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Method for synthesizing diethylene glycol methyl hexyl ether

A technology of diethylene glycol and methylhexyl ether, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of ether, etc. It can solve the problems of difficult to realize large-scale production, difficult control of sodium alkoxide reaction, low conversion rate of sodium alkoxide, etc. problems, to achieve the effect of low toxicity, high yield and high purity

Inactive Publication Date: 2017-05-10
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the above-mentioned third method can overcome the corrosivity of sulfuric acid in the first two methods, the high price of dimethyl carbonate, the large shortcoming of production cost, but because the third method generates the reaction of sodium alkoxide is not easy to control, the reaction of converting into sodium alkoxide The conversion rate is not high, it is difficult to realize large-scale production, so for actual production, the solution to be solved is to design a kind of synthetic diethylene glycol methyl with low toxicity, easy control of the reaction process, easy realization of large-scale production, and comprehensive beneficial effects. Hexyl ether route

Method used

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  • Method for synthesizing diethylene glycol methyl hexyl ether
  • Method for synthesizing diethylene glycol methyl hexyl ether
  • Method for synthesizing diethylene glycol methyl hexyl ether

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Embodiment 1

[0023] Embodiment one: a kind of method for synthesizing diethylene glycol methylhexyl ether provided by the present invention comprises the following steps, (1) raw material sodium hydroxide is placed in the reactor, then dilute hydrochloric acid solution is slowly added dropwise into the reactor In the reaction, the reaction generates sodium chloride, and the chemical reaction equation is:

[0024] NaOH+HCl→NaCl+H 2 O;

[0025] (2) Add diethylene glycol monohexyl ether dropwise to the reaction kettle in step (1), heat the reaction kettle to 80° C., and continuously feed hydrogen into the reaction kettle, and connect the reaction kettle to a reflux device to recover the reaction kettle Hydrochloric acid, the sodium alkoxide intermediate product that obtains is passed in the next stage reactor, and described chemical reaction equation is:

[0026] C 6 h 13 (OCH 2 CH 2 ) 2 OH+NaCl→C 6 h 13 (OCH 2 CH 2 ) 2 ONa+HCl;

[0027] (3) Coating graphite layer in the secondar...

Embodiment 2

[0038] Embodiment two: the method for synthesizing diethylene glycol methylhexyl ether disclosed by the present invention comprises the following steps, (1) putting the raw material sodium hydroxide in the reactor, then slowly adding dilute hydrochloric acid solution dropwise into the reactor for reaction The mass ratio of sodium hydroxide and hydrochloric acid is 1:0.5 to react to generate sodium chloride, and the end point of the reaction can be controlled by a pH indicator. The sufficient time for this reaction is 2h, and the chemical reaction equation is:

[0039] NaOH+HCl→NaCl+H 2 O;

[0040] (2) Add diethylene glycol monohexyl ether dropwise to the reactor in step (1), heat the reactor to 120°C, and continuously feed hydrogen into the reactor, the flow rate of hydrogen is 3ml / min, diethylene glycol The mass ratio of glycol monohexyl ether to sodium chloride is 1:1.5, and the reaction kettle is connected with the reflux device to recover the hydrochloric acid generated b...

Embodiment 3

[0052] Embodiment three: the method for synthesizing diethylene glycol methylhexyl ether disclosed by the present invention comprises the following steps, (1) putting the raw material sodium hydroxide in the reactor, then slowly adding dilute hydrochloric acid solution dropwise into the reactor for reaction , the mass ratio of sodium hydroxide and hydrochloric acid is 1:1 and reacts to generate sodium chloride, and the reaction terminal can be controlled by a pH indicator. The sufficient time for this reaction is 1.5h, and the chemical reaction equation is:

[0053] NaOH+HCl→NaCl+H 2 O;

[0054] (2) Add diethylene glycol monohexyl ether dropwise to the reactor in step (1), heat the reactor to 100°C, and continuously feed hydrogen into the reactor, the flow rate of hydrogen is 5ml / min, diethyl ether The mass ratio of glycol monohexyl ether to sodium chloride is 1:2, the reaction kettle is connected with the reflux device to recover the hydrochloric acid generated by the reacti...

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Abstract

The invention discloses a method for synthesizing diethylene glycol methyl hexyl ether. The method comprises the following steps: (1) putting a raw material, namely sodium hydroxide, into a reaction kettle, adding a diluted hydrochloric acid solution into the reaction kettle slowly and dropwise and reacting to produce sodium chloride; (2) adding diethylene glycol monohexyl ether into the reaction kettle in the step (1) dropwise, and introducing the obtained sodium alcoholate intermediate product into the next level of reaction kettle; (3) coating the secondary reaction kettle, in which the sodium alceholate intermediate product is put, with a graphite layer, introducing methyl iodide into the secondary reaction kettle and reacting to obtain a final product, namely the diethylene glycol methyl hexyl ether; (4) after the reaction in the step (3), cooling to room temperature, standing and layering, and performing pressure-reducing filtration on the upper layer liquid to obtain the final product, namely the diethylene glycol methyl hexyl ether. The method has the advantages that the diethylene glycol methyl hexyl ether is synthesized by innovatively adopting the new raw material; the whole synthesis method is stable in reaction and easy to operate; the obtained final product has high yield and high purity; the method is suitable for industrialized production and breaks through bottleneck for commercial popularization of the products.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a method for synthesizing diethylene glycol methylhexyl ether. Background technique [0002] Diethylene glycol methylhexyl ether is a high-boiling organic solvent with excellent performance. It is widely used in the production of dyes, resins, paints, cleaning agents, and special inks. As a precious metal extraction agent, it is also used in the extraction and separation of gold and palladium. , it can be miscible with most alcohols, ketones, ethers, halogenated hydrocarbons, etc., and has good solubility to alkali metal hydroxides, so it also has important applications in organic synthesis. The method for synthesizing diethylene glycol methylhexyl ether at present has: 1) take diethylene glycol monohexyl ether and methyl alcohol or diethylene glycol monomethyl ether and hexanol as raw material, and the concentrated sulfuric acid is the direct etherification method of c...

Claims

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Application Information

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IPC IPC(8): C07C41/01C07C43/11C01D3/04
CPCC07C41/01C01D3/04C07C41/26C07C43/11
Inventor 崔秀云李长江李伟伟史建俊方红霞
Owner HUANGSHAN UNIV
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