CN100369650C - Anti-oxidation filter device for separation of palladium-carbon catalyst - Google Patents

Anti-oxidation filter device for separation of palladium-carbon catalyst Download PDF

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CN100369650C
CN100369650C CNB2005100103085A CN200510010308A CN100369650C CN 100369650 C CN100369650 C CN 100369650C CN B2005100103085 A CNB2005100103085 A CN B2005100103085A CN 200510010308 A CN200510010308 A CN 200510010308A CN 100369650 C CN100369650 C CN 100369650C
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filter
pipeline
fixedly connected
palladium
valve
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CN1762535A (en
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黄玉东
宋元军
曹海琳
王剑飞
刘立洵
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The present invention discloses an anti-oxidation filtering device for separating a palladium-carbon catalyst, which relates to a filtering device for separating the palladium-carbon catalyst. The anti-oxidation filtering device solves the problems that a product medium filtered by a fusion funnel is easily oxygenized, and a millipore filter has the disadvantages of inexhaustive filtration and cockamamie operation. A reactor 2 is fixedly connected with a filter 1 by a first pipe passage 4, and the filter 1 is connected with a nitrogen regulating bag 19 by a sixth pipe passage 18 and is fixedly connected with a filter liquor collector 5 by a second control valve 7. The filter liquor collector 5 is fixedly connected with a nitrogen buffer tank 8 by a third pipe passage 9 and a nitrogen valve 10 and is fixedly connected with a vacuum buffer tank 11 by a fourth pipe passage 12 and a first vacuum valve 13, and the vacuum buffer tank 11 is fixedly connected with a vacuum pump 14 by a fifth pipe passage 16 and a second vacuum valve 15. The filter liquor collector 5 is fixedly connected with a liquor discharging valve 17, and the filter 1 and the filter liquor collector 5 are fixedly connected with a supporting frame. Thereby, the filtering device can prevent the obtained product medium from being oxygenized.

Description

The filter of anti-oxidation separation of palladium-carbon catalyst
Technical field:
The present invention relates to a kind of filter of separation of palladium-carbon catalyst, belong to chemical technology field; Be specifically related to a kind of filter of anti-oxidation separation of palladium-carbon catalyst.
Background technology:
In chemical process, for the thorough fast use solid catalyst that needs that chemical reaction is carried out.The normal palladium-carbon catalyst that uses in the hydrogenation reduction process; to carry out separating of product and palladium-carbon catalyst after chemical reaction finishes, in separation process regular meeting run into products therefrom in air dielectric easily oxidation and separate after the problem that can utilize again of palladium-carbon catalyst.Normal at present fusion funnel separation of palladium-carbon catalyst and the products therefrom of adopting.Because the fusion funnel adopts method separation of palladium-carbon catalyst and the products therefrom that directly filters, solution directly contacts with air in separation process, thereby has the problem of the easy oxidation of products therefrom medium; The employing millipore filter separation of palladium-carbon catalyst and the products therefrom that also have, owing to feeding manner under being of millipore filter employing, thereby there is filtration back easy residual material in millipore filter, filters not thorough, complex operation, the unmanageable problem of filter pressure.
Summary of the invention:
The objective of the invention is to adopt direct isolated by filtration palladium-carbon catalyst of fusion funnel and products therefrom, have the problem of the easy oxidation of products therefrom medium for solving; Adopt millipore filter separation of palladium-carbon catalyst and products therefrom, exist and filter back easy residual material in millipore filter, filter not thorough, complex operation, the unmanageable problem of filter pressure and the filter of a kind of anti-oxidation separation of palladium-carbon catalyst of providing.It comprises filter 1; It also comprises reactor 2, first control valve 3, first pipeline 4, filtrate collection 5, second control valve 7, nitrogen buffer tank 8, the 3rd pipeline 9, nitrogen valve 10, vacuum buffer tank 11, the 4th pipeline 12, first vacuum valve 13, vavuum pump 14, second vacuum valve 15, the 5th pipeline 16, bleeder valve 17, the 6th pipeline 18, nitrogen adjusting bag 19, bracing frame; Fixedly connected with the upper end of filter 1 by first pipeline 4 in the lower end of reactor 2, first control valve 3 is housed on first pipeline 4, the upper end of filter 1 is regulated bag 19 by the 6th pipeline 18 and nitrogen and is connected, fixedly connected with the upper end of filtrate collection 5 by second control valve 7 in the lower end of filter 1, the left upper end of filtrate collection 5 is fixedlyed connected with nitrogen buffer tank 8 by the 3rd pipeline 9, on the 3rd pipeline 9 nitrogen valve 10 is housed, the upper right side of filtrate collection 5 is fixedlyed connected with the bottom face of vacuum buffer tank 11 by the 4th pipeline 12, first vacuum valve 13 is housed on the 4th pipeline 12, the bottom face of vacuum buffer tank 11 is fixedlyed connected with vavuum pump 14 by the 5th pipeline 16, second vacuum valve 15 is housed on the 5th pipeline 16, fixedlys connected with bleeder valve 17 in the lower end of filtrate collection 5; Described filter 1 is fixedlyed connected with bracing frame respectively with filtrate collection 5.
The present invention has following beneficial effect: one, the present invention is because reactor is positioned at the top of filter, promptly adopt the mode that goes up charging, the mixed material of emitting from reactor enters in the filter, because nitrogen is regulated the pressure stability that the existence of bag can guarantee that filter is interior, close at bleeder valve and nitrogen valve, under the state that second control valve is opened, open first vacuum valve and second vacuum valve carries out suction filtration, filtrate is separated with solids (palladium-carbon catalyst), solids (palladium-carbon catalyst) is retained in filter plate top, and filtration back palladium-carbon catalyst carries out dry processing and can utilize once more; And filtrate enters into filtrate collection.Filter when finishing, close second control valve and first vacuum valve earlier, open nitrogen valve again and replenish nitrogen, make pressure in the filtrate collection be in state, by bleeder valve filtrate is put into other container and carry out next step operation greater than normal pressure to filtrate collection.Whole process makes filtration system be under the nitrogen protection and oxidized phenomenon can not occur because of the switch control processing step of each valve.Two, facts have proved too big variation is not arranged, and the specific area that adopts the fusion funnel directly to feed the isolated palladium-carbon catalyst of hydrochloric acid changes (referring to table 1) greatly by the specific area of the isolated palladium-carbon catalyst of filter of the present invention.
Table 1
Catalyst Specific area (m 2·g -1)
Original palladium-carbon catalyst 896.2
Adopt the fusion funnel directly to feed the isolated palladium-carbon catalyst of hydrochloric acid 186.1
Use the isolated palladium-carbon catalyst of filter of the present invention 891.8
Three, adopt fusion funnel hydrogenation products directly to feed the isolated palladium-carbon catalyst of hydrochloric acid and use the isolated palladium-carbon catalyst of filter of the present invention to carry out X-ray diffraction (XRD) map analysis, the result as shown in Figure 10.From the XRD figure as can be seen, carbon carrier on X-ray diffractogram, show as one wide and the diffraction maximum of disperse uses the isolated palladium-carbon catalyst of filter of the present invention that tangible palladium crystalline phase diffraction maximum is arranged.And adopt fusion funnel hydrogenation products to feed directly that palladium crystalline phase diffraction maximum has disappeared in the isolated palladium-carbon catalyst of hydrochloric acid, variation has taken place in this explanation palladium crystal phase structure.Using the active palladium in the isolated palladium-carbon catalyst of filter of the present invention is 0 valency, have only the palladium of 0 valence state just to have activity, and the valence state that adopts fusion funnel hydrogenation products directly to feed palladium in the isolated palladium-carbon catalyst of hydrochloric acid is+divalent, this explanation uses the isolated palladium-carbon catalyst of filter of the present invention still to have activity, can utilize once more, thereby avoided the inactivation of palladium-carbon catalyst, greatly reduced production cost.Four, filter of the present invention has simple in structure, processing ease, filtration is thorough, can prevent the advantage that the products therefrom medium is oxidized.
Description of drawings:
Fig. 1 is a general structure schematic diagram of the present invention, Fig. 2 front view that to be filter 1 fixedly connected with bracing frame with filtrate collection 5, Fig. 3 is the left view of Fig. 2, Fig. 4 is the right view of Fig. 2, and Fig. 5 is the main pseudosection of filter 1, and Fig. 6 is the vertical view of Fig. 5, Fig. 7 is the main pseudosection of filtrate collection 5, Fig. 8 is that vertical view, Fig. 9 of Fig. 7 is 4, the infrared spectrogram that the 6-diamino resorcin hydrochlorate records with pellet technique, and Figure 10 is an X-ray diffractogram.
The specific embodiment:
The specific embodiment one: in conjunction with Fig. 1, Fig. 2, Fig. 3 present embodiment is described, present embodiment is made up of filter 1, reactor 2, first control valve 3, first pipeline 4, filtrate collection 5, second control valve 7, nitrogen buffer tank 8, the 3rd pipeline 9, nitrogen valve 10, vacuum buffer tank 11, the 4th pipeline 12, first vacuum valve 13, vavuum pump 14, second vacuum valve 15, the 5th pipeline 16, bleeder valve 17, the 6th pipeline 18, nitrogen adjusting bag 19, bracing frame; Fixedly connected with the upper end of filter 1 by first pipeline 4 in the lower end of reactor 2, first control valve 3 is housed on first pipeline 4, the upper end of filter 1 is regulated bag 19 by the 6th pipeline 18 and nitrogen and is connected, fixedly connected with the upper end of filtrate collection 5 by second control valve 7 in the lower end of filter 1, the left upper end of filtrate collection 5 is fixedlyed connected with nitrogen buffer tank 8 by the 3rd pipeline 9, on the 3rd pipeline 9 nitrogen valve 10 is housed, the upper right side of filtrate collection 5 is fixedlyed connected with the bottom face of vacuum buffer tank 11 by the 4th pipeline 12, first vacuum valve 13 is housed on the 4th pipeline 12, the bottom face of vacuum buffer tank 11 is fixedlyed connected with vavuum pump 14 by the 5th pipeline 16, second vacuum valve 15 is housed on the 5th pipeline 16, fixedlys connected with bleeder valve 17 in the lower end of filtrate collection 5; Described filter 1 is fixedlyed connected with bracing frame respectively with filtrate collection 5.
The specific embodiment two: in conjunction with Fig. 1, Fig. 5, Fig. 6 present embodiment is described, the filter 1 of present embodiment is made up of loam cake 1-1, housing 1-2, filter plate 1-3, filter plate flange 1-4, last sealing ring 1-5, lower seal 1-6, left connecting plate 1-7, right connecting plate 1-8, material inlet pipe 1-9, nitrogen inlet tube 1-10; Fixedly connected with the lower surface of loam cake 1-1 in the upper surface of housing 1-2, sealing ring 1-5 is housed between the lower surface of the upper surface of housing 1-2 and loam cake 1-1, fixedly connected with the upper surface of filter plate flange 1-4 in the lower surface of housing 1-2, in the inner groove of filter plate flange 1-4 filter plate 1-3 is housed, between the inner groove end face of the excircle end face of filter plate 1-3 and filter plate flange 1-4 lower seal 1-6 is housed, the lower end of material inlet pipe 1-9 is contained in the housing 1-2 by the centre bore 1-1-1 on the loam cake 1-1, fixedly connected with the lower end of first pipeline 4 in the upper end of material inlet pipe 1-9, the lower end of nitrogen inlet tube 1-10 is contained in the housing 1-2, fixedly connected with an end of the 6th pipeline 18 in the upper end of nitrogen inlet tube 1-10, the lower end of filter plate flange 1-4 has the filtrate (liquid 1-4-1 that is connected with second control valve 7, and left-right symmetry is fixedly connected with left connecting plate 1-7 and right connecting plate 1-8 respectively on the outer wall of housing 1-2.That this filter 1 has is simple in structure, filter thoroughly, advantage of good sealing effect, and filter 1 employed workpiece-filter plate 1-3 is produced by Changchun glassware Co., Ltd, and its model is PT, and positive/negative pressure is 9.8 * 10 -4Pa.Other composition and annexation are identical with the specific embodiment one.
The specific embodiment three: in conjunction with Fig. 1, Fig. 5 present embodiment is described, the filter plate 1-3 of present embodiment adopts glass material to make, and the aperture Φ of filter plate 1-3 is 4~7 μ m.The aperture of filter plate 1-3 is chosen in this scope, can guarantee that palladium-carbon catalyst does not flow in the filtrate collection 5 with liquid, thereby has guaranteed that palladium-carbon catalyst thoroughly separates with products therefrom.Other composition and annexation are identical with the specific embodiment two.
The specific embodiment four: in conjunction with Fig. 1, Fig. 7, Fig. 8 present embodiment is described, the filtrate collection 5 of present embodiment is made up of cavity 5-1, left fixed head 5-2, right fixed head 5-3; Has the filtrate import 5-1-1 of fixedlying connected on the center of cavity 5-1 upper end with the lower end of second control valve 7, the upper end of cavity 5-1 has nitrogen inlet 5-1-2 that is connected with the 3rd pipeline 9 and the vacuum outlet 5-1-3 that is connected with the 4th pipeline 12, the lower end of cavity 5-1 has the tap hole 5-1-4 that is connected with bleeder valve 17, and left-right symmetry is fixedly connected with left fixed head 5-2 and right fixed head 5-3 respectively on the outer wall of cavity 5-1.Between filtrate import 5-1-1 in the present embodiment and second control valve 7, between tap hole 5-1-4 and the bleeder valve 17, between nitrogen inlet 5-1-2 and the 3rd pipeline 9 and between vacuum outlet 5-1-3 and the 4th pipeline 12 all employing be threaded.Adopt the filtrate collection 5 of said structure to have advantage simple in structure, easy for installation.Other composition and annexation are identical with the specific embodiment one.
The specific embodiment five: in conjunction with Fig. 1, Fig. 2, Fig. 3, Fig. 4 present embodiment is described, the bracing frame of present embodiment is made up of left front column 20-1, right front column 20-2, left back column 20-3, right back column 20-4, upper left suitable beam 20-5, left lower synbeam 20-6, upper right suitable beam 20-7, right lower synbeam 20-8, upper left tie-beam 20-9, lower-left tie-beam 20-10, upper right tie-beam 20-11, bottom right tie-beam 20-12; Be fixedly connected with upper left between left front column 20-1 and the left back column 20-3 respectively along beam 20-5 and left lower synbeam 20-6, be fixedly connected with upper right between right front column 20-2 and the right back column 20-4 respectively along beam 20-7 and right lower synbeam 20-8, fixedly connected with the end of upper left tie-beam 20-9 in the centre position of the medial surface 20-5-1 of upper left suitable beam 20-5, upper left tie-beam 20-9 is fixedlyed connected with described left connecting plate 1-7, fixedly connected with the end of upper right tie-beam 20-11 in the centre position of the medial surface 20-7-1 of upper right suitable beam 20-7, upper right tie-beam 20-11 is fixedlyed connected with described right connecting plate 1-8, fixedly connected with the end of lower-left tie-beam 20-10 in the centre position of the medial surface 20-6-1 of left side lower synbeam 20-6, lower-left tie-beam 20-10 is fixedlyed connected with described left fixed head 5-2, fixedly connected with the end of bottom right tie-beam 20-12 in the centre position of the medial surface 20-8-1 of right lower synbeam 20-8, bottom right tie-beam 20-12 is fixedlyed connected with described right fixed head 5-3.Adopt the bracing frame of this structure to have simple in structure, easy for installation, the reliable advantage of intensity, bracing frame is connected with filtrate collection 5 simply with filter 1, firm.Other composition and annexation are identical with the specific embodiment one.
The specific embodiment six: present embodiment is described in conjunction with Fig. 1, present embodiment is an isolated by filtration 4,6-diamino resorcin and palladium-carbon catalyst, 4, the 6-diamino resorcin is synthetic by following raw material reaction in reactor 2: adopt 2-chloro-4, the 6-dinitroresorcinol is raw material, is that solvent, palladium carbon are that catalyst carries out hydrogenating reduction under uniform temperature and pressure with the acetic acid aqueous solution, after reaction finishes, 4 of generation, 6-diamino resorcin are dissolved in the acetic acid solution and form mixed solution with palladium-carbon catalyst.Mixed solution enters into filter 1 and carries out isolated by filtration, and gained filtrate is passed into through filtrate collection 5 carries out acid out and handle and to make 4 in the hydrochloric acid solution, and the 6-diamino resorcin generates salt, obtains 4, the 6-diamino resorcin hydrochlorate.The palladium-carbon catalyst that separates carries out drying to be handled.To 4,6-diamino resorcin hydrochlorate element measured value (%) carries out analysis in table 2 with calculated value (%):
Table 2
Measured value (%) Calculated value (%)
C 33.73 33.80
H 4.61 4.75
N 13.21 13.15
As can be seen from Table 2, the measured value of its C, H and N and calculated value are very approaching.
From accompanying drawing 9 as can be seen: 1640cm -1, 1550cm -1Absworption peak for N-H and C=C; 3400cm -1~2500cm -1For-O-H and-NH 2Absworption peak; 1190cm -1Be C-O stretching vibration absworption peak; 860cm -1It is the absworption peak of four substituted benzene rings; The data that theory provides are 1643cm -1, 1540cm -1Absworption peak for N-H and C=C; 3450cm -1~2500cm -1For-O-H and-NH 2Absworption peak; 1210cm -1Be C-O stretching vibration absworption peak; 850cm -1It is the absworption peak of four substituted benzene rings.Can illustrate by above-mentioned measured value and theoretical value, the product 4 that uses filter of the present invention to obtain, the every index and the theoretical value of 6-diamino resorcin hydrochlorate are close.

Claims (5)

1. the filter of an anti-oxidation separation of palladium-carbon catalyst, it comprises filter (1); It is characterized in that it also comprises reactor (2), first control valve (3), first pipeline (4), filtrate collection (5), second control valve (7), nitrogen buffer tank (8), the 3rd pipeline (9), nitrogen valve (10), vacuum buffer tank (11), the 4th pipeline (12), first vacuum valve (13), vavuum pump (14), second vacuum valve (15), the 5th pipeline (16), bleeder valve (17), the 6th pipeline (18), nitrogen adjusting bag (19), a bracing frame; Fixedly connected with the upper end of filter (1) by first pipeline (4) in the lower end of reactor (2), first control valve (3) is housed on first pipeline (4), the upper end of filter (1) is regulated bag (19) by the 6th pipeline (18) and nitrogen and is connected, fixedly connected with the upper end of filtrate collection (5) by second control valve (7) in the lower end of filter (1), the left upper end of filtrate collection (5) is fixedlyed connected with nitrogen buffer tank (8) by the 3rd pipeline (9), nitrogen valve (10) is housed on the 3rd pipeline (9), the upper right side of filtrate collection (5) is fixedlyed connected with the bottom face of vacuum buffer tank (11) by the 4th pipeline (12), first vacuum valve (13) is housed on the 4th pipeline (12), the bottom face of vacuum buffer tank (11) is fixedlyed connected with vavuum pump (14) by the 5th pipeline (16), second vacuum valve (15) is housed on the 5th pipeline (16), fixedlys connected with bleeder valve (17) in the lower end of filtrate collection (5); Described filter (1) is fixedlyed connected with bracing frame respectively with filtrate collection (5).
2. the filter of anti-oxidation separation of palladium-carbon catalyst according to claim 1, it is characterized in that described filter (1) by loam cake (1-1), housing (1-2), filter plate (1-3), filter plate flange (1-4), go up sealing ring (1-5), lower seal (1-6), left connecting plate (1-7), right connecting plate (1-8), material inlet pipe (1-9), nitrogen inlet tube (1-10) and form; Fixedly connected with the lower surface of loam cake (1-1) in the upper surface of housing (1-2), sealing ring (1-5) is housed between the lower surface of the upper surface of housing (1-2) and loam cake (1-1), fixedly connected with the upper surface of filter plate flange (1-4) in the lower surface of housing (1-2), filter plate (1-3) is housed in the inner groove of filter plate flange (1-4), lower seal (1-6) is housed between the inner groove end face of the excircle end face of filter plate (1-3) and filter plate flange (1-4), the lower end of material inlet pipe (1-9) is contained in the housing (1-2) by the centre bore (1-1-1) on the loam cake (1-1), fixedly connected with the lower end of first pipeline (4) in the upper end of material inlet pipe (1-9), the lower end of nitrogen inlet tube (1-10) is contained in the housing (1-2), fixedly connected with an end of the 6th pipeline (1 8) in the upper end of nitrogen inlet tube (1-10), the lower end of filter plate flange (1-4) has the filtrate (liquid (1-4-1) that is connected with second control valve (7), and left-right symmetry is fixedly connected with left connecting plate (1-7) and right connecting plate (1-8) respectively on the outer wall of housing (1-2).
3. the filter of anti-oxidation separation of palladium-carbon catalyst according to claim 2 is characterized in that described filter plate (1-3) adopts glass material to make, and the aperture (Φ) of filter plate (1-3) is 4~7 μ m.
4. the filter of anti-oxidation separation of palladium-carbon catalyst according to claim 2 is characterized in that described filtrate collection (5) is made up of cavity (5-1), left fixed head (5-2), right fixed head (5-3); Has the filtrate import (5-1-1) of fixedlying connected on the center of cavity (5-1) upper end with the lower end of second control valve (7), the upper end of cavity (5-1) has nitrogen inlet (5-1-2) that is connected with the 3rd pipeline (9) and the vacuum outlet (5-1-3) that is connected with the 4th pipeline (12), the lower end of cavity (5-1) has the tap hole (5-1-4) that is connected with bleeder valve (17), and left-right symmetry is fixedly connected with left fixed head (5-2) and right fixed head (5-3) respectively on the outer wall of cavity (5-1).
5. the filter of anti-oxidation separation of palladium-carbon catalyst according to claim 4, it is characterized in that described bracing frame by left front column (20-1), right front column (20-2), left back column (20-3), right back column (20-4), upper left along beam (20-5), left lower synbeam (20-6), upper rightly form along beam (20-7), right lower synbeam (20-8), upper left tie-beam (20-9), lower-left tie-beam (20-10), upper right tie-beam (20-11), bottom right tie-beam (20-12); Be fixedly connected with upper left between left front column (20-1) and the left back column (20-3) respectively along beam (20-5) and left lower synbeam (20-6), be fixedly connected with upper right between right front column (20-2) and the right back column (20-4) respectively along beam (20-7) and right lower synbeam (20-8), fixedly connected with an end of upper left tie-beam (20-9) in the centre position of the medial surface (20-5-1) of upper left suitable beam (20-5), upper left tie-beam (20-9) is fixedlyed connected with described left connecting plate (1-7), fixedly connected with an end of upper right tie-beam (20-11) in the centre position of the medial surface (20-7-1) of upper right suitable beam (20-7), upper right tie-beam (20-1 1) is fixedlyed connected with described right connecting plate (1-8), fixedly connected with an end of lower-left tie-beam (20-10) in the centre position of the medial surface (20-6-1) of left side lower synbeam (20-6), lower-left tie-beam (20-10) is fixedlyed connected with described left fixed head (5-2), fixedly connected with an end of bottom right tie-beam (20-12) in the centre position of the medial surface (20-8-1) of right lower synbeam (20-8), bottom right tie-beam (20-12) is fixedlyed connected with described right fixed head (5-3).
CNB2005100103085A 2005-09-07 2005-09-07 Anti-oxidation filter device for separation of palladium-carbon catalyst Active CN100369650C (en)

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CN101728234B (en) * 2008-10-29 2012-04-18 沈阳芯源微电子设备有限公司 Vacuum buffer device
CN110918004B (en) * 2019-12-20 2024-04-12 湖南双阳高科化工有限公司 Palladium-carbon filtering and recycling system and recycling method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1090215A (en) * 1993-01-29 1994-08-03 钱志光 Continuous dual-chamber filter
US20050167351A1 (en) * 2004-01-29 2005-08-04 Herman Peter K. Liquid additive slow-release apparatus driven by a filter pressure gradient

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1090215A (en) * 1993-01-29 1994-08-03 钱志光 Continuous dual-chamber filter
US20050167351A1 (en) * 2004-01-29 2005-08-04 Herman Peter K. Liquid additive slow-release apparatus driven by a filter pressure gradient

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