anhydrous aluminum trichloride is used as a catalyst, and reaction liquid after the acylation reaction is injected into a buffer tank 1. Adding dilute hydrochloric acid from a dilute hydrochloric acid preparation tank 2 into a mixer 3, stirring, slowly adding acylation reaction liquid from a buffer tank 1 into the mixer 3, and mixing with prepared acid water according to the proportion of 1: 1, continuously feeding the mixture into a mixer, fully stirring and mixing the mixture by a mixer 3, continuously feeding the mixture into a first hydrolysis kettle 4 and a second hydrolysis kettle 5, keeping the temperature of materials in the kettles at about 80 ℃, and keeping the temperature for 2 hours to fully hydrolyze the material solution. The first hydrolysis kettle 4 and the second hydrolysis kettle 5 are heated by circulating water in a jacket, the temperature is maintained at 80-90 ℃, the mixed solution is preheated and hydrolyzed in the first hydrolysis kettle 4, and the mixed solution is further hydrolyzed in the second hydrolysis kettle 5; the hydrolyzed material liquid continuously enters a hydrolysis separation tank 6 to separate an organic phase and a water phase, and the separated water phase aluminum trichloride solution enters an aluminum trichloride solution tank 7 and is pumped out of the system; the organic phase enters a water washing tank 8, and the reaction is carried out according to the following steps of 1: 1, continuously adding hot water with the temperature of 80 ℃, stirring, further washing, continuously separating a water phase from a mixed solution of an organic phase and water after washing, adding the mixed solution into a separator 9, adding the water phase into a washing water collecting tank 11, pumping the mixed solution into a dilute hydrochloric acid preparation tank 2 by using a pump to prepare dilute hydrochloric acid, and then feeding the diluted hydrochloric acid into a mixer 3 for hydrolysis; and (3) feeding the organic phase out of the separator 9 into a crude product collecting tank 10 to obtain a mesitylene solution of 2,4, 6-trimethyl benzoic acid, and sending the mesitylene solution to a crystallizing device for cooling, crystallizing and centrifugal separation to obtain crystals of the 2,4, 6-trimethyl benzoic acid, wherein the crystals are used as raw materials for acyl chlorination reaction or are sold as products.
The mixer 3 adopts cold water to control the temperature, so that the mixing reaction is carried out at normal temperature; the first hydrolysis kettle 4 and the second hydrolysis kettle 5 adopt external jacket circulating water for temperature control, and circulating water enters from a circulating water inlet at the bottom of the jacket and is discharged from a water outlet at the upper part of the jacket; the mixer 3, the first hydrolysis kettle 4 and the second hydrolysis kettle 5 are stirred by adopting stirrers, the mixer 3 controls normal temperature operation, and the hydrolysis kettle keeps the temperature in the kettle at 80 ℃; the material flow rate is suitable for maintaining hydrolysis reaction for 2 hours; the hydrolyzed material enters a hydrolysis separation tank 6, and the standing time is 2 hours; and (3) allowing the mesitylene solution of 2,4, 6-trimethylbenzoic acid after the aluminum trichloride aqueous phase is separated to enter a water washing tank 8, adding a proper amount of water, stirring and washing, allowing the solution to enter a separator 9, standing for 2 hours, and separating washing water and the mesitylene solution of 2,4, 6-trimethylbenzoic acid.
TABLE 1 comparison of products of equal-scale batch and continuous hydrolysis of 2,4, 6-trimethylbenzoic acid
Comparison of product quality
In the intermittent hydrolysis process, hydrochloric acid and acylation reaction liquid are directly added into a hydrolysis kettle for hydrolysis reaction, and aluminum trichloride chelated on product molecules is slow to hydrolyze and is not washed cleanly, so that the product quality is influenced.
The continuous hydrolysis adopts a mixer to fully mix, and the two stages of hydrolysis kettles can ensure that the aluminum trichloride chelated on the product molecules is hydrolyzed more easily and is washed cleanly, and the product quality is improved.
The product content of the 2,4, 6-trimethyl benzoic acid obtained by the two methods is 98.77 percent by a continuous hydrolysis method and 91.92 percent by a batch method.
Test example 2
Raw materials such as mesitylene and the like are subjected to acylation reaction under the condition that anhydrous aluminum trichloride is used as a catalyst, and reaction liquid after the acylation reaction is injected into a buffer tank 1. Adding dilute hydrochloric acid from a dilute hydrochloric acid preparation tank 2 into a mixer 3, stirring, slowly adding acylation reaction liquid from a buffer tank 1 into the mixer 3, and mixing with prepared acid water at normal temperature and normal pressure according to the ratio of 1: 1, continuously feeding the mixture into a mixer, fully stirring and mixing the mixture by a mixer 3, continuously feeding the mixture into a first hydrolysis kettle 4 and a second hydrolysis kettle 5, keeping the temperature of materials in the kettles at about 85 ℃, and keeping the temperature for 2 hours to fully hydrolyze the material solution. The first hydrolysis kettle 4 and the second hydrolysis kettle 5 are heated by circulating water in a jacket, the temperature is maintained to be 85-90 ℃, the mixed solution is preheated and hydrolyzed in the first hydrolysis kettle 4, and the mixed solution is further hydrolyzed in the second hydrolysis kettle 5; the hydrolyzed material liquid continuously enters a hydrolysis separation tank 6 to separate an organic phase and a water phase, and the separated water phase aluminum trichloride solution enters an aluminum trichloride solution tank 7 and is pumped out of the system; the organic phase enters a water washing tank 8, and the reaction is carried out according to the following steps of 1: 1, continuously adding hot water with the temperature of 85 ℃, stirring, further washing, continuously separating a water phase from a mixed solution of an organic phase and water after washing, adding the mixed solution into a separator 9, adding the water phase into a washing water collecting tank 11, pumping the mixed solution into a dilute hydrochloric acid preparation tank 2 by using a pump to prepare dilute hydrochloric acid, and then feeding the diluted hydrochloric acid into a mixer 3 for hydrolysis; and (3) feeding the organic phase out of the separator 9 into a crude product collecting tank to obtain a mesitylene solution of 2,4, 6-trimethyl benzoic acid, and sending the mesitylene solution to a crystallizing device for cooling, crystallizing and centrifugal separation to obtain crystals of the 2,4, 6-trimethyl benzoic acid, wherein the crystals are used as raw materials for acyl chlorination reaction or are sold as products.
The mixer 3 adopts cold water to control the temperature, so that the mixing reaction is carried out at normal temperature; the first hydrolysis kettle 4 and the second hydrolysis kettle 5 adopt external jacket circulating water for temperature control, and circulating water enters from a circulating water inlet at the bottom of the jacket and is discharged from a water outlet at the upper part of the jacket; the mixer 3, the first hydrolysis kettle 4 and the second hydrolysis kettle 5 are stirred by adopting stirrers, the mixer 3 controls normal temperature and normal pressure, and the hydrolysis kettle keeps the temperature in the kettle at 85 ℃; the material flow rate is suitable for maintaining hydrolysis reaction for 2 hours; the hydrolyzed material enters a hydrolysis separation tank 6, and the standing time is 2 hours; and (3) allowing the mesitylene solution of 2,4, 6-trimethylbenzoic acid after the aluminum trichloride aqueous phase is separated to enter a water washing tank 8, adding a proper amount of water, stirring and washing, allowing the solution to enter a separator 9, standing for 2 hours, and separating washing water and the mesitylene solution of 2,4, 6-trimethylbenzoic acid.
TABLE 2 comparison of products of equal-scale batch and continuous hydrolysis of 2,4, 6-trimethylbenzoic acid
Comparison of product quality
In the intermittent hydrolysis process, hydrochloric acid and acylation reaction liquid are directly added into a hydrolysis kettle for hydrolysis reaction, and aluminum trichloride chelated on product molecules is slow to hydrolyze and is not washed cleanly, so that the product quality is influenced.
The continuous hydrolysis adopts a mixer to fully mix, and the two stages of hydrolysis kettles can ensure that the aluminum trichloride chelated on the product molecules is hydrolyzed more easily and is washed cleanly, and the product quality is improved.
The product content of the 2,4, 6-trimethyl benzoic acid obtained by using the device of the utility model to carry out continuous hydrolysis is 98.95 percent, while the product content of the traditional batch hydrolysis kettle is 91.92 percent.
Claims (6)
1. A continuous hydrolysis device for producing acylation liquid of 2,4,6 trimethyl benzoic acid by acylation reaction is characterized by comprising a mixer (3), a first hydrolysis kettle (4), a second hydrolysis kettle (5), a hydrolysis separation tank (6), a water washing tank (8) and a separator (9);
the lower end of the mixer (3) is connected with the first hydrolysis kettle (4) through a pipeline, and the outlet of the first hydrolysis kettle (4) is connected with the feed liquid inlet of the second hydrolysis kettle (5) through a pipeline; a feed liquid outlet of the second hydrolysis kettle (5) is connected with a feed liquid inlet of the hydrolysis separation tank (6) through a pipeline; a feed liquid outlet of the hydrolysis separation tank (6) is respectively connected with a feed liquid inlet of the aluminum trichloride solution storage tank (7) and a feed liquid inlet of the washing tank (8) through pipelines; the outlet of the washing tank (8) is connected with the feed liquid inlet of the separator (9) through a pipeline; the outlet of the separator (9) is respectively connected with a crude product collecting tank (10) and a washing water collecting tank (11) through pipelines.
2. The continuous hydrolysis device according to claim 1, wherein stirrers are arranged in the mixer (3), the first hydrolysis kettle (4) and the second hydrolysis kettle (5); the side wall is provided with a jacket.
3. Continuous hydrolysis device according to claim 1, characterized in that the feed inlet of the separator (9) is located at the top of the separator (9).
4. The continuous hydrolysis apparatus as claimed in claim 1, wherein the upper end of the mixer (3) is connected to the buffer tank (1) and the diluted hydrochloric acid preparation tank (2).
5. The continuous hydrolysis device according to claim 1, wherein the tail gas discharge ports of the first hydrolysis kettle (4), the second hydrolysis kettle (5), the hydrolysis separation tank (6), the washing tank (8) and the washing collection tank (11) are connected with a tail gas discharge system through pipelines.
6. The continuous hydrolysis apparatus as claimed in claim 1, wherein the washing tank (8) is provided with a washing water inlet connected to a water inlet line.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269108A (en) * | 2020-01-20 | 2020-06-12 | 泰安渤洋化工科技有限公司 | Continuous hydrolysis device and method for 2,4,6 trimethyl benzoic acid acylation liquid |
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2020
- 2020-01-20 CN CN202020128934.4U patent/CN211546371U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269108A (en) * | 2020-01-20 | 2020-06-12 | 泰安渤洋化工科技有限公司 | Continuous hydrolysis device and method for 2,4,6 trimethyl benzoic acid acylation liquid |
| CN111269108B (en) * | 2020-01-20 | 2023-08-22 | 泰安渤洋化工科技有限公司 | Continuous hydrolysis device and method for 2,4,6 trimethyl benzoic acid acylation liquid |
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