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
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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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