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Treatment method of waste water produced in process for producing caprolactam by utilizing toluene method

A treatment method, the technology of caprolactam, is applied in the direction of water/sewage multi-stage treatment, water/sludge/sewage treatment, chemical instruments and methods, etc. It can solve the problems of ineffective recycling, difficult treatment, complex chemical composition, etc., and achieve Good environmental and economic benefits, good combustion calorific value, simple recovery method

Active Publication Date: 2012-08-22
TIANJIN FUTESI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic waste water is a black viscous liquid with an unpleasant smell, and its chemical composition is complex. It is a high-concentration organic waste water that is difficult to treat. It has great pollution to the environment and cannot be discharged directly.
Because organic sewage contains organic matter, it can be used as fuel for combustion. At present, the main treatment method at home and abroad is incineration. However, because it contains substances that are difficult to burn, special methods and equipment must be used for combustion. This method consumes a lot of energy. The valuable components in the waste liquid are not effectively recycled, causing serious pollution to the environment and equipment.

Method used

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  • Treatment method of waste water produced in process for producing caprolactam by utilizing toluene method
  • Treatment method of waste water produced in process for producing caprolactam by utilizing toluene method
  • Treatment method of waste water produced in process for producing caprolactam by utilizing toluene method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Get 100g of toluene method to produce caprolactam process waste water, adjust the pH value to 8-9 with 20% (mass percentage) NaOH solution under room temperature and normal pressure, add solvent II acetone 60g, have solid to separate out, filter in batches, collect filtrate and filter residue, filter residue Wash with 2 g of anhydrous methanol until off-white, dry at 40-50°C, and weigh to obtain 9 g of crude cyclohexyl formic acid sulfonate.

[0028] The collected filtrate is distilled under normal pressure, and the cut acetone of 50-70 ℃ is collected, which can be reused; the remaining liquid is distilled under reduced pressure (200-600mmHg) to remove 60% (mass percentage) moisture, and then at room temperature and normal pressure Add the solvent 1 toluene 7g of residue 20% (mass percentage) down, carry out extraction separation and obtain organic phase and water phase, concentrate organic phase, weigh after vacuum-drying treatment, through 1 HNMR, 13 CNMR and IR iden...

Embodiment 2

[0031] Take 100g of this organic wastewater, adjust the pH value to 8-9 with NaOH at room temperature and normal pressure, add solvent II acetone 80g, solids are precipitated, filter in batches, collect the filtrate and filter residue, and wash the filter residue with 2g of anhydrous methanol to off-white, 40 After drying at -50°C, it was weighed to obtain 11 g of crude cyclohexyl formic acid sulfonate.

[0032] Distill the collected filtrate under normal pressure, collect the distillate acetone at 50-70°C for reuse; distill the remaining liquid to remove 60% water (mass percentage) under reduced pressure (200-600mmHg), and then add it at room temperature and normal pressure Residue 20% (mass percentage) solvent Ibenzene 7g, carry out extraction separation to obtain organic phase and water phase, concentrate organic phase, obtain caprolactam 2.5g through vacuum drying. The aqueous phase was further concentrated and dried in vacuo to give 29 g of a black solid.

[0033] Take 1...

Embodiment 3

[0035] Take 100g of this organic wastewater, adjust the pH value to 8-9 with NaOH at room temperature and normal pressure, add solvent II acetone 120g, solids are precipitated, filter in batches, collect the filtrate and filter residue, and wash the filter residue with 2g of anhydrous methanol until off-white, 40 After drying at -50°C, it was weighed to obtain 12.5 g of crude cyclohexyl formic acid sulfonate.

[0036] Distill the collected filtrate under normal pressure, collect the distillate acetone at 50-70°C for reuse; distill the remaining liquid to remove 60% water (mass percentage) under reduced pressure (200-600mmHg), and then add it at room temperature and normal pressure The remaining 30% (mass percentage) solvent I cyclohexane 10g was extracted and separated to obtain an organic phase and an aqueous phase, the organic phase was concentrated, and 2.2 g of caprolactam was obtained through vacuum drying. The aqueous phase was further concentrated and dried under vacuum...

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Abstract

The invention provides a treatment method of waste water produced in process for producing caprolactam by utilizing a toluene method. The treatment method comprises the steps of: adding acetone into the waste water to be treated, implementing the filtering after solid is precipitated, washing the filter residue to gray white with absolute methanol, drying the absolute methanol to obtain cyclohexyl formate and sulfonate, and extracting the caprolactam. By utilizing the method, valuable organic substances and combustion pollutants in the waste water can be separated to obtain caprolactam and cyclohexyl formate and sulfonate, and chemical engineering products with high additional value can be obtained through subsequent further processing; and the content of organisms in the waste water alsocan be reduced, so that the treated waste water can be mixed with other waste water to be discharged after being further treated by a waste water treatment system, and residues after the separation and extraction can be used as fuel after being concentrated. The treatment method has good environmental-protection benefit and economic benefit.

Description

technical field [0001] The invention relates to a method for treating waste water, in particular to a method for treating waste water in a toluene process for producing caprolactam. Background technique [0002] A large amount of waste water and by-products are produced in the production process of caprolactam by the toluene method. The composition of these waste water is complex, and the main pollutants are: caprolactam, ammonium sulfate, toluene, benzoic acid, cyclohexyl carboxylate, cyclohexyl formate sulfonate, etc. Cyclohexyl carboxylate sulfonate is the main chemical with small amounts of caprolactam and other chemicals. The organic waste water liquid is a black viscous liquid with an unpleasant smell and complex chemical composition. It is a high-concentration organic waste water that is difficult to treat. It has great pollution to the environment and cannot be discharged directly. Because organic sewage contains organic matter, it can be used as fuel for combustion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04C02F9/10C10L1/00C07C309/27C07C303/44C07D223/10
Inventor 卢忠林程怀文杨辉
Owner TIANJIN FUTESI TECH DEV
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