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Process for preparing dimethyl sulfate by discontinuous process

A technology of dimethyl sulfate and batch method, which is applied in the preparation of sulfate, organic chemistry and other directions, can solve the problems of methanol market fluctuation and high raw material prices, and achieve the effects of low operating costs, lower energy consumption, and lower consumption.

Inactive Publication Date: 2009-04-15
HANERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention provides a kind of technology simple, the technology that methane oxidizes intermittent method with low operation cost to prepare dimethyl sulfate, to overcome the defects such as high raw material price existing in the traditional preparation technology of dimethyl sulfate, subject to the relatively large fluctuation of methanol market, and The corresponding process parameters are given to provide the basis for further industrialization experiments

Method used

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  • Process for preparing dimethyl sulfate by discontinuous process
  • Process for preparing dimethyl sulfate by discontinuous process
  • Process for preparing dimethyl sulfate by discontinuous process

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Such as figure 1 The process flow shown, weigh 0.2gI 2 , and place it in the autoclave, according to I:SO 3 The molar ratio is 1:430. Measure 30ml of liquid sulfur trioxide with a measuring cylinder, place it in the autoclave, and seal the autoclave. Replace the air in the autoclave three times with argon, then feed Ar-containing methane gas (argon volume percentage is 5%) in the autoclave until the pressure in the autoclave is 3 MPa, heat the autoclave to 175 ° C, stop the reaction after 180 min, and wait for The still temperature is down to room temperature, and its gas phase composition is measured by gas chromatography. After measuring, the gas in the still is emptied, and the still is opened, and the reaction solution therein is poured out and carried out underpressure distillation to obtain dimethyl sulfate, such as figure 2 measured. Depend on image 3 , Figure 4 Determination and calculation showed that the gas-phase methane conversion rate was 47.80%, an...

Embodiment 2

[0034] Weigh 0.3gI 2 , and place it in the autoclave, according to I:SO 3 The molar ratio is 1:288. Measure 30ml of liquid sulfur trioxide with a measuring cylinder, place it in the autoclave, and seal the autoclave. Replace the air in the autoclave three times with argon, then feed Ar-containing methane gas into the autoclave (the volume percentage of argon is 5%) until the pressure in the autoclave is 2 MPa, heat the autoclave to 130 ° C, and stop the reaction after 150 min. The temperature of the kettle was lowered to room temperature, and its gas phase composition was measured by gas chromatography. After the measurement, the gas in the kettle was emptied, and the kettle was opened, and the reaction solution therein was poured out for rectification under reduced pressure. The gas-phase methane conversion rate was measured to be 59.94%, and the yield of dimethyl sulfate was 94.07%.

Embodiment 3

[0036] Take by weighing 0.35g sodium iodide, and it is placed in autoclave, according to I: SO 3 The molar ratio is 1:288, and 17.5 L of gaseous sulfur trioxide is introduced into the autoclave, and the autoclave is sealed. Replace the air in the autoclave with argon three times, then feed Ar-containing civil natural gas (5% by volume of argon) into the autoclave until the pressure in the autoclave is 2MPa, heat the autoclave to 160°C, and stop the reaction after 3min. The temperature of the kettle is lowered to room temperature, and its gas phase composition is measured by gas chromatography. After the measurement, the gas in the kettle is emptied, and the kettle is opened, and the reaction solution therein is poured out for ordinary distillation. The gas-phase methane conversion rate was measured to be 32.37%, and the yield of dimethyl sulfate was 97.71%.

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Abstract

The invention discloses a process for preparing dimethyl sulfate by using a batch process, which belongs to the field of preparing dimethyl sulfate. According to a molar raio of I: SO3 of 1:86-430, catalyst iodine or iodine compound and sulfur trioxide or compound containing dissociative sulfur trioxide are put into a high pressure reaction kettle; then gas containing methane of about 1-3MPa is led into the high pressure reaction kettle; at the temperature of 130-175 DEG C, the reaction lasts for 3-480min; and then the obtained mixture from the reaction is distilled in liquid phase to get the product dimethyl sulfate. The process has the reaction process which is easy to be controlled, the reaction condition is moderate, the safety is high, and the process is simple and efficient and is applicable to industrial production.

Description

technical field [0001] The invention relates to a process for preparing dimethyl sulfate by a batch method, in particular to a process for preparing dimethyl sulfate by a batch method of methane oxidation. Background technique [0002] Dimethyl sulfate is an important methylating reagent, which is used as an important raw material for the manufacture of drugs (caffeine, antipyrine, etc.), dyes, and spices. The traditional production process is as follows: methanol reacts with sulfuric acid to generate methyl hydrogen sulfate, and further reacts with methanol to generate dimethyl ether, reacts dimethyl ether with sulfur trioxide to generate dimethyl sulfate, and then undergoes vacuum distillation to obtain the finished product. [0003] It can be seen from the above traditional production process that the production of dimethyl sulfate uses methanol as raw material, and the production cost fluctuates under the influence of methanol price, while the traditional methanol produc...

Claims

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Application Information

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IPC IPC(8): C07C305/08C07C303/24
Inventor 肖钢侯晓峰李锋伟
Owner HANERGY TECH
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