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Sulfonation equipment and method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene

A technology of p-toluenesulfonic acid and sulfur trioxide, which is applied to the preparation of sulfonic acid, chemical instruments and methods, chemical/physical/physicochemical processes, etc. It can solve problems affecting product quality, no heat transfer structure, and small cooling area , to achieve the effects of stable product quality, improved mass transfer efficiency, and small equipment volume

Active Publication Date: 2015-03-25
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

North University of China (CN 101570500) applied the high-gravity rotating packed bed to the sulfonation of toluene to produce better p-toluenesulfonic acid products, but because the cooling area of ​​the rotating packed bed is small and the reaction occurs at the packing rotor, However, there is no heat transfer structure at the packing rotor, which makes heat transfer lag and affects product quality. Therefore, further innovation and improvement of the rotating packing bed structure is required.

Method used

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  • Sulfonation equipment and method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene
  • Sulfonation equipment and method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene

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Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: the sulfonation of toluene

[0038] use figure 2 The plant scheme shown performs toluene sulfonation. Adjust the rotating speed of the rotating packed bed 4 to 1200r / min, the raw material toluene is cooled to -5°C to 0°C through the heat exchanger 41 before entering the rotating packed bed 4, and the flow rate of the toluene entering the system is 18 kg / h (the spray density is 9 meters 3 / m 2 .h), the flow rate of the mixed gas containing 6% sulfur trioxide (v / v) (the rest is dry air) is 30Nm 3 / h, after the two raw materials are rapidly mixed and reacted in the rotating packed bed 4, they enter the constant temperature reactor 38 through the rotating packed bed liquid outlet 18 and continue to complete the reaction (aging) at a suitable temperature (5-10) °C to obtain Product enters product storage tank 39 . The molar ratio of sulfur trioxide and toluene added to the reaction system is 0.41:1. The para-position content in the toluenesulfonic acid p...

Embodiment 2

[0039] Embodiment 2: the sulfonation of toluene

[0040] use figure 2 The plant scheme shown performs the sulfonation of toluene. Adjust the rotational speed of the rotary packed bed 4 to 1500 r / min. Before entering the rotary packed bed 4, the raw material toluene is cooled to 0°C-5°C through the heat exchanger 41, and the flow rate of the toluene entering the system is 18 kg / h, containing sulfur trioxide 8% (v / v) mixture (the rest is dry air) with a flow rate of 25 Nm 3 / h, after the two raw materials are quickly mixed and reacted in the rotating packed bed 4, the product enters the constant temperature reactor 38 through the liquid outlet 18 of the rotating packed bed and continues to complete the reaction (aging) at a suitable temperature (5-10) °C , get the product into the product storage tank 39. The molar ratio of sulfur trioxide and toluene added to the reaction system is 0.45:1. The para-position content in the toluenesulfonic acid produced by the reaction accou...

Embodiment 3

[0041] Embodiment 3: Sulfonation of toluene

[0042] use figure 2 The plant scheme shown performs the sulfonation of toluene. Adjust the rotational speed of the rotary packed bed 4 to 1800 r / min, and the raw material toluene is cooled to -5°C to 0°C through the heat exchanger 41 before entering the rotary packed bed 4, and the flow rate of the toluene entering the system is 18 kg / h, containing three The flow rate of sulfur oxide 10% (v / v) mixture (the rest is dry air) is 15 Nm 3 / h, after the two raw materials are rapidly mixed and reacted in the rotating packed bed 4, the product enters the constant temperature reactor 38 through the liquid outlet 18 of the rotating packed bed and continues to complete the reaction (aging) at a suitable temperature (5-10) °C. The resulting product enters product storage tank 39 . The molar ratio of sulfur trioxide and toluene added to the reaction system is 0.34:1. The para-position content in the toluenesulfonic acid produced by the rea...

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Abstract

The invention belongs to the technical field of production of p-toluenesulfonic acid, and provides sulfonation equipment and a method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene for solving the problems of methods for preparing the p-toluenesulfonic acid by using the gaseous sulfur trioxide as a sulfonating agent for sulfonating toluene in the prior art. The sulfonation reaction is completed at a time by the efficient mass transfer characteristics of a rotary packed bed, a liquid phase product is not circulated to inhibit side reaction, and the rotary packed bed is characterized in that a heat transfer structure is arranged at a packing rotor of the rotary packed bed to quickly remove heat generated in the reaction and ensure that the reaction is carried out within a regulated temperature range, so that the side reaction is inhibited, the purity of the p-toluenesulfonic acid is improved, the yield of the p-toluenesulfonic acid is increased and the purposes of improving the production efficiency, reducing the energy consumption and reducing the environmental pollution are achieved.

Description

technical field [0001] The invention belongs to the technical field of producing p-toluenesulfonic acid, and in particular relates to a sulfonation equipment and a preparation method for preparing p-toluenesulfonic acid by sulfonating toluene with sulfur trioxide in the gas phase. Background technique [0002] P-toluenesulfonic acid (4-methylbenzenesulfonic acid) is an important organic chemical raw material and intermediate, widely used in the manufacture of surfactants, pharmaceuticals, pesticides and dye intermediates, p-cresol, resins and other substances. p-Toluenesulfonic acid is derived from toluene sulfonation. According to the different sulfonating agents used, the industrial p-toluenesulfonic acid production process can be divided into three types: sulfuric acid method, oleum method and sulfur trioxide method. When concentrated sulfuric acid or fuming sulfuric acid is used as sulfonating agent for sulfonation reaction, water will be generated during the reaction p...

Claims

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Application Information

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IPC IPC(8): B01J19/28B01J4/00C07C303/06C07C309/30
CPCB01J19/0013B01J19/002B01J19/28B01J2219/00054C07C303/06C07C309/30
Inventor 袁志国刘有智申红艳罗莹高璟张巧玲栗秀萍焦纬洲祁贵生康小峰
Owner ZHONGBEI UNIV
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