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Recovery and treatment method of rough steaming residue from p-cresol production

A technology for recovery and treatment of p-cresol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as waste, inability to carry out distillation, inability to distill out phenol, etc., and achieve obvious economic benefits and no Discharge of three wastes and the effect of solving process limitations

Active Publication Date: 2015-11-18
LIANYUNGANG KEMING CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, a premise of using direct high-temperature distillation for the rough steaming residue treatment is that there should not be too much sodium toluenesulfonate in it, otherwise the sodium toluenesulfonate will foam at high temperature during distillation and the distillation cannot be carried out. The presence and encapsulation of salt will prevent some phenols from being distilled
Therefore, the current residue treatment method has great limitations. Based on the fact that the alkali fusion reaction is completely normal or good, as long as the production is abnormal, a little more sodium toluenesulfonate will not be able to be processed in the alkali fusion material.
Moreover, only part of the mixed phenols were recovered, and the sodium toluenesulfonate with the same high economic value was not recovered, which is actually a waste

Method used

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  • Recovery and treatment method of rough steaming residue from p-cresol production

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Experimental program
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Effect test

Embodiment 1

[0020] The recovery treatment method of this p-cresol production crude steaming residue, its step comprises:

[0021] (1) the rough steaming residue is put into the ground tank and stirred and cooled to normal temperature, then pumped to the filter tank for vacuum suction filtration, and the sodium toluenesulfonate solid obtained by suction filtration is directly recycled;

[0022] (2) the filtrate obtained by suction filtration is delivered to the reactor, and the pH value is adjusted to 7.5 with sulfuric acid;

[0023] (3) Add toluene to the filtrate according to the amount of 70 g of toluene per 100 g of filtrate, and stir at about 60 ° C for 30 minutes to extract, so that the phenol in the filtrate is extracted by toluene as much as possible;

[0024] (4) Standing for stratification, taking the upper layer of toluene to extract the organic phase, distilling, separating and recovering toluene and mixed phenols, taking the lower layer of water phase and putting it into an ev...

Embodiment 2

[0028] The recovery treatment method of this p-cresol production crude steaming residue, its step comprises:

[0029] (1) the rough steaming residue is put into the ground tank and stirred and cooled to normal temperature, then pumped to the filter tank for vacuum suction filtration, and the sodium toluenesulfonate solid obtained by suction filtration is directly recycled;

[0030] (2) the filtrate obtained by suction filtration is delivered to the reactor, and the pH value is adjusted to 7 with sulfuric acid;

[0031] (3) Add toluene to the filtrate according to the amount of adding 50g toluene per 100g filtrate, and stir at 50°C for 60 minutes to extract, so that the phenol in the filtrate is extracted by toluene as much as possible;

[0032] (4) Stand for stratification, take the upper layer of toluene to extract the organic phase, distill, separate and recover toluene and mixed phenols, take the lower layer of water phase and put it into an evaporation concentration kettle...

Embodiment 3

[0036] The recovery treatment method of this p-cresol production crude steaming residue, its step comprises:

[0037] (1) the rough steaming residue is put into the ground tank and stirred and cooled to normal temperature, then pumped to the filter tank for vacuum suction filtration, and the sodium toluenesulfonate solid obtained by suction filtration is directly recycled;

[0038] (2) the filtrate obtained by suction filtration is delivered to the reactor, and the pH value is adjusted to 8 with sulfuric acid;

[0039] (3) Add toluene to the filtrate according to the amount of adding 80g toluene per 100g filtrate, and stir at 70°C for 10 minutes to extract, so that the phenol in the filtrate is extracted by toluene as much as possible;

[0040] (4) standing for stratification, extracting the organic phase with toluene from the upper layer, distilling, separating and recovering toluene and mixed phenols, taking the lower layer of water phase and putting it into an evaporative c...

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Abstract

The invention provides a paracresol production crude distillation residue recovery treatment method which comprises the following steps: extracting crude distillation residues with toluene, stratifying, distilling the supernatant organic phase to respectively recover toluene and mixed phenols, and concentrating the understratum water phase by evaporation to obtain the sodium toluene sulfonate solid. The method has the following advantages: 1. environmental protection: the extraction-concentration-crystallization technique is adopted to treat the residues, thereby solving the technical limitation and ensuring immediate treatment of the residues and no discharge of three wastes; and 2. higher economical efficiency: the direct high-temperature distillation technique and water washing technique can only recover part of phenols in the residues and can not easily recover the sodium toluene sulfonate, but the method provided by the invention can respectively recover most phenols and sodium toluene sulfonate in the residues, and thus, has obvious economic benefit.

Description

technical field [0001] The invention relates to a method for recovering and treating p-cresol production crude steaming residue. Background technique [0002] In the production of p-cresol, the sodium salt of toluenesulfonate reacts with sodium hydroxide at high temperature to generate sodium cresol. After adding water for digestion, the aqueous solution of sodium phenate is sulfurized with dioxide, and the two phases are separated to obtain acidic crude phenol. After the crude phenol is adjusted to a pH value of 7-8 with aqueous sodium carbonate, the aqueous phase is separated to obtain basic crude phenol. Alkaline crude phenol distillation (coarse steaming for short) removes water and residue to obtain mixed phenols, and then obtains p-cresol products through rectification. [0003] Sodium cresyl must be left to stand for stratification after being sulfurated with carbon dioxide and adjusting the pH value with aqueous sodium carbonate. During stratification, the crude phe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/68C07C37/72C07C39/07C07C303/44C07C309/30
CPCC07C37/68C07C37/72C07C39/07C07C303/44C07C309/30
Inventor 彭俊涛陈敬财
Owner LIANYUNGANG KEMING CHEM CO LTD