IE83667B1 - A process for removing pyrophoric catalyst - Google Patents
A process for removing pyrophoric catalystInfo
- Publication number
- IE83667B1 IE83667B1 IE2000/1042A IE20001042A IE83667B1 IE 83667 B1 IE83667 B1 IE 83667B1 IE 2000/1042 A IE2000/1042 A IE 2000/1042A IE 20001042 A IE20001042 A IE 20001042A IE 83667 B1 IE83667 B1 IE 83667B1
- Authority
- IE
- Ireland
- Prior art keywords
- catalyst
- filter
- pyrophoric
- reaction vessel
- rich material
- Prior art date
Links
- 239000003054 catalyst Substances 0.000 title claims description 42
- 238000000034 method Methods 0.000 title claims description 13
- 238000005984 hydrogenation reaction Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 11
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 230000000717 retained Effects 0.000 claims description 6
- 239000007868 Raney catalyst Substances 0.000 claims description 4
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000010923 batch production Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000036633 rest Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Description
A process for removing pyrophoric catalyst
Introduction
The invention relates to a factory scale process for carrying out a hydrogenation
reaction.
Hydrogenation reactions are frequently carried out in the presence of a pyrophoric
catalyst such as Raney Nickel. This presents a serious difficulty because flammable
liquids such as methanol or ethanol are often used as hydrogenation solvents. The
removal of the catalyst from the reaction mixture after the hydrogenation reaction is
complete, presents serious difficulties. Generally the reaction mixture is passed
through a filter, the catalyst is filtered out and removed in a closed circuit.
Handling of the resultant catalyst presents difficulties and the commonly used
multiplate filters, which necessitate generation of hazardous dry material, require
extensive safety precautions and extended operation times to facilitate safe removal
of the catalyst.
DE—A-4325682 (= US5,690,836) describes a method for removing a catalyst such as
Raney Nickel from hydrogenation reaction product. The reaction product is passed
through a hollow tubular filter medium which is back—washable. The process is
described on a laboratory scale and is not suitable for large factory scale use.
There is therefore a need for an improved process for carrying out a hydrogenation
reaction which will overcome these problems.
Statements of Invention
According to the invention there is provided a batch process for carrying out a
hydrogenation reaction comprising the steps of:—
mixing a pyrophoric catalyst with reactants and solvents to form a reaction
mixture in a reaction vessel;
adding hydrogen to the reaction vessel;
after hydrogenation, removing the desired hydrogenation product from the
reaction vessel;
delivering the pyrophoric catalyst-rich material from the reaction vessel to a
pressure filter comprising a container having an upper rim closable by a
removable lid, the container having a removable filter bag and the
pyrophoric-rich material being retained in the bag;
adding water to the pyrophoric catalyst—rich material in the filter to saturate
the pyrophoric catalyst—rich material on the filter;
opening the lid; and
removing the filter bag containing the spent pyrophoric material from the
pressure filter in a water wet form.
In a preferred embodiment of the invention the pressure filter is a single platc
pressure filter, the catalyst being held in the filter in a wet form.
In one embodiment the catalyst is Raney Nickel.
Preferably the contents of the reaction vessel are decanted after hydrogenation, the
desired hydrogenation product being substantially removed while allowing the
catalyst—rich material to settle at the bottom of the vessel.
Preferably the reaction vessel is an agitated vessel, the agitator being stopped to
allow the catalyst to settle at the bottom of the vessel.
In one embodiment of the invention the process includes the step of washing the
catalyst—rich material in the filter with a solvent to recover residual desired
hydrogenation product.
Detailed Description of the Drawings
The invention will be more clearly understood from the following description given
by way of example only with reference to the accompanying drawings in which:—
Fig.1 is a perspective view from the front of a filter apparatus used in the
process of the invention;
Fig.2 is a perspective view from the side of the filter apparatus of Fig. l;
Fig.3A is an exploded perspective view of a removable filter bag and
associated clamping band;
Fig. 3B is a perspective view of the filter bag in position;
Fig. 4 is a top view of a clam—shell lid of the filter apparatus of Fig. 1; and
Fig. 5 is a cross—sectional view of the filter apparatus of the invention.
Detailed Description
The invention will be more clearly understood from the following description given
by way of example only.
We have found a new method of removing a spent pyrophoric reaction catalyst from
a reaction mixture, safely, cheaply and rapidly using a single plate pressure filter.
In the process, after hydrogenation, the reaction mixture is decanted, the desired
hydrogenation product is substantially removed and catalyst rich material which
settles at the bottom of the vessel is delivered to a single plate pressure filter. The
spent catalyst is retained in the filter bag on the filter plate while the product rich
solvent is led away from the bottom outlet of the pressure filter to a receiving vessel.
The retained catalyst material is washed with a solvent to recover residual product
and then washed with water to saturate the catalyst material which is then safely and
easily transferred to drums and stored under water awaiting recovery.
Referring to Figs. 1 to 5 there is illustrated a filter apparatus 1 of the invention. The
filter apparatus 1 comprises a container having a domed base 2, a generally
cylindrical sidewall 3 terminating in an upper rim 4 closed by a removable lid 5
having lifting lugs 6. The lid 5 is fixed in pressure—tight engagement with the
sidewall 3 by flange engaging screw clamps 7 and an embedded
polytetrafluoroethene gasket 8.
The filter container has a single removable, perforated filter plate 9 which is
supported in spaced-apart relation from the base 2 by supports 12. The base 2 has an
outlet 10 below the filter plate 9. The outlet 10 is fitted with an outlet valve 13 for
discharge of product—rich solvent.
The lid 5 has several fittings including a main catalyst inlet line 15, a decant inlet
valve 16 and a water wash inlet line 17. A light port 18, a sight glass 19, pressure
relief line 20 and a nitrogen purge line 21 are also provided. An earth clip 22 is
located on the lid 5.
The filter container has two jacketed coils 30 with inlet and outlets 31, 32. The
jackets may be heated or cooled, as required, to heat or cool the contents of the filter
container. A hot water pressure release device 23 and a hot water overflow 27 are
also provided.
Referring especially to Fig. 3 there is illustrated a removable filter bag 40 of
water/solvent permeable material, typically of acid resistant polypropylene
monofilament or multifilament weave (about 10 micron pores), with a top rim 41
held in position against the side wall 3 of the filter container by a band 11. A
releasable ring clamp 42 is provided on the band 11. The clamp 42 is adjustable to
maximise the diameter of band 11 and thus tighten the filter bag rim 41 against the
filter sidewall 3. The bottom of the filter bag 40 rests on a perforated filter plate 9
which is supported by a filter plate support 12. The filter is inerted by first applying a
vacuum and then breaking the vacuum with nitrogen. Most of the contents of a
reaction vessel after settling are pressure decanted from the reaction vessel and fed
into the closed single plate pressure filter apparatus 1 through an inlet line 16.
Liquid free of catalyst is discharged through the bottom outlet valve 13 and
transferred to a receiving vessel. The residual catalyst in the reaction vessel is fed to
the filter through the larger inlet line 15 followed by a solvent wash to recover
residual product. The spent catalyst is retained in a filter bag 40 while the desired
product is drained off and removed, by applying pressure to the apparatus 1, through
to a receiving vessel via the outlet valve 13. Water is then added through the wash
inlet line 17 to wash out residual solvent to waste and to saturate the retained catalyst
material. The pressure in the filter apparatus 1 is released and the lid 5 is removed
by passing a chain through the lugs 6 and hoisting the lid 5 off. Water saturated
catalyst is scooped directly to drums and stored under water. Alternatively the filter
bag 40 is lifted out and the water wet catalyst is removed and stored for disposal.
The filter bag 40 may be reused. Alternatively the filter bag 40 is lifted out of the
pressure filter and the bag containing catalyst charged to a drum where it is stored
under water and sent for catalyst recovery.
The filter container is mounted on a wheeled chassis 50 so that the filter apparatus
may be easily moved from one location to another.
The invention provides a simple, cheap and rapid method for removing spent
pyrophoric catalyst from hydrogenation catalyst-rich material. The filter apparatus is
cheap to set up and maintain. By keeping the pyrophoric catalyst water wet the
catalyst does not pose a safety hazard and may be easily taken from the filter
apparatus 1 directly or in removable filter bags 40 and safely and easily transferred
to drums containing water for storage and recovery.
The invention is not limited to the embodiments hereinbefore described which may
be varied in detail.
Claims (2)
1. A batch process for carrying out a hydrogenation reaction comprising the steps of :- mixing a pyrophoric catalyst with reactants and solvents to form a reaction mixture in a reaction vessel; adding hydrogen to the reaction vessel; after hydrogenation, removing the desired hydrogenation product from the reaction vessel; delivering the pyrophoric catalyst—rich material from the reaction vessel to a pressure filter comprising a container having an upper rim closable by a removable lid, the container having a removable filter bag and the pyrophoric—rich material being retained in the bag; adding water to the pyrophoric catalyst—rich material in the filter to saturate the pyrophoric catalyst—rich material on the filter; opening the lid; and removing the filter bag containing the spent pyrophoric material from the pressure filter in a water wet form.
2. A process as claimed in claim 1 including the step of washing the catalyst- rich material in the filter with a solvent to recover residual desired hydrogenation product. A process as claimed in claim 1 or 2 wherein the pressure filter is a single plate pressure filter, the catalyst being held in the filter in a wet form. A process as claimed in any preceding claim wherein the catalyst is Raney Nickel. A process as claimed in any preceding claim wherein the contents of the reaction vessel are decanted after hydrogenation, desired hydrogenation product being substantially removed while allowing the catalyst-rich material to settle in the bottom of the reaction Vessel. A process as claimed in any preceding claim wherein the reaction vessel is an agitated vessel, the agitator being stopped to allow the catalyst to settle at the bottom of the vessel.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IE2000/1042A IE83667B1 (en) | 2000-12-18 | A process for removing pyrophoric catalyst |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IEIRELAND17/12/19991999/1063 | |||
IE991063 | 1999-12-17 | ||
IE2000/1042A IE83667B1 (en) | 2000-12-18 | A process for removing pyrophoric catalyst |
Publications (2)
Publication Number | Publication Date |
---|---|
IE20001042A1 IE20001042A1 (en) | 2002-03-20 |
IE83667B1 true IE83667B1 (en) | 2004-11-17 |
Family
ID=
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CA2389561C (en) | A process for removing pyrophoric catalyst | |
US20020153328A1 (en) | Process for removing pyrophoric catalyst | |
IE83667B1 (en) | A process for removing pyrophoric catalyst | |
IE20001042A1 (en) | A process for removing pyrophoric catalyst | |
IES991061A2 (en) | An Apparatus for Carrying Out a Hydrogenation Reaction | |
IE83620B1 (en) | An apparatus for removing pyrophoric catalyst | |
EP0299681A2 (en) | Flask support system | |
AU2009310582B2 (en) | Separating devulcanized rubber | |
US11167451B2 (en) | Lewis base-mediated recovery of fibers from fiber reinforced polymers | |
IES991062A2 (en) | A process for removing a pyrophoric catalyst | |
CN218741178U (en) | Separation equipment for extracting helium from BOG gas | |
JPS6279819A (en) | Method and device for separating solid and liquid | |
JP5064299B2 (en) | Method for producing dry powder of porous polymer particles | |
WO2022260559A1 (en) | Lid device for transferring a contaminated catalyst slurry, catalyst washing system, hydrogenation reactor system and process for purifying a contaminated catalyst |