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Method for extracting o-phenylendiamine from waste water of o-phenylendiamine production

A technology for o-phenylenediamine and production wastewater, which is applied in the purification/separation of amino compounds, organic chemistry and other directions, can solve the problems of large o-phenylenediamine content, poor adsorption performance and high production cost, and achieves high removal rate and good Economic efficiency and good purity

Inactive Publication Date: 2006-11-22
陈义龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still has the following deficiencies: 1. After adopting hydrochloric acid desorption, it is necessary to desorb and regenerate the resin with low-carbon alcohol again, the process is complicated, and the production cost is higher
2. After hydrochloric acid desorption, only o-phenylenediamine hydrochloride can be obtained, and o-phenylenediamine cannot be obtained directly. If o-phenylenediamine is to be obtained, other processes need to be added; 3. The adsorption performance of the H series large-pore resin used Poor (the content of o-phenylenediamine in wastewater after adsorption treatment is still high)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Measure 100ml (about 70g) of XDA-1 macroporous resin into a glass adsorption column, take o-phenylenediamine production wastewater, and first filter it, and the filtering method is vacuum filtration or pressure filtration. At room temperature, the filtered wastewater passes through the glass adsorption column from bottom to top at a flow rate of 2BV / H, and the large-pore resin in the adsorption column adsorbs organic substances such as o-phenylenediamine in the wastewater, and the wastewater treatment capacity is 1200ml (12BV), the waste water is light yellow after flowing out through the glass column.

[0012] After testing, before the waste water passes through the glass column, the content of o-phenylenediamine is 6372 mg / l, and the waste water is directly distilled, and the measured value of CODcr in the distillate is 6425 mg / l. After the wastewater passed through the glass column, it was detected by spectrophotometry, and the content of o-phenylenediamine was 3.5 m...

Embodiment 2

[0016] Measure 100ml (about 70g) of XDA-200 large-pore resin into a glass adsorption column, take o-phenylenediamine production wastewater, first filter the wastewater by vacuum filtration or pressure filtration, and filter it at 25-35 At ℃, the filtered wastewater passes through the glass column from bottom to top at a flow rate of 2.5BV / H, and the large-pore resin in the glass column adsorbs organic substances such as o-phenylenediamine in the wastewater. The wastewater treatment capacity is 1200ml (12BV ), the waste water was pale yellow after flowing out through the glass column.

[0017] After testing, before the waste water passes through the glass column, the content of o-phenylenediamine is 5856 mg / l. After the waste water passes through the glass column, it is detected by spectrophotometry, and the content of o-phenylenediamine is reduced to 7.5 mg / l. The removal rate of o-phenylenediamine is 99.8%. Then by distilling the waste water, the measured value of CODcr in t...

example 3

[0021] Using two adsorption columns in series for adsorption and single-column desorption, the specific steps are as follows:

[0022] 1. Adsorption process—Use two adsorption columns of the same specification (Φ1000×5000), mark them as I column and II column, and fill each adsorption column with 2500Kg (about 3600L) of XDA-1 large-pore resin. At ℃, the waste water from the production of o-phenylenediamine (content: 6149mg / l) was filtered to remove impurities, and then the pump was used to pump 7.2m 3 / h flow into the adsorption column. The adsorption adopts the adsorption method of two columns I and II connected in series and countercurrent. The I column is the front column and the II column is the back column. That is, the waste water enters through the bottom of the I column, flows out from the top of the I column, and then enters from the bottom of the II column, and then enters from the II column. Column top outflow. After the wastewater is treated by adsorption, the co...

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Abstract

This invention relates to a method for extracting o-phenylenediamine from waste water of o-phenylenediamine production. Wherein: filtrate the waste water containing o-phenylenediamine, and load it on the absorption column filled with macroreticular resin which absorbs o-phenylenediamine and other organic compounds in the waste water, and then elute with ethanol solution to desorb the o-phenylenediamine and form the desorption solution, distill the desorption solution to remove the ethanol, cool the residual liquid after distillation at controlled temperature to precipitate the o-phenylenediamine crystals, and then obtain the o-phenylenediamine by filtration. This invention is characterized of high clearance of o-phenylenediamine in the waste water, high-purity of recovered o-phenylenediamine, simple and rational process. It accomplishes the object of turning waste to be useful, solves the waste discharging problem, and has a good economical benefit.

Description

technical field [0001] The invention relates to wastewater treatment and utilization technology, in particular to a method for extracting o-phenylenediamine from wastewater extracted from o-phenylenediamine production. Background technique [0002] O-phenylenediamine is an important intermediate of pesticides and dyes. It is mainly prepared from o-nitrochlorobenzene through amination under high temperature and high pressure and reduction with alkali sulfide. Using the above method, 8 to 10 tons of waste water (CODcr is about 100,000 to 120,000 mg / l) will be discharged for every ton of o-phenylenediamine produced, the main components of which are: 0.5 to 1% o-phenylenediamine, 16 ~18%, alkali sulfide 1~2%, etc. O-phenylenediamine production wastewater has a high value of extraction and utilization. At present, the treatment and utilization of this type of wastewater is mainly used as a raw material for the production of soda. However, in the process of using it to produce s...

Claims

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Application Information

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IPC IPC(8): C07C211/51C07C209/86
Inventor 陈义龙
Owner 陈义龙
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