CN115557834A - Separation process of mixed butyraldehyde - Google Patents
Separation process of mixed butyraldehyde Download PDFInfo
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- CN115557834A CN115557834A CN202110752194.0A CN202110752194A CN115557834A CN 115557834 A CN115557834 A CN 115557834A CN 202110752194 A CN202110752194 A CN 202110752194A CN 115557834 A CN115557834 A CN 115557834A
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Abstract
The invention relates to a separation process for preparing mixed butyraldehyde by low-pressure carbonyl synthesis, belonging to the technical field of chemical separation. According to the separation process of the mixed butyraldehyde, a reaction product of a oxo reactor enters the middle part of a butyraldehyde isomer tower through a feed inlet after being subjected to catalyst separation and compression, the light component in the reaction product is less than or equal to 4wt%, the ratio of n-isobutyraldehyde is 10-13, the light component is extracted from the top of a light component removal section at the top of the tower, isobutyraldehyde is extracted from the lateral line at the upper part of the tower, and a n-butyraldehyde mixture is extracted from the bottom of the tower. The invention has the advantages of small equipment investment, simple operation, low energy consumption and high concentration of isobutyraldehyde products.
Description
Technical Field
The invention relates to a separation process for preparing mixed butyraldehyde by low-pressure carbonyl synthesis, belonging to the technical field of chemical separation.
Background
N-butyraldehyde is a colorless transparent liquid at normal temperature, has a suffocation odor, and is commonly used as an intermediate for resins, plastic plasticizers, vulcanization accelerators, insecticides and the like.
Isobutyraldehyde is colorless liquid at normal temperature and has pungent smell, and is an important raw material in chemical production, is commonly used for synthesizing cellulose ester, essence, perfume and the like, can be used for preparing rubber vulcanization accelerators and anti-aging agents, and is a raw material for producing isobutanol, neopentyl glycol, methacrylic acid (MAA) and Methyl Methacrylate (MMA).
The industrial production of butyraldehyde takes propylene and synthesis gas as raw materials, stable butyraldehyde is generated through the oxo synthesis reaction, and then the stable butyraldehyde is fractionated to obtain the products of n-butyraldehyde and isobutyraldehyde. There are three main industrial production processes for butyraldehyde: (1) high pressure cobalt process; (2) medium pressure rhodium processes; (3) a low pressure rhodium process. The boiling point of n-butyraldehyde is 75.7 ℃, the boiling point of isobutyraldehyde is 64.0 ℃, and a precise rectification method is generally adopted for separating mixed butyraldehyde, but the existing three-tower or two-tower rectification equipment has large investment and high energy consumption.
CN112299979A discloses a method for extracting isobutyraldehyde, which comprises a butyraldehyde isomer rectifying tower and an isobutyraldehyde rectifying tower, wherein a mixture containing n-butyraldehyde and isobutyraldehyde is primarily separated in the butyraldehyde isomer rectifying tower, a mixture of n-butyraldehyde and isobutyraldehyde is extracted from the top of the tower, and n-butyraldehyde is extracted from the bottom of the tower; the mixture of n-isobutyraldehyde and isobutyraldehyde enters an isobutyraldehyde rectifying tower for purification, isobutyraldehyde is extracted from the side line, and n-butyraldehyde is extracted from the tower bottom. The method has large equipment investment, and the side line operation has high requirement on the purity of isobutyraldehyde in the mixed butyraldehyde.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a separation process of mixed butyraldehyde, which has the advantages of small equipment investment, simple operation, low energy consumption and high concentration of isobutyraldehyde products.
The invention provides a separation process of a carbonyl synthesis reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components, wherein each component is separated by using a butyraldehyde isomerate tower with an added light component removing section, the concentration of the isobutyraldehyde is more than or equal to 99.6 percent (wt) after separation, and the concentrations of the light components and the isobutyraldehyde in the n-butyraldehyde are less than or equal to 0.01 percent (wt).
The basic production process of the invention is as follows: and (2) a reaction product of the oxo-synthesis reactor enters the middle part of a butyraldehyde isomer tower through a feed inlet after being subjected to catalyst separation and compression, wherein the light component in the reaction product is less than or equal to 4% (wt), the ratio of n-butyraldehyde to iso-butyraldehyde is 10-13, the light component is extracted from the top of a light component removal section at the top of the tower, isobutyraldehyde is extracted from the lateral line at the upper part of the tower, and a n-butyraldehyde mixture is extracted from the bottom of the tower.
The device is characterized in that a light component removing section is arranged at the top of the butyraldehyde isomerate tower, a light component outlet at the top of the light component removing section is sequentially connected with a condenser, a reflux tank and a reflux pump through pipelines, the reflux pump is connected with a reflux port of the butyraldehyde isomerate tower, a light component product extraction line is arranged at the top of the reflux tank, an isobutyraldehyde product extraction line is arranged at the upper part of the butyraldehyde isomerate tower, a reboiler is connected with the bottom of the butyraldehyde isomerate tower, and a n-butyraldehyde mixture extraction line is arranged at the bottom of the butyraldehyde isomerate tower.
The butyraldehyde isomerate tower is a plate rectifying tower, and adopts a fixed valve tray, the number of the trays is 119, a feed inlet is positioned on the 54 th tray, and a side draw outlet is positioned on the 10 th tray.
The light component removing section is based on the original butyraldehyde isomerate tower, the plate number of the tower is increased by 9, the top of the tower is increased, and a solid valve tray is adopted.
The fixed valve tray is a semi-elliptical valve body formed by directly stamping a tray structural material, and has the characteristics of being beneficial to reducing the liquid level gradient of liquid, reducing liquid back mixing on the tray and enhancing the mass transfer efficiency.
The operating conditions of the rectifying tower are as follows: the pressure at the top of the tower is 0.12-0.20 MPa, preferably 0.16MPa; the lateral extraction temperature is 72-84 ℃, and the optimal temperature is 78-79 ℃; the temperature of the top of the tower is controlled to be between 66 and 75 ℃, and preferably between 69 and 71 ℃; the temperature of the tower kettle is controlled to be 97-109 ℃, preferably 100-103 ℃; the reflux ratio is controlled to be 40 to 42.
The top products of the butyraldehyde isomerate tower mainly comprise water, carbon dioxide, propylene and propane, the side-stream products mainly comprise isobutyraldehyde, and the bottom products mainly comprise n-butyraldehyde, isobutanol, n-butanol and the like.
In conclusion, the beneficial effects of the invention are as follows:
the invention provides a separation process of a carbonyl synthesis reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components. And (3) feeding the mixed product into the middle part of a butyraldehyde isomerate tower with a light component removing section, extracting the light component from the top of the light component removing section through rectification, extracting isobutyraldehyde from the side line of the upper part of the tower, and extracting a n-butyraldehyde mixture from the bottom of the tower. After separation, the concentration of isobutyraldehyde is more than or equal to 99.6 percent (wt), the concentration of light components and isobutyraldehyde in n-butyraldehyde is less than or equal to 0.01 percent (wt), and the mixture of the light components, isobutyraldehyde and n-butyraldehyde is completely separated. The method is improved from a double-tower process to a single-tower process, and has the advantages of less equipment investment, low device and object consumption and energy consumption and simple operation.
Drawings
FIG. 1 is a schematic diagram of a butyraldehyde isomer column of the present invention;
FIG. 2 is a schematic view of a valve body of a fixed valve tray;
in the figure: 1. a butyraldehyde isomerate column; 2. a light component removal section; 3. a condenser; 4. a reflux tank; 5. a reflux pump; 6. a reboiler; 7. a light component product extraction line; 8. an isobutyraldehyde product production line; 9. and a n-butyraldehyde mixture extraction line.
Detailed Description
The present invention is further illustrated by the following examples, but the present invention is not limited to these examples. The spirit and scope of the present invention will be fully understood from the examples, further understanding the process features of the present invention.
As shown in figure 1, a mixed product enters the middle of a butyraldehyde isomer tower 1, light components and isobutyraldehyde are separated out through rectification and a light component removal section 2, the light components are condensed into a gas-liquid phase mixture through a condenser 3 and enter a reflux tank 4, the gas-phase light components are extracted from a light component product extraction line 7 at the top of the tank, the liquid phase returns to the butyraldehyde isomer tower 1 through a reflux pump 5, isobutyraldehyde products are extracted from an isobutyraldehyde product extraction line 8 at the upper part of the tower, and a n-butyraldehyde mixture is extracted from a n-butyraldehyde mixture extraction line 9 at the bottom of the tower.
The rectifying tower is a plate rectifying tower, and adopts valve fixing trays, the number of the trays is 119, a feed inlet is positioned on the 54 th tray, and a lateral line extraction outlet is positioned on the 10 th tray.
The light component removing section 2 is a rectifying section with 9 tower plates, is added at the top of the butyraldehyde isomeride tower 1, and adopts a solid valve tower tray.
The fixed valve tower plate is a semi-elliptical valve body formed by directly stamping a tower plate structural material, and has the characteristics of being beneficial to reducing the liquid level gradient of liquid, reducing the liquid back-mixing on the tower plate and enhancing the mass transfer efficiency.
According to the process flow, the operating conditions of the butyraldehyde isomer tower are as follows: the pressure at the top of the tower is 0.12-0.20 MPa, the temperature at the side line extraction is 72-84 ℃, the temperature at the top of the tower is controlled at 66-75 ℃, the temperature at the bottom of the tower is controlled at 97-109 ℃, and the reflux ratio is controlled at 40-42.
Examples 1 to 5
Isobutyraldehyde was extracted according to the above process, with the butyraldehyde isomerate column feed composition in each example as follows in table 1:
examples 1-5 butyraldehyde isomer column operating conditions were:
example 1: the pressure at the top of the tower is 0.16MPa, the temperature of the side-draw is 78.5 ℃, the temperature at the top of the tower is 70.3 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 40.1.
Example 2: the pressure at the top of the tower is 0.16MPa, the temperature at the side extraction is 78.5 ℃, the temperature at the top of the tower is 70.2 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 39.9.
Example 3: the pressure at the top of the tower is 0.16MPa, the temperature at the side extraction is 78.5 ℃, the temperature at the top of the tower is 70.3 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 40.0.
Example 4: the pressure at the top of the tower is 0.16MPa, the temperature at the side extraction is 78.5 ℃, the temperature at the top of the tower is 70.3 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 40.0.
Example 5: the pressure at the top of the tower is 0.16MPa, the temperature at the side extraction is 78.5 ℃, the temperature at the top of the tower is 70.3 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 40.0.
TABLE 1 butyraldehyde isomerate column feed composition
The isobutyraldehyde product analyzed after separation by the process of the present invention is shown in table 2 below:
TABLE 2 side-line isobutyraldehyde product analysis data
The purity of the isobutyraldehyde product after separation is high, and the purity and the impurity content of the isobutyraldehyde meet the indexes of corresponding industrial standard superior products.
Example 6
The same process flow and feed composition as in example 1 were used, with the operating conditions of the butyraldehyde isomerate column being: the pressure at the top of the tower is 0.16MPa, the temperature at the side extraction is 78.5 ℃, the temperature at the top of the tower is 70.1 ℃, the temperature at the bottom of the tower is 102.0 ℃, and the mass reflux ratio is 39.6.
The simulation is carried out by chemical simulation software Aspen Plus, the mass concentration of the isobutyraldehyde product is controlled to be 99.60%, the energy consumption of the example 6 is converted into standard oil by GB/T50441-2016, and the result is shown in Table 3.
TABLE 3 energy consumption and product yield consumed in example 6
Comparative example 1
In the comparative example, a conventional float valve tray is used for replacing a fixed valve tray, the rectification method described in example 6 is used for refining the oxo reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components, the mixed feed composition and the same product purity requirement in example 6 are adopted, and the mixed product amount is 24.85t/h.
The floating valve tray is characterized in that a valve plate capable of moving up and down is arranged at each sieve pore, when the air speed of the sieve pores is too high, the valve plate is jacked up and ascended, when the pore speed is low, the valve plate descends due to self weight, and the lifting position of the valve plate is automatically adjusted along with the air quantity; the process flow of the comparative example is the same as that of example 6, all the equipment needing to be heated adopts steam for heating, and all the equipment needing to be cooled adopts condensed water for cooling.
The results of the simulation of example 6 and comparative example 1 by the chemical simulation software Aspen Plus and the conversion of energy consumption by GB/T50441-2016, the conversion of energy consumption of example 6 and comparative example 1 to standard oil, and the comparison of the isobutyraldehyde product concentrations of example 6 and comparative example 1 are shown in table 4.
Table 4 comparative table of energy consumption consumed by the distillation process of example 6 and comparative example 1
As can be seen from Table 4, the mixed butyraldehyde separation process for the direct rectification of the butyraldehyde isomerate tower with the added light component removal section has the advantages that when a oxo-synthesis reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components is treated, the isobutyraldehyde product has high purity and the energy-saving effect is good. Compared with the floating valve tray used in the comparative example 1, the concentration of the isobutyraldehyde product is qualified, the purity of the isobutyraldehyde superior product in the industrial standard HG/T4965-2016 is higher than 99.2wt%, and the energy is saved by about 6%.
Comparative example 2
In the comparative example, the conventional rectification method of removing light components and separating n-isobutyraldehyde first and then refining the oxo reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components is adopted, the mixed feed composition and the same product purity requirement in the example 6 are adopted, and the mixed product amount is 24.85t/h.
The existing conventional mixed butyraldehyde separation process flow is as follows: the mixed product enters the middle part of a light component removal tower, the tower top pressure of the light component removal tower is 0.38MPaG, the tower top temperature is 86.5 ℃, the tower bottom pressure is 0.41MPaG, the tower kettle temperature is 130.0 ℃, the mass reflux ratio is 6.0, the rectification is carried out, the tower top gas phase is condensed into a gas-liquid phase mixture through a condenser, the gas-liquid phase mixture enters a reflux tank, the gas-phase light component product is extracted from the top of the tank, the liquid phase returns to the rectifying tower through a reflux pump, the normal-iso-butyraldehyde mixture without light components enters the middle part of a butyraldehyde isomerate tower through a light component removal tower kettle liquid pump, the tower top pressure of the butyraldehyde isomerate tower is 0.60MPaG, the tower top temperature is 80.0 ℃, the tower bottom pressure is 0.64MPaG, the tower bottom temperature is 101.0 ℃, the mass reflux ratio is 30, the rectification is carried out, the tower top gas phase is condensed into a gas-liquid phase mixture through the condenser, the reflux tank enters the reflux tank, a condensed liquid phase passes through a reflux pump, a part of isobutyraldehyde is extracted as an iso-isobutyraldehyde product, a part of isobutyraldehyde product, a part returns to the rectifying tower as a reflux liquid, a part returns to the rectifying tower as a reflux liquid, and a heavy component mixture from the rectifying tower is extracted from the heavy component removal tower; all the equipment needing to be heated are heated by adopting steam, and all the equipment needing to be cooled are cooled by adopting condensed water.
Comparative example 3
The rectification method in patent CN112299979A is adopted to refine the oxo-synthesis reaction products of light components, iso-butyraldehyde, n-butyraldehyde and heavy components, the mixed feed composition and the same product purity requirement in example 6 are adopted, and the mixed product amount is 24.85t/h; the process parameters were simulated exactly according to the data disclosed in example 1 of patent CN112299979 a.
The temperature of the bottom of the isobutyraldehyde rectifying tower is controlled at 103.0 ℃, the temperature of the top of the tower is controlled at 75.9 ℃, the pressure of the top of the tower is 0.15MPa, and the temperature of the lateral line is 77.5 ℃ to obtain the isobutyraldehyde product.
The tower temperature of a butyraldehyde isomer rectifying tower is controlled at 106.0 ℃, the tower top temperature is controlled at 81.5 ℃, the tower top pressure is 0.15MPa, and the reflux ratio is controlled at 3.0:1.
example 6 and comparative examples 2 to 3 were each calculated in terms of isobutyraldehyde yield of 99% and purity of 99.6%, simulated by chemical simulation software Aspen Plus, and energy consumption converted by GB/T50441-2016 to convert the energy consumption of example 6 and comparative examples 2 to 3 to standard oils for comparison, and the results are shown in Table 5.
TABLE 5 comparison of energy consumption consumed by the rectification Processes of example 6 and comparative examples 2-3
As can be seen from Table 5, the mixed butyraldehyde separation process for the direct rectification of the butyraldehyde isomerate column with the added light component removal section has the obvious energy-saving characteristic when treating a oxo-synthesis reaction product containing light components, isobutyraldehyde, n-butyraldehyde and heavy components. Compared with the conventional rectification method for removing light components and separating normal and iso-butyraldehyde firstly and then in the comparative example 2, the energy consumption of the device is reduced by about 19 percent, 10 tower plates are added to a butyraldehyde isomeride tower, but equipment such as one rectification tower, two heat exchangers, one pump and the like is reduced, and the equipment investment is saved; compared with the rectification method of the prior patent CN112299979A, the energy consumption is reduced by about 42 percent.
Claims (8)
1. A separation process of mixed butyraldehyde, which is characterized in that: and (2) a reaction product of the oxo reactor enters the middle part of a butyraldehyde isomer tower (1) through a feed inlet after being subjected to catalyst separation and compression, wherein the light component in the reaction product is less than or equal to 4wt%, the ratio of n-isobutyraldehyde is 10-13, the light component is extracted from the top of a light component removal section (2) at the top of the tower, isobutyraldehyde is extracted from the lateral line at the upper part of the tower, and a n-butyraldehyde mixture is extracted from the bottom of the tower.
2. The process according to claim 1, wherein the mixed butyraldehyde separation process comprises: the top of the butyraldehyde isomery tower (1) is provided with a light component removing section (2), a light component outlet at the top of the light component removing section (2) is sequentially connected with a condenser (3), a reflux tank (4) and a reflux pump (5) through pipelines, the reflux pump (5) is connected with a reflux port of the butyraldehyde isomery tower (1), a light component product extraction line (7) is arranged at the top of the reflux tank (4), an isobutyraldehyde product extraction line (8) is arranged at the upper part of the butyraldehyde isomery tower (1), a reboiler (6) is connected with the bottom of the butyraldehyde isomery tower (1), and a n-butyraldehyde mixture extraction line (9) is arranged at the bottom of the butyraldehyde isomery tower (1).
3. The process according to claim 1, wherein the mixed butyraldehyde separation process comprises: the butyraldehyde isomerate tower (1) is a plate-type rectifying tower, and adopts a fixed valve tray, the number of the trays is 119, a feed inlet is positioned on the 54 th tray, and a side draw outlet is positioned on the 10 th tray.
4. The process according to claim 1, wherein the mixed butyraldehyde separation process comprises: the light component removing section (2) is a rectifying section with 9 tower plates and adopts a fixed valve tower tray.
5. The process according to claim 3 or 4, wherein the mixed butyraldehyde separation process comprises: the valve fixing tray is a semi-elliptical valve body formed by directly stamping a tray plate structural material.
6. The process according to claim 1, wherein the mixed butyraldehyde separation process comprises: the operating conditions of the butyraldehyde isomerate tower (1) are as follows: the pressure at the top of the tower is 0.12-0.20 MPa; the lateral extraction temperature is 72-84 ℃, the top temperature is controlled at 66-75 ℃, the temperature of the tower bottom is controlled at 97-109 ℃, and the reflux ratio is controlled at 40-42.
7. The process according to claim 6, wherein the mixed butyraldehyde separation process comprises: the operating conditions of the butyraldehyde isomerate tower (1) are as follows: the pressure at the top of the tower is 0.16MPa; the side line extraction temperature is 78-79 ℃, the top temperature is controlled at 69-71 ℃, and the bottom temperature is controlled at 100-103 ℃.
8. The process according to claim 1, wherein the mixed butyraldehyde separation process comprises: the top product of the butyraldehyde isomer column (1) comprises water, carbon dioxide, propylene and propane, the side draw product comprises isobutyraldehyde, and the bottom product comprises n-butyraldehyde, isobutanol and n-butanol.
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| CN102580337A (en) * | 2012-01-19 | 2012-07-18 | 天津大学 | Mixed butyraldehyde separation device and application of packed towers |
| CN111302922A (en) * | 2020-03-27 | 2020-06-19 | 北京诺维新材科技有限公司 | Rectification separation method and rectification system |
| CN112299979A (en) * | 2020-11-27 | 2021-02-02 | 南京诚志清洁能源有限公司 | Method for extracting isobutyraldehyde |
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| CN102580337A (en) * | 2012-01-19 | 2012-07-18 | 天津大学 | Mixed butyraldehyde separation device and application of packed towers |
| CN111302922A (en) * | 2020-03-27 | 2020-06-19 | 北京诺维新材科技有限公司 | Rectification separation method and rectification system |
| CN112299979A (en) * | 2020-11-27 | 2021-02-02 | 南京诚志清洁能源有限公司 | Method for extracting isobutyraldehyde |
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