Novel synthetic process of p-phenylene dimethyl ether

A technology of terephthalic ether and a new process, which is applied in the field of new synthesizing terephthalic ether, can solve the problems of high total production cost, high price, increased production cost and the like, and achieves improvement of reaction yield and reduction of production cost. , the effect of reducing the production process

Inactive Publication Date: 2009-01-21
舒景林
View PDF0 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the product mainly has two synthesis routes of methylation of dimethyl sulfate under normal pressure and pressure methylation of methyl halide. The route of methylation of dimethyl sulfate under normal pressure uses hydroquinone as the starting material It is obtained by forming a salt with a strong base in an alkaline medium and then replacing it with dimethyl sulfate. The process yield is high, the product quality is stable, and the reaction conditions are mild. However, the raw material dimethyl sulfate is a highly toxic product, and the price is relatively high. High, and the utilization rate of the methyl group in dimethyl sulfate is only 50%, the remaining methyl group after generating monomethyl sulfate sodium salt no longer participates in the reaction, so the unit consumption of dimethyl sulfate is higher, which not only increases production cost, and increased the difficulty of wastewater treatment; due to the cost of raw materials, haloalkane used in the pressurized methylation process of halomethane is cheap and easy-to-get monochloromethane, and hydroquinone in a strong alkaline medium under pressure The raw material monochloromethane used in this process is cheap, but the reaction needs to be carried out under pressure, the equipment investment is high, and the reaction yield is low, and the total production cost is still high; the above two processes all have a common The disadvantage is that there are still some monomethylated products p-hydroxyanisole in the product, and it needs to be further refined to obtain high-content p-phenylenedimethyl ether finished product

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Novel synthetic process of p-phenylene dimethyl ether
  • Novel synthetic process of p-phenylene dimethyl ether
  • Novel synthetic process of p-phenylene dimethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 300ml of water, 30g of hydroquinone, and 55g of sodium hydroxide with a concentration of 30% into a 500ml four-neck flask, stir and raise the temperature to 55°C in a water bath, and slowly add 45g of dimethyl sulfate dropwise at this temperature for about half an hour , after the dropwise addition, keep warm for one hour, slowly add 25g of 30% sodium hydroxide solution about 15-20 minutes after the finish of the keep warm, then continue to heat up to 102-103°C for 5 hours, after the reflux, turn the reflux device Change it to a distillation device, and feed direct steam to carry out distillation at the same time. After the distillate is clarified and no product is distilled out, the reaction is over. Collect the distillate, filter and dry after cooling, and obtain 31g of the product, with a yield of 90.2%. It is 55.3°C.

Embodiment 2

[0024] Add 300ml of water, 30g of hydroquinone, and 65g of sodium hydroxide with a concentration of 30% into a 500ml four-neck flask, stir and raise the temperature to 55°C in a water bath, and slowly add 45g of dimethyl sulfate dropwise at this temperature for about half an hour After the dropwise addition, keep the temperature for one hour, slowly add 15g of 30% sodium hydroxide solution about 15-20 minutes after the heat preservation, then continue to heat up to 102-103°C for 5 hours, after the reflux, turn the reflux device Change it to a distillation unit, and feed direct steam to carry out distillation simultaneously. After the distillate is clarified and no product is distilled out, the reaction is finished. The distillate is collected, filtered and dried after cooling to obtain 29.8g of product, and the yield is 86.7%. The freezing point is 54.8°C.

Embodiment 3

[0026] Add 300ml of water, 30g of hydroquinone, and 55g of sodium hydroxide with a concentration of 30% into a 500ml four-neck flask, stir and raise the temperature to 55°C in a water bath, and slowly add 50g of dimethyl sulfate dropwise at this temperature for about half an hour , after the dropwise addition, keep warm for one hour, slowly add 25g of 30% sodium hydroxide solution about 15-20 minutes after the finish of the keep warm, then continue to heat up to 102-103°C for 5 hours, after the reflux, turn the reflux device Change it to a distillation unit, and feed direct steam to carry out distillation simultaneously. After the distillate is clarified and no product is distilled out, the reaction is finished. Collect the distillate, filter and dry after cooling, and obtain 30.7g of product, with a yield of 89.3%. The freezing point is 55.4°C.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
freezing pointaaaaaaaaaa
freezing pointaaaaaaaaaa
freezing pointaaaaaaaaaa
Login to view more

Abstract

The invention relates to a novel process for synthesizing p-xylene glycol dimethyl ether. The synthesis method takes hydrochinone and dimethyl sulfate as raw materials, and obtains the product through substitution inside an alkaline medium. Moreover, the synthesis method has the technological characteristics that by means of the principle of equilibrium shifting, the product is moved out of a reaction system during reaction, thereby accelerating reaction and ensuring complete reaction; in the prior synthesis process, the auxiliary raw material dimethyl sulfate no longer participates in reaction when reacted to generate monomethyl sodium sulfate, and the theoretical utilization rate of dimethyl sulfate is only 50 percent; therefore, the method greatly increases the utilization rate of dimethyl sulfate, and reduces the consumption of dimethyl sulfate by 40 percent; meanwhile, reaction yield is also increased to a certain extent; moreover, because the process makes use of the special characteristics of azeotropic distillation of the product and water, the product obtained during reaction can be moved out in time, while the reaction raw materials and intermediate product para hydroxyanisole are stored in a reactor in the form of sodium salts in the alkaline medium and do not enter the product when distilled out along with water vapor; therefore, the product has extremely high purity and can be obtained without adopting the prior alcohol refining; and the novel process ensures greatly simplified production process, higher production safety, lower production cost and labor intensity and better operating environment for workers, thereby having significant social benefit and economic benefit.

Description

technical field [0001] The invention relates to a new process for synthesizing p-xylylene dimethyl ether. More specifically, it uses the principle of equilibrium movement to move the product out of the reaction system at the same time as the reaction. While speeding up the reaction and improving the utilization rate and yield of raw materials, the cumbersome post-treatment and refining process in the original process is reduced, and high-quality products are obtained. P-Phenylene Dimethyl Ether Products. Background technique [0002] P-xylylene dimethyl ether is also known as 1,4-xylylene dimethyl ether, p-dimethoxybenzene, hydroquinone dimethyl ether and hydroquinone dimethyl ether, etc. Its molecular formula is: C 8 h 10 o 2 , Molecular weight: 138.17, with aromatic smell, is a relatively common organic synthetic raw material, often used in the synthesis and preparation of spices, daily chemicals, food, tobacco flavors, etc., and can also be used as an anti-wind erosion...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/205C07C41/16
Inventor 舒景林
Owner 舒景林
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products