Method for separating and purifying benzenediol isomer

A technology for purifying catechol and isomers, which is applied in the field of separating and purifying catechol isomers, and can solve the problem of increased investment in solvent ratio production equipment, undisclosed crystallization and purification of catechol, and different crystallization and purification methods. problems, to achieve the effect of reducing investment in production equipment, increasing dissolving capacity, and reducing production costs

Pending Publication Date: 2022-03-11
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, US4239921 (A), CN102643169A disclose a kind of technology of toluene solvent crystallization and purification of resorcinol, but the low boiling point of the used solvent toluene will lead to excessive volatilization loss in the production process, and the high proportion of solvent will also lead to increased investment in production equipment. Large, high production cost, and this technology is mainly suitable for the purification of crude resorcinol obtained by the synthesis method. At the same time, this technology is only for the purification of resorcinol, and it is not disclosed that it can be used for Crystallization and purification of diphenols, the crystallization and purification methods of the two are obviously different

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  • Method for separating and purifying benzenediol isomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0033](1) The aromatic hydrocarbon solvent is a benzene solvent with a boiling point of 136-176°C, for example: the aromatic hydrocarbon solvent includes but not limited to ethylbenzene, xylene isomers, trimethylbenzene isomers, , At least one of the isomers of propylbenzene and methylethylbenzene.

[0034] (2) The polar solvent uses alcohols with a boiling point of 105-176°C, ketones with a boiling point of 105-176°C or esters with a boiling point of 105-176°C; the alcohols include but are not limited to n-butyl At least one of alcohol, isobutanol, methyl isobutyl carbinol (abbreviated as MIBC), n-pentanol, isoamyl alcohol, n-hexanol, n-heptanol, 2-heptanol; the ketones include but Not limited to at least one of methyl isobutyl ketone and cyclohexanone; the esters include but not limited to at least one of n-butyl acetate, isobutyl acetate, n-pentyl acetate, and isoamyl acetate .

[0035] (3) The crude product of catechol can be the crude product of catechol with a purity o...

Embodiment 1

[0046] A method for separating and purifying hydroquinone isomers is used to separate and purify hydroquinone monomers from a certain gasified phenol slag purchased in the market. The components of the gasified phenol slag are shown in Table 1 below:

[0047] Table 1

[0048] Components of gasified phenol residue Content / wt% Catechol 31.4 Resorcinol 25.1 Quinol 16.8 4-Methylcatechol 16.2 benzoic acid 3.0 2-naphthol 1.5 2-Methylquinoline 1.3 Trimethylphenol 0.4 5-indanol 1.6 Ethyl quinone 2.7

[0049] The method for separating and purifying hydroquinone isomers may comprise the following steps:

[0050] Step A1, rectification: Take 20kg of the above gasified phenol slag and carry out vacuum rectification, the pressure at the top of the tower is 10kPa absolute pressure, the theoretical plate of the rectification tower is 30, the reflux ratio is fixed at 20, and the cooling medium at the top of the tower i...

Embodiment 2

[0053] A method for separating and purifying hydroquinone isomers, used to separate and purify hydroquinone monomers from the gasified phenol slag described in Embodiment 1 of the present invention, may include the following steps:

[0054] Step B1 is the same as Step A1 in Embodiment 1 of the present invention.

[0055] Step B2: Add 80 g of cumene solvent to 100 g of the crude catechol product, heat to dissolve the material completely, slowly cool down to 50° C. for crystallization, keep for 2 hours, separate by suction filtration to obtain 75 g of filter cake, and then filter the The cake was dried under vacuum at 100°C to obtain 64 g of pure catechol product. After testing: the catechol content of the pure catechol product is 99.9wt%.

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Abstract

The invention discloses a method for separating and purifying a benzenediol isomer. The method comprises the following steps: crystallizing and purifying at least one of a catechol crude product, a hydroquinone crude product or a resorcinol crude product by adopting a solvent crystallization method; the catechol crude product is subjected to crystallization purification by adopting an aromatic hydrocarbon solvent or a mixed solvent, the hydroquinone crude product is subjected to crystallization purification by adopting a polar solvent or a mixed solvent, the resorcinol crude product is subjected to crystallization purification by adopting a mixed solvent, solid-liquid separation is performed after crystallization to remove a solution so as to obtain a filter cake, and then the filter cake is subjected to vacuum drying at a melting point, so that the product is obtained. A pure product with the content of 99% or above can be obtained. According to the method, the benzenediol monomer product with the purity of 99% or above can be separated and purified, the dissolving capacity of the solvent is improved, the volatilization loss of the solvent is reduced, the solvent proportion is reduced, the energy consumption of solvent recovery is saved, the investment of production equipment is reduced, and the whole separation and purification process is mild in condition, simple to operate, low in production cost and suitable for industrial production. And the economic benefit is improved.

Description

technical field [0001] The invention relates to the technical field of gasification phenol processing, in particular to a method for separating and purifying hydroquinone isomers. Background technique [0002] Gasified phenol slag is rich in quinone isomers with high added value, accounting for 5-10% of the raw material of gasified phenol. In gasified phenol raw materials, after small cresols and xylenols are extracted, useful diphenols are enriched in the phenol residue, and the total content of valuable isomers usually reaches more than 50% of the phenol residue. [0003] Since there are as many as dozens of diphenol isomers, such as quinone, methylquinone, ethylquinone, dimethylquinone, etc. contained in the gasified phenol residue, the composition is complex and the boiling point Very close, for example, the difference between the boiling points of resorcinol and hydroquinone is only 5°C, and it is impossible to directly separate resorcinol and hydroquinone by rectifica...

Claims

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Application Information

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IPC IPC(8): C07C37/84C07C39/08
CPCC07C37/84C07B2200/09C07C39/08
Inventor 熊杰明岳爱鹏江浩何运良
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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