CN113262509A - Treatment system and treatment method for isobutanol recovered from diisobutyl preparation process - Google Patents
Treatment system and treatment method for isobutanol recovered from diisobutyl preparation process Download PDFInfo
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Abstract
The invention relates to the technical field of diisobutyl ester production, and discloses a treatment system for isobutanol recovered in a diisobutyl ester preparation process and a treatment method for isobutanol, aiming at the problem that the reuse of isobutanol is influenced by the high content of color and luster substances in the isobutanol recovered in the existing diisobutyl ester preparation process. The treatment system and the treatment method can effectively purify the isobutanol recovered in the diisobutyl ester production, the recovery rate of the isobutanol is high, the purity is high, the sulfur test color can reach below 15#, the production application of the diisobutyl ester is met, the process structure is simple, and positive economic benefits and environmental protection benefits are achieved.
Description
Technical Field
The invention relates to the technical field of diisobutyl ester production, in particular to a treatment system for recovering isobutanol in a diisobutyl ester preparation process and a treatment method for the isobutanol.
Background
The diisobutyl ester is produced with phthalic anhydride and isobutyl alcohol as material and through heating reaction in the presence of sulfuric acid catalyst to produce coarse ester, neutralizing with sodium carbonate in neutralizing position, vacuum dealcoholizing in dealcoholizing tower, and filtering in filter press to eliminate impurity and to obtain the product. And treating the wastewater generated by esterification and neutralization by a wastewater treatment tower, recovering isobutanol, and using the recovered isobutanol as a raw material again. The sulfur test color of the recovered alcohol generated in the esterification working section and the wastewater recovery working section is very high, because under the reaction condition, impurities in the recovered alcohol continuously generate thermal cracking and oxidation reactions to generate unsaturates, the unsaturates are further polymerized to form colored substances, the color of the esterified crude ester is adversely affected by the byproducts, the color of the recovered alcohol sulfur in the esterification phase separator and the recovered phase separator is larger than 100# through regular sampling and detection of isobutanol recovered in the esterification and dealcoholization working sections, the content of the byproducts is increased progressively along with the recycling and reusing of the recovered isobutanol, the components are complex day by day, and the quality of the diisobutyl ester is seriously affected. In addition, solid waste generated by the diisobutyl ester production system mainly comes from low-boiling-point substances and high-boiling-point substances generated by treating and recycling alcohol. Therefore, how to treat the isobutanol recovered in the diisobutyl preparation and reduce the solid waste yield are of great significance for the diisobutyl production.
Disclosure of Invention
Aiming at the problem that the reuse of isobutanol is influenced by the high content of color substances in the isobutanol recovered in the existing diisobutyl preparation process, the invention aims to provide a treatment system for the isobutanol recovered in the diisobutyl preparation process, which can effectively reduce the content of the color substances in the isobutanol and improve the purity of the isobutanol, and meanwhile, the purity and the recovery rate of the isobutanol are high.
Another object of the present invention is to provide a method for treating recovered isobutanol using the treatment system described above.
The technical scheme provided by the invention is as follows:
a treatment system for isobutanol recovered from a diisobutyl preparation process comprises a pretreatment kettle (1), a pretreatment tower (2), a pretreatment phase separator (4), a primary low-boiling tank (5), a second fraction tank (6), a front isobutanol tank (7), a low-boiling kettle (10), a low-boiling tower (11), a low-boiling phase separator (13), a rear isobutanol tank (14) and a secondary low-boiling tank (15), which are sequentially arranged along the material flow direction;
the top of the pretreatment kettle is provided with a first feed inlet (18), a first discharge outlet (19) and a second feed inlet (20), and the bottom of the pretreatment kettle is provided with a second discharge outlet (21);
the top of the pretreatment tower is provided with a third discharge hole (23), the upper part of the pretreatment tower is provided with a fifth feed hole (26), and the bottom of the pretreatment tower is provided with a fifth discharge hole (27) and a third feed hole (22);
a fourth feed inlet (24) and a fourth discharge outlet (25) are formed in the pretreatment phase splitter;
the first discharge hole is communicated with the third feed hole through a feed pipeline, the fifth discharge hole is communicated with the second feed hole through a discharge pipeline, the third discharge hole is communicated with the fourth feed hole through a feed pipeline, and the fourth discharge hole is communicated with the fifth feed hole through a return pipeline;
the fourth discharge hole is also respectively communicated with the front isobutanol groove, the second fraction groove and the primary low-boiling groove through a feeding pipeline;
a sixth feeding hole (28), a sixth discharging hole (29) and a seventh feeding hole (30) are formed in the top of the low-boiling kettle, and a seventh discharging hole (31) is formed in the bottom of the low-boiling kettle;
the lower part of the low-boiling tower is provided with an eighth feed inlet (32), the bottom of the low-boiling tower is provided with a tenth discharge outlet (37), the upper part of the low-boiling tower is provided with a decimal feed inlet (36), and the top of the low-boiling tower is provided with an eighth discharge outlet (33);
a ninth feeding hole (34) and a ninth discharging hole (35) are formed in the low-boiling phase separator;
a low-boiling material outlet is formed in the primary low-boiling tank and is communicated with a sixth feeding hole through a feeding pipeline, a sixth discharging hole is communicated with an eighth feeding hole through a feeding pipeline, and the bottom of a tenth discharging hole is communicated with a seventh feeding hole through a return pipeline;
the eighth discharge hole is communicated with the ninth feed hole through a discharge pipeline, and the ninth discharge hole is communicated with the tenth feed hole through a return pipeline;
the ninth discharge hole is also communicated with the back isobutanol groove and the secondary low-boiling groove through a discharge pipeline.
The treatment for recovering isobutanol of the invention is different from the purification treatment for isobutanol of other occasions, such as the purification treatment for preparing isobutanol by an isobutyraldehyde hydrogenation method, mainly because the organic impurity components and the content of the isobutanol are different. The recovered isobutanol to be treated by the invention is derived from the diisobutyl preparation process, such as esterification reaction and neutralization reaction, wherein the generated impurities are subjected to continuous thermal cracking and oxidation reaction to generate unsaturates, and the unsaturates are further polymerized to form colored substances, and the color of the esterified crude ester is adversely affected by the byproducts. According to the impurity components and content characteristics in the recovered isobutanol, an inventor team repeatedly tries to use a rectifying still, a rectifying tower and a phase splitter together, and adopts a double-rectifying mode to effectively treat the recovered isobutanol, the recovery rate of the isobutanol can reach 90 percent, even more than 96 percent, the purity is high, the color impurity content is greatly reduced, the color number can reach below 15#, and the requirement of diisobutyl ester production on the raw material of the isobutanol is completely met.
Preferably, the temperature of the pretreatment kettle is 80-113 ℃; the temperature of the low-boiling kettle is 80-113 ℃. The pretreatment kettle is used for carrying out first separation of recovered isobutanol, the generated gas phase enters a subsequent separation process, and the high-boiling residue is separated from the pretreatment kettle to be one of solid waste sources; the low-boiling kettle separates the components in the primary low-boiling tank, the generated gas phase enters a subsequent separation process, and the high-boiling substance is separated from the primary treatment kettle to be one of solid waste sources.
Preferably, the number of the tower plates of the pretreatment tower is 28-32; the number of the tower plates of the low-boiling tower is 28-32. Controlling the appropriate number of trays is important to maintain the desired analytical results.
Preferably, the first low boiling tank collects a front fraction when the tower top temperature of the pretreatment tower is 86-107 ℃, the second distillate tank collects a middle fraction when the tower top temperature of the pretreatment tower is 107-108 ℃, and the front isobutanol tank collects a back fraction when the tower top temperature of the pretreatment tower is higher than 108 ℃. The isobutanol in the front isobutanol tank can be reused, the material in the first low-boiling tank is a low-boiling material with the sulphur test color of more than 200#, the content of the isobutanol is 50-60 wt%, further treatment is needed, and the material in the second fraction tank is determined according to the quality of the isobutanol.
Preferably, the secondary low-boiling tank collects a front fraction when the tower top temperature of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects a back fraction when the tower top temperature of the low-boiling tower is higher than 108 ℃. The isobutanol in the isobutanol groove can be reused, and the isobutanol content in the material of the secondary low-boiling-point groove is 30-40% and is a main solid waste source.
Preferably, the flow ratio of the material refluxed from the pretreatment phase separator to the pretreatment column to the total material introduced from the pretreatment phase separator into the isobutanol tank, the second fraction tank and the primary low-boiling tank is 1:1 to 1.2.
Preferably, the flow ratio of the material refluxed from the low-boiling phase separator to the pretreatment column to the total material introduced from the low-boiling phase separator into the post-isobutanol tank and the secondary low-boiling tank is 1:1 to 1.2.
A method for treating isobutanol recovered from a diisobutyl preparation process by using the treatment system comprises the following steps:
(1) delivering isobutanol recovered from diisobutyl preparation into a pretreatment kettle through a first feed port for heating, delivering generated gas phase into a pretreatment tower through a first discharge port and a third feed port, and discharging high-boiling substances generated in the pretreatment kettle from a second discharge port;
(2) the gas phase in the pretreatment tower enters the pretreatment phase separator from the third discharge hole to separate a water phase and an organic phase, when the temperature of the tower top of the pretreatment tower is more than or equal to 86 ℃, the organic phase in the pretreatment phase separator partially reflows to the pretreatment tower from the fourth discharge hole, and one part of the organic phase is collected into a primary low-boiling tank, a second fraction tank or a front isobutanol tank, wherein the primary low-boiling tank collects a front fraction when the temperature of the tower top of the pretreatment tower is 86-107 ℃, and the isobutanol tank collects a back fraction when the temperature of the tower top of the pretreatment tower is higher than 108 ℃;
(3) the organic phase collected in the primary low-boiling tank enters a low-boiling kettle through a sixth feeding hole, the gas phase generated in the low-boiling kettle enters a low-boiling tower through a sixth discharging hole, the gas phase generated in the low-boiling tower enters a low-boiling phase separator through an eighth discharging hole to separate a water phase and the organic phase, one part of the organic phase flows back to the low-boiling tower through a ninth discharging hole, the other part of the organic phase is collected in a back isobutanol tank or a secondary low-boiling tank, wherein the secondary low-boiling tank collects front fraction when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fraction when the temperature of the top of the low-boiling tower is higher than 108 ℃;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting low-boiling-point substances in the secondary low-boiling-point groove and high-boiling-point substances in the treatment kettle and the low-boiling-point kettle to obtain solid waste.
In the above process, since the initially recovered isobutanol contains 10 to 15wt% of water, the organic phase in the pre-treatment phase separator needs to be subjected to total reflux water separation at an initial stage.
Preferably, the method of the invention further comprises the step (3) of adding 10-15 wt% of water into the low-boiling kettle. Because the isobutanol content of the materials in the primary low-boiling tank is reduced, the impurity content is increased (the sulfur test color is more than 200 #), the water content is reduced to 1-5 wt%, and after further water is required to be added, the water and the low-boiling impurities and ether are subjected to azeotropic distillation, high-content impurities are extracted from the tower top and enter a secondary low-boiling tank.
As a preference of the process of the present invention, the treatment is ended when the temperature in the former treatment vessel or the low-boiling vessel is more than 113 ℃.
The invention has the following beneficial effects:
the treatment system and the treatment method can effectively purify the isobutanol recovered in the diisobutyl ester production, the recovery rate of the isobutanol is high, the purity is high, the sulfur test color can reach below 15#, the production application of the diisobutyl ester is met, the process structure is simple, and positive economic benefits and environmental protection benefits are achieved.
Drawings
FIG. 1 is a process flow diagram of the treatment system of the present invention.
In the figure: 1. a pretreatment kettle, 2, a pretreatment tower, 3, an overhead condenser, 4, a pretreatment phase separator, 5, a primary low-boiling tank, 6, a second fraction tank, 7, a front isobutanol tank, 8, a recovered alcohol feed pump, 9, a low-boiling feed pump, 10, a low-boiling kettle, 11, a low-boiling tower, 12, a low-boiling overhead condenser, 13, a low-boiling phase separator, 14, a secondary low-boiling tank, 15, a rear isobutanol tank, 18, a first feed inlet, 19, a first discharge outlet, 20, a second feed inlet, 21, a second discharge outlet, 22, a third feed inlet, 23, a third discharge outlet, 24, a fourth feed inlet, 25, a fourth discharge outlet, 26, a fifth feed inlet, 27, a fifth discharge outlet, 28, a sixth feed inlet, 29, a sixth discharge outlet, 30, a seventh feed inlet, 31, a seventh discharge outlet, 32, an eighth feed inlet, 33, an eighth discharge outlet, 34, a ninth feed inlet, 35, and a ninth discharge outlet, 36. a tenth material port, 37 and a tenth material port.
Detailed Description
The following further describes the embodiments of the present invention.
The starting materials used in the present invention are commercially available or commonly used in the art, unless otherwise specified, and the methods in the following examples are conventional in the art, unless otherwise specified.
A treatment system for isobutanol recovered from a diisobutyl preparation process comprises a pretreatment kettle 1, a pretreatment tower 2, a pretreatment phase separator 4, a primary low-boiling tank 5, a second fraction tank 6, a front isobutanol tank 7, a low-boiling kettle 10, a low-boiling tower 11, a low-boiling phase separator 13, a rear isobutanol tank 14 and a secondary low-boiling tank 15 which are sequentially arranged along the material flow direction, as shown in figure 1.
The top of the pretreatment kettle is provided with a first feeding hole 18, a first discharging hole 19 and a second feeding hole 20, the bottom of the pretreatment kettle is provided with a second discharging hole 21, and the temperature of the pretreatment kettle is 80-113 ℃. The pretreatment tower is a packed tower, the number of tower plates is 28-32, the top of the pretreatment tower is provided with a third discharge hole 23, the upper part of the pretreatment tower is provided with a fifth feed hole 26, and the bottom of the pretreatment tower is provided with a fifth discharge hole 27 and a third feed hole 22; the pretreatment phase separator is provided with a fourth feed inlet 24 and a fourth discharge outlet 25.
The top of the low-boiling kettle is provided with a sixth feeding hole 28, a sixth discharging hole 29 and a seventh feeding hole 30, the bottom of the low-boiling kettle is provided with a seventh discharging hole 31, and the temperature of the low-boiling kettle is 80-113 ℃. The lower part of the low-boiling tower is provided with an eighth feed inlet 32, the bottom of the low-boiling tower is provided with a tenth discharge outlet 37, the upper part of the low-boiling tower is provided with a tenth discharge outlet 36, and the top of the low-boiling tower is provided with an eighth discharge outlet 33; and a ninth feeding hole 34 and a ninth discharging hole 35 are arranged on the low-boiling phase separator.
The first feed port is communicated with a pipeline for conveying the recovered isobutanol, and the recovered isobutanol is conveyed into the pretreatment kettle through the first feed port by a recovered alcohol feed pump 8; the first discharge hole is communicated with the third feed hole through a feed pipeline, the fifth discharge hole is communicated with the second feed hole through a discharge pipeline, the third discharge hole is communicated with the fourth feed hole through a feed pipeline, a tower top condenser 3 is further arranged on a pipeline for communicating the third discharge hole with the fourth feed hole, and the fourth discharge hole is communicated with the fifth feed hole through a return pipeline; the fourth discharge hole is also communicated with the front isobutanol groove, the second fraction groove and the primary low-boiling groove through a feeding pipeline respectively.
A low-boiling material outlet is arranged on the primary low-boiling tank and is communicated with the sixth feeding hole through a feeding pipeline, and a low-boiling feeding pump 9 is arranged on the feeding pipeline; the sixth discharge hole is communicated with the eighth feed inlet through a feed pipeline, and the tenth discharge hole is communicated with the seventh feed inlet through a return pipeline; the eighth discharge hole is communicated with the ninth feed hole through a discharge pipeline, a low-boiling tower top condenser 12 is arranged on the discharge pipeline, and the ninth discharge hole is communicated with the tenth feed hole through a return pipeline; the ninth discharge hole is also communicated with the back isobutanol groove and the secondary low-boiling groove through a discharge pipeline.
When the recovered isobutanol is treated, the recovered isobutanol enters a pretreatment kettle through a recovered alcohol feeding pump, gas phase generated from the pretreatment kettle enters a pretreatment tower, and high-boiling residues in the pretreatment kettle are treated from a bottom ladle. Heavy components at the bottom of the pretreatment tower flow back to the pretreatment kettle, gas-phase light components enter a pretreatment phase separator through a tower top condenser to be subjected to water phase and organic phase separation, when the tower top temperature of the pretreatment tower is lower than 86 ℃, organic phases in the pretreatment phase separator flow back completely, when the tower top temperature of the pretreatment tower is higher than 86 ℃, organic phases in the pretreatment phase separator partially flow back to the pretreatment tower, and are partially collected into an isobutanol tank, a second fraction tank or a primary low boiling tank, and the flow ratio of backflow to extraction is controlled to be 1: 1-1.2, specifically: the primary low-boiling tank collects front distillate when the tower top temperature of the pretreatment tower is 86-107 ℃, the second distillate tank collects middle distillate when the tower top temperature of the pretreatment tower is 107-108 ℃, and the front isobutanol tank collects back distillate when the tower top temperature of the pretreatment tower is higher than 108 ℃.
And (3) feeding low-boiling residues in the primary low-boiling tank into a low-boiling kettle through a low-boiling feed pump, feeding a gas phase generated from the low-boiling kettle into a low-boiling tower, wherein the number of tower plates of the low-boiling tower is 28-32, and treating the high-boiling residues in the low-boiling kettle from a bottom ladle. Heavy components at the bottom of the low-boiling tower flow back to the low-boiling kettle, gas-phase light components in the low-boiling tower enter a low-boiling phase separator through an eighth discharge port and a condenser at the top of the low-boiling tower, the low-boiling phase separator is used for separating an organic phase from a water phase, the water phase is discharged from the bottom, one part of the organic phase flows back to the low-boiling tower, one part of the organic phase is extracted into a back isobutanol groove or a secondary low-boiling groove, the flow ratio of backflow to extraction is 1: 1-1.2, and the method specifically comprises the following steps: and the secondary low-boiling tank collects front distillate when the temperature of the top of the low-boiling tower is 86-108 ℃, the back isobutanol tank collects back distillate when the temperature of the top of the low-boiling tower is higher than 108 ℃, and the treatment is finished when the temperature of the front treatment kettle or the low-boiling kettle is higher than 113 ℃.
Specific application example 1 of the treatment of isobutanol recovered from a diisobutyl ester production process using the treatment system described above, the steps were as follows:
(1) recovering isobutanol from wastewater generated in an esterification section and a neutralization section of diisobutyl ester after being treated by a wastewater treatment tower, continuously feeding 147 tons of the recovered isobutanol into a pretreatment kettle through a first feed port for heating, wherein the temperature of the pretreatment kettle is 80 ℃, the mass concentration of the isobutanol in the recovered isobutanol is 85%, the balance of the wastewater, color substances and solid wastes is 150#, feeding gas phase generated in the pretreatment kettle into the pretreatment tower through a first discharge port and a third feed port, the number of tower plates of the pretreatment tower is 30, and high-boiling substances generated in the pretreatment kettle are discharged from a second discharge port;
(2) the gas phase in the pretreatment tower enters the pretreatment phase separator from the third discharge hole to separate a water phase and an organic phase, when the tower top temperature of the pretreatment tower is lower than 86 ℃, the organic phase in the pretreatment phase separator totally reflows to the pretreatment tower, when the tower top temperature of the pretreatment tower rises to above 86 ℃, one part of the organic phase in the pretreatment phase separator reflows to the pretreatment tower, and the other part is extracted, wherein the flow ratio of the reflowing to the extracting is 1:1, and the extraction method comprises the following steps: the primary low-boiling tank collects front fraction when the tower top temperature of the pretreatment tower is 86-107 ℃, the isobutanol tank collects rear fraction when the tower top temperature of the pretreatment tower is higher than 108 ℃, and the secondary fraction tank collects fraction when the tower top temperature of the pretreatment tower is 107-108 ℃; when the temperature of the front treatment kettle is higher than 113 ℃, the treatment is finished;
(3) the organic phase collected in the primary low-boiling tank enters a low-boiling kettle through a sixth feeding hole, the temperature of the low-boiling kettle is 108 ℃, 10wt% of water of materials in the low-boiling kettle is added into the low-boiling kettle, the gas phase generated in the low-boiling kettle enters a low-boiling tower through a sixth discharging hole, the gas phase generated in the low-boiling tower enters a low-boiling phase separator through an eighth discharging hole to separate a water phase and an organic phase, one part of the organic phase reflows to the low-boiling tower through a ninth discharging hole, the other part of the organic phase is collected in a back isobutanol tank or a secondary low-boiling tank, the flow ratio of the reflowing to the collecting is 1:1, and the collecting method comprises the following steps: the secondary low-boiling tank collects front fractions when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fractions when the temperature of the top of the low-boiling tower is higher than 108 ℃; when the temperature in the low-boiling kettle is higher than 113 ℃, finishing the treatment;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting high-boiling-point substances in the low-boiling-point treatment kettle and the low-boiling-point kettle in the secondary low-boiling-point groove to obtain solid waste.
In the application example, the recovery rate of the isobutanol is 96.5 percent, the purity is 98.8 percent, and the sulfur test color is less than or equal to 15 #.
Specific application example 2 of the treatment of isobutanol recovered from a diisobutyl ester production process using the treatment system described above, the steps were as follows:
(1) recovering isobutanol from wastewater generated in an esterification section and a neutralization section of diisobutyl ester after being treated by a wastewater treatment tower, continuously feeding 147 tons of the recovered isobutanol into a pretreatment kettle through a first feed port for heating, wherein the temperature of the pretreatment kettle is 112 ℃, the mass concentration of the isobutanol in the recovered isobutanol is 85%, the balance of the wastewater, color substances and solid wastes is 150#, feeding gas phase generated in the pretreatment kettle into the pretreatment tower through a first discharge port and a third feed port, the number of tower plates of the pretreatment tower is 30, and high-boiling substances generated in the pretreatment kettle are discharged from a second discharge port;
(2) and the gas phase in the pretreatment tower enters the pretreatment phase separator from the third discharge hole to separate a water phase and an organic phase, when the tower top temperature of the pretreatment tower is lower than 86 ℃, the organic phase in the pretreatment phase separator totally reflows to the pretreatment tower, the tower top temperature of the current treatment tower rises to 86 ℃, one part of the organic phase in the pretreatment phase separator reflows to the pretreatment tower, and the other part of the organic phase is extracted, wherein the flow ratio of the reflowing to the extracting is 1:1.1, and the extraction method comprises the following steps: the primary low-boiling tank collects front fraction when the tower top temperature of the pretreatment tower is 86-107 ℃, the isobutanol tank collects rear fraction when the tower top temperature of the pretreatment tower is higher than 108 ℃, and the secondary fraction tank collects fraction when the tower top temperature of the pretreatment tower is 107-108 ℃; when the temperature of the front treatment kettle is higher than 113 ℃, the treatment is finished;
(3) the organic phase collected in the primary low-boiling tank enters a low-boiling kettle through a sixth feeding hole, the temperature of the low-boiling kettle is 112 ℃, 15wt% of water of materials in the low-boiling kettle is added into the low-boiling kettle, the gas phase generated in the low-boiling kettle enters a low-boiling tower through a sixth discharging hole, the gas phase generated in the low-boiling tower enters a low-boiling phase separator through an eighth discharging hole to separate a water phase and an organic phase, one part of the organic phase reflows to the low-boiling tower through a ninth discharging hole, the other part of the organic phase is collected in a back isobutanol tank or a secondary low-boiling tank, the flow ratio of the reflowing to the collecting is 1:1.1, and the collecting method comprises the following steps: the secondary low-boiling tank collects front fractions when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fractions when the temperature of the top of the low-boiling tower is higher than 108 ℃; when the temperature in the low-boiling kettle is higher than 113 ℃, finishing the treatment;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting high-boiling-point substances in the low-boiling-point treatment kettle and the low-boiling-point kettle in the secondary low-boiling-point groove to obtain solid waste.
In the application example, the recovery rate of the isobutanol is 96.2 percent, the purity is 99.1 percent, and the sulfur test color is less than or equal to 15 #.
Specific application example 3 of the treatment of isobutanol recovered from a diisobutyl ester production process using the treatment system described above, the steps were as follows:
(1) recovering isobutanol from wastewater generated in an esterification section and a neutralization section of diisobutyl ester after being treated by a wastewater treatment tower, continuously feeding 147 tons of the recovered isobutanol into a pretreatment kettle through a first feed port for heating, wherein the temperature of the pretreatment kettle is 100 ℃, the mass concentration of the isobutanol in the recovered isobutanol is 85%, the balance of the wastewater, color substances and solid wastes is 150#, feeding gas phase generated in the pretreatment kettle into the pretreatment tower through a first discharge port and a third feed port, the number of tower plates of the pretreatment tower is 30, and high-boiling substances generated in the pretreatment kettle are discharged from a second discharge port;
(2) and the gas phase in the pretreatment tower enters the pretreatment phase separator from the third discharge hole to separate a water phase and an organic phase, when the tower top temperature of the pretreatment tower is lower than 86 ℃, the organic phase in the pretreatment phase separator totally reflows to the pretreatment tower, the tower top temperature of the current treatment tower rises to 86 ℃, one part of the organic phase in the pretreatment phase separator reflows to the pretreatment tower, and the other part of the organic phase is extracted, wherein the flow ratio of the reflowing to the extracting is 1:1.2, and the extraction method comprises the following steps: the primary low-boiling tank collects front fraction when the tower top temperature of the pretreatment tower is 86-107 ℃, the isobutanol tank collects rear fraction when the tower top temperature of the pretreatment tower is higher than 108 ℃, and the secondary fraction tank collects fraction when the tower top temperature of the pretreatment tower is 107-108 ℃; when the temperature of the front treatment kettle is higher than 113 ℃, the treatment is finished;
(3) and (2) feeding the organic phase collected in the primary low-boiling tank into a low-boiling kettle through a sixth feeding hole, wherein the temperature of the low-boiling kettle is 100 ℃, adding 14wt% of water of materials in the low-boiling kettle into the low-boiling kettle, feeding the gas phase generated in the low-boiling kettle into a low-boiling tower through a sixth discharging hole, feeding the gas phase generated in the low-boiling tower into a low-boiling phase separator through an eighth discharging hole to separate a water phase and an organic phase, refluxing one part of the organic phase to the low-boiling tower through a ninth discharging hole, collecting the other part of the organic phase in a back isobutanol tank or a secondary low-boiling tank, and controlling the flow ratio of reflux to the collected part of the organic phase to be 1: 1-1.2, wherein the collection method comprises the following steps: the secondary low-boiling tank collects front fractions when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fractions when the temperature of the top of the low-boiling tower is higher than 108 ℃; when the temperature in the low-boiling kettle is higher than 113 ℃, finishing the treatment;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting high-boiling-point substances in the low-boiling-point treatment kettle and the low-boiling-point kettle in the secondary low-boiling-point groove to obtain solid waste.
In the application example, the recovery rate of the isobutanol is 96.8 percent, the purity is 99.3 percent, and the sulfur test color is less than or equal to 10 #.
Specific application example 4 of the treatment of isobutanol recovered from a diisobutyl ester production process using the treatment system described above, the steps were as follows:
(1) recovering isobutanol from wastewater generated in an esterification section and a neutralization section of diisobutyl ester after being treated by a wastewater treatment tower, continuously feeding 147 tons of the recovered isobutanol into a pretreatment kettle through a first feed port for heating, wherein the temperature of the pretreatment kettle is 80 ℃, the mass concentration of the isobutanol in the recovered isobutanol is 85%, the balance of the wastewater, color substances and solid wastes is 150#, feeding gas phase generated in the pretreatment kettle into the pretreatment tower through a first discharge port and a third feed port, the number of tower plates of the pretreatment tower is 30, and high-boiling substances generated in the pretreatment kettle are discharged from a second discharge port;
(2) and the gas phase in the pretreatment tower enters the pretreatment phase separator from a third discharge hole to separate a water phase and an organic phase, when the tower top temperature of the pretreatment tower is lower than 86 ℃, the organic phase in the pretreatment phase separator totally reflows to the pretreatment tower, the tower top temperature of the current treatment tower rises to 86 ℃, one part of the organic phase in the pretreatment phase separator reflows to the pretreatment tower, and the other part of the organic phase is extracted, wherein the flow ratio of the reflowing to the extracting is 1:1, and the extraction method comprises the following steps: the primary low-boiling tank collects front fraction when the tower top temperature of the pretreatment tower is 86-107 ℃, the isobutanol tank collects rear fraction when the tower top temperature of the pretreatment tower is higher than 108 ℃, and the secondary fraction tank collects fraction when the tower top temperature of the pretreatment tower is 107-108 ℃; when the temperature of the front treatment kettle is higher than 113 ℃, the treatment is finished;
(3) the organic phase collected in the primary low-boiling tank enters a low-boiling kettle through a sixth feeding hole, the temperature of the low-boiling kettle is 108 ℃, the gas phase generated in the low-boiling kettle enters a low-boiling tower through a sixth discharging hole, the gas phase generated in the low-boiling tower enters a low-boiling phase separator through an eighth discharging hole to separate a water phase and the organic phase, one part of the organic phase reflows to the low-boiling tower through a ninth discharging hole, the other part of the organic phase is collected in a back isobutanol tank or a secondary low-boiling tank, the flow ratio of the reflowing to the collected organic phase is 1:1, and the extraction method comprises the following steps: the secondary low-boiling tank collects front fractions when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fractions when the temperature of the top of the low-boiling tower is higher than 108 ℃; when the temperature in the low-boiling kettle is higher than 113 ℃, finishing the treatment;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting high-boiling-point substances in the low-boiling-point treatment kettle and the low-boiling-point kettle in the secondary low-boiling-point groove to obtain solid waste.
In the application example, the recovery rate of the isobutanol is 90.5 percent, the purity is 91.8 percent, and the color of the sulfur test is less than or equal to 30 #.
Claims (10)
1. The treatment system for the isobutanol recovered from the diisobutyl preparation process is characterized by comprising a pretreatment kettle (1), a pretreatment tower (2), a pretreatment phase separator (4), a primary low-boiling tank (5), a second fractionation tank (6), a front isobutanol tank (7), a low-boiling kettle (10), a low-boiling tower (11), a low-boiling phase separator (13), a rear isobutanol tank (14) and a secondary low-boiling tank (15) which are sequentially arranged along the material flow direction;
the top of the pretreatment kettle is provided with a first feed inlet (18), a first discharge outlet (19) and a second feed inlet (20), and the bottom of the pretreatment kettle is provided with a second discharge outlet (21);
the top of the pretreatment tower is provided with a third discharge hole (23), the upper part of the pretreatment tower is provided with a fifth feed hole (26), and the bottom of the pretreatment tower is provided with a fifth discharge hole (27) and a third feed hole (22);
a fourth feeding hole (24) and a fourth discharging hole (25) are formed in the treatment phase splitter;
the first discharge hole is communicated with the third feed hole through a feed pipeline, the fifth discharge hole is communicated with the second feed hole through a discharge pipeline, the third discharge hole is communicated with the fourth feed hole through a feed pipeline, and the fourth discharge hole is communicated with the fifth feed hole through a return pipeline;
the fourth discharge hole is also respectively communicated with the front isobutanol groove, the second fraction groove and the primary low-boiling groove through a feeding pipeline;
a sixth feeding hole (28), a sixth discharging hole (29) and a seventh feeding hole (30) are formed in the top of the low-boiling kettle, and a seventh discharging hole (31) is formed in the bottom of the low-boiling kettle;
the lower part of the low-boiling tower is provided with an eighth feed inlet (32), the bottom of the low-boiling tower is provided with a tenth discharge outlet (37), the upper part of the low-boiling tower is provided with a decimal feed inlet (36), and the top of the low-boiling tower is provided with an eighth discharge outlet (33);
a ninth feeding hole (34) and a ninth discharging hole (35) are formed in the low-boiling phase separator;
a low-boiling material outlet is formed in the primary low-boiling tank and is communicated with a sixth feeding hole through a feeding pipeline, a sixth discharging hole is communicated with an eighth feeding hole through a feeding pipeline, and the bottom of a tenth discharging hole is communicated with a seventh feeding hole through a return pipeline;
the eighth discharge hole is communicated with the ninth feed hole through a discharge pipeline, and the ninth discharge hole is communicated with the tenth feed hole through a return pipeline;
the ninth discharge hole is also communicated with the back isobutanol groove and the secondary low-boiling groove through a discharge pipeline.
2. The system for the treatment of isobutanol recovered from a diisobutyl preparation process according to claim 1, wherein the temperature of the pre-treatment tank is 80 to 113 ℃; the temperature of the low-boiling kettle is 80-113 ℃.
3. The system for handling isobutanol recovered from a diisobutyl preparation process according to claim 1, wherein the number of trays of the pretreatment column is 28 to 32; the number of the tower plates of the low-boiling tower is 28-32.
4. The system according to claim 1 or 3, wherein the first low-boiling tank collects a front cut fraction at an overhead temperature of the pre-treatment column of 86 to 107 ℃, the second cut tank collects a middle cut fraction at an overhead temperature of the pre-treatment column of 107 to 108 ℃, and the front isobutanol tank collects a back cut fraction at an overhead temperature of the pre-treatment column of more than 108 ℃.
5. The system for handling isobutanol recovered from a diisobutyl production process according to claim 1 or 3, wherein the secondary low-boiling tank collects a front fraction when the overhead temperature of the low-boiling column is 86 to 108 ℃, and the post-isobutanol tank collects a post fraction when the overhead temperature of the low-boiling column is higher than 108 ℃.
6. The system for treating isobutanol recovered from a diisobutyl ester production process according to claim 1, wherein the flow ratio of the material returned from the pretreatment phase separator to the pretreatment column to the total material introduced from the pretreatment phase separator into the isobutanol tank, the second fraction tank and the primary low-boiling tank is 1:1 to 1.2.
7. The system for treating isobutanol recovered from a diisobutyl production process according to claim 1, wherein the flow ratio of the material refluxed from the low-boiling phase separator to the low-boiling column to the total material introduced from the low-boiling phase separator into the secondary low-boiling tank is 1:1 to 1.2.
8. A method of treating isobutanol recovered from a diisobutyl preparation process using the treatment system of any one of claims 1 to 7, comprising the steps of:
(1) delivering isobutanol recovered from diisobutyl preparation into a pretreatment kettle through a first feed port for heating, delivering generated gas phase into a pretreatment tower through a first discharge port and a third feed port, and discharging high-boiling substances generated in the pretreatment kettle from a second discharge port;
(2) the gas phase in the pretreatment tower enters the pretreatment phase separator from the third discharge hole to separate a water phase and an organic phase, when the temperature of the tower top of the pretreatment tower is more than or equal to 86 ℃, the organic phase in the pretreatment phase separator partially reflows to the pretreatment tower from the fourth discharge hole, and one part of the organic phase is collected into a primary low-boiling tank, a second fraction tank or a front isobutanol tank, wherein the primary low-boiling tank collects a front fraction when the temperature of the tower top of the pretreatment tower is 86-107 ℃, and the isobutanol tank collects a back fraction when the temperature of the tower top of the pretreatment tower is higher than 108 ℃;
(3) the organic phase collected in the primary low-boiling tank enters a low-boiling kettle through a sixth feeding hole, the gas phase generated in the low-boiling kettle enters a low-boiling tower through a sixth discharging hole, the gas phase generated in the low-boiling tower enters a low-boiling phase separator through an eighth discharging hole to separate a water phase and the organic phase, one part of the organic phase flows back to the low-boiling tower through a ninth discharging hole, the other part of the organic phase is collected in a back isobutanol tank or a secondary low-boiling tank, wherein the secondary low-boiling tank collects front fraction when the temperature of the top of the low-boiling tower is 86-108 ℃, and the back isobutanol tank collects back fraction when the temperature of the top of the low-boiling tower is higher than 108 ℃;
(4) collecting isobutanol in the front isobutanol groove and the rear isobutanol groove to obtain purified isobutanol, and collecting high-boiling-point substances in the low-boiling-point treatment kettle and the low-boiling-point kettle in the secondary low-boiling-point groove to obtain solid waste.
9. The method according to claim 8, wherein step (3) further comprises adding water in an amount of 10 to 15wt% based on the weight of the low-boiling material in the low-boiling tank.
10. The process for the treatment of isobutanol recovered from the diisobutyl preparation process of claim 8, wherein the treatment is terminated when the temperature in the front-treatment tank or the low-boiling tank is more than 113 ℃.
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