CN101367050A - Safe and environment friendly method and equipment for improving dehydrogenation catalyst preparation - Google Patents
Safe and environment friendly method and equipment for improving dehydrogenation catalyst preparation Download PDFInfo
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- CN101367050A CN101367050A CNA2007101203200A CN200710120320A CN101367050A CN 101367050 A CN101367050 A CN 101367050A CN A2007101203200 A CNA2007101203200 A CN A2007101203200A CN 200710120320 A CN200710120320 A CN 200710120320A CN 101367050 A CN101367050 A CN 101367050A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to a method and a device for improving the safety and environment protection in the preparation process of a benzene hydrogenation catalyst. The method comprises the following steps: a signal of temperature inside a reactor is acquired and fed back to a temperature control circuit which instructs a micropressure and overpressure solenoid valve to control the flow of cooling water so as to control the temperature inside the reactor; a signal of pressure inside the reactor is acquired and fed back to a pressure control circuit which instructs a micropressure and overpressure solenoid valve to open to discharge the overpressure cyclohexane gas into a heat exchanger, and the condensed cyclohexane gas is recovered for use. The temperature for the complexation reaction of benzene hydrogenation homogeneous catalyst is accurate to +-2 DEG C from +-10 DEG C. The pressure fluctuation is accurate to +-0.02Mpa from +-0.08Mpa. Particularly, the overpressure cyclohexane gas can be discharged into a recovery system automatically, so environment pollution is avoided.
Description
Technical field
The present invention relates to a kind of method and apparatus that improves Safety and Environmental Protection in the benzene homogeneous hydrogenation catalyst preparation process.
Background technology
Before the present invention, the patent No. is in 88105065 the technology, selecting the compound of metallic nickel for use when the preparation benzene hydrogenating homogeneous catalyst is major catalyst, trialkyl aluminium is co-catalyst, weak organic acid is the 3rd component, NaOH is the process intermediate feed, and its technical process mainly is divided into two steps: the complex reaction of half-finished salt-forming reaction and finished catalyst.In the complexing technical process, the cyclohexane solution of semi-finished product isooctyl acid nickel and trialkyl aluminium generation complex reaction, the complex compound that is generated is added aging agent and is made HC-402-2 type benzene hydrogenating homogeneous catalyst.Reaction temperature during the preparation catalyst is 0~200 ℃, cyclohexane is respectively 50 ℃, 100 ℃, 150 ℃ vapour pressure: 0.0352Mpa, 0.1547Mpa, 0.5625Mpa, technology in the past is that employing logical cooling water in the chuck of reactor comes decrease temperature and pressure, a manual purge valve also is installed on reactor, if the increased water flow amount does not make reaction pressure descend yet, then open the vapour pressure that purge valve emptying cyclohexane produces, such method of operating reaction pressure control is unstable, also bring accident potential, the cyclohexane of discharging is contaminated environment again.
Summary of the invention
The objective of the invention is to adopt collection reactor temperature parameter to regulate cooling water magnetic valve discharge and control reactor temperature, cyclohexane gas for unusual superpressure is then discharged by minute-pressure superpressure magnetic valve, and imports in condenser and the receiving tank by pipeline.
The present invention program gathers the reactor temperature signal, feed back to temperature control loop, by temperature control loop instruction minute-pressure superpressure solenoid control cooling water flow control reactor temperature, gather the reactor pressure signal, feed back to pressure control loop, open jumping by pressure control loop instruction minute-pressure superpressure magnetic valve, discharge the interior superpressure cyclohexane gas of reactor and enter heat exchanger, utilize again after the condensed cyclohexane liquids recovery.
The inventive method realizes by following process equipment: a pressure gauge and a thermometer are installed in the top at complex reaction still 1, one end of pressure gauge and thermometer is connected with complex reaction still 1, the other end is connected with the switch of minute-pressure superpressure magnetic valve 4, one end of minute-pressure superpressure magnetic valve 4 connects complex reaction still 1, the other end is connected with heat exchanger 2, and heat exchanger 2 is connected with cyclohexane recycling can 3 with cooling water respectively.
Good effect of the present invention is: the control of the complex reaction temperature of benzene hydrogenating homogeneous catalyst by original ± 10 ℃ be accurate to ± 2 ℃, pressure oscillation is accurate to ± 0.02Mpa by original ± 0.08Mpa, and particularly superpressure cyclohexane gas can enter automatically to be both in the recovery system and avoid contaminated environment.
Description of drawings
Fig. 1 process flow diagram of the present invention.
Wherein: 1, complex reaction still 2, heat exchanger 3, cyclohexane recycling can 4, minute-pressure superpressure magnetic valve 5, thermometer 6, pressure gauge
Concrete thing mode
Embodiment 1
The present invention installs a pressure gauge 6 and a thermometer 5 at the top of complex reaction still 1, one end of pressure gauge 6 and thermometer 5 is connected with complex reaction still 1, the other end is connected with the switch of minute-pressure superpressure magnetic valve 4, one end of minute-pressure superpressure magnetic valve 4 connects complex reaction still 1, the other end is connected with heat exchanger 2, and heat exchanger 2 is connected with cyclohexane recycling can 3 with cooling water respectively.
Minute-pressure superpressure magnetic valve: DF1-2 220V type.
Adopt batch process to produce HC-402-2 type benzene hydrogenating homogeneous catalyst, the cyclohexane solution of semi-finished product isooctyl acid nickel and triethyl aluminum generation complex reaction, reaction temperature is controlled at 45 ± 2 ℃, the take-off value of DF1-2 220V type minute-pressure superpressure magnetic valve is set at 0.03 ± 0.005Mpa, the reactor pressure show value is 0.03Mpa, do not produce the superpressure phenomenon in the reactor, the adjusting number of times of cooling water is one to secondary by lowering for original three to five times, and a spot of cyclohexane gas enters recovery system by minute-pressure superpressure magnetic valve.Process equipment is with embodiment 1.
Embodiment 3
Adopt batch process to produce HC-402-2 type benzene hydrogenating homogeneous catalyst, the cyclohexane solution of semi-finished product isooctyl acid nickel and triethyl aluminum generation complex reaction, reaction temperature is controlled at 50 ± 2 ℃, the take-off value of DF1-2 220V type minute-pressure superpressure magnetic valve is set at 0.035 ± 0.005Mpa, the reactor pressure show value is 0.035Mpa, do not produce the superpressure phenomenon in the reactor, the adjusting number of times of cooling water is one to secondary by lowering for original three to five times, and a spot of cyclohexane gas enters recovery system by minute-pressure superpressure magnetic valve.Process equipment is with embodiment 1.
Adopt batch process to produce HC-402-2 type benzene hydrogenating homogeneous catalyst, the cyclohexane solution of semi-finished product isooctyl acid nickel and triethyl aluminum generation complex reaction, reaction temperature is controlled at 55 ± 2 ℃, the take-off value of DF1-2 220V type minute-pressure superpressure magnetic valve is set at 0.038 ± 0.005Mpa, the reactor pressure show value is 0.038Mpa, do not produce the superpressure phenomenon in the reactor, the adjusting number of times of cooling water is one to secondary by lowering for original three to five times,, a spot of cyclohexane gas enters recovery system by minute-pressure superpressure magnetic valve.Process equipment is with embodiment 1.
Claims (2)
1. one kind is improved the method that benzene hydrogenating catalyst prepares safety and environmental protection, it is characterized in that: gather the reactor temperature signal, feed back to temperature control loop, by temperature control loop instruction minute-pressure superpressure solenoid control cooling water flow control reactor temperature, gather the reactor pressure signal, feed back to pressure control loop, open jumping by pressure control loop instruction minute-pressure superpressure magnetic valve, discharge the interior superpressure cyclohexane gas of reactor and enter heat exchanger, utilize again after the condensed cyclohexane liquids recovery.
2. a kind of equipment that benzene hydrogenating catalyst prepares safety and environmental protection that improves according to claim 1, it is characterized in that: a pressure gauge and a thermometer are installed in the top of complex reaction still 1, one end of pressure gauge and thermometer is connected with complex reaction still 1, the other end is connected with the switch of minute-pressure superpressure magnetic valve 4, one end of minute-pressure superpressure magnetic valve 4 connects complex reaction still 1, the other end is connected with heat exchanger 2, and heat exchanger 2 is connected with cyclohexane recycling can 3 with cooling water respectively.
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CNA2007101203200A CN101367050A (en) | 2007-08-16 | 2007-08-16 | Safe and environment friendly method and equipment for improving dehydrogenation catalyst preparation |
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CNA2007101203200A CN101367050A (en) | 2007-08-16 | 2007-08-16 | Safe and environment friendly method and equipment for improving dehydrogenation catalyst preparation |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107684929A (en) * | 2016-08-05 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of method for improving benzene hydrogenating homogeneous catalyst performance |
CN109745943A (en) * | 2019-02-27 | 2019-05-14 | 天津金牛电源材料有限责任公司 | Pressure security control equipment and control method in difluorophosphate preparation process |
CN110180593A (en) * | 2019-06-14 | 2019-08-30 | 昆明理工大学 | A method of improving benzene hydrogenating catalyst catalytic performance and stability |
-
2007
- 2007-08-16 CN CNA2007101203200A patent/CN101367050A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107684929A (en) * | 2016-08-05 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of method for improving benzene hydrogenating homogeneous catalyst performance |
CN107684929B (en) * | 2016-08-05 | 2020-12-22 | 中国石油化工股份有限公司 | Method for improving performance of benzene hydrogenation homogeneous catalyst |
CN109745943A (en) * | 2019-02-27 | 2019-05-14 | 天津金牛电源材料有限责任公司 | Pressure security control equipment and control method in difluorophosphate preparation process |
CN109745943B (en) * | 2019-02-27 | 2024-05-24 | 天津金牛新材料有限责任公司 | Pressure safety control equipment and control method in lithium difluorophosphate preparation process |
CN110180593A (en) * | 2019-06-14 | 2019-08-30 | 昆明理工大学 | A method of improving benzene hydrogenating catalyst catalytic performance and stability |
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Open date: 20090218 |