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Method for treating sewage generated by preparing methyl salicylate and resource recorery by composite technology

A technology for methyl salicylate and waste water production, applied in chemical instruments and methods, multi-stage water/sewage treatment, heating water/sewage treatment, etc.

Active Publication Date: 2007-12-05
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no report of a similar treatment method for methyl salicylate production wastewater in domestic and foreign literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 100ml (about 75 grams) of NDA-100 ultra-highly cross-linked macroporous adsorption resin and 100ml (about 75 grams) of NDA-99 composite functional adsorption resin (produced by Hebei Langfang Power Resin Factory) into two jacketed glasses. In the adsorption column (Φ32×360mm). The residue after the methyl salicylate production wastewater is stripped at room temperature (10~30℃) for 10~40min, first passes through the NDA-100 ultra-highly cross-linked macroporous adsorption resin bed at a flow rate of 6BV / h. The treatment capacity is 100BV / batch, and then the first-stage adsorption effluent is passed through the NDA-99 composite functional adsorption resin bed at a flow rate of 2BV / h, and the wastewater treatment capacity is 15BV / batch. The COD of the original wastewater is 58756mg / l, the COD after the stripping is 16328mg / l, the salicylic acid content is about 1000mg / l, the sulfosalicylic acid content is about 7000mg / l; the COD after the primary adsorption treatment is 1...

Embodiment 2

[0020] Use two polypropylene adsorption columns (Φ160×1000mm) to replace the two glass adsorption columns in Example 1, and each column is filled with 10 kg (approximately 13L) of resin, which is 130 times the wastewater treatment volume in Example 1. By operation, the effect of adsorption treatment and segmented resource recovery consistent with Example 1 was obtained.

Embodiment 3

[0022] Choose two 316L stainless steel adsorption towers with the same specifications (Φ400×2400mm), and each tower is filled with 190 kg (about 250L) of NDA-100 resin; another three 316L stainless steel adsorption towers with the same specifications (Φ600×3600mm) (respectively numbered I, II, III), each tower is filled with 500 kg (about 670L) of NDA-99 resin. The residue after the methyl salicylate production wastewater is stripped at room temperature (10~30℃) for 1.5h (the COD is about 16534mg / l, the salicylic acid content is about 1000mg / l, and the sulfosalicylic acid content is about 7000mg / l) into the adsorption tower, the first-stage adsorption adopts a single tower filled with NDA-100 macroporous adsorption resin, the cocurrent adsorption and countercurrent desorption method, and the adsorption flow rate is controlled at 1.5m 3 / h, each batch is controlled at 25m 3 ; The two-stage adsorption adopts the method of two towers (I, II towers) filled with NDA-99 resin in series ...

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Abstract

A process for treating and reclaiming the sewage generated by preparing methyl salicylate includes such steps as steam stripping to recover methanol, macroreticular resin adsorption of salicylic acid and methyl salicylate, eluting to recover salicylic acid and methyl salicylate, selective adsorption of sulfonyl salicylic acid by functional resin, and eluting to recover sulfonyl salicylic acid.

Description

1. Technical Field [0001] The invention relates to a method for treating and recovering waste water produced in the production process of methyl salicylate, which is an important intermediate for medicines, pesticides, perfumes, and coatings. Specifically, it relates to salicylic acid in the wastewater from the production of methyl salicylate And its derivative sulfosalicylic acid and the method of enrichment, separation and recycling of organic solvent in it. 2. Background technology [0002] Methyl salicylate, also known as wintergreen oil, is an important intermediate of medicines, pesticides, perfumes and coatings. Industrially, it is prepared by esterification reaction of salicylic acid and methanol under sulfuric acid catalysis. For every ton of methyl salicylate produced, 10-30 tons of yellow-brown wastewater are discharged, and the COD in the wastewater is as high as 57000-59000mg / l. Contains methanol 20000-30000mg / l, salicylic acid and sulfosalicylic acid 7500-9800mg / l, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F9/02C02F1/04C02F1/28
Inventor 张全兴陈金龙刘福强程秀梅葛俊杰李爱民鲁俊东周家艳韩丽
Owner NANJING UNIV