CN111057012A - Method for removing residual iron ions in AABI (anaerobic-anoxic-oxic) by using chelating agent - Google Patents
Method for removing residual iron ions in AABI (anaerobic-anoxic-oxic) by using chelating agent Download PDFInfo
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- CN111057012A CN111057012A CN201911264615.4A CN201911264615A CN111057012A CN 111057012 A CN111057012 A CN 111057012A CN 201911264615 A CN201911264615 A CN 201911264615A CN 111057012 A CN111057012 A CN 111057012A
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- aabi
- chelating agent
- iron ions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/24—Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D235/26—Oxygen atoms
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Adding phosphoric acid and an antioxidant into a crude product of the AABI, then heating, adding the chelating agent during heating, heating to 80-95 ℃, adding activated carbon, keeping the temperature for 2.5-3h, carrying out heat filtration, filtering precipitates and the activated carbon, dropwise adding diketene into filtrate until the pH value is 5-6, separating out crystals, cooling and filtering to obtain the AABI qualified in alkali dissolution. Utilizing chelating agent EDTA, DTPA or NTA and residual Fe in AABI crude product3+/Fe2+And (3) reacting to generate solid precipitates, removing a small amount of residual iron ions in the reaction solution, and adding an activated carbon adsorption chelating agent to decolorize the reaction solution, so that the cold dissolution quality is improved, and the AABI qualification rate is improved.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis byproduct treatment, and particularly relates to a method for removing residual iron ions in AABI by using a chelating agent.
Background
During the synthesis of 5-acetoacetylaminobenzimidazolones (AABI)Iron reduction is required, and a small amount of iron ions remain in the reaction solution during filtration, which causes red color (Fe) in the cold dissolution process3+/Fe2+) And the color is unqualified, so that the invention removes iron ions in the AABI reaction solution to improve the cold dissolution quality.
Disclosure of Invention
The invention aims to provide a method for removing residual iron ions in AABI by using a chelating agent, which improves the product yield of the AABI.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for removing residual iron ions in AABI by using a chelating agent comprises the following steps: adding phosphoric acid and an antioxidant into the ABBI crude product, then heating, adding a chelating agent in the heating process, heating to 80-95 ℃, adding activated carbon, preserving heat for 2.5-3h, carrying out heat filtration, filtering precipitates and the activated carbon, dropwise adding diketene into the filtrate until the pH value is 5-6, separating out crystals, cooling and filtering to obtain the AABI qualified in alkaline solution.
Specifically, the mass ratio of the AABI crude product to the phosphoric acid to the antioxidant is 1: 2.5-3: 0.2-0.25.
Specifically, the antioxidant is one of BHT (dibutylhydroxytoluene), BHA (butylhydroxyanisole) and sodium sulfite.
Specifically, the chelating agent is one of EDTA (ethylene diamine tetraacetic acid), DTPA (diethyltriaminepentaacetic acid), NTA (nitrilotriacetic acid), and preferably EDTA.
Specifically, the addition amount of the chelating agent is 0.2-1% of the mass of the crude product of AABI.
Specifically, the addition temperature of the chelating agent is 80 ℃.
Specifically, the temperature for cooling and filtering is 45-50 ℃.
The invention has the following beneficial effects: the invention utilizes chelating agent EDTA, DTPA or NTA and residual Fe in AABI crude product3+/Fe2+And (3) reacting to generate solid precipitates, removing a small amount of residual iron ions in the reaction solution, and adding an activated carbon adsorption chelating agent to decolorize the reaction solution, so that the cold dissolution quality is improved, and the AABI qualification rate is improved.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the scope of the present invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.
Example 1
Adding 250kg of crude ABBI into a decoloring kettle, adding 750kg of phosphoric acid, adding 57.5kg of antioxidant BHT57, opening a steam valve, opening an emptying valve, opening a circulating water inlet and outlet valve, heating to 80 ℃, opening a chelating agent head tank feeding valve, adding 2.5kg of chelating agent DTPA into a reaction kettle, closing the feeding valve after the feeding is finished, opening an activated carbon feeding valve after the reaction is carried out for 0.5h, adding 1kg of activated carbon, carrying out plate frame suction filtration after the reaction temperature is kept at 80 ℃ for 3h, transferring filtrate into an oxidation kettle, turning the temperature to 65-75 ℃ after the material is transferred, opening a diketene dropping valve for dropping, closing the dropping valve when the pH value is 5-6, opening the circulating water valve for cooling, opening a bottom valve of the oxidation kettle when the temperature is reduced to 48 ℃, opening a centrifuge for material throwing, conveying the thrown material to AABI for drying, and dissolving the product into yellow color, the product quality is qualified.
Example 2
Adding 250kg of crude ABBI product into a decoloring kettle, adding 625kg of phosphoric acid, adding 50kg of antioxidant BHA, opening a steam valve, opening an emptying valve, opening a circulating water inlet and outlet valve, heating to 80 ℃, opening a feeding valve of a chelating agent elevated tank, adding 2kg of chelating agent NTA into the reaction kettle, closing the feeding valve after the feeding is finished, opening an active carbon feeding valve after the reaction is carried out for 0.5h, adding 1kg of active carbon, keeping the temperature at 90 ℃ for 2.5h, carrying out plate frame suction filtration, transferring the filtrate into an oxidation kettle, opening a diketene dropwise adding valve for dropwise adding after the material transferring is finished, and when the pH value is 5-6, closing the dropwise adding valve, opening a circulating water valve for cooling, opening a bottom valve of the oxidation kettle when the temperature is reduced to 50 ℃, opening a centrifugal machine for throwing the materials, conveying the thrown materials to an AABI bipyramid for drying, and performing alkali dissolution on the dried product to obtain a yellow system, wherein the product quality is qualified.
Example 3
Adding 250kg of crude ABBI into a decoloring kettle, adding 650kg of phosphoric acid, adding 62.5kg of sodium sulfite as an antioxidant, opening a steam valve, opening an emptying valve, opening a circulating water inlet and outlet valve, heating to 80 ℃, opening a feeding valve of a chelating agent head tank, adding 1.25kg of chelating agent EDTA into a reaction kettle, closing the feeding valve after feeding, opening an activated carbon feeding valve after reacting for 0.5h, adding 1kg of activated carbon, carrying out plate frame suction filtration after keeping the reaction temperature at 95 ℃ for 2.8h, transferring filtrate into an oxidation kettle, opening a ketene dimer dropping valve for dropping after transferring, closing the dropping valve when the pH value is 5-6, opening the circulating water valve for cooling, opening a bottom valve of the oxidation kettle when the temperature is 45 ℃, opening a centrifuge for dropping, transferring the dropped material, conveying the dropped material to AABI to dry, dissolving the product in alkali to yellow color, the product quality is qualified.
Example 4
Adding 250kg of crude ABBI product into a decoloring kettle, adding 700kg of phosphoric acid, adding antioxidant BHT55kg, opening a steam valve, opening an emptying valve, opening a circulating water inlet and outlet valve, heating to 80 ℃, opening a feeding valve of the chelating agent head tank, adding 0.55kg of chelating agent EDTA into the reaction kettle, after the feeding is finished, the feeding valve is closed, the activated carbon feeding valve is opened after the reaction is carried out for 0.5h, 1kg of activated carbon is fed, keeping the reaction temperature at 85 ℃ for 3h, performing plate-frame suction filtration, transferring the filtrate into an oxidation kettle, opening a diketene dropwise adding valve for dropwise addition after the material transfer is finished, and when the pH value is 5-6, closing the dropwise adding valve, opening a circulating water valve for cooling, opening a bottom valve of the oxidation kettle when the temperature is reduced to 47 ℃, opening a centrifugal machine for throwing the materials, conveying the thrown materials to an AABI bipyramid for drying, and performing alkali dissolution on the dried product to obtain a yellow system, wherein the product quality is qualified.
The present invention is not limited to the above embodiments, and any structural changes made under the teaching of the present invention shall fall within the scope of the present invention, which is similar or similar to the technical solutions of the present invention.
The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (7)
1. A method for removing residual iron ions in AABI by using a chelating agent is characterized by comprising the following steps: adding phosphoric acid and an antioxidant into the ABBI crude product, then heating, adding a chelating agent in the heating process, heating to 80-95 ℃, adding activated carbon, preserving heat for 2.5-3h, carrying out heat filtration, dropwise adding diketene into the filtrate until the pH value is 5-6, then cooling and filtering to obtain the AABI qualified in alkaline solution.
2. The method for removing residual iron ions in AABI by using chelating agent as claimed in claim 1, wherein the mass ratio of the AABI crude product, phosphoric acid and antioxidant is 1: 2.5-3: 0.2-0.25.
3. The method for removing residual iron ions in AABI of claim 1 or claim 2, wherein the antioxidant is one of BHT, BHA and sodium sulfite.
4. The method for removing residual iron ions from AABI of claim 1, wherein said chelating agent is one of EDTA, DTPA, NTA.
5. The method for removing residual iron ions from AABI by using a chelating agent as claimed in claim 1, wherein the chelating agent is added in an amount of 0.2-1% by mass based on the crude AABI product.
6. The method for removing residual iron ions from AABI of claim 1, wherein the chelating agent is added at a temperature of 80 ℃.
7. The method for removing residual iron ions from AABI by using a chelating agent as claimed in claim 1, wherein the temperature of the reduced temperature filtration is 45-50 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911264615.4A CN111057012A (en) | 2019-12-11 | 2019-12-11 | Method for removing residual iron ions in AABI (anaerobic-anoxic-oxic) by using chelating agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911264615.4A CN111057012A (en) | 2019-12-11 | 2019-12-11 | Method for removing residual iron ions in AABI (anaerobic-anoxic-oxic) by using chelating agent |
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| CN111057012A true CN111057012A (en) | 2020-04-24 |
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