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Method used of high efficiency separation and purification of 1-methylnaphthalene

A methylnaphthalene, high-efficiency technology, applied in chemical instruments and methods, distillation purification/separation, crystallization purification/separation, etc., to achieve high temperature resistance, simple separation, and low price

Active Publication Date: 2019-02-01
PENG CHEN NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the yield of the same product needs further improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for efficiently separating and purifying 1-methylnaphthalene, comprising the following steps:

[0026] (1) Dissolve the magnesium-based hydrotalcite material in an aqueous solution of polyethylene glycol, slowly raise the temperature to 40-50°C, stir and mix for 1 hour, then cool to room temperature, and filter to obtain a polyethylene glycol-modified magnesium-based hydrotalcite material ; Wherein, the mass ratio of magnesium-based hydrotalcite material to polyethylene glycol is 4:0.13;

[0027] (2) Prepare sodium edetate solution, add the polyethylene glycol-modified magnesium-based hydrotalcite material prepared above, stir and mix for 20 minutes at 4000 rpm, then add zinc chloride, stir until the solid dissolves, A dispersion is obtained; the dispersion is concentrated and then vacuum-dried to obtain a catalyst; wherein, the mass ratio of sodium edetate, polyethylene glycol-modified magnesium-based hydrotalcite material, and zinc chloride is 0.3:2:0.5 ;

...

Embodiment 2

[0032] A method for efficiently separating and purifying 1-methylnaphthalene, comprising the following steps:

[0033] (1) Dissolving the magnesium-based hydrotalcite material in an aqueous solution of polyethylene glycol, slowly raising the temperature to 40-50° C., stirring and mixing for 5 hours, cooling to room temperature, and filtering to obtain a polyethylene glycol-modified magnesium-based hydrotalcite material; Among them, the mass ratio of magnesium-based hydrotalcite material to polyethylene glycol is 4:0.16;

[0034] (2) Prepare sodium edetate solution, add the polyethylene glycol-modified magnesium-based hydrotalcite material prepared above, stir and mix for 60 minutes at 7000 rpm, then add zinc chloride, stir until the solid dissolves, A dispersion is obtained; the dispersion is concentrated and then vacuum-dried to obtain a catalyst; wherein, the mass ratio of sodium edetate, polyethylene glycol-modified magnesium-based hydrotalcite material, and zinc chloride i...

Embodiment 3

[0039] A method for efficiently separating and purifying 1-methylnaphthalene, comprising the following steps:

[0040] (1) Dissolve the magnesium-based hydrotalcite material in an aqueous solution of polyethylene glycol, slowly raise the temperature to 40-50°C, stir and mix for 1.5 hours, then cool to room temperature, and filter to obtain polyethylene glycol-modified magnesium-based hydrotalcite Material; Wherein, the mass ratio of magnesium-based hydrotalcite material, polyethylene glycol is 4:0.14;

[0041] (2) Prepare sodium edetate solution, add the polyethylene glycol-modified magnesium-based hydrotalcite material prepared above, stir and mix for 30 minutes at 4500 rpm, then add zinc chloride, stir until the solid dissolves, A dispersion is obtained; the dispersion is concentrated and then vacuum-dried to obtain a catalyst; wherein, the mass ratio of sodium edetate, polyethylene glycol-modified magnesium-based hydrotalcite material, and zinc chloride is 0.35:2:0.5 ;

...

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PUM

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Abstract

The invention discloses a method used for high efficiency separation and purification of 1-methylnaphthalene. The method comprises following steps: firstly, magnesium-based hydrotalcite is taken as araw material, polyethylene glycol is adopted for surface modification, sodium ethylene diamine tetracetate and zinc chloride are added for modification so as to obtain a catalyst; naphthalene oil fractions are subjected to sulphur removing and primary distillation, and 230 to 270 DEG C fractions are collected, the catalyst is added into the collected fractions for reaction, and an obtained filtrate is collected; the filtrate is subjected to intermittent vacuum rectification, and 237 to 241 DEG C crystallizable fractions and 241 to 245 DEG C noncrystallizable fractions are collected; the collected crystallizable fractions are refrigerated to -10 to -20 DEG C, and are subjected to centrifugation processing, and an obtained filtered solution is collected; the filtered solution and the noncrystallizable fractions are mixed, and are washed with concentrated sulfuric acid with a mass concentration of 95 to 98%, alkali neutralization is carried out, washing and removing of water are carried out, fractionation is carried out in a distillation column, and 241 DEG C lower fractions are collected, and are subjected to low temperature refrigeration to remove crystals so as to obtain 1-methylnaphthalene. The method is simple in operation, and high in product yield and purity.

Description

technical field [0001] The invention relates to the field of preparation of methylnaphthalene, in particular to a method for efficiently separating and purifying 1-methylnaphthalene. Background technique [0002] 1-Methylnaphthalene, colorless oily liquid, has a smell similar to naphthalene, insoluble in water, soluble in most organic solvents such as ethanol and ether. Store in a cool, ventilated warehouse. Keep away from fire and heat sources. The storage temperature should not exceed 32°C, and the relative humidity should not exceed 80%. 1-Methylnaphthalene can be used as a raw material for organic synthesis such as surfactants, water reducers, dispersants, and drugs. It can be used as a printing and dyeing carrier for polyvinyl chloride fiber and polyester, as a heat carrier and solvent, as a surfactant, as an extraction agent for sulfur, and as a raw material for the production of plasticizers and fiber dyeing aids. [0003] At present, the preparation method of 1-m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07C7/00C07C7/04C07C7/14C07C15/24
CPCB01J31/26C07C7/005C07C7/04C07C7/14C07C15/24
Inventor 谈勇谈俊江晓龙
Owner PENG CHEN NEW MATERIALS TECH CO LTD
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