CN113277983A - Treatment method of 5-aminobenzimidazole ketone mother liquor - Google Patents
Treatment method of 5-aminobenzimidazole ketone mother liquor Download PDFInfo
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- CN113277983A CN113277983A CN202110394076.7A CN202110394076A CN113277983A CN 113277983 A CN113277983 A CN 113277983A CN 202110394076 A CN202110394076 A CN 202110394076A CN 113277983 A CN113277983 A CN 113277983A
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- mother liquor
- aminobenzimidazole
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- concentrated solution
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 34
- -1 5-aminobenzimidazole ketone Chemical class 0.000 title claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 20
- WFRXSXUDWCVSPI-UHFFFAOYSA-N 3h-benzimidazol-5-amine Chemical compound NC1=CC=C2NC=NC2=C1 WFRXSXUDWCVSPI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 238000004064 recycling Methods 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000005984 hydrogenation reaction Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 4
- KQNZKBRSEJLVEO-UHFFFAOYSA-N 3-oxo-n-(2-oxobenzimidazol-5-yl)butanamide Chemical compound C1=C(NC(=O)CC(=O)C)C=CC2=NC(=O)N=C21 KQNZKBRSEJLVEO-UHFFFAOYSA-N 0.000 claims description 3
- 238000004042 decolorization Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 8
- 239000010815 organic waste Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- MYONAGGJKCJOBT-UHFFFAOYSA-N benzimidazol-2-one Chemical compound C1=CC=CC2=NC(=O)N=C21 MYONAGGJKCJOBT-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000007868 Raney catalyst Substances 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 229910000564 Raney nickel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention belongs to the technical field of wastewater treatment, and particularly relates to a treatment method of 5-aminobenzimidazole ketone mother liquor. The treatment method is simple and convenient to operate, high in safety coefficient and low in cost; the content of organic waste and COD in the treated wastewater is obviously reduced, the recovery of solid matters in the mother liquor wastewater can be realized, and the burden of subsequent treatment is reduced. A method for treating 5-aminobenzimidazole mother liquor comprises the following steps: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, adding phosphoric acid and decoloring, adding liquid alkali and diacetone, carrying out heat preservation reaction and filtration, carrying out heat preservation reaction on the diacetone, cooling and precipitating salt, and the like.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a treatment method of 5-aminobenzimidazole ketone mother liquor.
Background
5-aminobenzimidazole ketone is a main intermediate for synthesizing benzimidazolone pigments at present. The benzimidazolone pigment is an azo type high-grade organic pigment with wide application, and has excellent light resistance, weather fastness, heat stability, migration resistance and solvent resistance. Because the 5-aminobenzimidazole ketone contains cyclic phthalidyl in a molecule, intermolecular and intramolecular hydrogen bonds are easy to form, so that the pigment has excellent performance, and is suitable for the paint industry to manufacture various industrial paints, car primary finishes, building coatings, polyethylene polymerization coloring and the like.
At present, the method for producing 5-aminobenzimidazole ketone at home and abroad is mainly prepared by condensation, nitration and reduction of o-phenylenediamine and urea, wherein the reduction step adopts relatively mature catalytic hydrogenation reduction: usually, Raney nickel or palladium carbon is used for reduction, the reaction conversion rate is high, side reactions are small, the product quality and the recovery rate are greatly improved, the environmental pollution is small, the catalyst can be recycled, and almost no solid waste is generated. But the process has obvious defects, the amount of wastewater is large, and the process is not easy to apply; the wastewater contains a large amount of macromolecular BI and other refractory substances, and has high COD, deep chromaticity and high treatment cost. Therefore, it is highly desirable to provide a method for treating 5-aminobenzimidazole mother liquor, which can effectively reduce the treatment cost and the burden of subsequent treatment.
Disclosure of Invention
The invention provides a treatment method of 5-aminobenzimidazole ketone mother liquor, which is simple and convenient to operate, high in safety coefficient and low in cost; the content of organic waste and COD in the treated wastewater is obviously reduced, the recovery of solid matters in the mother liquor wastewater can be realized, and the burden of subsequent treatment is reduced.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for treating a 5-aminobenzimidazole mother liquor comprises the following steps:
step 1: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, and recycling fractions;
step 2: adding phosphoric acid into the concentrated solution obtained in the step 1; heating and adding a granular activated carbon decoloring column for decoloring to obtain filtrate A;
and step 3: adding liquid caustic soda into the filtrate A obtained in the step 2; dropwise adding diacetone, carrying out heat preservation reaction, cooling, filtering and recovering a filter cake to obtain a filtrate B;
and 4, step 4: adding liquid caustic soda into the filtrate B obtained in the step 3 to adjust the pH value, and cooling to separate out salt; discharging and recovering the separated salt, and performing biochemical treatment on the residual wastewater.
Preferably, the fraction recycling in the step 1 is recycling for fraction hydrogenation.
Preferably, the evaporation concentration equipment used in the process of evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain the concentrated solution in the step 1 is an MVR evaporator;
the mass of the concentrated solution obtained by evaporation and concentration is 10-15% of that of the 5-aminobenzimidazole mother liquor.
Preferably, the mass of the phosphoric acid added in the step 2 is 0.6-0.8% of the mass of the concentrated solution.
Preferably, in the step 2 of decoloring treatment, the temperature is increased to 80-85 ℃, and the decoloring retention time of the granular activated carbon decoloring column is 10-30 min.
Preferably, the mass of the liquid alkali added in the step 3 is 30% of the mass of the filtrate A.
Preferably, in the step 3, in the heat preservation reaction process of dropwise adding the diacetone, the temperature required by the heat preservation reaction is 70-80 ℃, the heat preservation time is 10-20min, and the molar ratio of the dropwise adding diacetone to the filtrate A is 1: 1.08; and 3, in the cooling and filtering process in the step 3, the cooling temperature is not higher than 40 ℃, and the filter cake recovered by filtering is 5-acetoacetylaminobenzimidazolone.
Preferably, in the step 4, the pH value is adjusted to pH =9-10 during the pH value adjustment by adding liquid alkali.
Preferably, in the process of cooling and separating out salt in the step 4, the temperature range of cooling is 35-40 ℃, and the salt separated out by discharging and recycling is 12-hydrate disodium hydrogen phosphate.
The invention provides a method for treating 5-aminobenzimidazole ketone mother liquor, which comprises the following steps: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, adding phosphoric acid and decoloring, adding liquid alkali and diacetone, carrying out heat preservation reaction and filtration, carrying out heat preservation reaction on the diacetone, cooling and precipitating salt, and the like. The method for treating the 5-aminobenzimidazole mother liquor with the characteristics of the steps is simple and convenient to operate, high in safety coefficient and low in cost; the content of organic waste and COD in the treated wastewater is obviously reduced, the recovery of solid matters in the mother liquor wastewater can be realized, and the burden of subsequent treatment is reduced.
Detailed Description
The invention provides a treatment method of 5-aminobenzimidazole ketone mother liquor, which is simple and convenient to operate, high in safety coefficient and low in cost; the content of organic waste and COD in the treated wastewater is obviously reduced, the recovery of solid matters in the mother liquor wastewater can be realized, and the burden of subsequent treatment is reduced.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides a method for treating 5-aminobenzimidazole ketone mother liquor. Specifically, the processing method comprises the following steps:
step 1: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, and recycling fractions.
In a preferred embodiment of the present invention, an MVR evaporator is preferably used as an evaporation and concentration device used in the process of evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, and the mass of the concentrated solution obtained after evaporation and concentration is preferably 10-15% of the mass of the 5-aminobenzimidazole mother liquor. Further examples are as follows: measuring 5000kg of 5-aminobenzimidazole ketone mother liquor (the main components of the mother liquor are about 0.3 percent), and evaporating and concentrating by utilizing an MVR evaporator; wherein, the vacuum degree of the system is controlled at-0.04 MPa in the distillation process, and the 80-92 ℃ fraction (about 4300kg in mass, about 86% in proportion) is recovered by applying mechanically.
Step 2: adding phosphoric acid into the concentrated solution obtained in the step 1; heating and adding a granular activated carbon decoloring column for decoloring to obtain filtrate A;
as a more preferable embodiment of the invention, the mass of the added phosphoric acid is preferably 0.6-0.8% of the mass of the concentrated solution; in the decoloring treatment step, the temperature is preferably raised to 80-85 ℃, and the decoloring retention time of the granular activated carbon decoloring column is preferably 10-30 min. Further examples are as follows: transferring the concentrated solution (about 700 kg) to a reaction kettle, stirring, adding phosphoric acid (about 5 kg), heating to 80-85 ℃, feeding into a granular activated carbon decolorizing column at a certain flow rate for decolorizing, wherein the retention time of the granular activated carbon decolorizing column is 10-30 min; and after the decolorization is finished, taking out the ineffective granular activated carbon, drying the ineffective granular activated carbon in a kiln, pickling and then reusing the ineffective granular activated carbon, and continuously carrying out subsequent treatment on the filtrate A.
And step 3: adding liquid caustic soda into the filtrate A obtained in the step 2; dropwise adding diacetone, carrying out heat preservation reaction, cooling, filtering and recovering a filter cake to obtain a filtrate B;
in a more preferred embodiment of the present invention, the amount of the alkali solution added is preferably 30% by mass of the filtrate A. In the thermal insulation reaction process of dropwise adding the diacetone, the temperature required by the thermal insulation reaction is preferably 70-80 ℃, the thermal insulation time is preferably 10-20min, and the molar ratio of the dropwise adding the diacetone to the filtrate A is 1: 1.08; and in the cooling and filtering process, the cooling temperature is not higher than 40 ℃. Further examples are as follows: adding liquid caustic soda (about 3 kg) into the filtrate A, heating to 70-80 ℃, slowly dropwise adding diacetone (about 8 kg), preserving heat for 20min after dropwise adding, cooling to below 40 ℃, discharging and filtering, vacuumizing the filtrate into another reaction kettle, washing a filter cake with water to be neutral, and drying and weighing the filter cake AABI (5-acetoacetylaminobenzimidazolone) (about 19.6 kg); the filter cake has slightly yellow alkali-soluble color value of 1, the content of 99.17 percent and 317ppm of main impurities, and meets the quality requirement.
And 4, step 4: adding liquid caustic soda into the filtrate B obtained in the step 3 to adjust the pH value, and cooling to separate out salt; discharging and recovering the separated salt, and performing biochemical treatment on the residual wastewater.
In a preferred embodiment of the present invention, the PH is preferably adjusted to PH =9-10 during the PH adjustment by adding liquid caustic soda. And in the process of cooling, separating out and salifying, the temperature range of cooling is 35-40 ℃, and the separated salt is 12-hydrated disodium hydrogen phosphate after discharging and recycling. Further examples are as follows: to filtrate B was added liquid caustic (about 37 kg) to adjust the PH of filtrate B to PH = 9-10. After stirring and cooling to 35-40 ℃, discharging and recovering salt (colorless flaky crystals, 12-hydrated disodium hydrogen phosphate (Na2HPO4.12H2O) about 16.3 kg).
In addition, the fraction obtained by distillation in the MVR evaporator is preferably recovered by hydrogenation. Examples are as follows: the distillate from the MVR evaporator (about 4000 k) was taken and subjected to mechanical hydrotreatment: adding the fraction into a hydrogenation kettle, adding 5-nitrobenzimidazole ketone (about 200 kg) and palladium-carbon catalyst (about 1.5 kg) into the hydrogenation kettle, stirring after nitrogen replacement, heating to 110 ℃ at 100 ℃, continuously introducing hydrogen for reaction after hydrogen replacement is finished, and maintaining the hydrogen pressure at 0.5 Mpa; after the reaction is finished, sampling and performing central control, replacing the quality inspection with nitrogen after the quality inspection meets the central control requirement, separating the catalyst through a titanium rod filter, and cooling the filtrate to 35 ℃ under the protection of nitrogen; filtering by a filter press, storing the filtrate in a storage tank under the protection of nitrogen, air-blowing and squeezing the filter cake, sampling and detecting, and carrying out flash evaporation and drying on the filter cake to obtain the 5-aminobenzimidazole ketone (about 146.7 kg) with the yield of 88.1 percent. As a control, the hydrogenation yield without pure water was 81%; by comparison, the recycling rate of hydrogenation reuse is 7 percent.
The quality of the 5-aminobenzimidazole ketone obtained by the two recovery modes is detected, and the detection result is as follows:
| amino value/% | 5-amino content/%) | 5-nitro impurities/%) | Yield/% | Appearance of the product | |
| Hydrogenation for mechanical use | 98.43 | 98.67 | 0.2116 | 88.1 | White-like crystal |
| Hydrogenation of pure water | 98.51 | 98.69 | 0.2201 | 81 | White-like crystal |
According to the comparison of the detection results, the quality of the (5-aminobenzimidazole ketone) product after fraction hydrogenation recycling reaches the normal product water, and the recovery rate is improved.
The invention provides a method for treating 5-aminobenzimidazole ketone mother liquor, which comprises the following steps: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, adding phosphoric acid and decoloring, adding liquid alkali and diacetone, carrying out heat preservation reaction and filtration, carrying out heat preservation reaction on the diacetone, cooling and precipitating salt, and the like. The method for treating the 5-aminobenzimidazole mother liquor with the characteristics of the steps is simple and convenient to operate, high in safety coefficient and low in cost; the content of organic waste and COD in the treated wastewater is obviously reduced, the recovery of solid matters in the mother liquor wastewater can be realized, and the burden of subsequent treatment is reduced.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. The method for treating the 5-aminobenzimidazole mother liquor is characterized by comprising the following steps of:
step 1: evaporating and concentrating the 5-aminobenzimidazole mother liquor to obtain a concentrated solution, and recycling fractions;
step 2: adding phosphoric acid into the concentrated solution obtained in the step 1; heating and adding a granular activated carbon decoloring column for decoloring to obtain filtrate A;
and step 3: adding liquid caustic soda into the filtrate A obtained in the step 2; dropwise adding diacetone, carrying out heat preservation reaction, cooling, filtering and recovering a filter cake to obtain a filtrate B;
and 4, step 4: adding liquid caustic soda into the filtrate B obtained in the step 3 to adjust the pH value, and cooling to separate out salt; discharging and recovering the separated salt, and performing biochemical treatment on the residual wastewater.
2. The method for treating the 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein the recycling of the fraction in the step 1 is recycling of the fraction for hydrogenation.
3. The method for treating the 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein the evaporation concentration equipment used in the process of evaporating and concentrating the 5-aminobenzimidazole ketone mother liquor to obtain the concentrated solution in the step 1 is an MVR evaporator;
the mass of the concentrated solution obtained by evaporation and concentration is 10-15% of that of the 5-aminobenzimidazole mother liquor.
4. The method for treating a 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein the mass of the phosphoric acid added in the step 2 is 0.6-0.8% of the mass of the concentrated solution.
5. The method for treating the 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein in the step 2 of the decolorization treatment, the temperature is increased to 80-85 ℃, and the decolorization retention time of the granular activated carbon decolorizing column is 10-30 min.
6. The method for treating the 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein the mass of the liquid alkali added in the step 3 is 30% of the mass of the filtrate A.
7. The method for treating 5-aminobenzimidazole ketone mother liquor according to claim 1, wherein in the step 3, the temperature required for the heat preservation reaction is 70-80 ℃ and the heat preservation time is 10-20min in the heat preservation reaction process of dropwise adding the diacetone, and the molar ratio of the dropwise added diacetone to the filtrate A is 1: 1.08; and 3, in the cooling and filtering process in the step 3, the cooling temperature is not higher than 40 ℃, and the filter cake recovered by filtering is 5-acetoacetylaminobenzimidazolone.
8. The method for treating the mother liquor of 5-aminobenzimidazole according to claim 1, wherein the pH value is adjusted to pH =9-10 during the pH value adjustment by adding liquid alkali in the step 4.
9. The method for treating the mother liquor of 5-aminobenzimidazole according to claim 1, wherein in the step 4, the temperature is reduced to 35-40 ℃ during the salt precipitation, and the salt separated by discharging and recovering is 12-disodium hydrogen phosphate hydrate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979948A (en) * | 2021-12-15 | 2022-01-28 | 山东汇海医药化工有限公司 | Method for recovering AABI from mother liquor of AABI reduction process |
| CN114369066A (en) * | 2021-12-09 | 2022-04-19 | 山东汇海医药化工有限公司 | Method for recycling 5-acetoacetylaminobenzimidazolone mother liquor |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| BR7602622A (en) * | 1975-04-29 | 1976-11-23 | Hoechst Ag | PROCESS FOR THE PREPARATION OF 5-ACETOACETYLAMINOBENIMIDAZOLONE |
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| CN113979948B (en) * | 2021-12-15 | 2024-02-06 | 山东汇海医药化工有限公司 | Method for recovering AABI from AABI reduction process mother liquor |
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