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Preparation process and reaction device for synthesizing sodium dodecyl diphenyl ether disulfonate

A technology of dodecyl diphenyl ether and sodium disulfonate, which is applied in the preparation of sulfonate, the preparation of sulfonic acid, and the chemical/physical/physical-chemical stationary reactor, etc., can solve the problem that the molar ratio cannot be satisfied and increase production Cost, affecting product appearance and other issues, to avoid local peroxidation, avoid volatilization, and reduce viscosity

Pending Publication Date: 2019-12-03
南雄市汉科化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method is to drop liquid SO 3 Adding reactants for reaction may easily cause local peroxidation to form black substances. Usually the produced products are darker in color and affect the appearance of the product
Second, during the dropwise addition, SO 3 It will volatilize, causing the molar ratio between the sulfonating agent and the reactant to fail to meet the requirements of the reaction, resulting in the generation of by-products, affecting the quality of the finished product, and increasing the production cost

Method used

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  • Preparation process and reaction device for synthesizing sodium dodecyl diphenyl ether disulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Such as figure 1 The shown reaction device includes a reaction kettle 1, a stirring device, a nozzle 3 and a peristaltic pump (not shown in the figure). The reactor has a reactant feed port 11, a sulfur trioxide feed port 12, and an installation port 13 at the top of the reactor 1 for installing a stirring device. Stirring device comprises motor 4 and stirring paddle 5. The motor 4 is installed on the installation port 13 , the stirring paddle 5 is located in the reactor 1 , and one end with the paddle extends close to the bottom of the reactor 1 . The nozzle 3 is located in the reactor 1 and close to the bottom of the reactor 1 . The nozzle 3 is connected with the sulfur trioxide raw material device (not shown in the figure) through the feed pipe 2 and the peristaltic pump. The nozzle is made of corrosion-resistant materials, such as polytetrafluoroethylene, 316L stainless steel, high-silicon cast iron, corrosion-resistant alloy materials, etc. The feed pipe 2 pass...

Embodiment 2

[0029] Place the reaction kettle in the water bath of the water bath. 71.4 g of dodecyl diphenyl ether and 300 g of dichloromethane were added to the reactor 1 from the reactant feed port 11 in advance. Take 40.5 grams of sulfur trioxide according to the molar ratio of dodecyl diphenyl ether to sulfur trioxide 1:2.2, and add 532 grams of dichloromethane to prepare a dichloromethane solution of sulfur trioxide with a mass fraction of 7%. The reaction kettle 1 was placed in a water bath, the temperature of the water bath was controlled at 40°C, and it was transported to the nozzle 3 according to the feeding speed of the peristaltic pump 40r / min for spray sulfonation. After the sulfonation was completed, the reaction system was kept warm and aged for 1 hour, and samples were taken to measure the acid value.

[0030] Add an appropriate amount of sodium hydroxide solution to the reaction system for neutralization, the volume of the sodium hydroxide solution is 8 times the volume o...

Embodiment 3

[0032] Place the reaction kettle in the water bath of the water bath. Add 74.07 g of dodecyl diphenyl ether and 300 g of dichloromethane in advance. Prepare 40.1 grams of sulfur trioxide according to the molar ratio of 1:2.1, and add 530 grams of solvent to prepare a 7% dichloromethane solution. The reaction kettle 1 was placed in a water bath, the temperature of the water bath was controlled at 30° C., and the spray sulfonation was carried out at a feeding speed of 50 r / min by a peristaltic pump. After the sulfonation is completed, heat preservation and aging for 1 hour, and take samples to measure the acid value.

[0033] Add an appropriate amount of sodium hydroxide solution to the reaction system for neutralization, the volume of the sodium hydroxide solution is 8 times the volume of the reaction system, extract and filter, and vacuum-dry the obtained aqueous phase to obtain the crude sodium salt of dodecyl diphenyl ether disulfonate product, then dissolve the crude prod...

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Abstract

The invention discloses a preparation process for synthesizing sodium dodecyl diphenyl ether disulfonate. The preparation process comprises the following steps: adding dodecyl diphenyl ether and a solvent into a reaction kettle in advance until the liquid level submerges a nozzle arranged in the reaction kettle, conveying a sulfonating agent to the nozzle, carrying out spraying and feeding under the liquid level, reacting the atomized sulfonating agent with the dodecyl diphenyl ether, and adding a sodium hydroxide solution after the reaction is finished to generate sodium dodecyl diphenyl ether disulfonate. The invention further discloses a reaction device for synthesizing the sodium dodecyl diphenyl ether disulfonate. Liquid sulfur trioxide is fed under liquid through the nozzle, so thaton one hand, volatilization of the liquid sulfur trioxide can be avoided; on the other hand, the contact area of reaction materials and sulfur trioxide is increased through atomization of the liquid sulfur trioxide, and local peroxidation is avoided; and therefore, the obtained sodium dodecyl diphenyl ether disulfonate finished product is light in color and is transparent.

Description

technical field [0001] The invention relates to a sulfonation reaction, in particular to a preparation process for synthesizing dodecyl diphenyl ether disulfonic acid sodium salt. The invention also relates to the reaction device used in the process. Background technique [0002] Sulfur trioxide (SO 3 ) sulfonation is currently performed with SO 3 A direct sulfonation reaction method of aromatic hydrocarbons as a sulfonating agent, divided into gaseous SO according to the different forms of the sulfonating agent 3 Sulfonation method, liquid SO 3 Sulfonation method, SO 3 Solvent sulfonation and SO 3 Complex positioning sulfonation method. Among them, liquid SO 3 The sulfonation method has high yield, no waste acid, simple post-treatment, and is suitable for sulfonation of inactive aromatic compounds. However, the method is to drop liquid SO 3 Adding reactants for reaction may easily cause local peroxidation to form black substances. Usually, the produced products are...

Claims

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Application Information

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IPC IPC(8): C07C309/42C07C303/06C07C303/32B01J19/18
CPCC07C303/06C07C303/32B01J19/18C07C309/42
Inventor 王汉锋张晓明谢亚飞聂秀梅
Owner 南雄市汉科化工科技有限公司
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