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A method for synthesizing dodecylbenzenesulfonic acid in a circulating microreactor

A technology of dodecylbenzenesulfonic acid and dodecylbenzenesulfonate, which is applied in the field of fine chemical raw material synthesis, can solve the problems of incomplete mixing of dodecylbenzene and sulfonating agent, long aging time of waste acid, and hot spots and other problems, to avoid excessive local concentration, increase the ratio, and prevent by-products

Active Publication Date: 2020-05-22
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing high-purity dodecylbenzenesulfonic acid, aiming to solve the problems of incomplete mixing of dodecylbenzene and sulfonating agent, hot spots, many side reactions and waste in the existing production process. A series of problems such as high acidity and long aging time, further improving the conversion rate of dodecylbenzene to dodecylbenzenesulfonic acid in the production process, making the preparation process more safe, efficient and pollution-free

Method used

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  • A method for synthesizing dodecylbenzenesulfonic acid in a circulating microreactor
  • A method for synthesizing dodecylbenzenesulfonic acid in a circulating microreactor

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Embodiment 1

[0035] (1) Evaporate sulfur trioxide from 20% oleum, prepare the material liquid A that mass fraction is about 5wt%, use the acid-base titration method to determine the concentration of the substance of sulfur trioxide to be 1.01mol / L, configure the mole For dodecylbenzene feed solution B with a concentration of 1.0mol / L, the concentration ratio of sulfur trioxide to dodecylbenzene is 1.01:1.

[0036] (2) Maintain the temperature of the water bath and the temperature of the storage tank 2 at a constant temperature of 30°C. Feed liquid A and feed liquid B are passed into the microporous disperser at a feed flow rate of 1ml / min and 10ml / min respectively, wherein A is the dispersed phase and B is the continuous phase. The structure of the microporous dispersing reactor is as follows: figure 2 shown. The reaction coil is a stainless steel tube with a length of 0.1 m and an inner diameter of 2 mm, and the feeding time of the liquid A is 20 min. The yield of dodecylbenzenesulfoni...

Embodiment 2

[0039] (1) evaporate sulfur trioxide from 20% oleum, be mixed with the feed liquid A that mass fraction is about 7.5wt%, use the acid-base titration method to determine the concentration of the substance of sulfur trioxide to be 1.2261mol / L, configure For dodecylbenzene feed solution B with a molar concentration of 1.2140mol / L, the concentration ratio of sulfur trioxide to dodecylbenzene is 1.01:1.

[0040] (2) Maintain the temperature of the water bath at a constant temperature of 50° C., and the storage tank 2 is not heated. Feed liquid A and feed liquid B are passed into the microporous disperser at a feed flow rate of 10ml / min and 50ml / min respectively, wherein A is the dispersed phase and B is the continuous phase. The structure of the microporous disperser is as follows: figure 2 shown. The reaction coil is a polytetrafluoroethylene tube with a length of 1 m and an inner diameter of 2 mm, and the residence time of the mixed solution in the microreactor is 3.14 s. Feed...

Embodiment 3

[0043] 1) Evaporate sulfur trioxide from 20% oleum, prepare feed liquid A with a mass fraction of about 7.5wt%, use acid-base titration to determine the concentration of sulfur trioxide as 1.2261mol / L, configure the molar For dodecylbenzene feed solution B with a concentration of 1.1681mol / L, the concentration ratio of sulfur trioxide to dodecylbenzene is 1.05:1.

[0044] 2) The temperature of the water bath is maintained at a constant temperature of 50°C, and the storage tank 2 is not heated. Feed liquid A and feed liquid B are passed into the microporous disperser at a feed flow rate of 10ml / min and 50ml / min respectively, wherein A is the dispersed phase and B is the continuous phase. The structure of the microporous disperser is as follows: figure 2 shown. The microreactor uses a polytetrafluoroethylene tube with a length of 5 m and an inner diameter of 1 mm, and the feeding time of the liquid A is 10 min. The yield of dodecylbenzenesulfonic acid was determined to be 79....

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Abstract

The invention discloses a technology for synthesizing dodecylbenzene sulfonic acid in a circulating microreactor. The technology is characterized in that a dodecylbenzene solution and a sulfonating agent which is a sulfur trioxide solution are rapidly mixed in a microporous dispersion reactor so as to realize sulfonation process; the obtained product flows back and is mixed with dodecylbenzene, and the mixture circularly enters a microreactor for further reacting; after sulfur trioxide is fed, the mixture is aged for 30-50min, and then the solvent which is 1, 2-dichloroethane is recovered by rotary evaporating so as to obtain the dodecylbenzene sulfonic acid product. According to the technology, the microporous dispersion technology is carried out to fully mix dodecylbenzene and the sulfonating agent, so that byproducts produced due to high local concentration of sulfur trioxide can be effectively avoided; moreover, the reaction temperature can be accurately controlled, so that local overheat due to heat produced in the reaction can be avoided; the reaction process and the ageing process are combined, so that the conversion rate of dodecylbenzene is increased; the dodecylbenzene sulfonic acid in the main product is up to 98% by mass; and the product is basically free from waste acid; and the product is easily separated.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemical raw materials, and in particular relates to a method for preparing dodecylbenzenesulfonic acid through dodecylbenzene sulfonation in a circulating microreactor. Background technique [0002] Dodecylbenzenesulfonic acid is an anionic surfactant, which is often used as a raw material for various detergents, or for the production of linear alkylbenzenesulfonic acid sodium salt, ammonium salt, and ethanolamine salt, and can also be used as an amino drying agent. Lacquer curing catalyst. Among them, sodium dodecylbenzene sulfonate can be used as a surfactant in EOR chemical flooding, but the cost of surfactant is an important factor limiting the development of EOR. [0003] The sulfonating agent used in the existing dodecylbenzene sulfonation process includes more than 90% concentrated sulfuric acid, sulfuryl chloride or sulfur trioxide in liquid / gas state. The technical process us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/06C07C309/31B01J19/00
Inventor 徐建鸿耿宇昊黄晋培
Owner TSINGHUA UNIV
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