CN106631682B - Device and method for separating water from 2-chloro-1, 2-tetrafluoropropane - Google Patents
Device and method for separating water from 2-chloro-1, 2-tetrafluoropropane Download PDFInfo
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- CN106631682B CN106631682B CN201611268138.5A CN201611268138A CN106631682B CN 106631682 B CN106631682 B CN 106631682B CN 201611268138 A CN201611268138 A CN 201611268138A CN 106631682 B CN106631682 B CN 106631682B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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Abstract
The invention relates to a device and a method for separating water from 2-chloro-1, 2-tetrafluoropropane. The equipment and the method for separating water from 2-chloro-1, 2-tetrafluoropropane comprise a degassing tower, a phase separator and a rectifying tower, wherein a discharge hole at the bottom of the degassing tower is connected with a feed inlet at the top of the phase separator, which is arranged at the top of the phase separator, through a pipeline, and a discharge regulating valve of the degassing tower is arranged on the pipeline between the discharge hole at the bottom of the degassing tower and the feed inlet at the top of the phase separator. The equipment and the method for separating water from 2-chloro-1, 2-tetrafluoropropane solve the problems of difficult separation of water in HCFC-244bb, long subsequent molecular sieve dehydration time, short service life and the like in the prior art, ensure that the water content in the quality index of HCFC-244bb extracted from the top of a rectifying tower is less than 100ppm, facilitate the improvement of the molecular sieve dehydration efficiency, and ensure that the water content after molecular sieve drying is less than 10ppm.
Description
Technical Field
The invention relates to a device and a method for separating water from 2-chloro-1, 2-tetrafluoropropane.
Background
2-chloro-1, 2-tetrafluoropropane (HCFC-244 bb) is used as an intermediate for producing 2, 3-tetrafluoropropene, and the water content in the quality index is an important quality index, and is required to be less than 10ppm. Because the conversion rate of HCFC-244bb in the current 2, 3-tetrafluoropropene production is not high, the catalyst has high requirements on impurities, and the HCFC-244bb with large flow is required to be subjected to water alkali elution to remove impurities and acidity. The water content of HCFC-244bb is saturated after washing with water and alkali, clear water is separated out in the middle tank after compression, the light component is removed in a degassing tower, the heavy component is removed in a rectifying tower, the water is removed by a molecular sieve, and the 2, 3-tetrafluoropropene is generated in the next step after the heavy component is removed in the rectifying tower. The dehydration effect of the medium with the water content below 200ppm is better for the molecular sieve, the dehydration effect of the medium with the water content above 500ppm is less ideal, the lower the water content is, the shorter the dehydration time is, and the service life of the molecular sieve is longer. Because the HCFC-244bb has large circulation flow and short buffering time, the HCFC-244bb is difficult to be discharged in a middle tank, a degassing tower kettle and a rectifying tower kettle, the moisture content of the rectified finished product is high, the molecular sieve has long dehydration time, and the service life of the molecular sieve is short, so that the large-scale production is influenced.
Disclosure of Invention
The invention provides equipment and a method for separating water from 2-chloro-1, 2-tetrafluoropropane, which are used for effectively improving dehydration effect and solve the problems in the prior art.
The invention is realized by the following technical scheme:
the equipment for separating water from 2-chloro-1, 2-tetrafluoropropane comprises a degassing tower, a phase separator and a rectifying tower, wherein a discharging hole at the bottom of the degassing tower is connected with a feeding hole at the top of the phase separator through a pipeline, a discharging regulating valve of the degassing tower is arranged on the pipeline between the discharging hole at the bottom of the degassing tower and the feeding hole at the top of the phase separator, a thermocouple and a remote interface meter are arranged in the phase separator, a condensing jacket is arranged on the outer side of the lower part of the phase separator, a refrigerant inlet pipe is arranged at the bottom of the condensing jacket, a discharging hole at the bottom of the phase separator is connected with a rectifying tower feeding hole arranged in the middle of the rectifying tower through a pipeline, a discharging regulating valve of the phase separator is arranged on the pipeline between the discharging hole at the bottom of the phase separator and the feeding hole of the rectifying tower, and a plurality of liquid discharging pipes communicated with the phase separator are arranged on one side of the upper part of the phase separator.
A process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into a degassing tower from the middle part of the degassing tower at a flow rate of 15-20kg/h, controlling the pressure at the top of the degassing tower to be 0.3-1.6MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering the product after removing the light components in the HCFC-244bb crude product to a phase separator by pressure difference, controlling the temperature in the phase separator to be 0-80 ℃ and the pressure to be 0.2-1.4Mpa, so that the interface layering height of the moisture and the HCFC-244bb is 20-90% of the liquid level height in the phase separator;
(3) The water in the upper layer of the phase separator is discharged through a liquid discharge pipe, HCFC-244bb in the lower layer is pressed into a rectifying tower for rectification through the pressure difference at the bottom of the phase separator at the flow rate of 15-20kg/h, the pressure at the top of the rectifying tower is controlled to be 0.1-1.2MPa, and qualified HCFC-244bb is recovered from the top of the rectifying tower in a reflux way after 2h of rectification.
The beneficial effects of the invention are as follows: the equipment and the method for separating water from 2-chloro-1, 2-tetrafluoropropane solve the problems of difficult separation of water in HCFC-244bb, long subsequent molecular sieve dehydration time, short service life and the like in the prior art, ensure that the water content in the quality index of HCFC-244bb extracted from the top of a rectifying tower is less than 100ppm, facilitate the improvement of the molecular sieve dehydration efficiency, and ensure that the water content after molecular sieve drying is less than 10ppm; the pressure and temperature in the phase separator are comprehensively controlled by the pressure transmitter and the thermocouple, so that the delamination of water and 2-chloro-1, 2-tetrafluoropropane is facilitated, and the separation effect of bright water is further improved.
Drawings
The invention is further described below with reference to the accompanying drawings.
Fig. 1 is a schematic structural view of the present invention.
In the figure, 1, a degasser, 2, a phase separator, 3, a rectifying tower, 4, a discharge hole at the bottom of the degasser, 5, a feed hole at the top of the phase separator, 6, a discharge regulating valve of the degasser, 7, a thermocouple, 8, a remote interface meter, 9, a condensing jacket, 10, a refrigerant inlet pipe, 11, a discharge hole at the bottom of the phase separator, 12, a feed hole of the rectifying tower, 13, a discharge regulating valve of the phase separator, 14, a drain pipe, 15 and a pressure transmitter.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present invention will be described in detail below with reference to the following detailed description and the accompanying drawings.
As shown in FIG. 1, the device for separating water from 2-chloro-1, 2-tetrafluoropropane comprises a degasser 1, a phase separator 2 and a rectifying tower 3, wherein a degasser bottom discharge port 4 arranged at the bottom of the degasser 1 is connected with a phase separator top feed port 5 arranged at the top of the phase separator 2 through a pipeline, a degasser discharge regulating valve 6 is arranged on the pipeline between the degasser bottom discharge port 4 and the phase separator top feed port 5, a thermocouple 7 and a remote interface meter 8 are arranged in the phase separator 2, a condensing jacket 9 is arranged at the outer side of the lower part of the phase separator 2, a refrigerant inlet pipe 10 is arranged at the bottom of the condensing jacket 9, a rectifying tower feed port 12 arranged at the middle of the rectifying tower 3 is connected with the phase separator bottom discharge port 11, a phase separator discharge regulating valve 13 is arranged on the pipeline between the phase separator bottom discharge port 11 and the rectifying tower feed port 12, a plurality of discharge pipes 14 communicated with the phase separator 2 are arranged at one side of the upper part of the phase separator 2, and a pressure transmitter 15 is arranged at the top of the phase separator 2.
Example 1:
a process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into the degasser 1 from the middle part of the degasser 1 at a flow rate of 20kg/h, controlling the pressure at the top of the degasser 1 at 0.8MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering a product from which light components in HCFC-244bb crude products are removed to a phase separator 2 through pressure difference, introducing 0 ℃ frozen brine into a condensing jacket 9 of the phase separator 2, enhancing the separation effect of water and HCFC-244bb, controlling the temperature in the phase separator 2 to be 10 ℃ through controlling the valve opening of a discharge regulating valve 6 of a degassing tower and a discharge regulating valve 13 of the phase separator, controlling the pressure to be 0.6MPa through a pressure transmitter 15 and a thermocouple 7, enabling obvious layering of water and HCFC-244bb to occur, displaying a layering interface through a remote interface meter 14, enabling the layering height of the water and HCFC-244bb interface to be 50% of the liquid level height in the phase separator 2, and discharging upper water when a liquid discharge pipe 14 is used for different liquid levels;
(3) The water in the upper layer of the phase separator 2 is discharged through a liquid discharge pipe 14, HCFC-244bb in the lower layer is pressed into a rectifying tower 3 by pressure difference at the bottom of the phase separator 2 at the flow rate of 20kg/h for rectification, the pressure at the top of the rectifying tower 3 is controlled to be 0.4MPa, after 2h of rectification, qualified HCFC-244bb is extracted by reflux from the top of the rectifying tower 3, and sampling analysis is carried out.
Testing moisture by using a moisture meter through a Karl Fischer reagent, and measuring that the moisture content of HCFC-244bb at the top of the rectifying tower 3 is 78ppm; the water content of HCFC-244bb is 8ppm after molecular sieve dehydration for 2 h.
Example 2:
a process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into the degasser 1 from the middle part of the degasser 1 at a flow rate of 20kg/h, controlling the pressure at the top of the degasser 1 at 0.8MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering a product from which light components in HCFC-244bb crude products are removed to a phase separator 3 through pressure difference, introducing 0 ℃ frozen brine into a condensing jacket 9 of the phase separator 2, enhancing the separation effect of water and HCFC-244bb, controlling the pressure in the phase separator 2 to be 0.6MPa and the temperature to be 5 ℃ through controlling the valve opening of a discharge regulating valve 6 of a degassing tower and a discharge regulating valve 13 of the phase separator and controlling the pressure in the phase separator 2 to be 0.6MPa by a pressure transmitter 15 and a thermocouple 7, so that the layering height of the interface between water and HCFC-244bb is 50% of the liquid level height in the phase separator, and discharging water on the upper layer when a liquid discharge pipe 14 is used for different liquid levels;
(3) The water in the upper layer of the phase separator 2 is discharged through a liquid discharge pipe 14, HCFC-244bb in the lower layer is pressed into a rectifying tower 3 for rectification through the pressure difference at the bottom of the phase separator 2 at the flow rate of 15kg/h, the pressure at the top of the rectifying tower 2 is controlled to be 0.4MPa, after 2h of rectification, qualified HCFC-244bb is extracted by reflux from the top of the rectifying tower 3, and sampling analysis is carried out.
Testing moisture by using a moisture meter through a Karl Fischer reagent, and measuring that the moisture content of HCFC-244bb at the top of the rectifying tower 3 is 60ppm; the molecular sieve is dehydrated for 1.5 hours, and the moisture content of HCFC-244bb is 7ppm.
Example 3:
a process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into the degasser 1 from the middle part of the degasser 1 at a flow rate of 15kg/h, controlling the pressure at the top of the degasser 1 at 0.8MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering a product from which light components in HCFC-244bb crude products are removed to a phase separator 2 through pressure difference, introducing 0 ℃ frozen brine into a condensing jacket 9 of the phase separator 2, enhancing the separation effect of water and HCFC-244bb, controlling the temperature in the phase separator 2 to be 5 ℃ through controlling the valve opening of a discharge regulating valve 6 of a degassing tower and a discharge regulating valve 13 of the phase separator, controlling the pressure to be 0.6MPa through a pressure transmitter 15 and a thermocouple 7, and enabling the layering height of the interface between water and HCFC-244bb to be 50% of the liquid level height in the phase separator, wherein a liquid discharge pipe 14 is used for discharging upper water when different liquid levels are obtained;
(3) The water in the upper layer of the phase separator 2 is discharged through a liquid discharge pipe 14, HCFC-244bb in the lower layer is pressed into a rectifying tower 3 for rectification through the pressure difference at the bottom of the phase separator 2 at the flow rate of 15kg/h, the pressure at the top of the rectifying tower 3 is controlled to be 0.4MPa, after 2h of rectification, qualified HCFC-244bb is extracted by reflux from the top of the rectifying tower 3, and sampling analysis is carried out.
Testing moisture by using a moisture meter through a Karl Fischer reagent, and measuring that the moisture content of HCFC-244bb at the top of the rectifying tower 3 is 56ppm; the water content of HCFC-244bb was 6ppm by molecular sieve dehydration for 1.5 h.
Example 4:
a process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into the degasser 1 from the middle part of the degasser 1 at a flow rate of 20kg/h, controlling the pressure at the top of the degasser 1 at 0.3MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering a product from which light components in HCFC-244bb crude products are removed to a phase separator 3 through pressure difference, introducing 0 ℃ frozen brine into a condensing jacket 9 of the phase separator 2, enhancing the separation effect of water and HCFC-244bb, controlling the pressure in the phase separator 2 to be 0.2MPa through controlling the valve opening of a discharge regulating valve 6 of a degassing tower and a discharge regulating valve 13 of the phase separator and controlling the pressure transmitter 15 and a thermocouple 7 to be 80 ℃ so that the layering height of the interface between water and HCFC-244bb is 20% of the liquid level height in the phase separator, and discharging water on the upper layer when a liquid discharge pipe 14 is used for different liquid levels;
(3) The water in the upper layer of the phase separator 2 is discharged through a liquid discharge pipe 14, HCFC-244bb in the lower layer is pressed into a rectifying tower 3 for rectification through the pressure difference at the bottom of the phase separator 2 at the flow rate of 15kg/h, the pressure at the top of the rectifying tower 2 is controlled to be 0.1MPa, after 2h of rectification, qualified HCFC-244bb is extracted by reflux from the top of the rectifying tower 3, and sampling analysis is carried out.
Testing moisture by using a moisture meter through a Karl Fischer reagent, and measuring that the moisture content of HCFC-244bb at the top of the rectifying tower 3 is 80ppm; the water content of HCFC-244bb was 9ppm by molecular sieve dehydration for 1.5 h.
Example 5:
a process for separating water from 2-chloro-1, 2-tetrafluoropropane comprising the steps of:
(1) Adding the HCFC-244bb crude product rich in water into the degasser 1 from the middle part of the degasser 1 at a flow rate of 20kg/h, controlling the pressure at the top of the degasser 1 at 1.6MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering a product from which light components in HCFC-244bb crude products are removed to a phase separator 3 through pressure difference, introducing 0 ℃ frozen brine into a condensing jacket 9 of the phase separator 2, enhancing the separation effect of water and HCFC-244bb, controlling the pressure in the phase separator 2 to be 1.4MPa by controlling the opening of a discharge regulating valve 6 of a degassing tower and a discharge regulating valve 13 of the phase separator and controlling the pressure in a pressure transmitter 15 and a thermocouple 7 to be 0 ℃ so that the layering height of the interface between water and HCFC-244bb is 90% of the liquid level height in the phase separator, and discharging upper water when a liquid discharge pipe 14 is used for different liquid levels;
(3) The water in the upper layer of the phase separator 2 is discharged through a liquid discharge pipe 14, HCFC-244bb in the lower layer is pressed into a rectifying tower 3 for rectification through the pressure difference at the bottom of the phase separator 2 at the flow rate of 15kg/h, the pressure at the top of the rectifying tower 2 is controlled to be 1.2MPa, after 2h of rectification, qualified HCFC-244bb is extracted by reflux from the top of the rectifying tower 3, and sampling analysis is carried out.
Testing moisture by using a moisture meter through a Karl Fischer reagent, and measuring that the moisture content of HCFC-244bb at the top of the rectifying tower 3 is 79ppm; the water content of HCFC-244bb was 9ppm by molecular sieve dehydration for 1.5 h.
The present invention is not described in detail in the present application, and is well known to those skilled in the art. Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (1)
1. A process for separating water from 2-chloro-1, 2-tetrafluoropropane, characterized by: the method comprises the following steps:
(1) Adding the HCFC-244bb crude product rich in water into a degassing tower from the middle part of the degassing tower at a flow rate of 15-20kg/h, controlling the pressure at the top of the degassing tower to be 0.8MPa, and removing light components in the HCFC-244bb crude product;
(2) Delivering the product after removing the light components in the HCFC-244bb crude product to a phase separator by pressure difference, controlling the temperature in the phase separator to be 5 ℃ or 10 ℃ and the pressure to be 0.6Mpa, so that the interface layering height of the moisture and the HCFC-244bb is 50% of the liquid level height in the phase separator;
(3) Discharging water at the upper layer of the phase separator through a liquid discharge pipe, pressing HCFC-244bb at the lower layer into a rectifying tower from the bottom of the phase separator through pressure difference at a flow rate of 15-20kg/h for rectifying, controlling the top pressure of the rectifying tower to be 0.4MPa, rectifying for 2h, and then reflux-extracting qualified HCFC-244bb from the top of the rectifying tower; the water content in HCFC-244bb extracted from the top of the rectifying tower is less than 100ppm and the water content after molecular sieve drying is not more than 8ppm;
the equipment for separating water from 2-chloro-1, 2-tetrafluoropropane comprises a degassing tower, a phase separator and a rectifying tower, wherein a discharging hole at the bottom of the degassing tower is connected with a feeding hole at the top of the phase separator through a pipeline, a discharging regulating valve of the degassing tower is arranged on the pipeline between the discharging hole at the bottom of the degassing tower and the feeding hole at the top of the phase separator, a thermocouple and a remote transmission interface meter are arranged in the phase separator, a condensing jacket is arranged on the outer side of the lower part of the phase separator, a refrigerant inlet pipe is arranged at the bottom of the condensing jacket, a discharging hole at the bottom of the phase separator is connected with a rectifying tower feeding hole at the middle part of the rectifying tower through a pipeline, a discharging regulating valve of the phase separator is arranged on the pipeline between the discharging hole at the bottom of the phase separator and the feeding hole of the rectifying tower, and a plurality of liquid discharging pipes communicated with the phase separator are arranged on one side of the upper part of the phase separator.
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| CN201611268138.5A CN106631682B (en) | 2016-12-31 | 2016-12-31 | Device and method for separating water from 2-chloro-1, 2-tetrafluoropropane |
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| WO2020029053A1 (en) * | 2018-08-07 | 2020-02-13 | 南通百川新材料有限公司 | Method for recovering n-methylpyrrolidone from lithium ion battery |
| CA3157432A1 (en) * | 2019-11-06 | 2021-05-14 | Honeywell International Inc. | Azeotrope or azeotrope-like compositions of 2-chloro-1,1,1,2-tetrafluoropropane (hcfc-244bb) and water |
| CN111170906B (en) * | 2020-02-25 | 2022-07-12 | 北京凯瑞英科技有限公司 | Molecular sieve dehydration system for dimethyl sulfoxide and dehydration method thereof |
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| CN203002028U (en) * | 2012-12-18 | 2013-06-19 | 泰兴市梅兰化工有限公司 | Novel phase separator for removing water in difluoromono chloroethane |
| CN103328423A (en) * | 2010-11-16 | 2013-09-25 | 霍尼韦尔国际公司 | Process for producing 2,3,3,3-tetrafluoropropene |
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| CN206494865U (en) * | 2016-12-31 | 2017-09-15 | 山东华安新材料有限公司 | The equipment of separation water in a kind of tetrafluoropropane from 2 chlorine 1,1,1,2 |
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| CN103328423A (en) * | 2010-11-16 | 2013-09-25 | 霍尼韦尔国际公司 | Process for producing 2,3,3,3-tetrafluoropropene |
| CN203002028U (en) * | 2012-12-18 | 2013-06-19 | 泰兴市梅兰化工有限公司 | Novel phase separator for removing water in difluoromono chloroethane |
| CN103626626A (en) * | 2013-11-01 | 2014-03-12 | 西安近代化学研究所 | Separating method of mixture of hydrogen fluoride and 2-chlorine-1,1,1,2-tetrafluoropropane |
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