CN210303646U - Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid - Google Patents

Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid Download PDF

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CN210303646U
CN210303646U CN201920822721.9U CN201920822721U CN210303646U CN 210303646 U CN210303646 U CN 210303646U CN 201920822721 U CN201920822721 U CN 201920822721U CN 210303646 U CN210303646 U CN 210303646U
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tail gas
kettle body
oxygen
warm water
water
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CN201920822721.9U
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李兴华
李卫明
陈雪飞
张亮
闫炯
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SUQIAN KESI CHEMICAL CO Ltd
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SUQIAN KESI CHEMICAL CO Ltd
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Abstract

To tertiary butylbenzene formic acid oxidation reaction device of inerting that adds water, including the reation kettle body, still include the moisturizing device, oxygen concentration on-line measuring appearance, tail gas outlet oxygen flow meter, the moisturizing device includes the warm water case, the warm water flowmeter, the governing valve, the inlet channel, inlet channel one end is connected with the warm water case, the inlet channel other end is linked together with reation kettle body top, the warm water flowmeter, the governing valve is installed on the inlet channel in proper order, the common control moisturizing volume, oxygen concentration on-line measuring appearance is installed at reation kettle body top, tail gas outlet oxygen flow meter installs on the tail gas pipeline, tail gas pipeline one end communicates with the reation kettle body mutually, still be provided with the condenser on the tail. The utility model discloses guarantee to be in the reaction process of para-tertiary butyl toluene oxidation to para-tertiary butyl benzoic acid kettle top gas phase space oxygen concentration in real time below the LOC of para-tertiary butyl toluene, can not form the explosive mixture to tertiary butyl toluene and oxygen at the kettle top, realize the safe high-efficient production of para-tertiary butyl benzoic acid.

Description

Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid
Technical Field
The utility model belongs to the technical field of chemical reaction equipment, concretely relates to tert-butylbenzene formic acid oxidation reaction inertization device that adds water.
Background
The p-tert-butyl benzoic acid is an important organic synthesis intermediate, is widely applied to the industries of chemical synthesis, cosmetics, flavors, fragrances and the like, and is mainly prepared by the reaction of p-tert-butyl toluene and oxygen molecules. In the prior art, the production method of p-tert-butyl benzoic acid is that p-tert-butyl toluene is put into a reaction kettle, a catalyst is added, jacket steam is adopted to heat the material to a certain temperature (130 ℃), a method of introducing pure oxygen under liquid is adopted to carry out oxidation reaction, and unreacted oxygen is discharged through a tail gas system. In the reaction process, due to the fact that the temperature of the reaction kettle is high, the evaporation amount of the p-tert-butyl toluene is large, the p-tert-butyl toluene and oxygen are mixed in a gas phase space at the top of the reaction kettle to form an explosive mixture of the p-tert-butyl toluene and the oxygen, and the safe operation of the oxidation reaction of the p-tert-butyl toluene is greatly influenced.
SUMMERY OF THE UTILITY MODEL
To the not enough of background art, the utility model discloses research and design has added water inerting device to tert-butylbenzoic acid oxidation reaction, its aim at: provides an oxidation reaction water adding inerting device which can realize the safe and efficient production of p-tert-butyl benzoic acid.
The technical solution of the utility model is as follows:
to tertiary butylbenzene formic acid oxidation reaction water inerting device, including the reation kettle body, its characterized in that: the device comprises a warm water tank, a warm water flowmeter, an adjusting valve and a water inlet pipeline, wherein one end of the water inlet pipeline is connected with the warm water tank, the other end of the water inlet pipeline is communicated with the top of the reaction kettle body, the warm water flowmeter and the adjusting valve are sequentially arranged on the water inlet pipeline to jointly control the water supplementing quantity, the oxygen concentration online detector is arranged at the top of the reaction kettle body, is used for detecting the oxygen concentration value at the top in the reaction kettle body in real time, the tail gas outlet oxygen flowmeter is arranged on a tail gas pipeline, be used for real-time detection tail gas oxygen flow, tail gas pipeline one end and reation kettle body communicate mutually, still are provided with the condenser on the tail gas pipeline, and the condenser is used for gaseous phase water, gaseous phase organic solvent condensation for only oxygen passes through the tail gas pipeline and flows, and measures through tail gas export oxygen flow meter.
The oxygen concentration online detector, the tail gas outlet oxygen flow meter and the warm water flow meter are all connected with the controller through lines.
The utility model has the advantages that: the utility model has the advantages of reasonable structure, novel design, its oxygen concentration numerical value of the real-time on-line measuring appearance of oxygen concentration of reation kettle top setting, the tail gas export oxygen flowmeter real-time detection tail gas oxygen flow that sets up on the tail gas pipeline, the controller can calculate its water yield that needs to be supplemented, warm water flowmeter on through the inlet channel, the governing valve common control moisturizing volume, guarantee to tertiary butyl toluene oxidation to be in the reaction process of p-tertiary butyl benzoic acid cauldron top gas phase space oxygen concentration in real time below the LOC of p-tertiary butyl toluene, can not form the explosive mixture to tertiary butyl toluene and oxygen at the cauldron top, realize the safe efficient production to tertiary butyl benzoic acid, and has very high practical value.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Wherein: 1. the reaction kettle comprises a reaction kettle body, 2, an oxygen concentration online detector, 3, a tail gas outlet oxygen flow meter, 4, a warm water tank, 5, a warm water flow meter, 6, a regulating valve, 7, a water inlet pipeline, 8, a tail gas pipeline, 9 and a condenser.
Detailed Description
The invention is further described with reference to the following drawings and specific embodiments.
As shown in figure 1, the water adding and inerting device for the oxidation reaction of tert-butylbenzoic acid comprises a reaction kettle body 1, a water supplementing device, an oxygen concentration online detector 2 and a tail gas outlet oxygen flow meter 3, wherein the water supplementing device comprises a warm water tank 4, a warm water flow meter 5, a regulating valve 6 and a water inlet pipeline 7, one end of the water inlet pipeline 7 is connected with the warm water tank 4, the other end of the water inlet pipeline 7 is communicated with the top of the reaction kettle body 1, the warm water flow meter 5 and the regulating valve 6 are sequentially installed on the water inlet pipeline 7 to jointly control the water supplementing amount, the oxygen concentration online detector 2 is installed on the top of the reaction kettle body 1 and is used for detecting the oxygen concentration value at the top in the reaction kettle body 1 in real time, the tail gas outlet oxygen flow meter 3 is installed on a tail gas pipeline 8 and is used for detecting the oxygen flow, the condenser 9 is used for condensing gas phase water and gas phase organic solvent, so that only oxygen flows out through the tail gas pipeline 8 and is measured through the tail gas outlet oxygen flow meter 3, and the oxygen concentration online detector 2, the tail gas outlet oxygen flow meter 3 and the warm water flow meter 5 are all in line connection with a controller (not marked in the figure).
The specific using process is as follows: in the actual use process, the reaction kettle body 1 for oxidizing the tert-butyl toluene starts to carry out oxygen introduction reaction, an oxygen concentration online detector 2 at the top of the reaction kettle body 1 detects the oxygen concentration value in real time, simultaneously transmits a signal to a controller, a condenser 9 is used for condensing gas-phase water and gas-phase organic solvent, so that only oxygen flows out through a tail gas pipeline 8, a tail gas outlet oxygen flow meter 3 arranged on the tail gas pipeline 8 detects the tail gas oxygen flow in real time and transmits the signal to the controller, the controller can calculate the total gas amount in the reaction kettle body 1 and the temperature water amount to be supplemented according to the oxygen concentration value at the top of the reaction kettle body 1 and the tail gas oxygen flow, the controller transmits the signal to a temperature water flow meter 5, the water supplementing amount is simultaneously controlled by a regulating valve 6 and the temperature water flow meter 5 on a water inlet pipeline 7, and the total gas amount and the oxygen concentration value in the reaction kettle body 1 are, adding warm water, and gasifying the mixture into steam (the volume of the steam gasified into steam is enlarged by 1600 times) to dilute the oxygen concentration, for example, if the detected value of the top oxygen concentration in the reaction kettle body 1 is 20%, and the tail gas flow of the tail gas outlet oxygen flow meter 3 is 6m for thin film cultivation, the total gas phase weight of the top water, the organic solvent gas phase and the oxygen can be reversely deduced to be 30m for thin film cultivation; at this moment, if the volume after quantitative water gasification is added into the kettle is 100m, then the total gas phase volume is 130m, then the concentration of oxygen is 6 ÷ 130=0.046, the oxygen concentration volume ratio is about 4.6%, it is below expected oxygen concentration (5% or 10%), the water gasification in warm water is water vapor and carries out concentration dilution to oxygen, and then the oxygen concentration at the top in the inerting reaction kettle body 1, be in below LOC to tert-butyltoluene in real time with top gas phase space oxygen concentration in the top in reaction kettle body 1, avoid forming explosive mixture at the top of reaction kettle body 1, guarantee that the reaction can be safely carried out, realize the safe and efficient production to tert-butylbenzoic acid.
To sum up, the utility model discloses reach anticipated effect.
The basic principles and the main features of the invention and the advantages of the invention have been shown and described above, it will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, but that the invention may be embodied 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 (2)

1. To tertiary butylbenzene formic acid oxidation reaction water inerting device, including the reation kettle body, its characterized in that: the device comprises a warm water tank, a warm water flowmeter, an adjusting valve and a water inlet pipeline, wherein one end of the water inlet pipeline is connected with the warm water tank, the other end of the water inlet pipeline is communicated with the top of the reaction kettle body, the warm water flowmeter and the adjusting valve are sequentially arranged on the water inlet pipeline to jointly control the water supplementing quantity, the oxygen concentration online detector is arranged at the top of the reaction kettle body, is used for detecting the oxygen concentration value at the top in the reaction kettle body in real time, the tail gas outlet oxygen flowmeter is arranged on a tail gas pipeline, be used for real-time detection tail gas oxygen flow, tail gas pipeline one end and reation kettle body communicate mutually, still are provided with the condenser on the tail gas pipeline, and the condenser is used for gaseous phase water, gaseous phase organic solvent condensation for only oxygen passes through the tail gas pipeline and flows, and measures through tail gas export oxygen flow meter.
2. The water inerting apparatus for the p-tert-butylbenzoic acid oxidation reaction according to claim 1, wherein: the oxygen concentration on-line detector, the tail gas outlet oxygen flow meter and the warm water flow meter are all connected with the controller through lines.
CN201920822721.9U 2019-06-03 2019-06-03 Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid Active CN210303646U (en)

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CN201920822721.9U CN210303646U (en) 2019-06-03 2019-06-03 Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid

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CN201920822721.9U CN210303646U (en) 2019-06-03 2019-06-03 Water adding inerting device for oxidation reaction of p-tert-butylbenzoic acid

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112479861A (en) * 2020-12-10 2021-03-12 成家钢 Liquid-phase normal-pressure catalytic oxygen oxidation safety method and oxygen oxidation safety reaction equipment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112479861A (en) * 2020-12-10 2021-03-12 成家钢 Liquid-phase normal-pressure catalytic oxygen oxidation safety method and oxygen oxidation safety reaction equipment

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