CN110156705A - A kind of method of benzotriazole Synthesis liquid acidification tail gas resource utilization - Google Patents
A kind of method of benzotriazole Synthesis liquid acidification tail gas resource utilization Download PDFInfo
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- CN110156705A CN110156705A CN201910449742.5A CN201910449742A CN110156705A CN 110156705 A CN110156705 A CN 110156705A CN 201910449742 A CN201910449742 A CN 201910449742A CN 110156705 A CN110156705 A CN 110156705A
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- tail gas
- bta
- resource utilization
- synthesis liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/16—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms condensed with carbocyclic rings or ring systems
- C07D249/18—Benzotriazoles
Abstract
The invention belongs to the technical fields of petrochemical industry, it is related to a kind of method of benzotriazole (abbreviation BTA) Synthesis liquid acidification tail gas resource utilization, more specifically, it is related to being acidified tail gas (nitrogen oxides) with BTA Synthesis liquid as starting material, pressurized absorption, nitrogen oxides is recycled, the method for BTA is directly synthesized.
Description
Technical field
The invention belongs to the technical fields of petrochemical industry, are related to a kind of benzotriazole (abbreviation BTA) Synthesis liquid acidification tail
The method of gas resource utilization is acidified tail gas (nitrogen oxides) for starting material, through adding more particularly, to BTA Synthesis liquid
Pressure absorbs, and recycles nitrogen oxides, directly synthesizes the method for BTA.
Background technique
Benzotriazole (CAS:95-14-7) is the light brown acicular crystal of white, is a kind of important fine chemical product,
It has many uses, and is mainly used for the rust and corrosion of metal (silver, copper, lead, nickel, zinc etc.), is also used as coating and adds
Add agent, the preservative of synthetic detergent, anti-coagulants, synthetic dyestuffs intermediate etc., downstream application is extensive.
Patent (CN105237488A) discloses a kind of synthetic method of benzotriazole, passes through o-phenylenediamine and nitrous acid
Sodium pressurization one-step synthesis benzotriazole, but vent gas treatment scheme is not proposed, the scheme of resource utilization is not proposed.
The present invention provides a kind of method of benzotriazole Synthesis liquid acidification tail gas resource utilization, do not appear in the newspapers in document
Road.Specifically, by BTA Synthesis liquid tune acid nitrogen oxide in tail gas through compressor compresses into reaction kettle, synthesize BTA, reach money
The purpose that source utilizes.The present invention almost realizes the zero-emission of nitrogen oxides in BTA production process, and there is nitrogen oxides to utilize
Rate height, strong operability, environmental pollution is small, economy is strong, the advantages of being easily industrialized.
Summary of the invention
The present invention provides a kind of methods of benzotriazole Synthesis liquid acidification tail gas resource utilization.Specifically, with BTA
It is starting material that Synthesis liquid, which is acidified tail gas (nitrogen oxides), and nitrogen oxides is recycled in pressurized absorption, directly synthesis BTA.
It is an object of the invention to study a kind of method of BTA Synthesis liquid acidification tail gas resource utilization, there is nitrogen oxidation
Object utilization rate height, strong operability, environmental pollution is small, economy is strong, the advantages of being easily industrialized.
A kind of method of BTA Synthesis liquid acidification tail gas resource utilization, including the following steps:
(1) BTA reaction solution acidification tail gas is pressurizeed through compressor, reaches certain pressure and temperature；
(2) it by a certain amount of water, sodium nitrite, o-phenylenediamine investment reaction kettle, is dispersed with stirring at a certain temperature；
(3) oxygen and compressed tail gas are passed through reaction kettle, reacted under certain condition, obtain BTA reaction after reaction
Liquid.
In above-mentioned steps (1), the described compressor pressurization rear molding atmospheric pressure is 0.1~10MPa, preferably temperature be 20~
100℃；
In above-mentioned steps (2), the water: the weight ratio of sodium nitrite is 1:0.1~1:1, sodium nitrite: o-phenylenediamine
The ratio between the amount of substance be 0.5:1~1.1:1；
In above-mentioned steps (2), the temperature for being dispersed with stirring control is 0~150 DEG C；
In above-mentioned steps (3), the compressed tail gas dosage is 0.1~2.0 times of amount of the substance of o-phenylenediamine；
In above-mentioned steps (3), the oxygen pressure be 0.1~0.5MPa, dosage be preferably exhaust gas species amount 0.1~
0.5 times, system pressure is 0~0.2MPa after being passed through oxygen；
In above-mentioned steps (3), preferred 240-290 DEG C of the reaction temperature, soaking time preferably 2~6h, reaction pressure
Preferably 2~6MPa.
Tail gas compression absorbs after the reaction of a series of complex, product is controlled based on sodium nitrite, for synthesizing
BTA.In view of practical operation, controlling flow of oxygen makes slow oxidative absorption, 0~0.2MPa of final control system pressure, to protect
No oxygen residual (oxygen bottom product colour difference) in card system, it is ensured that nitrogen oxides is slightly excessive, then completes BTA synthesis, to protect
Hinder normal reaction.
The present invention has the advantage that
A kind of method of benzotriazole Synthesis liquid acidification tail gas resource utilization, will be acidified tail gas pressurizing absorption, recycling
Nitrogen oxides is directly used in BTA synthesis, to realize the almost zero-emission of the acidification resource utilization of tail gas, nitrogen oxides
Purpose.Meaning of the present invention is: nitrogen oxides tail gas resource utilization does not have significant impact, while raw material to reaction yield
The usage amount of sodium nitrite can also save 5~10% in original basis.With nitrogen oxides utilization rate height, strong operability, ring
The border small, economy of pollution is strong, the advantages of being easily industrialized.
Specific embodiment
The following examples are illustrated in more detail the present invention, rather than limitation of the invention further.It removes
Non- to be otherwise noted, " % " therein is " quality % ".
Embodiment 1
BTA synthesis: by 295kg o-phenylenediamine, 213kg sodium nitrite, 370kg water is placed in 1000L autoclave, and nitrogen is set
It changes, is warming up to 260 DEG C after mixing evenly, insulation reaction 3h.After heat preservation, cool down pressure release, releases brown supernatant liquid
877kg analyzes to obtain o-phenylenediamine conversion ratio 100%, BTA yield 98.9%.Carry out BTA synthesis, reaction solution tune acid with this technique
Acidification, tail gas are used for resource utilization.
Acidification and exhaust collection: above-mentioned reaction solution 430kg25% hydrochloric acid being acidified, controls 60~70 DEG C of reaction temperature,
Terminal system pH=4~6 are acidified, gained tail gas is used for resource utilization through compressor pressurized collection.
Embodiment 2
Tail gas resource utilization: the tail gas of embodiment 1 is forced into 1.1MPa through compressor, at this time compressed tail gas temperature
50~60 DEG C of degree.O-phenylenediamine 29.5kg is put into 100L reaction kettle, sodium nitrite 20.5kg, water 37kg are warming up to 50 DEG C
Stirring.Acidification tail gas is filled with into reaction kettle by compressor, pressure and compressor on kettle is made to reach 1.1MPa.Switch oxygen
Gas is slowly oxygenated, and system pressure slowly declines at this time, until pressure drops to 0.1MPa, stops oxygenation.Reaction kettle is warming up to
270 DEG C of insulation reaction 3h.Reaction terminates, and cool down pressure release, and tail gas collects reuse with compressor.Brown transparency liquid is released about in kettle
87kg.Through analyzing o-phenylenediamine conversion ratio 100%, BTA yield 98.2%.
Embodiment 3
The tail gas of embodiment 1 is forced into 3MPa through compressor, 50~60 DEG C of exhaust temperature after control compression at this time.It is past
O-phenylenediamine 29.5kg, sodium nitrite 19kg, water 37kg are put into 100L reaction kettle, are warming up to 50 DEG C of stirrings.Pass through compressor
It is filled with acidification tail gas into reaction kettle, pressure and compressor on kettle is made to reach 3MPa.Switch oxygen, is slowly oxygenated, at this time body
It is that pressure slowly declines, until pressure drops to 0.1MPa, stops oxygenation.Reaction kettle is warming up to 270 DEG C of insulation reaction 3h.Reaction
Terminate, cool down pressure release, and tail gas collects reuse with compressor.Brown transparency liquid about 87kg is released in kettle.Through analyzing o-phenylenediamine
Conversion ratio 100%, BTA yield 97.9%.
Embodiment 4-7
Change compressed tail gas pressure on the basis of embodiment 2, change sodium nitrite inventory, other conditions are constant, knot
Fruit is as follows:
Embodiment 8-10
Embodiment 2 is acidified exhaust collection compression, nitrogen oxides tail gas is applied according to 2 reaction process of embodiment, realizes nitrogen
Oxide recycles, as a result as follows:
Content of the present invention is not limited in embodiment content of the present invention.
Specific case used herein is expounded structure of the invention and embodiment, the explanation of above embodiments
It is merely used to help understand the core idea of the present invention.It should be pointed out that for those skilled in the art,
Without departing from the principles of the invention, can be with several improvements and modifications are made to the present invention, these improvement and modification are also fallen
Enter in the protection scope of the claims in the present invention.
Claims (7)
1. a kind of method of BTA Synthesis liquid acidification tail gas resource utilization, feature with, including the following steps:
(1) BTA reaction solution acidification tail gas is pressurizeed through compressor, reaches certain pressure and temperature；
(2) it by a certain amount of water, sodium nitrite, o-phenylenediamine investment reaction kettle, is dispersed with stirring at a certain temperature；
(3) oxygen and compressed tail gas are passed through reaction kettle, reacted under certain condition, obtain BTA reaction solution after reaction.
2. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (1), the compressor pressurization rear molding atmospheric pressure is 0.1~10MPa, and temperature is 20~100 DEG C.
3. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (2), the water: the weight ratio of sodium nitrite is 1:0.1~1:1, sodium nitrite: the ratio between amount of substance of o-phenylenediamine
For 0.5:1~1.1:1.
4. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (2), the temperature for being dispersed with stirring control is 0~150 DEG C.
5. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (3), the compressed tail gas dosage is 0.1~2.0 times of amount of the substance of o-phenylenediamine.
6. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (3), the oxygen pressure is 0.1~0.5MPa, and dosage is 0.1~0.5 times of amount of exhaust gas species, is passed through body after oxygen
Be pressure be 0~0.2MPa.
7. the method for BTA Synthesis liquid according to claim 1 acidification tail gas resource utilization, feature with above-mentioned step
Suddenly in (3), the reaction temperature is 240-290 DEG C, and soaking time is 2~6h, and reaction pressure is 2~6MPa.
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Citations (6)
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| CN1864812A (en) * | 2006-04-24 | 2006-11-22 | 南京大学 | A nitric oxides (NOX) waste pollution control in industrial process and resource reclaiming method |
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| US20140171658A1 (en) * | 2011-12-16 | 2014-06-19 | Chemtreat Inc. | Methods for triazole synthesis |
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| CN105237488A (en) * | 2015-11-13 | 2016-01-13 | 如皋市金陵化工有限公司 | Synthesis method of benzotriazole |
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2019
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| CN1864812A (en) * | 2006-04-24 | 2006-11-22 | 南京大学 | A nitric oxides (NOX) waste pollution control in industrial process and resource reclaiming method |
| CN101095998A (en) * | 2006-06-26 | 2008-01-02 | 山东金城医药化工有限公司 | Recovery utilization method of furfuran amine salt waste gases |
| CN102247748A (en) * | 2011-06-30 | 2011-11-23 | 湖北省宏源药业有限公司 | Treatment method and treatment system of tail gas from glyoxylic acid production by nitric acid oxidation of glyoxal |
| US20140171658A1 (en) * | 2011-12-16 | 2014-06-19 | Chemtreat Inc. | Methods for triazole synthesis |
| CN104628664A (en) * | 2015-02-05 | 2015-05-20 | 甘肃众亨新材料科技股份有限公司 | Method for continuously producing benzotriazole |
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Application publication date: 20190823 |