CN1331070A - Process for separating methylisobutanone synthesized from acetone - Google Patents
Process for separating methylisobutanone synthesized from acetone Download PDFInfo
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Abstract
A separation process for synthesizing methylisobutanone from acetone features that the 2-methylphentane tower, acetone recovering tower phase separators, dewatering tower for removing H2O and DAA, and MIBK product tower are used. Its advantages include high purity of product (not containing acetone in it) and saving energy.
Description
The invention relates to a separation method for synthesizing methyl isobutyl ketone (MIBK) from Acetone (AC), which has the characteristics of low consumption, high product quality and the like.
MIBK is a colorless, transparent liquid and excellent industrial solvent, and has wide industrial application, such as nitrocellulose and tetracycline solvents; also used for high-efficiency separation reagents of inorganic salts and the like.
The traditional method for producing MIBK is the acetone three-step process. Namely a first step: generating one molecule of diacetone alcohol (DAA) by two molecules of acetone under the action of an alkaline catalyst; the second step is that: dehydrating a molecule of DAA under the action of an acid catalyst to generate Mesityl Oxide (MO); the third step: MO is reacted with a selective hydrogenation catalyst to produce MIBK. The specific reaction formula is as follows: the first step is as follows: (1) the second step is that: (2) the third step: (3)
the technology for synthesizing MIBK by using an acetone one-step method is industrialized in 1968, and at the end of sixties, German Texaco company develops a novel catalyst which has the double functions of dehydration and hydrogenation, so that the three-step reaction is completed in one step, and firstly, two molecules of acetone are condensed and dehydrated on an acid center of the catalyst to generate MO; the MO is then rapidly hydrogenated at the hydrogenation center of the catalyst to produce MIBK. The course of the reaction can be represented by the following formula:
2CH3COCH3→(CH3)2C＝CHCOCH3＋H2O
↓H2
(CH3)2CHCH2COCH3
documents 1 (Jinling petrochemical, 1987 (5): 25) and 2 (Jinling petrochemical 1997, 3: 14) introduce the production process of Xide Hibernia and the production process of Japan Deshan Cao, the separation processes in the two production processes are basically the same and both adopt three-tower processes, namely, the first tower is an acetone recovery tower, and the acetone which is excessive in reaction is recovered and recycled; the second tower is a dehydrating tower, water generated by reaction is azeotropic with MIBK, and water is removed in an azeotrope form; the third tower is a product tower, products are produced at the top of the tower, and heavy components are produced at the bottom of the tower.
Two major problems were found when organizing production according to the above separation scheme: 1. the 2-methylpentane (2-MPA) column is absent. Under normal reaction conditions, 2-MPA with the content of less than 1.0w percent is contained in the reaction liquid, the separation is carried out according to a three-tower flow disclosed by the literature, a 2-MPA tower is not provided, and the 2-MPA cannot be separated from the system and can only be entrained in acetone to circulate and accumulate in the system. In the initial stage of production, when the 2-MPA in the circulating material is less than 1.0 w%, the production structure is not affected by shutdown, along with the lengthening of continuous production time, when the 2-MPA in the circulating material is more than 1.0 w%, the 2-MPA and acetone form azeotrope, and the azeotrope is evaporated from the top of the tower, and the temperature of the top of the tower is no longer 56 ℃ of the original acetone boiling point, but 47 ℃ of the two azeotropic temperatures, so that the original design operation conditions and purposes of the tower are completely changed, a large amount of acetone is left in the tower kettle, and finally the separation system is shut down. 2. The product (MIBK) has low purity (about 98.5-99.3 w%) and limited application range. The product contains about 1.0% of DAA, and has a boiling point of 168 deg.C, but is characterized by easy decomposition at 95 deg.C. The operation condition of the dehydration tower designed according to the conventional method is that the top of the tower is 88 ℃, namely the azeotropic temperature of water and MIBK, the bottom of the tower is 120 ℃, so that DAA in the reaction liquid is only partially decomposed into acetone which is evaporated from the top of the dehydration tower, and a part of the undecomposed DAA is brought into the MIBK product tower and is decomposed into acetone in the MIBK product tower, and the MIBK is evaporated from the top of the dehydration tower, so that the purity of the MIBK product fluctuates between 98.5 and 99.3w percent, and the purity is difficult to reach more than 99.5w percent. The product purity is limited, and the application range of the product is greatly influenced.
Document 2 (Jinling petrochemical 1997, 3: 14) describes a process for the one-step synthesis of MIBK from acetone, which is separated into a four-column process, with the addition of a 2-MPA column, which better solves the first of the above problems, but the second remains.
The invention aims to provide a novel product separation method aiming at the problem that the product carries acetone and the quality is influenced, so as to improve the purity of the product and expand the application range of the product.
The technical scheme of the invention is as follows:
reacting raw material acetone in the presence of hydrogen-containing gas and a catalyst, separating the hydrogen-containing gas from reactants through a gas-liquid separator, cooling the reactants through a condenser, feeding the reactants into a 2-methylpentane tower, evaporating 2-methylpentane and acetone from the tower top in an azeotrope form (the azeotrope under normal pressure comprises 56 w% of 2-methylpentane and 44 w% of acetone), feeding kettle liquid into an acetone recovery tower, evaporating excessive acetone from the top of the acetone recovery tower, feeding the kettle liquid into a first phase separator, separating a water phase and an oil phase, and feeding the oil phase into a dehydration tower. In the dehydration tower, water and methyl isobutyl ketone are distilled from the top of the tower in an azeotrope form (the azeotrope composition of the water is 75 w% of methyl isobutyl ketone and 25 w% of water under normal pressure), then the water and the methyl isobutyl ketone enter a second phase separator, after phase separation, a water phase is separated from the bottom of the second phase separator, an oil phase is used as reflux of the dehydration tower, a water phase is discharged from a device, the kettle liquid of the dehydration tower enters a methyl isobutyl ketone tower, the methyl isobutyl ketone is distilled from the top of the tower, and the recombined components are remained in the kettle liquid; wherein the top of the dehydrating tower also has the function of removing one molecule of diacetone alcohol, one molecule of diacetone alcohol is decomposed into acetone (accounting for less than 1.0w percent of the totaloverhead distillate) in the dehydrating tower, and the acetone and the azeotrope of the methyl isobutyl ketone (the azeotrope under normal pressure of the water and the methyl isobutyl ketone has the composition of 75w percent of the methyl isobutyl ketone and 25w percent of the water) are evaporated out from the top of the dehydrating tower.
The heavy component is a mixture of diisobutyl ketone (DIBK) and mesitylene (TMB).
The dehydration tower is generally designed conventionally, namely an external-hanging tubular reboiler is adopted for heating the tower kettle. In this column, water azeotropes with MIBK and evaporates from the top of the column, a small amount of water being removed from the feed in this way. Thus the tower is madeBy single use, only removing H2O, no effect of eliminating DAA.
In order to achieve the dual functions of dehydration and DAA dehydration of the dehydration tower of the invention, the following method can be adopted according to the characteristics that about 1 percent of DAA is contained in the material and the acetone is easily decomposed at the temperature of 95 ℃ under normal pressure:
the tower kettle shape and the heating mode of the tower are changed. (1) The original vertical kettle is changed into a horizontal kettle, the volume of the kettle is increased, the retention time of materials in the kettle is increased, the DAA has sufficient time to be decomposed into acetone, the retention time of the materials in the kettle is 1.0-2.5 h, the top temperature is 87-88 ℃, and the kettle temperature is 124-126 ℃; (2) the original external hanging type tube array reboiler is changed into the steam heating of the coil pipe arranged in the kettle, so that the purpose is to increase the heat transfer effect and facilitate the DAA decomposition to generate acetone. Thus, the small amount of acetone produced by DAA decomposition is also accompanied by H2O-MIBK azeotropyThe substances are evaporated from the top of the tower and enter a phase separator, after phase separation, oil phase reflows, water phase can be sent to a wastewater treatment plant for treatment, and the materials in the tower bottom are sent to a MIBK product tower.
Of course, according to the characteristics of the dehydration tower of the present invention, other methods can be adopted to achieve the dual functions of dehydration and DAA removal of the dehydration tower of the present invention.
The acetone which is excessive in reaction is evaporated from the top of the acetone recovery tower and then can be sent back to the reaction system; the acetone recovery tower bottom liquid is sent to a phase separator, and after phase separation, the water phase can be sent to a wastewater treatment plant for recovering MIBK; the oil phase is sent to a dehydration column. In the dehydration tower, water and MIBK are subjected to azeotropic distillation, and the quantity of the azeotrope is small; simultaneously, DAA is decomposed into acetone in the tower, and is evaporated out from the tower top together with the azeotrope, and enters a phase separator, and after phase separation, an oil phase (generally, mainly MIBK and acetone accounting for less than 1.0 w% of the whole tower top evaporated product) is taken as reflux of the tower; the aqueous phase (generally containing MIBK<1.0 w%) can be sent to a wastewater treatment plant for recycling MIBK.
The invention has the advantages that:
1. the product quality is improved. The purity of the MIBK is improved to over 99.5 percent from the original 98.5 to 99.3 percent.
2. The separation process belongs to a low-consumption and economical system. Removing the impurities in the prior artSingle function of water tower is changed into removing H2The O/DAA removing double-function tower avoids the problem of rebuilding a tower for removing DAA, does not increase investment and operation energy consumption basically while improving the product quality, and belongs to an energy-saving separation process.
FIG. 1 is a schematic flow diagram of the separation process of the present invention.
The technical solution of the present invention is further described below with reference to the accompanying drawings and specific embodiments:
1. examples the case of the starting materials used:
table 1 is the composition of the feed from the reaction system to the separation system.
TABLE 1 raw material composition
| Name (R) | Composition, w% |
| H2O | 5.76 |
| 2-MPA | 0.32 |
| AC | 63.05 |
| MIBK | 29.00 |
| DAA | 0.28 |
| DIBK | 1.10 |
| TMB | 0.50 |
2. The flow conditions are as follows:
the material from the reaction system is firstly sent to a 2-MPA tower to carry out azeotropic distillation on 1, 2-MPA and AC, and the 2-MPA is evaporated from the tower top in an azeotrope form; the residue is sent to an acetone recovery tower 2. The acetone which is excessive in reaction is evaporated from the top of the acetone recovery tower 2 and is sent back to the reaction system; the residue in the acetone recovery tower 2 is sent to a phase separator 3, and after phase separation, the water phase (containing MIBK<1.0 w%) is sent to a wastewater treatment plant for recovering MIBK; the oil phase is sent to the dehydration column 4. In this column, water azeotropes with MIBK (the azeotrope amounts are small); meanwhile, DAA is decomposed into acetone in the tower, and is evaporated out from the top of the tower together withthe azeotrope, and enters a phase separator 5, and after phase separation, the oil phase is taken as the reflux of the tower; the water phase (containing MIBK less than 1.0 w%) is sent to a wastewater treatment plant for recycling MIBK. The bottoms from column 4 are fed to a MIBK product column 6 where MIBK is distilled from the top of the column and the heavies are retained in the bottoms.
3. The operating conditions of each column were:
the detailed operating conditions of the columns of the separation system are shown in Table 2.
TABLE 2 operating conditions of the columns of the separation System
| 2-methyl pentane tower | Acetone recovery tower | Removing H2O tower | MIBK product tower | |
| Operating pressure | Atmospheric pressure | Atmospheric pressure | Atmospheric pressure | Atmospheric pressure |
| The temperature at the top of the column,. degree.C | 47 | 56 | 88 | 117 |
| Column bottom temperature,. degree.C | 60 | 90 | 125 | 180 |
| Reflux ratio, V | 110 | 2.0 | 4.0 | 4.0 |
4. The result of the separation:
4.12-methylpentane column
The column functions to remove 2-MPA. The feed composition is shown in table 1.
The 2-MPA and acetone are azeotroped, the azeotropic point is 47 ℃, the 2-MPA is distilled from the top of the tower in the form of azeotrope, the composition of the azeotrope is 56-MPA 56W percent and the acetone content is 44W percent (normal pressure). The kettle liquid for removing the 2-MPA tower comprises the following components: h2O 5.79w％，AC 63.46w％，MIBK 29.15w％，DIBK 1.10w％，TMB 0.50w％，DAA 0.26w％。
Although the content of acetone in the azeotrope is high, the yield of the azeotrope is very small, and for example, a set of 1000t/aMIBK production device only produces 2-3 Kg of azeotrope in one hour. The azeotrope has two uses, one is used as solvent for common paint and the other is used as fuel for burning, and the molecule of the azeotrope consists of carbon, oxygen and hydrogen, so that the burning process produces no pollution to air.
4.2 acetone recovery tower
The tower is used for recovering and recycling the unreacted acetone. The bottoms composition of the 2-MPA column is the composition of the column feed.
The material from which the 2-MPA was removed was sent to an acetone recovery column where acetone was distilled off from the top of the column with a purity>99.5 w%; the bottom liquid contains no acetone as much as possible, AC is less than 1.0 w% so as to prevent the influence on the subsequent separation of MIBK, and simultaneously, water generated in the reaction is remained in the tower bottom as much as possible. The kettle liquid is sent to a phase separator 3, and after phase separation, the water phase is sent to a wastewater treatment plant, wherein the water phase only accounts for 10-15 w% of the oil phase; the oil phase is sent to dehydrationIn column 4, the oil phase composition is: h20.93 w% of O, 0.97 w% of acetone, 0. 92.17 w% of MIBK, 0.84w% of DAA0 and 5.09 w% of heavy component.
4.3 removal of H2O tower
The column functions to strip H from the feed2O and DAA. The composition of the oil phase taken out of the phase separator 3 is the composition of the column feed.
In the tower, water and MIBK are subjected to azeotropic distillation, the quantity of the azeotrope is small, the azeotrope only accounts for 5.0 w% of the feeding material, and the composition is as follows: MIBK is less than 5%, and the balance is H2O; while DAA is decomposed in the column to acetone, evaporated with entrainer from the top of the column, cooled and passed to phase separator 5 where the oil phase (MIBK53 w%, AC40 w%, H) is phase separated2O7.0 w%, atmospheric) as reflux to the column; aqueous phase (containing MIBK1.0 w%, H)2O98 w%, the remainder being AC) to a wastewater treatment plant for MIBK recovery. The tower bottoms are sent to a product tower, which comprises the following components: h2O0.11w%, AC0.01w%, MIBK 94.53w%, heavy component 5.35 w%.
4. MIBK product tower
By removing H2The material treated by the O tower enters a MIBK product tower 6 for normal rectification, the problem that the product is influenced by the evaporation of acetone from the tower top is avoided in the rectification process, the product with the purity of over 99.5 percent can be obtained from the tower top only by leaving heavy components in the tower, and the product is obtained at the tower bottomThe heavies were<1.0 w% MIBK, the balance being a mixture of DIBK and TMB. The heavy components at the tower bottom have two purposes, and one can be used as an ink solvent; and the second can be used as boiler fuel. Table 1 shows the operating conditions and the operating results of the dehydration/DAA removal column and the product column before and after the reforming.
TABLE 3 DeH before andafter reforming2Operating conditions and operating results of O/DAA stripping column and product column
| Original process operation strip Piece | Operating pressure, MPa | Atmospheric pressure | |||||
| The temperature at the top of the column,. degree.C | 88 | ||||||
| Column bottom temperature,. degree.C | 120 | ||||||
| The invention is a process operation Conditions for working | Operating pressure, MPa | Atmospheric pressure | |||||
| The temperature at the top of the column,. degree.C | 88 | ||||||
| Column bottom temperature,. degree.C | 125 | ||||||
| H2O | Acetone (II) | MIBK | DAA | Heavy component | |||
| Original separation process | Feed to the dehydration column, w% | 0.93 | 0.97 | 92.17 | 0.84 | 5.09 | |
| Kettle outlet of dehydration tower Material content w% | 0.11 | 0.01 | 93.75 | 0.78 | 5.35 | ||
| MIBK Product(s) Tower top Discharging | Production of One month | 0.13 | 0.39 | 99.30 | 0.18 | ||
| Production of After a month | 0.11 | 1.17 | 98.52 | 0.20 | |||
| Flow of the invention | Feed to the dehydration column, w% | 1.46 | 0.12 | 92.27 | 0.96 | 5.19 | |
| Discharging the materials from the dehydration tower kettle, w％ (product tower feed) | 0.11 | 0.01 | 94.53 | 5.35 | |||
| MIBK product overhead Discharging by weight percent (the whole production week Phase) | 0.12 | 0.003 | 99.64 | 0.24 | |||
As can be seen from the data in Table 3, DAA is subjected to H removal after the original dehydration tower is modified by applying the technical scheme of the invention2The decomposition in the O/DAA removing tower is very clean, the problem that the product of the MIBK product tower is influenced by acetone is solved, and no addition is madeThe product purity is improved under the condition of the new tower, which shows that the separation process has the characteristics of energy consumption saving, product quality improvement and the like. Meanwhile, the product quality in the whole production period is more than 99.5%, the device is convenient to operate, the product application range is enlarged, and the device has market competitiveness.
Claims (4)
1. A separation method for synthesizing methyl isobutyl ketone from acetone comprises the steps of reacting raw material acetone in the presence of hydrogen-containing gas and catalyst, separating hydrogen-containing reactant by a gas-liquid separator, cooling by a condenser,feeding the reactant into a 2-methyl pentane tower (1), distilling 2-methyl pentane and acetone from the tower top in an azeotrope form, feeding the tower bottom kettle liquid into an acetone recovery tower (2), distilling excessive acetone from the tower top of the acetone recovery tower (2), feeding the tower bottom kettle liquid into a phase separator (3), separating a water phase and an oil phase, separating the water phase from the bottom of the phase separator (3), feeding the oil phase into a dehydration tower (4), distilling water and methyl isobutyl ketone from the tower top in an azeotrope form, feeding the water and the methyl isobutyl ketone into a phase separator (5), refluxing the oil phase as the tower (4) after phase separation, discharging the water phase from a device, feeding the tower (4) kettle liquid into a methyl isobutyl ketone tower (6), methyl isobutyl ketone is evaporated from the tower top, and the heavy components are remained in the kettle liquid; it is characterized in that the top of the dehydrating tower (4) also has the function of removing one molecule of diacetone alcohol, one molecule of diacetone alcohol is decomposed into acetone in the tower (4), and the acetone and the azeotrope of water and methyl isobutyl ketone are evaporated from the top of the tower.
2. A separation process for the synthesis of methyl isobutyl ketone from acetone according to claim 1, characterized in that the bottom of the dehydration column (4) is horizontal.
3. A separation process for the synthesis of methyl isobutyl ketone from acetone according to claim 1, characterized in that the operating conditions of the dehydration column (4) are: the retention time in the material kettle is 0.8-3.0 h, the operation pressure is normal pressure, the operation temperature is 87-88 ℃ at the top of the tower, and the tower kettle is 124-126 ℃.
4. A separation process for the synthesis of methyl isobutyl ketone from acetone according to claim 1, characterized in that the heating mode in the dehydration column (4) is steam coil heating in the bottom of the column.
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| WO2007069109A3 (en) * | 2005-12-14 | 2007-10-11 | Sasol Tech Pty Ltd | Method and apparatus for producing purified methyl isobutyl ketone |
| WO2007069110A3 (en) * | 2005-12-14 | 2007-10-11 | Sasol Tech Pty Ltd | Method and apparatus for producing purified methyl isobutyl ketone |
| CN100413837C (en) * | 2005-10-19 | 2008-08-27 | 中国石油化工股份有限公司 | Process for separating methylisobutanone synthesized from acetone |
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| CN107915615A (en) * | 2016-10-08 | 2018-04-17 | 万华化学集团股份有限公司 | The method that the MIBK of purification is prepared by industrial by-product waste liquid acetone |
| CN107915612A (en) * | 2016-10-08 | 2018-04-17 | 万华化学集团股份有限公司 | A kind of method for the MIBK that purification is prepared by industrial by-product waste liquid acetone |
| CN107915615B (en) * | 2016-10-08 | 2020-09-08 | 万华化学集团股份有限公司 | Method for preparing purified MIBK from industrial byproduct waste liquid acetone |
| CN109134227A (en) * | 2018-09-28 | 2019-01-04 | 万华化学集团股份有限公司 | A method of purification methyl iso-butyl ketone (MIBK) product |
| CN109134227B (en) * | 2018-09-28 | 2021-07-23 | 万华化学集团股份有限公司 | Method for refining methyl isobutyl ketone product |
| 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 |
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