CN103274913A - Method and device for producing methyl isobutyl ketone - Google Patents
Method and device for producing methyl isobutyl ketone Download PDFInfo
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- CN103274913A CN103274913A CN2013101515797A CN201310151579A CN103274913A CN 103274913 A CN103274913 A CN 103274913A CN 2013101515797 A CN2013101515797 A CN 2013101515797A CN 201310151579 A CN201310151579 A CN 201310151579A CN 103274913 A CN103274913 A CN 103274913A
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Abstract
The invention discloses a method and a device for producing methyl isobutyl ketone. The method comprises the following steps that a, acetone and hydrogen as raw materials are fed into a fixed bed reactor and undergo a reaction in the presence of a catalyst B621; the reaction products are subjected to condensation separation to produce hydrogen; and the condensed solution is fed into a follow-up separation system; b, the product solution is fed into a light component tower and is separated; and the tower bottom residues are fed into an acetone tower and then are separated; c, under the micro-negative pressure as acetone tower pressure, the heavy component at the tower bottom is fed into a dehydrating tower and then is dehydrated; and d, the light component obtained at the top of the dehydrating tower is fed into a waste water tower and then is treated so that an organic light component is obtained; and the product obtained at the bottom of the dehydrating tower is fed into a product tower and then is purified and the product obtained at the top of the product tower is methyl isobutyl ketone. Compared with the traditional one-step method, the method provided by the invention has a high average acetone conversion rate, simple processes and less by-products, realizes maximized recovery of raw materials and utilization of energy, and has low energy consumption and low raw material consumption.
Description
Technical field
The invention belongs to Chemical Manufacture Processes and apparatus technical field, relate generally to production technique and the equipment of methyl iso-butyl ketone (MIBK) MIBK.
Background technology
Methyl iso-butyl ketone (MIBK) (being called for short MIBK), it is a kind of colourless, nontoxic, stable chemical performance, purposes is medium-boiling solvent very widely, main as nitrocotton, polyvinyl chloride, polyvinyl acetate (PVA), polystyrene, Resins, epoxy, the natural and solvent of synthetic rubber, paint, coating and de-oiling, the photoghraphic coupler of colour film are also as the extraction agent of penicillin fermentation liquid and the separating agent of some organic salts.It also is the main raw material of rubber antioxidant 4020 and some organic syntheses simultaneously.Produce MIBK several different methods is arranged, mainly be acetone three-step approach and acetone single stage method, wherein the technical process of acetone three-step approach elongation MIBK is, acetone and NaOH enter reactor continuously, have reacted back device product and phosphoric acid and have worn out, and resolved acetone, remaining is the Pyranton mixture that contains 80%-90%, mix with Tripyrophosphoric acid more at Pyranton liquid, carry out rectifying then, and separate except acetone and purity be the mesityl oxide of 98%-99%; Mesityl oxide is carried out hydrogenation and rectifying simultaneously, with palladium make catalyzer, under certain temperature and pressure, obtain product MIBK, its productive rate reaches 90%.
The shortcoming of three-step approach is because each reaction conditions difference, and catalyst system therefor is also different, per pass conversion low (general about 15%) so whole process flow is oversize, product yield is low and energy consumption is high, and equipment requirements is anticorrosion, and FU volume production ability is low.Therefore less suitable acetone three-steps process at present.What majority was suitable for is the acetone single stage method.
The acetone single stage method was a kind of advanced operational path in 2008.Its principal feature is to utilize finish reaction process such as condensation of acetone, dehydration and hydrogenation high performance one step of catalyzer, obtains purpose product MIBK.Its reaction formula is as follows:
2CH3COCH3 + H2→CH3CH(CH3)CH2COCH3+H2O
This technology three-step approach of comparing, advantage such as it is higher relatively to have a transformation efficiency, and raw material consumption and energy consumption are lower is the present various countries technologies of development mutually unexpectedly.Single stage method has become the main flow synthetic technology of MIBK at present.MIBK device main body technology all is single stage method at present.
As shown in Figure 1, present single stage method MIBK device, main raw material is acetone and hydrogen, adopt and carry the Pd catalyzer, target product is MIBK, and by product is Virahol, unreacted acetone, 2-methylpentane, water, diisobutyl ketone, mesityl oxide, methyl isobutyl alcohol (hydrogenation products of MIBK), heavy constituent (the above acetone polymerisate of 3 molecules) etc.The single stage method building-up reactions is used tubular reactor, 7 tower process are adopted in the rectifying of reactor outlet, process comprises that acetone rectification cell, MIBK refined unit, acetone reclaim and diisobutyl ketone purifying 3 parts, technical process is as follows: reaction product is introduced into acetone dehydrogenation tower, light constituent is discharged from cat head, and main component is 2-methylpentane and acetone, sends into the acetone extract tower, water is cooked extraction agent, and extraction liquid removes acetone recovery tower recovery acetone wherein.The material of discharging at the bottom of the acetone dehydrogenation Tata enters water-and-oil separator.The organic phase of discharging from phase separator is removed the MIBK lightness-removing column, and water removes rectifying acetone and reclaims.The material of discharging at the bottom of the MIBK lightness-removing column tower removes the MIBK rectifying tower; The tower side line is measured MIBK, and content can reach 99.5%, and the quality mark can reach the premium grads standard less than 0.1%.
The diisobutyl ketone that the MIBK rectifier bottoms is discharged is delivered to the diisobutyl ketone tower and is separated by light constituent, at the bottom of the tower in the exportable oil that acts as a fuel of component use.Single stage method MIBK produces and to exist that the low by product of transformation efficiency is many, reactor product separates difficulty, complicated operation, hydrogen consumption are big.
Summary of the invention
Goal of the invention: at problem and the defective of above-mentioned existence, the invention provides production technique and the equipment of the methyl iso-butyl ketone (MIBK) that a kind of flow process is simple, transformation efficiency is high, by product is few, energy consumption is low.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of methyl iso-butyl ketone (MIBK) production technique, may further comprise the steps: a, raw material acetone and hydrogen are sent into fixed-bed reactor react, temperature of reaction is 120～180 ℃, reaction pressure is 5.0～8.0MPa, adopts the B621 catalyzer; The reaction product that obtains after the reaction obtains hydrogen through condensation separation earlier, and sends hydrogen recycle back to fixed-bed reactor; The solution that condensation obtains enters subsequent separation system; B, described product solution are sent into lights column and are separated, and it is 0.2～0.3MPa that tower is pressed, and cat head obtains by product 2-methylpentane, and still liquid then enters the acetone tower and separates at the bottom of the tower; C, acetone Tata be voltage-controlled be made as little negative pressure-5～-30KPa, the acetone column overhead obtains light constituent acetone, the heavy constituent that obtain at the bottom of the tower are sent into dehydration tower and are dewatered; The light constituent that d, dehydration column overhead obtain is sent to the waste water tower and handles, and obtains organic light constituent; The product that obtains at the bottom of the dehydration Tata is sent into the product tower and is purified, and product column overhead temperature is 110～130 ℃, and the product column overhead obtains the product methyl iso-butyl ketone (MIBK).
As preferably, described waste water column overhead temperature is 75～90 ℃.
As preferably, separate the light constituent acetone recycle utilization that obtains from the acetone column overhead among the step c and send fixed-bed reactor back to.
As preferably, tower top temperature is 52～58 ℃ in the described dehydration tower, and column bottom temperature is 65～80 ℃.
As preferably, the tower bottoms temperature is 165～200 ℃ in the described product tower.
Another purpose of the present invention has provided the methyl iso-butyl ketone (MIBK) production process equipment of above-mentioned correspondence, comprise fixed-bed reactor, lights column, acetone tower, dehydration tower, waste water tower and product tower, wherein liquid outlet is connected with dehydration tower with lights column, acetone tower successively at the bottom of the fixed-bed reactor still; Dehydration column overhead is connected with the waste water tower by pipeline, is connected with the product tower by pipeline at the bottom of the dehydration Tata; Liquid outlet is provided with condenser and hydrogen recovery branch road at the bottom of the described fixed-bed reactor still simultaneously, and this hydrogen recovery branch road the other end is communicated with the fixed-bed reactor dog-house.
As preferably, described hydrogen recovery branch road is provided with condenser and hydrogen gas compressor.
Beneficial effect: compared with prior art, the present invention has the following advantages: the traditional relatively single stage method of the present invention, and the average conversion height of acetone, and flow process is simple, by product is few, maximized recycling raw material and energy consumption, thus lower energy consumption and raw material consumption had.
Description of drawings
Fig. 1 is the prior art constructions synoptic diagram;
Fig. 2 is the structural representation of methyl iso-butyl ketone (MIBK) production process equipment of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention, should understand these embodiment only is used for explanation the present invention and is not used in and limits the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
As shown in Figure 1, the one-step method production process of a kind of methyl iso-butyl ketone (MIBK) MIBK, raw material acetone and hydrogen are preheating to 120 ℃, enter the fixed-bed reactor that the B621 catalyzer is housed, 120 ~ 180 ℃ of control temperature of reaction, reaction pressure control 5.0 ~ 8.0MPa, reacted solution enters the water cooler condensation, the uncooled hydrogen that gets off passes through the hydrogen recovery branch road and boosts to 9.0 ~ 10.0MPa by hydrogen gas compressor entering the fixed-bed reactor recycle by decompression; The liquid that condensation is got off enters subsequent separation system, and separates.
Condensed reaction solution enters the lights column initial gross separation and goes out light constituent, and the tower pressure-controlled is at 0.2 ~ 0.3MPa, and the cat head light constituent obtains byproduct of reaction 2-methylpentane, and still liquid enters the acetone tower at the bottom of the tower.Acetone Tata pressure-controlled little negative pressure-5～-30KPa, the cat head light constituent obtains 99% acetone, and enters the fixed-bed reactor recycle; Heavy constituent enter dehydration tower at the bottom of the tower, 52 ~ 58 ℃ of dehydration tower head temperature, 65 ~ 80 ℃ of column bottom temperatures, dehydration tower control atmospheric operation.Dehydration column overhead obtains light constituent waste water, and sends into the waste water tower and distill, 75 ~ 90 ℃ of tower top temperature controls, and still liquid enters the product tower at the bottom of the tower.
Product tower atmospheric operation, cat head obtains the methyl iso-butyl ketone (MIBK) of 99% concentration, 110 ~ 130 ℃ of control tower top temperatures, tower bottoms obtains heavy constituent, and the tower bottoms temperature is 165 ~ 200 ℃, and tower bottoms can be used as solvent and takes out or send to burning
Because this technology MIBK adopts novel B 621 catalyzer, this catalyst selectivity height, the average conversion of acetone is 30.86%.The average selectivity of MIBK is 94.92%.And this catalyzer has good heat resistance, and the temperature use range is wide, but the long-term operation of implement device; The new separation process scheme that adopts.Reacted MIBK only contains a spot of dimethylpentane, unnecessary unreacted acetone, a spot of organic light constituent and heavy constituent, compare 7 tower separating technologies with former one-step method production process MIBK, this technology only needs 5 towers can obtain product, flow process is simple, therefore it is low to separate power consumption, and the consumption of raw and auxiliary materials of MIBK must reduce.And this device acetone recycle utilizes, and dimethylpentane is sent outside as by product, separates a small amount of light constituent of obtaining and middle component or sends outside as byproduct, or send to boiler combustion.As the hydrogen of one of reaction product, the hydrogen of complete reaction does not recycle through the hydrogen pressure machine, the effective rate of utilization height of hydrogen, and the hydrogen unit consumption is low.
| Three-step approach | The Veba single stage method | The present invention | |
| Acetone (t) | 1.42 | 1.33~1.35 | 1.318 |
| Hydrogen (Nm3) | 674 | 502~590 | 447 |
| Water coolant (t) | 579 | 100 | 60 |
| Process water (t) | 0.417 | -- | -- |
| Power consumption (Kwh) | 309 | 450~550 | 340 |
| Steam (t) | 12.13 | 2.36~4.9 | 4.1 |
Table 1 starting material and power consumption contrast (in MIBK per ton)
The synopsis 1 of the consumption data that last table is tried out through actual production for this technology and three-step approach, single stage method.
Claims (7)
1. methyl iso-butyl ketone (MIBK) production technique is characterized in that may further comprise the steps:
A, raw material acetone and hydrogen are sent into fixed-bed reactor react, temperature of reaction is 120～180 ℃, and reaction pressure is 5.0～8.0MPa, adopts the B621 catalyzer; The reaction product that obtains after the reaction obtains hydrogen through condensation separation earlier, and sends hydrogen recycle back to fixed-bed reactor; The solution that condensation obtains enters subsequent separation system;
B, described product solution are sent into lights column and are separated, and it is 0.2～0.3MPa that tower is pressed, and cat head obtains by product 2-methylpentane, and still liquid then enters the acetone tower and separates at the bottom of the tower;
C, acetone Tata be voltage-controlled be made as little negative pressure-5～-30KPa, the acetone column overhead obtains light constituent acetone, the heavy constituent that obtain at the bottom of the tower are sent into dehydration tower and are dewatered;
The light constituent that d, dehydration column overhead obtain is sent to the waste water tower and handles, and obtains organic light constituent; The product that obtains at the bottom of the dehydration Tata is sent into the product tower and is purified, and product column overhead temperature is 110～130 ℃, and the product column overhead obtains the product methyl iso-butyl ketone (MIBK).
2. according to the described methyl iso-butyl ketone (MIBK) production technique of claim 1, it is characterized in that: described waste water column overhead temperature is 75～90 ℃.
3. according to the described methyl iso-butyl ketone (MIBK) production technique of claim 1, it is characterized in that: separate the light constituent acetone recycle utilization that obtains from the acetone column overhead among the step c and send fixed-bed reactor back to.
4. according to the described methyl iso-butyl ketone (MIBK) production technique of claim 1, it is characterized in that: tower top temperature is 52～58 ℃ in the described dehydration tower, and column bottom temperature is 65～80 ℃.
5. according to the described methyl iso-butyl ketone (MIBK) production technique of claim 1, it is characterized in that: the tower bottoms temperature is 165～200 ℃ in the described product tower.
6. described methyl iso-butyl ketone (MIBK) production process equipment of claim 1, it is characterized in that: comprise fixed-bed reactor, lights column, acetone tower, dehydration tower, waste water tower and product tower, wherein liquid outlet is connected with dehydration tower with lights column, acetone tower successively at the bottom of the fixed-bed reactor still; Dehydration column overhead is connected with the waste water tower by pipeline, is connected with the product tower by pipeline at the bottom of the dehydration Tata; Liquid outlet is provided with condenser and hydrogen recovery branch road at the bottom of the described fixed-bed reactor still simultaneously, and this hydrogen recovery branch road the other end is communicated with the fixed-bed reactor dog-house.
7. according to the described methyl iso-butyl ketone (MIBK) production process equipment of claim 6, it is characterized in that: described hydrogen recovery branch road is provided with condenser and hydrogen gas compressor.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130778A (en) * | 2015-08-31 | 2015-12-09 | 宁波镇洋化工发展有限公司 | Production process of methyl isobutyl ketone |
| CN107400046A (en) * | 2017-07-03 | 2017-11-28 | 湖北三里枫香科技有限公司 | Acetone liquid phase one-step method prepares the process of methyl iso-butyl ketone (MIBK) |
| CN110054555A (en) * | 2019-03-14 | 2019-07-26 | 镇江李长荣高性能材料有限公司 | A kind of purification isobutyrone Product Process and its equipment |
| CN110922317A (en) * | 2019-12-06 | 2020-03-27 | 万华化学集团股份有限公司 | Method for producing methyl isobutyl ketone by reactive distillation |
| CN112745206A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Combined process and device for producing MIBK and MIBC |
| CN115433063A (en) * | 2022-07-28 | 2022-12-06 | 南通江山农药化工股份有限公司 | Production method of metolachlor production raw material methoxy acetone |
| CN116253631A (en) * | 2023-02-15 | 2023-06-13 | 宁波宁咨绿色发展有限公司 | Rectification process for synthesizing methyl isobutyl ketone by energy-saving acetone one-step method |
| WO2023130930A1 (en) | 2022-01-04 | 2023-07-13 | 圣奥化学科技有限公司 | Method for preparing methyl isobutyl ketone |
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| CN1331070A (en) * | 2000-06-28 | 2002-01-16 | 中国石油化工集团公司 | Process for separating methylisobutanone synthesized from acetone |
| CN101376623A (en) * | 2007-08-31 | 2009-03-04 | 中国石油天然气股份有限公司 | Separation method of methyl isobutyl ketone synthetic liquid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1331070A (en) * | 2000-06-28 | 2002-01-16 | 中国石油化工集团公司 | Process for separating methylisobutanone synthesized from acetone |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130778A (en) * | 2015-08-31 | 2015-12-09 | 宁波镇洋化工发展有限公司 | Production process of methyl isobutyl ketone |
| CN107400046A (en) * | 2017-07-03 | 2017-11-28 | 湖北三里枫香科技有限公司 | Acetone liquid phase one-step method prepares the process of methyl iso-butyl ketone (MIBK) |
| CN107400046B (en) * | 2017-07-03 | 2023-03-31 | 湖北三里枫香科技有限公司 | Process method for preparing methyl isobutyl ketone by acetone liquid phase one-step method |
| CN110054555A (en) * | 2019-03-14 | 2019-07-26 | 镇江李长荣高性能材料有限公司 | A kind of purification isobutyrone Product Process and its equipment |
| CN112745206A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Combined process and device for producing MIBK and MIBC |
| CN110922317A (en) * | 2019-12-06 | 2020-03-27 | 万华化学集团股份有限公司 | Method for producing methyl isobutyl ketone by reactive distillation |
| CN110922317B (en) * | 2019-12-06 | 2022-11-08 | 万华化学集团股份有限公司 | Method for producing methyl isobutyl ketone by reactive distillation |
| WO2023130930A1 (en) | 2022-01-04 | 2023-07-13 | 圣奥化学科技有限公司 | Method for preparing methyl isobutyl ketone |
| CN115433063A (en) * | 2022-07-28 | 2022-12-06 | 南通江山农药化工股份有限公司 | Production method of metolachlor production raw material methoxy acetone |
| CN115433063B (en) * | 2022-07-28 | 2023-10-17 | 南通江山农药化工股份有限公司 | Production method of metolachlor production raw material methoxy acetone |
| CN116253631A (en) * | 2023-02-15 | 2023-06-13 | 宁波宁咨绿色发展有限公司 | Rectification process for synthesizing methyl isobutyl ketone by energy-saving acetone one-step method |
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Application publication date: 20130904 |