CN106397332A - Method for treating 5-nitrobenzimidazolone mother liquor by reduction with iron powder - Google Patents
Method for treating 5-nitrobenzimidazolone mother liquor by reduction with iron powder Download PDFInfo
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- CN106397332A CN106397332A CN201610763873.7A CN201610763873A CN106397332A CN 106397332 A CN106397332 A CN 106397332A CN 201610763873 A CN201610763873 A CN 201610763873A CN 106397332 A CN106397332 A CN 106397332A
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- iron powder
- benzimidazolinone
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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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Abstract
The invention discloses a method for treating 5-nitrobenzimidazolone-2 mother liquor by reduction with iron powder. An aqueous solution with hydrochloric acid added is used as a solvent, iron powder is added and temperature is reaised to 80-100 DEG C, and 5-nitrobenzimidazolone is added and insulation is carried out at 80-100 DEG C for 1-2 hours; after insulation, a sodium hydroxide solution is used for adjusting the pH value to 7-9, a catalyst is added, insulation is carried out for 10-30 minutes, and pumping filtration is carried out in order to obtain an aqueous solution of 5-nitrobenzimidazolone; the temperature of the solution is reduced to 30-45 DEG C, pumping filtration is carried out in order to obtain 5-nitrobenzimidazolone, and the filtrate is treated and used as a reduction solvent of 5-nitrobenzimidazolone continuously. A filtrate treatment method comprises the following steps: hydrochloric acid is added into the filtrate, after filtering, the filtrate is used as a solvent for reducing 5-nitrobenzimidazolone, iron powder is directly added, and a reduction reaction is carried out; reduction requirements are satisfied, and the purpose of repeat usage is realized.
Description
Technical field
The invention belongs to chemical mother liquid disposal field is and in particular at a kind of iron powder reducing 5-Nitro-2-benzimidazolinone mother solution
The method of reason.
Background technology
With water as solvent, produce a large amount of waste water with iron powder reducing 5-Nitro-2-benzimidazolinone, reduce one ton of 5- nitro benzo
Imidazolone water is about 8 sides, huge using simple distillation process power consumption, causes energy waste, so severe at present
Environmental Protection Situation under, solve wastewater problem extremely urgent.
In view of the restriction of above-mentioned technique and shortcoming, need to improve.
Content of the invention
It is an object of the invention to provide a kind of method of iron powder reducing 5-Nitro-2-benzimidazolinone mother liquid disposal.
The technical solution adopted for the present invention to solve the technical problems is：At iron powder reducing 5-Nitro-2-benzimidazolinone mother solution
The method of reason, comprises the following steps：
1) it is warming up to 80-100 DEG C after adding iron powder in aqueous hydrochloric acid solution, hydrochloric acid addition is the 0.1- of solvent water quality
2%, add 5-Nitro-2-benzimidazolinone and be incubated 1-2h at 80-100 DEG C, after the completion of insulation, adjust pH to 7- with sodium hydroxide solution
9, add catalyst, sucking filtration obtains the aqueous solution of 5-Amino-2-benzimidazolinone, obtain solid 5- aminobenzene by after solution cooling sucking filtration
And imidazolone, liquid is mother solution；
2) add in mother solution and account for filtration after the hydrochloric acid that its quality is 0.1-2%, filtrate is as 5-Nitro-2-benzimidazolinone
The solvent of reduction.
Specifically, described step 1) in iron powder addition be quantity of solvent 0.04-0.1%.
Specifically, described step 1) in the ratio of 5-Nitro-2-benzimidazolinone and the amount of the material of iron powder be 2:5-1:3.
Specifically, described step 1) in catalyst be sodium sulfite and activated carbon, the addition of sodium sulfite is molten
The 0.1-1% of agent weight, the addition of activated carbon is the 0.5-2% of weight of solvent.
The invention has the advantages that：The method of the present invention is filtered after solvent adds hydrochloric acid, solves universal
The problems such as wastewater flow rate existing is big, processing cost is high, energy waste, environmental pollution are big and production cost is high, improves filtrate quality,
There is no material and energy waste, reduce impurity and retain, improve solvent utilization rate, reduce production cost.
Specific embodiment
The following is the specific embodiment of the present invention, technical scheme is described further, but the present invention
Protection domain is not limited to these embodiments.Every change without departing substantially from present inventive concept or equivalent substitute are included in the present invention
Protection domain within.
Embodiment 1
It is warming up to 80 DEG C, hydrochloric acid addition is the 1% of solvent water quality, and iron powder adds after adding iron powder in aqueous hydrochloric acid solution
Enter amount for the 0.04% of quantity of solvent, add 5-Nitro-2-benzimidazolinone to be simultaneously incubated 1h, 5-Nitro-2-benzimidazolinone and ferrum at 90 DEG C
The ratio of the amount of the material of powder is 2:5, adjust pH to 8 with sodium hydroxide solution after the completion of insulation, add catalyst, catalyst is sulfurous
Sour hydrogen sodium and activated carbon, the addition of sodium sulfite is the 0.8% of weight of solvent, and the addition of activated carbon is weight of solvent
2%, sucking filtration obtains the aqueous solution of 5-Amino-2-benzimidazolinone, obtains solid 5-Amino-2-benzimidazolinone by after solution cooling sucking filtration,
Liquid is mother solution；Add in mother solution and filter after accounting for the hydrochloric acid that its quality is 0.1%, filtrate is as 5-Nitro-2-benzimidazolinone also
Former solvent.Product weight 105.3kg, yield 84.33%, purity 97.68%.
Reuse in 10 below reaction cycle of gained solvent, be not required to again salt adding acid.Result statistics is as follows：
Embodiment 2
It is warming up to 90 DEG C, hydrochloric acid addition is the 0.1% of solvent water quality, iron powder after adding iron powder in aqueous hydrochloric acid solution
Addition be quantity of solvent 0.1%, add 5-Nitro-2-benzimidazolinone and 100 DEG C be incubated 1h, 5-Nitro-2-benzimidazolinone with
The ratio of the amount of the material of iron powder is 1:3, adjust pH to 9 with sodium hydroxide solution after the completion of insulation, add catalyst, catalyst is Asia
Sodium bisulfate and activated carbon, the addition of sodium sulfite is the 0.1% of weight of solvent, and the addition of activated carbon is weight of solvent
0.5%, sucking filtration obtains the aqueous solution of 5-Amino-2-benzimidazolinone, by solution lower the temperature sucking filtration after solid 5- aminobenzimidazole
Ketone, liquid is mother solution；Add in mother solution and filter after accounting for the hydrochloric acid that its quality is 1%, filtrate is as 5-Nitro-2-benzimidazolinone
The solvent of reduction.Product weight 109.7kg, yield 87.86, purity 97.59%.
Embodiment 3
It is warming up to 100 DEG C, hydrochloric acid addition is the 2% of solvent water quality, iron powder after adding iron powder in aqueous hydrochloric acid solution
Addition be quantity of solvent 0.08%, add 5-Nitro-2-benzimidazolinone and 80 DEG C be incubated 2h, 5-Nitro-2-benzimidazolinone with
The ratio of the amount of the material of iron powder is 1.1:3, adjust pH to 7 with sodium hydroxide solution after the completion of insulation, add catalyst, catalyst is
Sodium sulfite and activated carbon, the addition of sodium sulfite is the 1% of weight of solvent, and the addition of activated carbon is weight of solvent
1%, sucking filtration obtains the aqueous solution of 5-Amino-2-benzimidazolinone, by solution lower the temperature sucking filtration after solid 5- aminobenzimidazole
Ketone, liquid is mother solution；Add in mother solution and filter after accounting for the hydrochloric acid that its quality is 2%, filtrate is as 5-Nitro-2-benzimidazolinone
The solvent of reduction.Product weight 109.6kg, yield 87.78, purity 97.54%.
Claims (4)
1. the method for iron powder reducing 5-Nitro-2-benzimidazolinone mother liquid disposal is it is characterised in that comprise the following steps：
1) it is warming up to 80-100 DEG C after adding iron powder in aqueous hydrochloric acid solution, hydrochloric acid addition is the 0.1-2% of solvent water quality,
Add 5-Nitro-2-benzimidazolinone and be incubated 1-2h at 80-100 DEG C, after the completion of insulation, adjust pH to 7-9 with sodium hydroxide solution, plus
Enter catalyst, sucking filtration obtains the aqueous solution of 5-Amino-2-benzimidazolinone, obtain solid 5- amino benzo miaow by after solution cooling sucking filtration
Oxazolone, liquid is mother solution；
2) add in mother solution and account for filtration after the hydrochloric acid that its quality is 0.1-2%, filtrate reduces as 5-Nitro-2-benzimidazolinone
Solvent.
2. the method for iron powder reducing 5-Nitro-2-benzimidazolinone mother liquid disposal according to claim 1 is it is characterised in that institute
State step 1) in iron powder addition be quantity of solvent 0.04-0.1%.
3. the method for iron powder reducing 5-Nitro-2-benzimidazolinone mother liquid disposal according to claim 1 is it is characterised in that institute
State step 1) in the ratio of 5-Nitro-2-benzimidazolinone and the amount of the material of iron powder be 2:5-1:3.
4. the method for iron powder reducing 5-Nitro-2-benzimidazolinone mother liquid disposal according to claim 1 is it is characterised in that institute
State step 1) in catalyst be sodium sulfite and activated carbon, the addition of sodium sulfite is the 0.1-1% of weight of solvent, lives
Property charcoal addition be weight of solvent 0.5-2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610763873.7A CN106397332A (en) | 2016-08-30 | 2016-08-30 | Method for treating 5-nitrobenzimidazolone mother liquor by reduction with iron powder |
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| CN201610763873.7A CN106397332A (en) | 2016-08-30 | 2016-08-30 | Method for treating 5-nitrobenzimidazolone mother liquor by reduction with iron powder |
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| CN201610763873.7A Pending CN106397332A (en) | 2016-08-30 | 2016-08-30 | Method for treating 5-nitrobenzimidazolone mother liquor by reduction with iron powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336825A (en) * | 2018-11-23 | 2019-02-15 | 山东汇海医药化工有限公司 | A method of improving 5-Amino-2-benzimidazolinone quality |
| 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 |
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| CN1100403A (en) * | 1994-05-07 | 1995-03-22 | 营口市江汇化工厂 | Iron powder-adding preparation process of 1.5,1.8-diamido naphthalene mixture |
| CN1397544A (en) * | 2001-07-12 | 2003-02-19 | 郑效农 | Process for preparing 4,4-diaminodiphenyl ether |
| CN101307023A (en) * | 2008-05-23 | 2008-11-19 | 东营市天正化工有限公司 | Production process of 5-acetyl acetamino benzimidazolone |
| JP2009191213A (en) * | 2008-02-15 | 2009-08-27 | Fujifilm Corp | Cyanine compound having cyclic amide group and near infrared absorbing composition containing the same |
| CN103664794A (en) * | 2013-12-30 | 2014-03-26 | 青岛双桃精细化工（集团）有限公司 | Preparation method for 5-acetoacetlamino benzimdazolone |
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2016
- 2016-08-30 CN CN201610763873.7A patent/CN106397332A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100403A (en) * | 1994-05-07 | 1995-03-22 | 营口市江汇化工厂 | Iron powder-adding preparation process of 1.5,1.8-diamido naphthalene mixture |
| CN1397544A (en) * | 2001-07-12 | 2003-02-19 | 郑效农 | Process for preparing 4,4-diaminodiphenyl ether |
| JP2009191213A (en) * | 2008-02-15 | 2009-08-27 | Fujifilm Corp | Cyanine compound having cyclic amide group and near infrared absorbing composition containing the same |
| CN101307023A (en) * | 2008-05-23 | 2008-11-19 | 东营市天正化工有限公司 | Production process of 5-acetyl acetamino benzimidazolone |
| CN103664794A (en) * | 2013-12-30 | 2014-03-26 | 青岛双桃精细化工（集团）有限公司 | Preparation method for 5-acetoacetlamino benzimdazolone |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336825A (en) * | 2018-11-23 | 2019-02-15 | 山东汇海医药化工有限公司 | A method of improving 5-Amino-2-benzimidazolinone quality |
| 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 |
| 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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Application publication date: 20170215 |