Synthesis method of methyl p-toluenesulfonate

A technology of methyl toluenesulfonate and a synthesis method, which is applied in the preparation of sulfonic acid ester, the preparation of sulfonic acid, chemical instruments and methods, etc., can solve problems such as many by-products, equipment corrosion, complicated process, etc. Increase the rate and reduce the effect of poisoning

Active Publication Date: 2019-01-18
南通沃兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The industrial synthesis of methyl p-toluenesulfonate usually uses concentrated sulfuric acid as a catalyst for direct esterification reaction, but there are many by-products when concentrated sulfuric acid is used as a catalyst, and the dilute sulfuric acid produced has serious corrosion on equipment, and the separation of products is complicated and the yield is low , serious pollution and other shortcomings
The reaction conditions are harsh, the process is complicated, and the product yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of synthetic method of methyl p-toluenesulfonate, the method comprises the following steps:

[0020] Step 1. Add 50g of toluene to a four-neck flask with a stirring reflux device, heat up to 120°C, add 35g of concentrated sulfuric acid with a concentration of 98% dropwise under reflux, add dropwise evenly within 30min, and continue heating under reflux;

[0021] Step 2, when no more water is separated from the reflux liquid, react for 4 hours to end the reaction. Lower the temperature and add 10 g of water and 20 g of ethanol as a mixed solvent at 60° C. After the crystals are precipitated, carry out suction filtration under reduced pressure to obtain p-toluenesulfonic acid;

[0022] Step 3. Add 100g of methanol to the reactor, add 3.0g of high-efficiency catalyst Fe-Zn / SBA-15, 100g of p-toluenesulfonic acid, slowly heat up to 70°C, start stirring, heat up to 85°C for reflux reaction for 3h; continue to heat up to 135°C ℃, start to drop 150g methanol;

[0023] ...

Embodiment 2

[0032] Step 3. Add 75g of methanol to the reactor, add 3.0g of high-efficiency catalyst Fe-Zn / SBA-15, 100g of p-toluenesulfonic acid, slowly heat up to 70°C, start stirring, heat up to 85°C for reflux reaction for 3h; continue to heat up to 135°C ℃, start dropwise adding 150g of methanol; the rest of the steps are the same as in Example 1.

Embodiment 3

[0034] Step 3. Add 50g of methanol to the reactor, add 3.0g of high-efficiency catalyst Fe-Zn / SBA-15, 100g of p-toluenesulfonic acid, slowly heat up to 70°C, start stirring, heat up to 85°C for reflux reaction for 3h; continue to heat up to 135°C ℃, start dropwise adding 150g of methanol; the rest of the steps are the same as in Example 1.

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PUM

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Abstract

The invention discloses a synthesis method of methyl p-toluenesulfonate. The synthesis method takes concentrated sulfuric acid, methanol, p-toluene sulfonic acid, FeCl3*H3O, zinc oxide and SBA-15 zeolite as main raw materials; and the methyl p-toluenesulfonate is obtained through a synthesis technology by adopting sulfonic acid esterification of the p-toluene sulfonic acid and methanol under the action of a catalyst Fe/Zn/SBA-15 through sulfonic acid esterification reaction. Compared with a manner of taking pure acid as a catalyst to obtain an unsatisfactory esterification effect and relatively low conversion rate and yield, the synthesis method takes the solid-phase loading catalyst Fe/Zn/SBA-15 to greatly improve the esterification conversion rate and yield of the p-toluene sulfonic acid.

Description

technical field [0001] The invention relates to a method for synthesizing methyl p-toluenesulfonate, which belongs to the field of chemical synthesis. Background technique [0002] Methyl p-toluenesulfonate (Methyl p-toluenesulfonate) CAS: 80-48-8 is an important organic chemical intermediate, mainly used in the synthesis of dyes and medicines. The industrial synthesis of methyl p-toluenesulfonate usually uses concentrated sulfuric acid as a catalyst for direct esterification reaction, but there are many by-products when concentrated sulfuric acid is used as a catalyst, and the dilute sulfuric acid produced has serious corrosion on equipment, and the separation of products is complicated and the yield is low , serious pollution and other shortcomings. The reaction conditions are harsh, the process is complicated, and the product yield is low. Therefore, finding a method for preparing methyl p-toluenesulfonate with simple process conditions, environmental friendliness and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J37/34C07C303/28C07C309/73C07C303/06C07C309/30
CPCB01J29/0333B01J37/343B01J37/346B01J2229/18C07C303/06C07C303/28C07C309/73C07C309/30
Inventor 孙强吴建国万海兵
Owner 南通沃兰化工有限公司
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