CN103450101B - Continuous purification process of methylbenzotriazole - Google Patents
Continuous purification process of methylbenzotriazole Download PDFInfo
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- CN103450101B CN103450101B CN201310166309.3A CN201310166309A CN103450101B CN 103450101 B CN103450101 B CN 103450101B CN 201310166309 A CN201310166309 A CN 201310166309A CN 103450101 B CN103450101 B CN 103450101B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a continuous purification process of methylbenzotriazole. The continuous purification process comprises the following steps of feeding a coarse material into a low fraction removing tower T1 through a pump P1 for gas-liquid exchange, feeding a high-boiling point material at the bottom of the tower to the middle part of a product tower through a heating part by virtue of a pump P2 for rectification and separation, and after the heat exchange of the material in the product tower, feeding a high-boiling point material part into a high-boiling material storage tank V5A/V5B through a pump P5, and then discharging the material. The continuous purification process of methylbenzotriazole is capable of improving the quality of the product, improving the productivity, saving energy and reducing consumption; the continuous purification process is stable in quality; therefore, the cost is reduced and the economic benefit is improved.
Description
Technical field
The present invention relates to a kind of continuous purifying technique of methyl benzotriazazole, belong to the purifying technique field of fine chemical product.
Background technology
Methyl benzotriazazole is mainly used as rust-preventive agent and the inhibiter of metal (as silver, copper, lead, nickel, zinc etc.), be widely used in slushing oil (fat) series products, be used for the vapour-phase inhibitor of Copper and its alloy, lubricating oil additive, circulating water treatment agent, automobile antifreeze solution.
In Chemicals production process, through multi-step chemical reaction, have various organic and inorganic impurities left in the finished product of production and affect the quality of the finished product.The method of purification that methyl benzotriazazole is conventional is that intermittent fractionation is purified, and product purity is not high, and after distillation, in residue, leftover materials are more, and product yield is not high, and quality is unstable.
Summary of the invention
The object of the invention is to solve the defect existed in prior art, a kind of continuous purifying technique of methyl benzotriazazole is provided, improves the quality of product.
The present invention is achieved through the following technical solutions:
The continuous purifying technique of methyl benzotriazazole is as follows: crude product material is pumped into de-low tower T1 by P1, carry out vapour-liquid exchange, low-boiling material front-end volatiles arrive top of tower E2 by exchanging, get off to exchange with ascending gas through being cooled to liquid state, the material that boiling point is high carries out the bottom that tower is got back in heat exchange, returned in tower by falling-film reboiler E1 heating and exchange, repeatedly exchanged by filler in de-low tower, reach a kind of balance, tower top lower boiling material is undertaken refluxing by reflux ratio controller E1 and takes out, high boiler material at the bottom of tower is sent in the middle part of product tower through hot spots by pump P2, carry out rectifying separation, front-end volatiles in tower top enter storage tank, automatically produced by pump P3.
Materials at bottom of tower is by entering in product tower T2 by flow F1 after heat exchange, pass through heat exchange, product steam cools through condenser E4, a part is separated by reflux ratio controller R2 and is entered products pot V3, partial reflux enter in tower with rise gas carry out exchange portions from, the storage tank V4 that the material returning at the bottom of tower enters tower bottom by pump P5 carry out circulation deliver to thin-film evaporator E3A E3B carry out heating and gasifying again, gas phase enters in tower carries out exchange separation, high boiler material part sends into the discharging of high boiling material storage tank by pump P5, product in tower top is separated by reflux ratio controller R2, enter storage tank V3, automatically produced by pump P6.
Preferably, de-low tower T1 theoretical plate number is 35 pieces.
De-low tower T1 tower top temperature controls at 140 DEG C, and column bottom temperature controls at 210 ± 3 DEG C.
De-low tower T1 tower top lower boiling material is undertaken reflux by 1:5-8 by reflux ratio controller R1 and takes out.
De-low tower T1 works in the vacuum system of vacuum pump P4, surge tank V2, and whole system vacuum tightness is 190-210Pa.
Preferably, product tower T2 theoretical tray is 40 pieces.
Product tower T2 tower top temperature controls at 190 DEG C, and column bottom temperature controls at 240 ± 3 DEG C.
Product tower T2 product is separated by 1:5-8 by reflux ratio controller R2.
Product tower T2 works in the vacuum system of vacuum pump P7, surge tank V6, and controlling whole system vacuum tightness is 18-22Pa.
The invention has the advantages that: the continuous rectification purifying technique that the invention provides a kind of methyl benzotriazazole, improve quality product, improve production capacity, energy-saving and cost-reducing, steady quality, thus reduce costs, increase economic benefit.
Accompanying drawing explanation
Fig. 1 is methyl benzotriazazole process for refining schema.
In figure, E1 is de-low tower reboiler, and E2 is de-low tower condenser; E3AB is product tower reboiler, and E4 is product tower condenser, and F1 is product tower feed condenses device, R1 is de-low tower reflux ratio control device, and R2 is de-low tower reflux ratio control device, and P2 is de-low tower bottoms recycle pump, P3 is low-boiling-point substance transfering material pump, and P4 is de-low tower vacuum pump, and P5 is product tower bottoms recycle pump, P6 is product transfering material pump, and P7 is product tower vacuum pump, and V1 is low-boiling-point substance storage, V2 is de-low tower vacuum tank, V5AB is high boiling material basin, and V3 is product storage tank, and V6 is product tower vacuum tank.
Embodiment
Below by specific embodiment, the present invention is elaborated.
Crude product is sent into by certain flow in de-low tower T1 by pump P1 at 110 ± 2 DEG C by crude product material, vapour-liquid exchange is carried out by wire packing, theoretical plate number is preferably 35 pieces, low-boiling material front-end volatiles arrive top of tower E2 by exchanging, get off to exchange with ascending gas through being cooled to liquid state, the material that boiling point is high carries out the bottom that tower is got back in heat exchange, returned in tower by falling-film reboiler E1 heating and exchange, repeatedly exchanged by filler in de-low tower, reach a kind of balance, tower top temperature controls at 140 DEG C, column bottom temperature controls at 210 ± 3 DEG C, tower top lower boiling material carries out refluxing and take out in the ratio of 1:6 by reflux ratio controller R1, high boiler material at the bottom of tower is sent into product tower T2 in the middle part of by certain flow part by pump P2 through heating, carry out rectifying separation.Front-end volatiles in tower top enter storage tank V1, reach certain flow and are automatically produced by pump P3, and whole tower T1 works in the vacuum system of vacuum pump P4, surge tank V2, and controlling whole system vacuum tightness is about 200Pa.
Materials at bottom of tower is by after heat exchange, control 210 ± 3 DEG C to control to enter in product tower T2 by certain flow F1, pass through heat exchange, product tower theoretical tray is preferably 40 pieces, tower top temperature controls at 190 DEG C, column bottom temperature controls at 240 ± 3 DEG C, product steam cools through condenser E4, a part to be separated according to the ratio of 1:6 by reflux ratio controller R2 and is entered products pot V3, partial reflux enter in tower with rise gas carry out exchange portions from, the storage tank V4 that the material returning at the bottom of tower enters tower bottom by pump P5 carry out circulation deliver to thin-film evaporator E3A E3B carry out heating and gasifying again, gas phase enters in tower carries out exchange separation by wire packing, high boiler material part sends into high boiling material storage tank V5A/V5B by pump P5, discharging.Product in tower top is separated by reflux ratio controller R2, enters storage tank V3, reaches certain flow and is automatically produced by pump P6.Whole product tower T2 works in the vacuum system of vacuum pump P7, surge tank V6, and controlling whole system vacuum tightness is about 20Pa.
The present invention can summarize with the specific form without prejudice to spirit of the present invention or principal character; above-mentioned embodiment is only in order to illustrate technical scheme of the present invention but not to limit design of the present invention and protection domain; those of ordinary skill of the present invention is modified to technical scheme of the present invention or equivalent replacement; and not departing from aim and the scope of technical scheme, it all should be encompassed in right of the present invention.
Claims (7)
1. the continuous purifying technique of a methyl benzotriazazole, it is characterized in that: the continuous purifying technique of methyl benzotriazazole is as follows: crude product material is pumped into de-low tower T1 by P1, carry out vapour-liquid exchange, low-boiling material front-end volatiles arrive top of tower E2 by exchanging, get off to exchange with ascending gas through being cooled to liquid state, the material that boiling point is high carries out the bottom that tower is got back in heat exchange, returned in tower by falling-film reboiler E1 heating and exchange, repeatedly exchanged by filler in de-low tower, reach a kind of balance, tower top lower boiling material is undertaken refluxing by reflux ratio controller E1 and takes out, high boiler material at the bottom of tower is sent in the middle part of product tower through hot spots by pump P2, carry out rectifying separation, front-end volatiles in tower top enter storage tank, automatically produced by pump P3,
Materials at bottom of tower is by entering in product tower T2 by flow F1 after heat exchange, pass through heat exchange, product steam cools through condenser E4, a part is separated by reflux ratio controller R2 and is entered products pot V3, partial reflux enter in tower with rise gas carry out exchange portions from, the storage tank V4 that the material returning at the bottom of tower enters tower bottom by pump P5 carry out circulation deliver to thin-film evaporator E3A E3B carry out heating and gasifying again, gas phase enters in tower carries out exchange separation, high boiler material part sends into the discharging of high boiling material storage tank by pump P5, product in tower top is separated by reflux ratio controller R2, enter storage tank V3, automatically produced by pump P6,
Described de-low tower T1 tower top temperature controls at 140 DEG C, and column bottom temperature controls at 210 ± 3 DEG C;
Described product tower T2 tower top temperature controls at 190 DEG C, and column bottom temperature controls at 240 ± 3 DEG C.
2. to require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: de-low tower T1 theoretical plate number is 35 pieces.
3. to require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: de-low tower T1 tower top lower boiling material passes through reflux ratio controller R1 and undertaken refluxing by 1: 5-8 and take out.
4. to require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: de-low tower T1 works in the vacuum system of vacuum pump P4, surge tank V2, and whole system vacuum tightness is 190-210Pa.
5. to require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: product tower T2 theoretical tray is 40 pieces.
6. to require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: product tower T2 product is separated by 1: 5-8 by reflux ratio controller R2.
7. will require the continuous purifying technique of a kind of methyl benzotriazazole described in 1 according to right, it is characterized in that: product tower T2 works in the vacuum system of vacuum pump P7, surge tank V6, controlling whole system vacuum tightness is 18-22Pa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310166309.3A CN103450101B (en) | 2013-05-08 | 2013-05-08 | Continuous purification process of methylbenzotriazole |
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| CN201310166309.3A CN103450101B (en) | 2013-05-08 | 2013-05-08 | Continuous purification process of methylbenzotriazole |
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| CN103450101A CN103450101A (en) | 2013-12-18 |
| CN103450101B true CN103450101B (en) | 2015-04-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105233519A (en) * | 2015-11-13 | 2016-01-13 | 如皋市金陵化工有限公司 | Gas-state TTA vacuumizing system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085664C (en) * | 1999-03-24 | 2002-05-29 | 徐道如 | Process for synthesizing methyl benzotriazazole |
| CN102757351A (en) * | 2012-07-18 | 2012-10-31 | 如皋市金陵化工有限公司 | Method for continuously purifying and refining ortho toludiamine |
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- 2013-05-08 CN CN201310166309.3A patent/CN103450101B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085664C (en) * | 1999-03-24 | 2002-05-29 | 徐道如 | Process for synthesizing methyl benzotriazazole |
| CN102757351A (en) * | 2012-07-18 | 2012-10-31 | 如皋市金陵化工有限公司 | Method for continuously purifying and refining ortho toludiamine |
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Effective date of registration: 20160526 Address after: 226500, 2, Xiangjiang Road, Changjiang town (Rugao port area), Nantong, Jiangsu, Rugao Patentee after: NANTONG BOTAO CHEMICAL CO., LTD. Address before: Jiang town Rugao City, Jiangsu province 226500 Nantong City Village Liaison Patentee before: Rugao Jinling Chemical Co., Ltd. |