CN112661731B - Device and method for decoloring and purifying maleic anhydride refined heavy components - Google Patents
Device and method for decoloring and purifying maleic anhydride refined heavy components Download PDFInfo
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- CN112661731B CN112661731B CN201910978696.8A CN201910978696A CN112661731B CN 112661731 B CN112661731 B CN 112661731B CN 201910978696 A CN201910978696 A CN 201910978696A CN 112661731 B CN112661731 B CN 112661731B
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Abstract
The invention relates to a device and a method for decoloring and purifying maleic anhydride refined heavy components, and belongs to the field of chemical industry. Firstly, extracting and decoloring refined heavy components of maleic anhydride, wherein an extraction raffinate is a chromogenic impurity phase, filter residues are chromogenic impurities after the extraction raffinate is filtered, filtrate and an extraction phase enter two-stage rectification, deep impurity removal is carried out in the first-stage rectification, an extractant is recovered in the second-stage rectification, and a maleic anhydride product is extracted. The method has the characteristics of high maleic anhydride recovery rate of over 90 percent, good quality of the recovered maleic anhydride product, mild operation conditions, recyclable extracting agent, low energy consumption and the like, has remarkable economic benefit, and has certain industrial application potential.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a device and a method for decoloring and purifying maleic anhydride refined heavy components.
Background
Maleic anhydride is an important organic chemical raw material and has wide application in the fields of synthetic resin industry, coating industry, pharmaceutical industry and the like. At present, the quality stability of a finished maleic anhydride product is poor due to the fact that the maleic anhydride product contains trace water, polymaleic anhydride and other impurities, so that the maleic anhydride product produced by the device needs to be rectified, heavy components produced in the rectifying process are high in purity, but brownish red in color and cannot be applied as the product, most of the industry adopts a batch distillation mode to recover the heavy components of the maleic anhydride, and the recovery rate is generally lower than 40%. Patent CN102702148A discloses a method for recovering maleic anhydride in maleic anhydride distillation still residue, which adopts intermittent and continuous distillation modes, and has certain economic benefit, but the recovery rate is lower and the energy consumption is higher; patent CN102836562A discloses a recycling system of kettle residue in maleic anhydride production, which adopts a mode of multiple rectification and distillation, and can recycle heavy components of maleic anhydride, but the process is long and the recycling rate needs to be further researched.
Disclosure of Invention
The invention provides a device and a method for decoloring maleic anhydride heavy components, and the method has the advantages of cyclic utilization of an extracting agent, mild treatment conditions, low energy consumption and remarkable economic benefit.
The purpose of the invention can be realized by the following technical scheme:
a method for decoloring and purifying heavy components refined from maleic anhydride comprises the steps of conveying a maleic anhydride raw material into an extraction kettle for extraction, obtaining a chromogenic impurity phase at the lower layer after extraction is finished, and filtering the chromogenic impurity phase to obtain a filtrate and chromogenic impurities respectively; and (3) conveying the filtrate obtained after the lower layer filtration and the upper extraction phase to a primary rectifying tower for rectification, conveying the product on the tower top after the first rectification to a secondary rectifying device for secondary rectification, recovering an extractant from the tower top after the secondary rectification, and obtaining a maleic anhydride product at the tower bottom.
The technical scheme of the invention is as follows: in the extraction process, the mass ratio of the extracting agent to the maleic anhydride raw material is 10: 1-1: 5, stirring for 10-60 min, and standing for 30-240 min after stirring is finished.
The technical scheme of the invention is as follows: in the extraction process, the mass ratio of the extracting agent to the maleic anhydride raw material is 1: 1-5, wherein the extracting agent is one or two of toluene, xylene, m-xylene, o-xylene and p-xylene.
The technical scheme of the invention is as follows: the operating pressure of the primary rectifying tower is 10-50 Kpa, and the operating temperature of the bottom of the primary rectifying tower is 110-200 ℃.
In some preferred embodiments: the operating pressure of the primary rectifying tower is 10-30 Kpa, and the operating temperature of the bottom of the primary rectifying tower is 130-150 ℃.
The technical scheme of the invention is as follows: the operating pressure of the secondary rectifying tower is 10-50 Kpa, and the operating temperature of the tower bottom of the secondary rectifying tower is 45-95 ℃.
In some preferred embodiments: the operation pressure of the secondary rectifying tower is 10-30 Kpa negative pressure.
The device comprises an extraction kettle, wherein the bottom end and the top end of the extraction kettle are connected with the middle part of a first-stage rectifying tower, the top part of the first-stage rectifying tower is connected with the middle part of a second-stage rectifying tower, the top part of the second-stage rectifying tower is connected with the middle part of the extraction kettle, and the bottom end of the second-stage rectifying tower is a product output end.
The invention has the beneficial effects that:
the invention adopts solid-liquid extraction to decolor heavy components of maleic anhydride, and the maleic anhydride product recovery rate can reach more than 90 percent and the melting color number can reach less than 20 through two-stage rectification and purification, and meanwhile, the method has the advantages of recyclable extracting agent, mild treatment conditions, low energy consumption and remarkable economic benefit.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
the utility model provides a device for refined heavy ends of maleic anhydride decoloration purification, the device includes the extraction cauldron, and the bottom and the top of extraction cauldron all link to each other with the middle part of one-level rectifying column, and the top of one-level rectifying column links to each other with the middle part of second grade rectifying column, and the top of second grade rectifying column links to each other with the middle part of extraction cauldron, and the bottom of second grade rectifying column is the product output end.
Example 1:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is toluene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extracting phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature of the bottom of a tower is 140 ℃, a product at the top of a tower is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature of the bottom of the tower is 45 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 95%, the purity reaches 99.97%, and the number of a molten color is 15.
Example 2:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is p-xylene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extraction phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 10Kpa, the operating temperature at the bottom of a tower is 130 ℃, a product at the top of a tower is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure 10Kpa, the operating temperature at the bottom of the tower is 69 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 93%, the purity reaches 99.97%, and the melting color number is 15.
Example 3:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is o-xylene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extraction phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure of 20Kpa, the operating temperature at the bottom of a tower is 140 ℃, a product at the top of a collecting tower is conveyed to a secondary rectifying device, the operating pressure is negative pressure of 20Kpa, the operating temperature at the bottom of the tower is 75 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 89%, the purity reaches 99.97%, and the melting color number is 15.
Example 4:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is m-xylene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extraction phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 25Kpa, the operating temperature at the bottom of a tower is 140 ℃, a product at the top of a collecting tower is conveyed to a secondary rectifying device, the operating pressure is negative pressure 25Kpa, the operating temperature at the bottom of the tower is 70 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 89%, the purity reaches 99.97%, and the melting color number is 15.
Example 5:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is benzene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extracting phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure of 30Kpa, the operating temperature of the bottom of a tower is 140 ℃, a product at the top of a tower is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure of 30Kpa, the operating temperature of the bottom of the tower is 90 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 91%, the purity reaches 99.97%, and the molten color number is 15.
Example 6:
the purity of a maleic anhydride raw material is 96.0%, an extracting agent is toluene, the raw material and the extracting agent are mixed and added into a 5L extraction kettle according to the mass ratio of 1:1, stirring is carried out for 15min, standing is carried out for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residue is chromogenic impurity, filtrate and an upper-layer extracting phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature of the bottom of a tower is 140 ℃, a product at the top of a tower is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature of the bottom of the tower is 45 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 93%, the purity reaches 99.97%, and the number of a molten color is 15.
Example 7:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is a mixture of toluene and p-xylene mixed according to the mass ratio of 2:1, the raw material and the extracting agent are mixed according to the mass ratio of 1:1 and added into a 5L extraction kettle, the mixture is stirred for 15min and kept stand for 60min, a lower-layer chromogenic impurity phase is discharged, the impurity phase is filtered, filter residues are chromogenic impurities, filtrate and an upper-layer extraction phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature at the bottom of a tower is 140 ℃, a product at the top of the tower is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature at the bottom of the tower is 45 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 94%, the purity is 99.97%, and the molten color number is 15.
Example 8:
the purity of a maleic anhydride raw material is 99.5%, an extracting agent is a mixture of benzene, toluene and p-xylene in a mass ratio of 1:2:1, the raw material and the extracting agent are mixed in a mass ratio of 1:1 and added into a 5L extraction kettle, the mixture is stirred for 15min and kept stand for 60min, a lower chromogenic impurity phase is discharged, the impurity phase is filtered, filter residues are chromogenic impurities, filtrate and an upper extraction phase are mixed and conveyed to a primary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature at the bottom of a tower is 140 ℃, a tower top product is collected and conveyed to a secondary rectifying device, the operating pressure is negative pressure 15Kpa, the operating temperature at the bottom of the tower is 45 ℃, the extracting agent is recovered at the top of the tower, a maleic anhydride product is obtained at the bottom of the tower, the recovery rate of the maleic anhydride product is 92%, the purity is 99.97%, and the melting color number is 15.
TABLE 1 data Table of the examples
Claims (6)
1. A method for decoloring and purifying heavy components refined from maleic anhydride is characterized by comprising the following steps: the method comprises the steps of conveying a maleic anhydride raw material into an extraction kettle for extraction, obtaining a chromogenic impurity phase at the lower layer after extraction is finished, and filtering the chromogenic impurity phase to respectively obtain a filtrate and chromogenic impurities; the filtrate obtained after the lower layer filtration and the upper layer extract phase are conveyed to a first-stage rectifying tower for rectification, the product at the top of the tower after the first rectification is finished is conveyed to a second-stage rectifying device for secondary rectification, the extractant is recovered at the top of the tower after the second rectification, and a maleic anhydride product is obtained at the bottom of the tower;
the extractant is one or two of toluene, m-xylene, o-xylene and p-xylene; in the extraction process, the mass ratio of the extracting agent to the maleic anhydride raw material is 10: 1-1: 5, stirring for 10-60 min, and standing for 30-240 min after stirring is finished.
2. The method for decoloring and purifying maleic anhydride refined heavy components according to claim 1, wherein the method comprises the following steps: in the extraction process, the mass ratio of the extracting agent to the maleic anhydride raw material is 1:1 to 5.
3. The method for decoloring and purifying maleic anhydride refined heavy components according to claim 1, wherein the method comprises the following steps: the operating pressure of the primary rectifying tower is 10-50 Kpa, and the operating temperature of the bottom of the primary rectifying tower is 110-200 ℃.
4. The method for decoloring and purifying maleic anhydride refined heavy components according to claim 3, wherein the method comprises the following steps: the operating pressure of the primary rectifying tower is 10-30 Kpa, and the operating temperature of the bottom of the primary rectifying tower is 130-150 ℃.
5. The method for decoloring and purifying maleic anhydride refined heavy components according to claim 1, wherein the method comprises the following steps: the operating pressure of the secondary rectifying tower is 10-50 Kpa, and the operating temperature of the tower bottom of the secondary rectifying tower is 45-95 ℃.
6. The method for decoloring and purifying maleic anhydride refined heavy components according to claim 5, wherein the method comprises the following steps: the operation pressure of the secondary rectifying tower is 10-30 Kpa negative pressure.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB879549A (en) * | 1958-07-31 | 1961-10-11 | Monsanto Chemicals | Purification of maleic anhydride |
| CN101514138A (en) * | 2008-02-20 | 2009-08-26 | 中国石油化工股份有限公司 | Decoloring agent and application thereof |
| CN103193739A (en) * | 2013-04-16 | 2013-07-10 | 北京秦唐工程有限公司 | Method for removing heavy and light impurities in maleic anhydride system |
| CN106178571A (en) * | 2016-08-31 | 2016-12-07 | 烟台国邦化工机械科技有限公司 | A kind of Azeotrope separation technique |
| CN109761940A (en) * | 2019-03-18 | 2019-05-17 | 淄博齐翔腾达化工股份有限公司 | Crude maleic anhydride continuous rectification apparatus and process |
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- 2019-10-15 CN CN201910978696.8A patent/CN112661731B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB879549A (en) * | 1958-07-31 | 1961-10-11 | Monsanto Chemicals | Purification of maleic anhydride |
| CN101514138A (en) * | 2008-02-20 | 2009-08-26 | 中国石油化工股份有限公司 | Decoloring agent and application thereof |
| CN103193739A (en) * | 2013-04-16 | 2013-07-10 | 北京秦唐工程有限公司 | Method for removing heavy and light impurities in maleic anhydride system |
| CN106178571A (en) * | 2016-08-31 | 2016-12-07 | 烟台国邦化工机械科技有限公司 | A kind of Azeotrope separation technique |
| CN109761940A (en) * | 2019-03-18 | 2019-05-17 | 淄博齐翔腾达化工股份有限公司 | Crude maleic anhydride continuous rectification apparatus and process |
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