Removing Catalyst Fines From Raney Nickel Catalyst Reactions

 

Raney nickel catalysts
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Whether you call it Raney nickel or Raney mud, this alloy of aluminum and nickel is a reagent common to many organic processes. Currently, most Raney nickel catalyst slurries are clarified with the use of manual plate or nutsche filters, bag filters, or cartridge filters. 

Yet any of these approaches require manual operations for cake discharge and cleaning between batches or campaigns. At the same time, they accrue high labor, maintenance and disposal costs  and  expose operators and the environment to toxic and hazardous solvents, solids and contaminated filter tools.  

BHS developed a more contained, cost-effective approach using batch-operated, pressure-filtration systems candle filters. 

A Candle Filter Primer

A candle filter is a pressure vessel filled with tubular filters called candles. The candle is comprised of a filtrate pipe, a perforated core with supporting tie rods, and a filter sock.

The filtrate pipe runs the length of the candle and ensures high liquid flow, as well as maximum distribution of the gas during cake discharge. The tie rods create an annular space between the filter sock and the perforated core, which helps maintain a low pressure drop during operation and promotes efficient expansion of the filter sock during cake discharge. The filter sock, made of various synthetic materials, is installed over the candle and can remove particles smaller than 1 micron (μm).

As the cake builds during operation, the candle filter’s removal efficiency increases, enabling removal of particles as small as approximately 0.5 μm. During operation, pressure from the reactor forces the slurry into the bottom of the pressure vessel. The solids build up on the outside of the filter sock, while the liquid filtrate flows into the candle through the registers and out of the vessel. This process continues until the maximum pressure drop, design cake thickness, minimum flow, or filtration time is reached. 

For concentrated cake discharge, low-pressure gas enters in the reverse direction through the registers and into the individual candles and expands the filter socks. This process breaks apart the cake, which detaches from the filter sock and falls into the vessel cone. The cake is then discharged as a concentrated slurry. 

Raney Nickel Catalyst with Candle Filters for Slurry Discharge

In this application, the current process after the reactor is gravity separation, hydrocyclones and then followed with cartridges and bag filters.  The specification for the process liquid (diamine and water) is less than 3 ppm catalyst.  This recovery process was inefficient and exposes the operators to the diamine and catalysts creating a safety hazard.  The average particle size is 2 um and amorphous crystals.   

Lab testing and pilot testing was conducted to determine a processing scheme that eliminates solvent exposure, reduces the maintenance and operation requirements of the current scheme and recovers the catalyst to less than 3 ppm.  The final design was a BHS slurry-discharge candle filter with 19 m2 of filtration area. 

Candle Filters for Raney nickel Slurry Discharge

BHS developed this approach working with a client whose process after the reactor included gravity separation, hydrocyclones, then followed with cartridges and bag filters. The specification for the process liquid (diamine and water) was less than 3 ppm catalyst. The average particle size was 2 um and amorphous crystals. Yet, this recovery process was inefficient and exposed operators to the diamine and catalysts, which created a safety hazard.  

BHS conducted lab  and pilot testing to determine a processing scheme that eliminated solvent exposure, reduced maintenance and operation requirements, and recovered the catalyst to less than 3 ppm. The final design was a BHS slurry-discharge candle filter with 19 m2 of filtration area. Learn more about this application in this article.