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A kind of multi-step acid analysis reclaims the method for 5-chlorosalicylic acid in the mother liquor waste water that produces 5-chlorosalicylic acid

A technology of chlorosalicylic acid and mother liquor, applied in chemical instruments and methods, water/sludge/sewage treatment, separation/purification of carboxylic acid compounds, etc., can solve the problem that 5-chlorosalicylic acid and salicylic acid cannot be recycled The effect of acid recovery needs to be strengthened, and the actual operation requirements of workers are relatively high, so as to achieve the effect of small footprint, reduced processing difficulty, and short process route

Active Publication Date: 2016-04-13
NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, the mother liquor waste water of producing 5-chlorosalicylic acid is usually processed by the complex extraction method, using EPT-1 as the complexing agent, kerosene as the diluent, and reclaiming the extractant with sodium hydroxide. This method section is loaded down with trivial details, to The actual operation requirements of workers are relatively high, and the treatment cost is also high; more importantly, this method cannot recycle 5-chlorosalicylic acid in the mother liquor wastewater, and its purpose is only to remove COD in the wastewater, failing to achieve clean production the goal of
[0005] After searching, the Chinese patent application number 201310168591.9, the application date is May 9, 2013, the name of the invention is: a method for recycling waste liquid from the production of 2-hydroxybenzoic acid-2-ethylhexyl ester, the application is open A method for recycling salicylic acid was developed. The wastewater produced in the esterification synthesis process was adjusted to a pH value of 2 with hydrochloric acid with a mass concentration of 30%, and the wastewater was fully stirred for half an hour. White crystals were precipitated in the wastewater, which were centrifuged and dehydrated to obtain salicylic acid. Acid crystals, the obtained salicylic acid crystals can be used as raw materials for the production of 2-hydroxybenzoic acid-2-ethylhexyl, this application reduces the consumption of salicylic acid raw materials, saves production costs, and reduces sewage treatment costs , but the application still needs to be strengthened in the recovery effect of salicylic acid

Method used

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  • A kind of multi-step acid analysis reclaims the method for 5-chlorosalicylic acid in the mother liquor waste water that produces 5-chlorosalicylic acid
  • A kind of multi-step acid analysis reclaims the method for 5-chlorosalicylic acid in the mother liquor waste water that produces 5-chlorosalicylic acid
  • A kind of multi-step acid analysis reclaims the method for 5-chlorosalicylic acid in the mother liquor waste water that produces 5-chlorosalicylic acid

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Effect test

Embodiment 1

[0028] In conjunction with the accompanying drawings, a method of multi-step acid analysis of this embodiment to recover 5-chlorosalicylic acid in the mother liquor wastewater producing 5-chlorosalicylic acid is applied to a chemical plant producing 5-chlorosalicylic acid in Binhai Recovery of 5-chlorosalicylic acid in discharged mother liquor wastewater. The recovery principle is as follows: concentrated hydrochloric acid or concentrated sulfuric acid is used to treat the mother liquid wastewater of synthetic 5-chlorosalicylic acid, and the dynamic balance between 5-chlorosalicylic acid sodium salt and 5-chlorosalicylic acid is forced to be changed by adding acid, and 5-chlorosalicylic acid is precipitated. Chlorosalicylic acid, so as to achieve the purpose of reclaiming 5-chlorosalicylic acid and removing COD of mother liquor wastewater. The parameters of the mother liquor wastewater used are as follows: w1-1 and w1-3 are mixed to form the raw water of the mother liquor wast...

Embodiment 2

[0041] A method of multi-step acid analysis of the present embodiment to recover 5-chlorosalicylic acid in the mother liquor wastewater producing 5-chlorosalicylic acid, the parameters of the mother liquor wastewater used are as follows: w1-1 and w1-3 are mixed to form the mother liquor wastewater raw water , water temperature 20°C, pH value 4.5, COD Cr The value is 91892mg / L, of which 5-chlorosalicylic acid is 30356mg / L.

[0042] The specific operations of the multi-step acid analysis of the present embodiment to reclaim and produce 5-chlorosalicylic acid in the mother liquor wastewater of 5-chlorosalicylic acid are:

[0043] (1) Mix the waste water w1-1 and w1-3 of the mother liquor produced in the production of 5-chlorosalicylic acid and pump it into the acidification stirring tank I, add industrial concentrated sulfuric acid dropwise, and stir mechanically to obtain the acidification solution A. The stirring time is 12 minutes, and the acidification solution is controlled ...

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Abstract

The invention discloses a method for recovering 5-chlorosalicylic acid from 5-chlorosalicylic acid production mother solution wastewater through multi-step acid precipitation, belonging to the technical field of chemical wastewater treatment. The method comprises the recovery steps: (1) mixing a mother solution of 5-chlorosalicylic acid, pumping the mother solution into an acidizing stirred tank I, dropwise adding concentrated hydrochloric acid or concentrated sulfuric acid, and uniformly stirring to obtain an acidizing liquid A; (2) centrifuging the acidizing liquid A to obtain a clear centrifugal liquid B and a granular centrifugal sediment; (3) dropwise adding concentrated hydrochloric acid or concentrated sulfuric acid into the clear centrifugal liquid B, and uniformly stirring to obtain an acidizing liquid C; (4) centrifuging the acidizing liquid C to obtain a clear centrifugal liquid D and a granular centrifugal sediment; and (5) sequentially repeating the acid precipitation operation in the step (3) and the centrifuging operation in the step (4) until the end of the recovery operation. The method is used for realizing the effective recovery of the 5-chlorosalicylic acid, also greatly reducing the COD (Chemical Oxygen Demand) in the mother solution wastewater and reducing the wastewater treatment difficulty and is strong in practicability.

Description

technical field [0001] The invention relates to the technical field of chemical wastewater treatment, more specifically, relates to a multi-step acid analysis method for recovering 5-chlorosalicylic acid in mother liquor wastewater produced from 5-chlorosalicylic acid. Background technique [0002] With the acceleration of urbanization and industrialization in my country, the ever-growing urban population has an increasing demand for chemical products, leading to an increase in the production scale and quantity of various chemical companies. The chemical sewage discharged by chemical enterprises in the production process has caused serious pollution to the urban water environment and its surrounding ecological environment. The difficulty of chemical wastewater treatment poses a severe challenge to environmental workers. During the "Twelfth Five-Year Plan" period, my country once again proposed the policy of chemical enterprises to upgrade their production processes and elimi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C65/05C07C51/50C02F9/04C02F101/34
CPCC02F9/00C02F2103/36C07C51/412C07C51/42C07C65/05
Inventor 戴建军卞为林周腾腾赵选英王文文
Owner NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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