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Recycling method of triethylamine and methylbenzene in combination of organophosphorus ester

A technology of organic phosphate ester and recovery method, which is applied in organic chemistry, amino compound purification/separation, distillation purification/separation, etc., can solve the problems of long recovery time, large equipment investment, and complicated process, so as to shorten the recovery time and reduce the Production cost, the effect of reducing environmental pollution

Active Publication Date: 2014-08-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high price and high toxicity of triethylamine, it is discharged together with toluene as a waste liquid, causing serious pollution and causing great pressure on the treatment of three wastes
[0003] CN1234373A discloses the purification of waste water containing triethylamine and other amines produced in the production process of phosphate esters by ozonation. These methods can achieve the purpose of removing ammonia nitrogen, but cannot effectively recycle organic amines in sewage use
CN101905941A discloses the use of oxidation, catalytic pyrolysis and separation and purification to convert triethylamine in sewage into diethylhydroxylamine and then achieve the purpose of recycling triethylamine in sewage, but the process is complicated, the recovery time is long, and equipment investment Many, the cost of conversion and recycling is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) The industrial waste liquid produced after 280ml of synthetic organophosphate is placed in a 500ml three-necked flask with a thermometer and a stirring device, at normal temperature, stirring;

[0021] (2) Slowly add industrial calcium oxide powder under stirring, measure the pH value of the solution with pH test paper after reacting for 10 minutes; If the pH value is 9-10, continue to add industrial powdered calcium oxide. After reacting for 10 minutes, when the measured pH value is about 11-12, stop processing industrial powdered calcium oxide and continue stirring for 10 minutes. Calcium oxide 35.5g;

[0022] (3) Remove the stirring device on the three-necked flask, add a heating mantle, a thorn-shaped distillation column, a condenser and other distillation devices, heat and distill, and collect the distillate at 60-120 ° C, namely triethylamine, water, and toluene.

[0023] (4) Put the collected triethylamine, toluene, and water mixed solution into another thre...

Embodiment 2

[0025] (1) The industrial waste liquid produced after 300ml of synthetic organophosphate is placed in a 500ml three-necked flask with a thermometer and a stirring device, at normal temperature, stirring;

[0026] (2) Slowly add industrial block calcium oxide under stirring, and measure the pH value of the solution with pH test paper after reacting for 10 minutes; the pH value is about 9, continue to add industrial block calcium oxide, stir for 10 minutes, and measure the pH value of the solution About 9 to 10, then continue to add industrial block calcium oxide, after 10 minutes of reaction, when the measured pH value is about 11 to 12, stop adding industrial block calcium oxide, continue stirring for 10 minutes, and process industrial block in the whole process Calcium oxide 45g;

[0027] (3) Remove the stirring device on the three-necked flask, add a heating mantle, a thorn-shaped distillation column, a condenser and other distillation devices, heat and distill, and collect ...

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Abstract

A recycling method of triethylamine and methylbenzene in combination of organophosphorus ester relates to technology for recycling triethylamine and methylbenzene from industrial waste water produced in combination of organophosphorus ester and resolves the technical problem of recycling of triethylamine and methylbenzene in industrial waste liquid. The recycling method includes the following steps: placing waste liquid produced combination of organophosphorus ester in a reactor, adding solid calcium oxide in stirring mode, conducting complete reaction, conducting heating and distillation after the pH value achieves 11-12, collecting distillate of 60-120 DEG C, adding a drying agent into collected mixed liquid of triethylamine, methylbenzene and water to conduct heating and backflow for 48 min to remove moisture and then conducting distillation again to obtain triethylamine and methylbenzene. The recycling rate is no smaller than 98%, methylbenzene is smaller than 0.005ppm in the industrial waste liquid after triethylamine and methylbenzene are recycled, and the recycled mixed liquid of triethylamine and methylbenzene can be applied to combination of organophosphorus ester.

Description

technical field [0001] The present invention relates to a process for recovering triethylamine and toluene in the synthesis of organophosphate, in particular to the recovery of triethylamine and toluene in waste water after the synthesis of organophosphate as an intermediate product in the synthesis of organophosphate polypropylene nucleating agent method. Background technique [0002] In chemical production, for industrial wastewater containing a variety of organic substances, it is very difficult to recover the organic substances in the wastewater and reduce the chroma and organic substances in the wastewater to the discharge standard. CN1803900 provides a mixed organophosphate polypropylene nucleating agent and its preparation method, which is applied to the modification of polypropylene resin. The synthesis of this organophosphate polypropylene nucleating agent is the reaction of substituted aryl phenols with a phosphorylating agent, esterification, hydrolysis, and salt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/05C07C209/86C07C15/06C07C7/04
Inventor 李伟徐耀辉顾民吕静兰褚海斌
Owner CHINA PETROLEUM & CHEM CORP