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Comprehensive treatment method of high-boiling residues

A comprehensive treatment and high boiling technology, applied in the direction of organic chemistry, can solve the problems of complex reaction, high reaction temperature, high cost of raw materials, etc., and achieve the effect of simple production method, high economic benefit and high use value

Active Publication Date: 2020-12-29
山东瑞康精化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN1810800A discloses a synthetic method of rhodamine B, which utilizes m-hydroxyl N,N-diethylaniline and anhydrous phthalic anhydride condensation reaction to To prepare rhodamine B, the cost of raw materials required for the reaction is high, the reaction is complicated, and the reaction temperature is relatively high, which is 170-180°C, and m-hydroxy N,N-diethylaniline needs to be added in 5 times; the patent involves The purity of the raw materials is high, and it is not a high-boiler that is difficult to handle

Method used

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  • Comprehensive treatment method of high-boiling residues
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  • Comprehensive treatment method of high-boiling residues

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Experimental program
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Effect test

Embodiment 1

[0040] Include the following steps:

[0041] (1) Dissolution and water separation: put into the dissolution kettle the high boiler (1565Kg) containing 40.2% 4-diethylamino ketoacid, 39.8% rhodamine B (1565Kg) and toluene (5477Kg) / min speed stirring and dissolving for 1.5 hours. After the dissolution is complete, let it stand for 30 minutes, separate the lower water layer, transfer the water layer to the waste water storage tank and enter the waste water treatment system, raise the temperature to 100°C, use a water separator to evaporate all the water in the high boiling matter, and make the reaction system The water content in it is less than 0.2%.

[0042] (2) Synthetic reaction: transfer the material to the reaction kettle after water separation, put (330Kg) m-hydroxyl N,N-diethylaniline with a concentration greater than 98.5% into the reaction kettle, stir at a speed of 100r / min, and control the temperature constantly 100°C, pressure 1.3Mpa, residence time 4.5 hours.

...

Embodiment 2

[0047] Include the following steps:

[0048] (1) Dissolution and water separation: put into the dissolution kettle the high boiler (1744Kg) containing 40.1% 4-diethylamino ketoacid, 40% rhodamine B (1744Kg) and toluene (6452Kg) / min speed stirring and dissolving for 2 hours. After the dissolution is complete, let it stand for 30 minutes, separate the lower water layer, transfer the water layer to the waste water storage tank and enter the waste water treatment system, raise the temperature to 100°C, and use a water separator to evaporate all the water in the high boiling matter to make the high boiling point The moisture content of the material is less than 0.2%.

[0049] (2) Synthesis reaction: transfer the material to the reactor after water separation, put (363Kg) m-hydroxy N,N-diethylaniline with a concentration greater than 98.5% into the reactor, stir at a speed of 100r / min, and control the temperature at a constant temperature of 110 °C, pressure 1.3Mpa, residence tim...

Embodiment 3

[0054] Include the following steps:

[0055] (1) Dissolution and water separation: put into the dissolution kettle the high boiler (1891Kg) containing 40.1% 4-diethylamino ketoacid, 39.9% rhodamine B (1891Kg) and toluene (6800Kg) / min speed stirring and dissolving for 2.5 hours. After the dissolution is complete, let it stand for 30 minutes, separate the lower water layer, transfer the water layer to the waste water storage tank and enter the waste water treatment system, raise the temperature to 100°C, and use a water separator to evaporate all the water in the high boiling matter to make the high boiling point The moisture content of the material is less than 0.2%.

[0056] (2) Synthesis reaction: transfer the material to the reaction kettle after water separation, put (396Kg) m-hydroxyl N,N-diethylaniline with a concentration greater than 98.5% into the reaction kettle, stir at a speed of 100r / min, and control the temperature constantly 115°C, pressure 1.5Mpa, residence t...

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Abstract

The invention provides a comprehensive treatment method of a high-boiling residue, which comprises the following steps: dissolving and separating water, and carrying out synthetic reaction. Accordingto the method, the substance 4-diethylaminoketo acid in the high-boiling residue is fully utilized in the reaction process, so that the waste of materials and the pollution to the environment are effectively avoided, and meanwhile, the generated rhodamine B has very high economic and utilization values; according to the method, most substances in the high-boiling residues are completely convertedinto rhodamine B, so that the economic value of the product is improved, the environmental pollution of the high-boiling residues is reduced, and very high economic benefits are brought to enterprises; the production method disclosed by the invention is relatively simple, does not need high equipment cost, does not adopt a catalyst, saves the production cost, and can achieve the yield of more than95%.

Description

technical field [0001] The invention relates to a comprehensive treatment method for high boilers, belonging to the technical field of chemical synthesis. Background technique [0002] During the large-scale industrial production of 4-diethylamino keto acid, some high boiling substances are produced. These high boiling substances are in a colloidal state, which is very sticky and difficult to decompose, polluting the environment. However, most of the organic matter 4-diethylamino ketoacid and rhodamine B contained in these high boilers have high utilization value, and this patent can convert the high boilers into rhodamine B through a certain method. [0003] Rhodamine B has high utilization value, is a kind of artificially synthesized red basic fluorescent dye, commonly known as flower pink, and its molecular formula is C 28 h 31 ClN 2 o 3 , the relative molecular mass is 479.28. The dye is often used as a fluorescent reagent and has been widely used in the fields of c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/82
CPCC07D311/82
Inventor 袁晋亭蔺黎明房雪琴袁航翟风南张慧翟全林
Owner 山东瑞康精化有限公司