CN106669279B - Filtering equipment for realizing catalyst separation in polytetramethylene glycol production - Google Patents
Filtering equipment for realizing catalyst separation in polytetramethylene glycol production Download PDFInfo
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- CN106669279B CN106669279B CN201710070906.4A CN201710070906A CN106669279B CN 106669279 B CN106669279 B CN 106669279B CN 201710070906 A CN201710070906 A CN 201710070906A CN 106669279 B CN106669279 B CN 106669279B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D36/04—Combinations of filters with settling tanks
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Abstract
The invention belongs to the technical field of chemical production equipment, and relates to a filtering device for separating a catalyst in polytetramethylene riddle glycol production, which comprises an upper barrel and a lower barrel which are connected in a sealing manner, wherein a tube plate is fixedly connected with the inner wall of the lower barrel, the upper surface of the tube plate is fixedly connected with a filter element, a first polytetrafluoroethylene gasket is arranged between the filter element and the tube plate, the upper part of the filter element is provided with a pressing plate, a plurality of screws extending vertically and upwards are fixed on the tube plate, the upper ends of the screws penetrate through corresponding through holes in the pressing plate, springs are sleeved at the upper ends of the screws, the lower ends of the springs are tightly pressed on the upper surface of the pressing plate, and the upper ends of the springs are tightly pressed on the bottom surfaces of nuts on the screws. The filter equipment works stably, and the service efficiency of the filter element is greatly improved.
Description
Technical Field
The invention belongs to the technical field of chemical production equipment, and relates to a filtering device for realizing catalyst separation in polytetramethylene glycol production.
Background
The filtering process of the filter achieves the purpose of filtering according to different molecular diameters of components in two or more mixed liquids. It is a common unit operation for filtering liquid mixture, has wide application in chemical, biological fermentation and pharmacy, can extract and enrich product, and can filter out part of other similar substances, so as to primarily purify the product, such as filtering yeast and by-products in beer production, and filtering phenolic substances in sewage. Meanwhile, high-value substances are recycled as far as possible, and the production running cost is effectively reduced, such as filtration of the heteropoly acid catalyst in PTMEG (polytetramethylene ether glycol) production and the like.
The prior PTMEG production catalyst separation equipment has the following defects: materials enter from the upper barrel of the device and enter and exit from the outside of the filter element, clear liquid is finally extracted from the lower barrel, heavy liquid is extracted from the upper barrel, in the operation process, the catalyst can be deposited on the tube plate and gradually solidified, and the solidified catalyst tightly wraps the filter element to cause the partial failure of the filter element; the joint of the filter element and the tube plate is generally sealed simply by adopting an O-shaped ring, and the catalyst leaks from the sealing part under certain pressure and enters into clear liquid, so that the catalyst is filtered and fails; after the filter is fed, the filter element is heated and bent by the high-temperature material, so that the filter membrane is damaged, and the catalyst passes through the filter element and enters into clear liquid; the catalyst in the clear liquid enters a PTMG (polytetramethylene glycol) product to promote the PTMG to generate thermal decomposition; the filter element is gradually blocked in the filtering process, the pressure difference is increased, the filter element needs to be replaced, and the filter element replacement period is frequent.
The existing equipment needs frequent on-site valve adjustment, and is frequently opened for internal cleaning to remove the solidified catalyst at the bottom, so that the catalyst is greatly wasted, time and labor are wasted, the environment is polluted, and certain safety risk exists;
the existing filter factory generally selects three devices to just reluctantly maintain the continuous production of the device, and certain investment is large.
The catalyst content in the clear liquid filtered by the existing filter is unstable, and the average content is about 70 ppm. The existing filter not only wastes a large amount of expensive catalyst, but also increases the difficulty of subsequent working sections in treating the catalyst, and the catalyst can enter PTMEG to cause thermal decomposition of products, so that the stability of a PTMEG production device and the improvement of the quality of the products are always restricted for a long time.
Disclosure of Invention
Aiming at the problems, the invention provides the filter equipment for separating the catalyst in the polytetramethylene riddle glycol production, and the filter equipment is stable in operation and greatly improves the use efficiency of the filter element.
According to the technical scheme of the invention: a filter equipment for realizing catalyst separation in polytetramethylene glycol production is characterized in that: the device comprises an upper barrel and a lower barrel which are connected in a sealing way, a tube plate is fixedly connected with the inner wall of the lower barrel, the upper surface of the tube plate is fixedly connected with a filter element, a first polytetrafluoroethylene gasket is arranged between the filter element and the tube plate, the upper part of the filter element is provided with a pressing plate, the tube plate is fixedly provided with a plurality of vertically and upwardly extending screw rods, the upper ends of the screw rods penetrate out from corresponding through holes on the pressing plate, springs are sleeved at the upper ends of the screw rods, the lower ends of the springs are tightly pressed on the upper surface of the pressing plate, the upper ends of the springs are tightly propped against the bottom surface of a nut on the screw rods, an annular distributor is arranged in the lower barrel and corresponds to the lower part of the tube plate, discharge holes of the distributor are inclined downwards and face to the inner wall of the lower barrel, a feed inlet of the distributor is connected with a feed pipeline, a first mass flow meter, a static mixer, a feed valve and a feed check valve are sequentially arranged on the feed pipeline along the material flowing direction, a collector is arranged below the distributor, a discharge hole of the collector is arranged above an outlet of the lower barrel, the outlet of the lower cylinder is fixedly connected with a second flange; the top of the upper cylinder body is provided with a backwashing feeding valve, a pressure gauge and a clear liquid discharging port, and a discharging valve and a sampling valve are arranged on a pipeline of the clear liquid discharging port; an emptying valve is arranged on the side wall of the lower cylinder body corresponding to the lower position of the tube plate, and the bottom of the lower cylinder body is connected with a delayer matched with the collector.
As a further improvement of the invention, the external thread joint of the filter element is matched and connected with an internal thread hole on the tube plate, and the first polytetrafluoroethylene gasket is arranged in the internal thread hole of the tube plate.
As a further improvement of the invention, the upper cylinder and the lower cylinder are tightly connected through a first flange.
As a further improvement of the invention, a second polytetrafluoroethylene gasket is arranged between the upper cylinder and the lower cylinder.
As a further development of the invention, the distributor has a larger diameter than the collector.
As a further improvement of the invention, steel linings are arranged inside and outside the filter element.
As a further improvement of the invention, the delaminating device comprises a sight glass, a backwashing discharge valve, a second mass flowmeter, a control valve and an interface meter, wherein the sight glass is arranged on the surface of the delaminating device and is used for observing the internal condition of the delaminating device, a branch pipeline, the second mass flowmeter and the control valve are sequentially arranged on a pipeline connected with a discharge port at the lower end of the delaminating device along the discharge direction, the backwashing discharge valve is arranged on the branch pipeline, a calibration probe of the interface meter is communicated with the inner cavity of the lower cylinder body, and a measurement probe of the interface meter is communicated with the inner cavity of the delaminating device.
As a further improvement of the invention, the top surface of the upper cylinder body is in a convex arc shape, and the bottom surface of the lower cylinder body is in a convex arc shape.
The invention has the technical effects that: the materials entering the filter are fully mixed in the static mixer and are dispersed in all directions by the distributor in the lower cylinder, so that the impact on the filter element can be effectively reduced, and the influence on the catalyst sedimentation can be reduced to the minimum extent. The material enters from the inside of the filter element and flows out from the outside, the catalyst is gradually concentrated in the internal channel of the filter element, and the catalyst naturally falls down by depending on gravity when reaching a certain concentration. The catalyst collector can collect the catalyst and guide the catalyst to the catalyst delayer, and meanwhile, the collector can prevent the influence of the disturbance of the liquid of the lower cylinder body on the catalyst to ensure the effective sedimentation and collection of the catalyst. The inner wall and the outer wall of the filter element are protected by steel mesh packages, so that the filter element can cope with the thermal deformation of high-temperature materials and can bear certain material pressure drop, the influence of the change of the temperature of the pressure plate and the upper spring with certain weight on the filter element can be automatically adjusted, and the stable operation of the change of the environment of the filter element is ensured. Moreover, an interface meter and a control valve are arranged on the catalyst delayer, so that the interface of the catalyst is stably controlled, the accompanying discharge of other materials is effectively reduced, and the operating efficiency of membrane filtration is greatly improved; the catalyst blanking control valve and the feed flowmeter are provided with a safety interlock, and when feeding is suddenly stopped in production operation, the catalyst control valve is immediately closed, so that the influence on next use caused by the fact that material flow in the filter is not emptied is prevented. When the pressure of the filter reaches 80KPa, the normal working pressure difference can be recovered by simply backwashing on site by using clear liquid materials.
In conclusion, the filter element can effectively ensure the service life of the filter element, the unique filter element and the installation design can avoid the filter element from being blocked by the solidified catalyst, and meanwhile, the filter element backwashing function is realized, and the use efficiency of the filter element is greatly improved. The collected catalyst can be automatically discharged after sedimentation and layering, and manual repeated adjustment on site is not needed. The final clear liquid catalyst is reduced by 4-7 times compared with the existing filtering equipment. The invention of the catalyst filter device thoroughly changes the design of the prior filter device, is simple and reasonable, convenient to operate, safe and continuous, and has outstanding effect
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings.
In fig. 1, the apparatus includes a first mass flow meter 1, a static mixer 2, a feed valve 3, a feed check valve 4, a tube plate 5, a second teflon gasket 6, an upper cylinder 7, a spring 8, a backwash feed valve 9, a pressure gauge 10, a discharge valve 11, a sampling valve 12, a pressure plate 13, a filter element 14, an external screw joint 15, a first teflon gasket 16, a first flange 17, an evacuation valve 18, a distributor 19, a lower cylinder 20, an interface meter 21, a second flange 22, a control valve 23, a collector 24, a delayer 25, a sight glass 26, a backwash discharge valve 27, a second mass flow meter 28, and the like.
As shown in figure 1, the invention is a filtering device for realizing the separation of catalyst in the production of polytetramethylene riddle glycol, which comprises an upper barrel 7 and a lower barrel 20 which are connected in a sealing way, a tube plate 5 is fixedly connected with the inner wall of the lower barrel 20, the upper surface of the tube plate 5 is fixedly connected with a filter element 14, a first polytetrafluoroethylene gasket 16 is arranged between the filter element 14 and the tube plate 5, the upper part of the filter element 14 is provided with a pressing plate 13, the tube plate 5 is fixedly provided with a plurality of screws which extend vertically and upwards, the upper ends of the screws penetrate through corresponding through holes on the pressing plate 13, the upper ends of the screws are sleeved with springs 8, the lower ends of the springs 8 are tightly pressed on the upper surface of the pressing plate 13, the upper ends of the springs 8 are tightly pressed on the bottom surface of nuts on the screws, an annular distributor 19 is arranged in the lower barrel 20 corresponding to the lower part of the tube plate 5, discharge holes of the distributor 19 are inclined downwards and face to the inner wall of the lower barrel 20, a feed inlet of the distributor 19 is connected with a feed pipe, a first mass flowmeter 1, a static mixer 2, a feeding valve 3 and a feeding check valve 4 are sequentially arranged on the feeding pipeline along the material flowing direction, a collector 24 is arranged below the distributor 19, a discharge hole of the collector 24 is arranged above an outlet of the lower barrel 20, and the outlet of the lower barrel 20 is fixedly connected with a second flange 22; the top of the upper cylinder 7 is provided with a backwashing feeding valve 9, a pressure gauge 10 and a clear liquid discharging port, and a discharging valve 11 and a sampling valve 12 are arranged on a pipeline of the clear liquid discharging port; the side wall of the lower cylinder 20 is provided with an emptying valve 18 corresponding to the lower position of the tube plate 5, and the bottom of the lower cylinder 20 is connected with a delayer 25 matched with a collector 24.
The external thread connector 15 of the filter element 14 is matched and connected with an internal thread hole on the tube plate 5, and the first polytetrafluoroethylene gasket 16 is arranged in the internal thread hole of the tube plate 5.
The upper cylinder 7 is tightly connected with the lower cylinder 20 through a first flange 17.
A second polytetrafluoroethylene gasket 6 is arranged between the upper cylinder 7 and the lower cylinder 20.
The distributor 19 has a larger diameter than the collector 24.
The filter element 14 is internally and externally provided with steel linings.
The delayer 25 comprises a sight glass 26, a backwashing discharge valve 27, a second mass flowmeter 28, a control valve 23 and an interface meter 21, wherein the sight glass 26 is arranged on the surface of the delayer 25 and is used for observing the internal condition of the delayer 25, a branch pipeline, a second flowmeter 28 and the control valve 23 are sequentially arranged on a pipeline connected with a discharge port at the lower end of the delayer 25 along the discharge direction, the backwashing discharge valve 27 is arranged on the branch pipeline, a calibration probe of the interface meter 21 is communicated with the inner cavity of the lower barrel 20, and a measurement probe of the interface meter 21 is communicated with the inner cavity of the delayer 25.
The top surface of the upper cylinder 7 is in a convex arc shape, and the bottom surface of the lower cylinder 20 is in a convex arc shape.
The use of the invention for the filtration of heteropolyacids from tetrahydrofuran polymer reactants is further illustrated below.
The ring opening polymerization of tetrahydrofuran is the basic polymerization reaction for producing polytetrahydrofuran, and heteropoly acid is selected as the catalyst in the polymerization reaction. In the continuous polymerization reaction, about 1.2% of the catalyst remains in the polymerization product, 72% of the unreacted tetrahydrofuran and 27.8% of the polytetrahydrofuran remain in the polymerization product, and the catalyst needs to be removed and recovered by filtration or the like. The heteropoly acid has high density and high viscosity, and under the condition of n-pentane serving as an extracting agent, the heteropoly acid in the material reaches a certain concentration, is saturated and gradually settles to cause layering. The heteropoly acid content in the mixed material is about 2000 ppm.
The polymerization reaction product which is mixed in the first step enters a catalyst filter through a first mass flow meter 1, and at the moment, a backwashing feeding valve 9 at the top of an upper cylinder 7 is opened to exhaust until the filter is filled.
The materials are metered by the first mass flow 1 and then enter the static mixer 2, the materials are downwards beaten to the inner wall of the cylinder body by 30 degrees by the built-in distributor 19 in the lower cylinder body 20, the materials are uniformly dispersed and then slowly enter the internal channel of the filter element 14, the catalyst is intercepted by the filter element 14 at the moment, other materials pass through the filter element 14, and clear liquid is continuously extracted from the upper cylinder body 7 to the subsequent working section after being filtered by the filter element 14.
With the continuous entering of the material containing the catalyst, the catalyst is filtered by the filter element 14, the concentration of the catalyst in the lower cylinder 20 is higher and higher, the catalyst is gradually saturated and slowly settles under the action of gravity, the collector 24 below the distributor 19 collects most of the settled catalyst and guides the collected catalyst to the inlet of the catalyst delayer 25 at the bottom, the catalyst is delaminated in the catalyst delayer 25, and the catalyst delamination effect can be obviously observed from the sight glass 26. A small amount of catalyst that fails to collect slowly flows into the stratifier 25 along the inner wall of the lower cylinder 20. When the catalyst interface reaches the mirror neutral position, the catalyst control valve 23 and the interface meter 21 are set to automatic, and the catalyst starts to be automatically discharged.
And in the continuous extraction process of the clear liquid, opening the sampling valve 12 for sampling, and analyzing the content of the catalyst.
When the pressure difference of the filter element reaches 80KPa, backwashing operation is carried out on site.
Filter partial debug log
Comparison table with the existing filter (taking 2000kg/h liquid cleaning amount as an example)
The same clear liquid extraction amount is adopted, the content of the heteropoly acid catalyst of the existing catalyst filter outlet material is about 70ppm, and after the inventive catalyst membrane filter is adopted, the content of the heteropoly acid at the outlet is about 12ppm, which is 1/6 of the existing process.
The catalyst separation and filtration equipment in PTMEG production provided by the invention has a simple scheme, can automatically and continuously discharge the catalyst, and has unique filter element installation and catalyst collection device design. The filter has the advantages of simple whole-process operation, safe, stable and reliable operation, greatly reduced production and operation cost, better market prospect and particular suitability for PTMEG production, biological fermentation and pharmaceutical engineering.
The above description is intended to be illustrative and not restrictive, and the scope of the invention is defined by the appended claims, which may be modified in any manner within the scope of the invention.
Claims (8)
1. A filter equipment for realizing catalyst separation in polytetramethylene glycol production is characterized in that: comprises an upper barrel (7) and a lower barrel (20) which are connected in a sealing way, a tube plate (5) is fixedly connected with the inner wall of the lower barrel (20), a filter element (14) is fixedly connected with the upper surface of the tube plate (5), a first polytetrafluoroethylene gasket (16) is arranged between the filter element (14) and the tube plate (5), a pressure plate (13) is arranged at the upper part of the filter element (14), a plurality of vertically and upwardly extending screws are fixed on the tube plate (5), the upper ends of the screws penetrate out from corresponding through holes on the pressure plate (13), springs (8) are sleeved at the upper ends of the screws, the lower ends of the springs (8) are tightly pressed on the upper surface of the pressure plate (13), the upper ends of the springs (8) are tightly pressed on the bottom surface of nuts on the screws, an annular distributor (19) is arranged in the lower barrel (20) corresponding to the lower part of the tube plate (5), discharge holes of the distributor (19) are inclined downwards and face the inner wall of the lower barrel (20), and a feed inlet of the distributor (19) is connected with a feed pipeline, a first mass flow meter (1), a static mixer (2), a feeding valve (3) and a feeding check valve (4) are sequentially arranged on the feeding pipeline along the material flowing direction, a collector (24) is arranged below the distributor (19), a discharge hole of the collector (24) is arranged above the outlet of the lower cylinder (20), and the outlet of the lower cylinder (20) is fixedly connected with a second flange (22); a backwashing feeding valve (9), a pressure gauge (10) and a clear liquid discharging port are arranged at the top of the upper barrel body (7), and a discharging valve (11) and a sampling valve (12) are arranged on a pipeline of the clear liquid discharging port; an emptying valve (18) is arranged on the side wall of the lower cylinder (20) corresponding to the lower position of the tube plate (5), and the bottom of the lower cylinder (20) is connected with a delayer (25) matched with the collector (24).
2. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: the external thread connector (15) of the filter element (14) is matched and connected with an internal thread hole in the tube plate (5), and the first polytetrafluoroethylene gasket (16) is arranged in the internal thread hole in the tube plate (5).
3. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: the upper cylinder body (7) is fixedly connected with the lower cylinder body (20) through a first flange (17).
4. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: and a second polytetrafluoroethylene gasket (6) is arranged between the upper cylinder (7) and the lower cylinder (20).
5. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: the distributor (19) has a larger diameter than the collector (24).
6. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: and steel linings are arranged inside and outside the filter element (14).
7. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: the delaminating device (25) comprises a sight glass (26), a backwashing discharge valve (27), a second mass flow meter (28), a control valve (23) and an interface meter (21), wherein the sight glass (26) is arranged on the surface of the delaminating device (25) and used for observing the internal condition of the delaminating device (25), a branch pipeline, the second mass flow meter (28) and the control valve (23) are sequentially arranged on a pipeline connected with a discharge port at the lower end of the delaminating device (25) along the discharge direction, the backwashing discharge valve (27) is arranged on the branch pipeline, a calibration probe of the interface meter (21) is communicated with the inner cavity of the lower barrel body (20), and a measurement probe of the interface meter (21) is communicated with the inner cavity of the delaminating device (25).
8. The filtration apparatus for effecting catalyst separation in the production of polytetramethylene glycol according to claim 1 wherein: the top surface of the upper cylinder body (7) is in an upward convex arc shape, and the bottom surface of the lower cylinder body (20) is in a downward convex arc shape.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710070906.4A CN106669279B (en) | 2017-02-09 | 2017-02-09 | Filtering equipment for realizing catalyst separation in polytetramethylene glycol production |
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| CN201710070906.4A CN106669279B (en) | 2017-02-09 | 2017-02-09 | Filtering equipment for realizing catalyst separation in polytetramethylene glycol production |
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| CN106669279B true CN106669279B (en) | 2022-04-22 |
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| CN110478951A (en) * | 2019-09-17 | 2019-11-22 | 四川北方红光特种化工有限公司 | A kind of technique and catalyst settler increasing catalyst sedimentation |
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