CN104803533B - Method for treating AABI (5-Acetoacetyl-amino-benzimidazolone) acylation wastewater - Google Patents

Method for treating AABI (5-Acetoacetyl-amino-benzimidazolone) acylation wastewater Download PDF

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CN104803533B
CN104803533B CN201510175708.5A CN201510175708A CN104803533B CN 104803533 B CN104803533 B CN 104803533B CN 201510175708 A CN201510175708 A CN 201510175708A CN 104803533 B CN104803533 B CN 104803533B
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aabi
waste water
acylated
wastewater
acylation
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CN104803533A (en
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牟应科
郑庚修
王乐强
张世凤
侯绪会
侯利国
宋师峰
李保铃
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HUIHAI MEDICAL CHEMICAL CO Ltd SHANDONG
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HUIHAI MEDICAL CHEMICAL CO Ltd SHANDONG
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Abstract

The invention relates to a method for treating AABI (5-Acetoacetyl-amino-benzimidazolone) acylation wastewater. The method mainly comprises the steps of basic hydrolysis, acetone distillation, triple effect evaporation and phosphorous removal with lime. The method is safe to operate and low in production cost, water collected from evaporation can meet the use requirement at an AABI acylation post and returns to the acylation post for repeated application, and environmental protection and saving are realized; the wastewater can be treated with a conventional biochemical technology after hydrolysis, distillation and phosphorous removal, 75%-88% of tons of wastewater produced in AABI production is reduced after adoption of the technology, and environmental protection benefits are remarkable.

Description

A kind of AABI is acylated the processing method of waste water
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of AABI is acylated the processing method of waste water.
Background technology
AABI (AABI) is the light colour pigment such as the high-grade organic pigment of synthesis is for example yellow, orange Key intermediate.Downstream pigment mainly has:C.I. pigment Yellow 12 0,151,154,175,180,181, orange 36,62 etc..
At present the method for the AABI of large-scale production both at home and abroad is by o-phenylenediamine and urea cyclization, nitrification, reduction, acylation Four steps obtain finished product AABI.But it is exactly that the wastewater flow rate for producing is very huge that the process route has a significantly defect, is put down One ton of AABI is often produced, 50 tons or so of waste water will be produced, the wastewater flow rate of wherein acylation step accounts for more than 90%.Acylated waste water In containing AABI, acetone, phosphate etc., it is impossible to directly carry out biochemical treatment.Simultaneously because it contains AABI, 5- of macromolecular The hardly degraded organic substances such as ABI, 5- acetamino benzimidazolone, chroma in waste water is big, and COD contents are high, and environmental protection treatment is very difficult.
In view of the restriction of above-mentioned processing method and shortcoming, need to be improved.
The content of the invention
It is an object of the invention to provide a kind of production technology is reasonable, wastewater discharge is little and water energy circulation and stress uses AABI is acylated the processing method of waste water.
The technical solution adopted for the present invention to solve the technical problems is:A kind of AABI is acylated the processing method of waste water, bag Include following steps:
1) liquid caustic soda of its 5-10wt% is accounted for addition in acylated waste water under normal temperature, regulation pH value is 8-9;
2) by step 1) waste water that regulates pH value is warming up to 80-105 DEG C, AABI, 5-ABI, 5- acetylamino benzo miaow The larger molecular organicses such as oxazolone decompose 2-5 hours;
3) in step 2) in larger molecular organicses decomposable process, the lower boiling organic principles such as acetone are collected, it is collected Organic principle separately purification processes;
4) by step 2) and step 3) process after waste water distilled with triple effect evaporator, steam and account for raw wastewater amount 75- 88% moisture;
5) to step 4) a certain amount of quick lime is added in remaining waste water after distillation, phosphate radical is changed into into calcium phosphate and is sunk It is filtered to remove behind shallow lake;
6) by step 5) process after waste water be incorporated to biochemical system and be further processed.
Preferably, the step 2) in temperature be preferably 85-95 DEG C, the alkaline decomposition of step (2) enters generally according to following formula OK:
The step 4) moisture that steams is back to acylated post and repeats to apply mechanically.
The step 5) in the addition of lime be the 2-3.5wt% for accounting for raw wastewater.
The invention has the advantages that:Simple and easy to control, safe operation of the invention, low production cost, relative to existing Technology, with advantages below:The water collected through basic hydrolysis, acetone distillation, triple effect evaporation disclosure satisfy that AABI is acylated hilllock The use requirement of position, returns to acylated post and repeats to apply mechanically, environmental protection and saving;The enough routines of waste water energy after hydrolysis, distillation, dephosphorization Biochemical technology processed;75-88% is reduced using AABI production tons waste water after the technology, environmental benefit is fairly obvious.
Specific embodiment
The specific embodiment of the present invention is the following is, technical scheme is described further, but the present invention Protection domain is not limited to these embodiments.Every change or equivalent substitute without departing substantially from present inventive concept is included in the present invention Protection domain within.
A kind of AABI is acylated the processing method of waste water, comprises the following steps:
1) liquid caustic soda of its 5-10wt% is accounted for addition in acylated waste water under normal temperature, regulation pH value is 8-9;
2) by step 1) waste water that regulates pH value is warming up to 80-105 DEG C, and preferably 85-95 DEG C, AABI, 5-ABI, 5- The larger molecular organicses such as acetamino benzimidazolone decompose 2-5 hours;
3) in step 2) in larger molecular organicses decomposable process, the lower boiling organic principles such as acetone are collected, it is collected Organic principle separately purification processes;
4) by step 2) and step 3) process after waste water distilled with triple effect evaporator, steam and account for raw wastewater amount 75- 88% moisture, the moisture for steaming is back to acylated post to be repeated to apply mechanically;
5) to step 4) lime for accounting for raw wastewater 2-3.5wt% is added in remaining waste water after distillation, phosphate radical is changed To be filtered to remove after calcium phosphate precipitation;
6) by step 5) process after waste water be incorporated to biochemical system and be further processed.
Specific embodiment 1
To in reactor add AABI be acylated waste water 500kg (phosphate content about 0.35%, AABI contents about 0.08%, About 1.48%) 5- acetamino benzimidazolones content, is subsequently adding liquid caustic soda 25kg, is warming up to 80-105 DEG C, and stirring decomposes 2.5 Hour (larger molecular organicses such as AABI, 5-ABI, 5- acetamino benzimidazolone remained in Decomposition Wastewater), decomposition it is same When collect low boiling distillate (about 38kg, content of acetone 54%, separately purification process);After the completion of decomposition, using triple effect evaporator Distillation waste water, collect -0.08MPa, (85%) about 425kg, account for 65-80 DEG C of cut, is back to acylated post.Distillation remainder Point, 4kg quick limes are added after being sufficiently stirred for, filter out and arrange remainder waste water after the calcium phosphate solid (about 6.5kg) of precipitation Putting to biochemical treatment tank carries out subsequent treatment.
The water that steams of gained has carried out the AABI acylation experimental verifications of 6 batches, as a result as shown in table 1, average yield 73.34%, purity 99.45%, impurity peaks 0.0072%, with the AABI products produced using fresh water yield (73.46%), Purity (99.23%) aspect is without significant difference, and it is qualified to be.
Table 1 steams water AABI and is acylated experimental result statistical form
The detached water return AABI acylations post that steams of embodiment 1 is applied mechanically, i.e., is used as solvent, detailed process (with As a example by the 6th batch in table 1) be:300kg is added to steam the catalyst of water, 20kg5-ABI, and respective numbers in reactor, Ketene dimer 15kg is added dropwise at 80-85 DEG C, 30 DEG C are cooled to after completion of dropping.Centrifuge rejection filter, filter cake steams water with 50kg Washing, obtains after drying finished product AABI22.95kg.Again Jing vacuum distillations obtain finished product AABI after precipitation, and its yield is 73.41%, purity is 99.43%, and impurity peaks are 0.0087%, reaches the level of normal product.

Claims (3)

1. a kind of AABI is acylated the processing method of waste water, it is characterised in that comprise the following steps:
1) liquid caustic soda of its 5-10wt% is accounted for addition in acylated waste water under normal temperature, regulation pH value is 8-9;
2) by step 1) waste water that regulates pH value is warming up to 80-105 DEG C, AABI, 5-ABI, 5- acetamino benzimidazolone Larger molecular organicses decompose 2-5 hours;
3) in step 2) in larger molecular organicses decomposable process, lower boiling organic principle is collected, collected organic principle is another Row purification processes;
4) by step 2) and step 3) process after waste water distilled with triple effect evaporator, steam and account for raw wastewater amount 75-88% Moisture;
5) to step 4) add a certain amount of lime after distillation in remaining waste water, the addition of lime for raw wastewater 2- 3.5wt%, phosphate radical is changed into after calcium phosphate precipitation and is filtered to remove;
6) by step 5) process after waste water be incorporated to biochemical system and be further processed.
2. AABI according to claim 1 is acylated the processing method of waste water, it is characterised in that the step 2) in temperature it is excellent Elect 85-95 DEG C as.
3. AABI according to claim 1 is acylated the processing method of waste water, it is characterised in that the step 4) water that steams Divide and be back to acylated post recycling.
CN201510175708.5A 2015-04-14 2015-04-14 Method for treating AABI (5-Acetoacetyl-amino-benzimidazolone) acylation wastewater Active CN104803533B (en)

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Denomination of invention: A treatment method of aabi acylation wastewater

Effective date of registration: 20211130

Granted publication date: 20170510

Pledgee: Dongying Hekou District sub branch of China Post Savings Bank Co.,Ltd.

Pledgor: SHANDONG HUIHAI PHARMACEUTICAL& CHEMICAL Co.,Ltd.

Registration number: Y2021980013568