CN110668935A - Method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin - Google Patents
Method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin Download PDFInfo
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- CN110668935A CN110668935A CN201911138508.7A CN201911138508A CN110668935A CN 110668935 A CN110668935 A CN 110668935A CN 201911138508 A CN201911138508 A CN 201911138508A CN 110668935 A CN110668935 A CN 110668935A
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- trimethoxybenzoic acid
- resin
- recovering
- resin column
- eluent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
The invention discloses a method for recovering 3,4, 5-trimethoxybenzoic acid from resin in wastewater, which comprises the following steps: adjusting the pH value of the 3,4, 5-trimethoxybenzoic acid waste mother liquor to 4-5, and removing impurities through a plate frame; press 3m3Conveying the waste mother liquor of the 3,4, 5-trimethoxybenzoic acid to a resin column at a speed of/h for adsorption; each resin column absorbs 100m3Then, eluting the 3,4, 5-trimethoxybenzoic acid adsorbed in the resin column; acidifying the eluent; centrifugally separating the eluent to obtain a crude product of the 3,4, 5-trimethoxybenzoic acid; refining and drying to obtain the finished product of the 3,4, 5-trimethoxybenzoic acid. The method for recovering 3,4, 5-trimethoxybenzoic acid from the resin has the advantages of high recovery rate, low energy consumption, high benefit and the like.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a method for recovering 3,4, 5-trimethoxybenzoic acid from resin in wastewater.
Background
The 3,4, 5-trimethoxybenzoic acid can be used as pharmaceutical and organic synthesis intermediate, and can be used for producing antibacterial synergistic agent trimethoprim and anxiolytic agent trimethoxy quinoline. The preparation process comprises the steps of carrying out methoxylation reaction on gallic acid and dimethyl sulfate to generate 3,4, 5-trimethoxybenzoic acid, and neutralizing, filtering and washing to obtain a fine product.
In the production process of 3,4, 5-trimethoxybenzoic acid, a large amount of waste water is generated by processes of filtering, washing and the like, the average amount of the waste water is 20t of waste water per t of products, and the waste water contains 3,4, 5-trimethoxybenzoic acid. The traditional wastewater treatment process is to recover 3,4, 5-trimethoxybenzoic acid in wastewater by a concentration method, and has the problems of time consumption, material consumption, labor consumption, high equipment corrosivity and the like.
In view of the above, there is a need to provide a new wastewater treatment process to solve the above technical problems.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for recovering 3,4, 5-trimethoxybenzoic acid from resin wastewater, and the method has the advantages of high recovery rate, low energy consumption, high yield and the like.
In order to solve the problems, the technical scheme of the invention is as follows:
a method for recovering 3,4, 5-trimethoxybenzoic acid from resin wastewater comprises the following steps:
step S1, adjusting the pH value of the 3,4, 5-trimethoxybenzoic acid waste mother liquor to 4-5, and removing impurities through a plate frame;
step S2, providing a resin column, pressing 3m3Conveying the waste mother liquor of the 3,4, 5-trimethoxybenzoic acid to a resin column at a speed of/h for adsorption;
step S3, absorbing 100m of resin in each resin column3Then, eluting the 3,4, 5-trimethoxybenzoic acid adsorbed in the resin column;
step S4, acidifying the eluent;
step S5, carrying out centrifugal separation on the eluent to obtain a crude product of the 3,4, 5-trimethoxybenzoic acid;
and step S6, refining and drying to obtain the finished product of the 3,4, 5-trimethoxybenzoic acid.
Further, the number of the resin columns was 4, and the number thereof was φ 1.2X 11 m.
Furthermore, the type of the resin used by the resin column is NKA-II.
Further, in the eluent acidification step, the pH value of the eluent is adjusted to 1-2.
Further, the filtering area of the plate frame is 30m2。
The method for recovering 3,4, 5-trimethoxybenzoic acid from waste water by using resin provided by the invention has the beneficial effects that:
the invention provides a method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin, the recovery rate can reach 99 percent, and the recovery rate is high; 3,4, 5-trimethoxybenzoic acid in the waste liquid is adsorbed by the resin, so that the energy consumption is low, the efficiency is high, and the cost is saved; the waste liquid is recycled, so that the environment is protected, and green production is realized.
Detailed Description
The following description of the present invention is provided to enable those skilled in the art to better understand the technical solutions in the embodiments of the present invention and to make the above objects, features and advantages of the present invention more comprehensible.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
A method for recovering 3,4, 5-trimethoxybenzoic acid from resin wastewater comprises the following steps:
step S1, adjusting the pH value of the 3,4, 5-trimethoxybenzoic acid waste mother liquor to 4-5, and removing impurities through a plate frame;
step S2, providing a resin column, pressing 3m3Conveying the waste mother liquor of the 3,4, 5-trimethoxybenzoic acid to a resin column at a speed of/h for adsorption;
step S3, absorbing 100m of resin in each resin column3Then, eluting the 3,4, 5-trimethoxybenzoic acid adsorbed in the resin column;
step S4, acidifying the eluent;
step S5, carrying out centrifugal separation on the eluent to obtain a crude product of the 3,4, 5-trimethoxybenzoic acid;
and step S6, refining and drying to obtain the finished product of the 3,4, 5-trimethoxybenzoic acid.
Further, the number of the resin columns was 4, and the number thereof was φ 1.2X 11 m.
Furthermore, the type of the resin used by the resin column is NKA-II.
Further, in the eluent acidification step, the pH value of the eluent is adjusted to 1-2.
Further, the filtering area of the plate frame is 30m2。
By the waste liquid recovery method, when the initial concentration of the 3,4, 5-trimethoxybenzoic acid in the waste liquid is 1%, the content of the 3,4, 5-trimethoxybenzoic acid in the waste liquid is 0.1% after resin adsorption, and the recovery rate reaches 99%.
In conclusion, the invention provides a method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin, the recovery rate can reach 99 percent, and the recovery rate is high; 3,4, 5-trimethoxybenzoic acid in the waste liquid is adsorbed by the resin, so that the energy consumption is low, the efficiency is high, and the cost is saved; the waste liquid is recycled, so that the environment is protected, and green production is realized. The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. Various changes, modifications, substitutions and alterations to these embodiments will occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (5)
1. A method for recovering 3,4, 5-trimethoxybenzoic acid from resin wastewater is characterized by comprising the following steps:
step S1, adjusting the pH value of the 3,4, 5-trimethoxybenzoic acid waste mother liquor to 4-5, and removing impurities through a plate frame;
step S2, providing a resin column, pressing 3m3Conveying the waste mother liquor of the 3,4, 5-trimethoxybenzoic acid to a resin column at a speed of/h for adsorption;
step S3, absorbing 100m of resin in each resin column3Then, eluting the 3,4, 5-trimethoxybenzoic acid adsorbed in the resin column;
step S4, acidifying the eluent;
step S5, carrying out centrifugal separation on the eluent to obtain a crude product of the 3,4, 5-trimethoxybenzoic acid;
and step S6, refining and drying to obtain the finished product of the 3,4, 5-trimethoxybenzoic acid.
2. A method of recovering 3,4, 5-trimethoxybenzoic acid from waste water by using resin as claimed in claim 1, wherein the number of resin columns is 4, and its model is phi 1.2 x 11 m.
3. The method of claim 2, wherein the type of the resin used in the resin column is NKA-II.
4. A method according to claim 1, wherein the pH of the eluate is adjusted to 1-2 in the step of acidifying the eluate.
5. The method of claim 1, wherein the filtration area of the plate frame is 30m2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911138508.7A CN110668935B (en) | 2019-11-20 | 2019-11-20 | Method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911138508.7A CN110668935B (en) | 2019-11-20 | 2019-11-20 | Method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin |
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| Publication Number | Publication Date |
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| CN110668935A true CN110668935A (en) | 2020-01-10 |
| CN110668935B CN110668935B (en) | 2022-06-21 |
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| CN201911138508.7A Active CN110668935B (en) | 2019-11-20 | 2019-11-20 | Method for recovering 3,4, 5-trimethoxybenzoic acid in wastewater by using resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683260A (en) * | 2021-08-24 | 2021-11-23 | 湖南棓雅生物科技有限公司 | Method for treating 3,4, 5-trimethoxybenzoic acid methyl ester wastewater |
| CN114195746A (en) * | 2021-12-30 | 2022-03-18 | 江苏清泉化学股份有限公司 | Method for recovering (Z) -2-methoxyimino-2-furanacetic acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519348A (en) * | 2009-04-10 | 2009-09-02 | 南京大学 | Process for reclaiming o-chlorobenzoic acid from mother liquor or waste water |
| CN109081777A (en) * | 2018-08-30 | 2018-12-25 | 西安金沃泰环保科技有限公司 | A kind of tetrafluorobenzoic aid Sewage treatment and processing method |
-
2019
- 2019-11-20 CN CN201911138508.7A patent/CN110668935B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519348A (en) * | 2009-04-10 | 2009-09-02 | 南京大学 | Process for reclaiming o-chlorobenzoic acid from mother liquor or waste water |
| CN109081777A (en) * | 2018-08-30 | 2018-12-25 | 西安金沃泰环保科技有限公司 | A kind of tetrafluorobenzoic aid Sewage treatment and processing method |
Non-Patent Citations (1)
| Title |
|---|
| 罗李华: "从TMP甲酯化废液中回收3,4,5-三甲氧基苯甲酸钠", 《化工环保》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683260A (en) * | 2021-08-24 | 2021-11-23 | 湖南棓雅生物科技有限公司 | Method for treating 3,4, 5-trimethoxybenzoic acid methyl ester wastewater |
| CN114195746A (en) * | 2021-12-30 | 2022-03-18 | 江苏清泉化学股份有限公司 | Method for recovering (Z) -2-methoxyimino-2-furanacetic acid |
| CN114195746B (en) * | 2021-12-30 | 2023-09-22 | 江苏清泉化学股份有限公司 | Method for recycling (Z) -2-methoxyimino-2-furanacetic acid |
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| CN110668935B (en) | 2022-06-21 |
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