Name: laboratory production of biofuels and biochemicals from a rapeseed oil through catalytic cracking conversion
Uploaded: 2016-09-02T15:00:00
Description: Watch this Scientific Journal Video about Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion at JoVE.com

The authors wish to thank the analytical laboratory of the CanmetENERGY Technology Centre for its technical support, and Suncor Energy Inc. for supplying the synthetic crude oil. Partial funding for this study was provided by Natural Resources Canada and government of Canada&#39;s interdepartmental Program of Energy Research and Development (PERD) with project ID A22.015. Yi Zhang would like to acknowledge his Natural Sciences and Engineering Research Council (NSERC) of Canada Visiting Fellowship from January 2015 to January 2016.

Caution: Please consult all relevant material safety data sheets (MSDS) before using the materials. Work with crude oil samples should only be done while wearing proper personal protective equipment (safety glasses, gloves, pants, closed-toe shoes, lab coat), and the opening, transfer and handling of crude samples should occur in a vented fumehood. Heated hydrocarbons can be flammable in air, and the reaction system should be carefully leak-checked prior to use with crude oil mixtures. The reactor can reach temperatures as high as 750 &#176;...

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The protocol described here utilizes cyclic operation of a single reactor containing a batch of fluidized catalyst particles to simulate feed oil cracking and catalyst regeneration. The oil to be cracked is preheated and fed from the top through an injector tube with its tip close to the bottom of the fluid bed. The vapor generated after catalytic cracking is condensed and collected in a receiver, and the liquid product collected is subsequently analyzed for simulated distillation to determine yields of fractions in diff...

There is strong global interest in both the private and public sectors to find efficient and economic means to produce transportation fuels from biomass-derived feedstocks. This interest is driven by a general concern over the substantial contribution of burning petroleum fossil fuels to greenhouse gas (GHG) emissions and its associated contribution to global warming. Also, there is strong political will in North America and Europe to displace foreign-produced petroleum with renewable domestic liquid fuels. In 2008, biofuels provided 1.8% of the world&#39;s transportation fuels1. In many developed countries, it is required that biofuels replace from 6% to 10% of petroleum fuels in the near future2. In Canada, regulations require an average renewable fuel content of 5% in gasoline starting December 15, 20103. The Renewable Energy Directive (RED) in Europe has also mandated a 10% renewable energy target for the European Union transport sector by 20204.
The challenge has been to develop and demonstrate a viable economic pathway to produce fungible transportation fuels from biomass. Biological sources include triglyceride-based biomass such as vegetable oils and animal fats, as well as waste cooking oil and cellulosic biomass such as wood chips, forest wastes, and agriculture residues. Over the past two decades, research has focused on the evaluation of biomass-derived oil processing using conventional fluid catalytic cracking (FCC)5-12, a technology responsible for producing most of the gasoline in a petroleum refinery. Our novel approach in this study is to co-process canola oil mixed with oil sands bitumen-derived feedstock. Normally, bitumen must be upgraded prior to refining, producing refinery feedstocks such as synthetic crude oil (SCO)&#8212;this processing route is particularly energy intensive, accounting for 68-78% of the GHG emissions from the SCO production13 and, in 2011, constituting 2.6% of Canada&#39;s total GHG emissions14. Replacing a portion of upgraded HGO with biofeed would reduce GHG emissions, since biofuel production involves a much smaller carbon footprint. Canola oil is chosen in this work because it is abundant in Canada and the US. This feedstock possesses a density and viscosity similar to those of HGOs while the contents of sulfur, nitrogen, and metals that could affect FCC performance or product quality are negligible. Moreover, this co-processing option offers significant technological and economic advantages as it would allow utilization of the existing refinery infrastructure and, hence, would require little additional hardware or modification of the refinery. In addition, there may be potential synergy that could result in product quality improvement when co-processing a highly aromatic bitumen feed with its straight-chain biomass counterpart. However, co-processing involves important technical challenges. These include the unique physical and chemical characteristics of bio-feeds: high oxygen content, paraffinic-rich composition, compatibility with petroleum feedstocks, fouling potential, etc.
This study provides a detailed protocol for the production of biofuels at laboratory scale from canola oil through catalytic cracking. A fully automated reaction system&#160;&#8211; referred to in this work as the laboratory test unit (LTU)15 &#8211; is used for this work. Figure 1 shows schematically how this unit operates. This LTU has become the industry standard for laboratory FCC studies. The objective of this study is to test the suitability of the LTU for cracking canola oil to produce fuels and chemicals with the goal of mitigating GHG emissions.
<img alt="Figure 1" src="/files/ftp_upload/54390/54390fig1.jpg" /> 
Figure 1: Conceptual illustration of the reactor. Illustration showing flow lines of the catalyst, feed, product, and diluent. <a href="https://www.jove.com/files/ftp_upload/54390/54390fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table border="0" cellpadding="0" cellspacing="0" width="818">
	<tbody>
		<tr height="168">
			<td height="168" style="height:168px;width:231px;">Advanced Cracking Evaluation (ACE) Unit</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">ACE R+ 46</td>
			<td dir="LTR" style="width:309px;">Assembled by Zeton Inc. SN:505-46;&#160; consisting of (1) a reactor; (2) catalyst addition system; (3) feed delivery system;&#160; (4) liquid collection system; (5) gas collection system; (6) gas analyzing system; (7) catalyst regeneration system; (8) CO catalytic convertor; (9) coke analyzing system</td>
		</tr>
		<tr height="126">
			<td height="126" style="height:126px;width:231px;">Reactor (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">V-105</td>
			<td style="width:309px;">A 1.6 cm ID stainless steel tube having a tapered conical bottom and with a diluent (nitrogen) flowing from the bottom to fluidize the catalyst and also serve as the stripping gas at the end of the run</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Catalyst Addition System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Six hoppers (V-120F, with respective valves) for addition of catalyst for up to 6 runs</td>
		</tr>
		<tr height="126">
			<td height="126" style="height:126px;width:231px;">Feed Delivery System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Consisting of feed bottle (V-100), syringe (FS-115), pump (P-100), and injector (with 1.125 inch injector height, i.e., the distance from the lowest point of the conical reactor bottom to the bottom end of the feed injector)</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:231px;">Liquid Collection System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Six liquid receivers (V-110F) immersed in a common coolant bath (Ethylene glycol/water mixture in 50:50 mass ratio) at about &#8211;15 &#176;C in a large tank (V-145)</td>
		</tr>
		<tr height="127">
			<td height="127" style="height:127px;width:231px;">Gas Collection System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Based on water displacement principle; consisting of gas collection vessel (V-150) with a motor-driven stirrer (MTR-100), and a weight scale (WT-100) for weighing the displaced water collected in a beaker (V100)&#160;</td>
		</tr>
		<tr height="101">
			<td height="101" style="height:101px;width:231px;">Gas Analyzing System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Key element being Agilent micro GC (model 3000A) with four capillary columns equipped with respective thermal conductivity detectors (TCDs)&#160;</td>
		</tr>
		<tr height="101">
			<td height="101" style="height:101px;width:231px;">Catalyst Regeneration System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">V-105</td>
			<td style="width:309px;">Spent catalyst in reactor being burned in situ in air at +700 &#176;C to ensure complete removal of carbon deposited on the catalyst</td>
		</tr>
		<tr height="109">
			<td height="109" style="height:109px;width:231px;">CO Catalytic Convertor&#160; (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">A reactor (V-140) with CuO as catalyst to oxidize any CO and hydrocarbons in exhausted flue gas to CO2 (to be analyzed by IR gas analyzer) and H2O (to be absorbed by a dryer)</td>
		</tr>
		<tr height="46">
			<td height="46" style="height:46px;width:231px;">Coke Analyzing System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Servomex (Model 1440C) IR analyzer for measuring CO2 in exhausted flue gas</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">R+MM Software Suite</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Including iFIX 3.5&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Agilent Micro GC</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;">3000A</td>
			<td style="width:309px;">For gas analysis after cracking</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Cerity Networked Data System</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Software for Agilent Micro GC</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">CO2 Gas Analyser</td>
			<td style="width:168px;">Servomex Inc.</td>
			<td style="width:111px;">1440C</td>
			<td style="width:309px;">SN: 01440C1C02/2900</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">NESLAB Refrigerated Bath</td>
			<td style="width:168px;">Themo Electron Corporation</td>
			<td style="width:111px;">RTE 740</td>
			<td style="width:309px;">SN: 104300061</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Orion&#160; Sage Syringe Pump</td>
			<td style="width:168px;">Themo Electron Corporation</td>
			<td style="width:111px;">M362</td>
			<td style="width:309px;">For delivering feed oil to injector tube</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Synthetic Crude Oil (SCO)&#160;</td>
			<td style="width:168px;">Suncor Energy Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Identified as Suncor OSA 10-4.1</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Catalyst P</td>
			<td style="width:168px;">Petro-Canada Refinery</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Equilibrium catalyst</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Balance</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">AB304-S</td>
			<td style="width:309px;">For weighing liquid product receivers</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Balance</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">XS8001S</td>
			<td style="width:309px;">For weighing water displaced by gas product</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Ethylene Glycol</td>
			<td style="width:168px;">Fisher Scientifc Inc.</td>
			<td style="width:111px;">CAS 107-21-1</td>
			<td style="width:309px;">Mixed with distilled water as coolant (50 v% )</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Drierite</td>
			<td style="width:168px;">W.A. Hammond Drierite Co. Ltd.</td>
			<td style="width:111px;">24001</td>
			<td style="width:309px;">For water absorption after CO catalytic converter</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">Copper Oxide</td>
			<td style="width:168px;">LECO Corporation</td>
			<td style="width:111px;">501-170</td>
			<td style="width:309px;">Catalyst for conversion of CO to CO2</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Toluene</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">CAS 108-88-3</td>
			<td style="width:309px;">For cleaning liquid receivers</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Acetone</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">CAS 67-64-1</td>
			<td style="width:309px;">For cleaning liquid receivers</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Micro GC Calibration Gas</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">SPG-25MX0015306</td>
			<td style="width:309px;">Multicomponent standard gas</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">19.8% CO2 Standard Gas</td>
			<td style="width:168px;">BOC Canada Ltd.</td>
			<td style="width:111px;">24069890</td>
			<td style="width:309px;">For calibration of IR analyzer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Argon Gas</td>
			<td style="width:168px;">Linde Canada ltd.</td>
			<td style="width:111px;">24001306</td>
			<td style="width:309px;">Grade 5.0 Purity</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Helium Gas</td>
			<td style="width:168px;">Linde Canada ltd.</td>
			<td style="width:111px;">24001333</td>
			<td style="width:309px;">Grade 5.0 Purity</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-15</td>
			<td style="width:309px;">Channel A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-03</td>
			<td style="width:309px;">Channel B</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-04</td>
			<td style="width:309px;">Channel C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-73</td>
			<td style="width:309px;">Channel D</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">HP 6890 GC</td>
			<td style="width:168px;">Hewlett-Packard Co.&#160;</td>
			<td style="width:111px;">G1530A</td>
			<td style="width:309px;">For simulated distillation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">ASTM 2887 Standard Sample</td>
			<td style="width:168px;">PAC L.P.</td>
			<td style="width:111px;">26650.150</td>
			<td style="width:309px;">For quality control in simulated distillation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">ASTM 2887 Standard Sample</td>
			<td style="width:168px;">PAC L.P.</td>
			<td style="width:111px;">25950.200</td>
			<td style="width:309px;">For calibration in simulated distillation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Column for GC 6890 (simulated distillation)</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;">CP7562</td>
			<td style="width:309px;">10m x 0.53mm x 1.2&#181;m, HP 6890 GC column</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Liquid Nitrogen</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">SPG-NIT1AC240LC</td>
			<td style="width:309px;">For use in simulated distillation&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Nitrogen</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">Bulk (building N2)</td>
			<td style="width:309px;">For use in ACE unit operation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Isotemp Programmable Furnace</td>
			<td style="width:168px;">Thermo Fisher Scientifc Inc.</td>
			<td style="width:111px;">10-750-126</td>
			<td style="width:309px;">For calcination of catalyst</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">GC Vials, Crimp Top</td>
			<td style="width:168px;">Chromatograghic Specialties Inc</td>
			<td style="width:111px;">C223682C</td>
			<td style="width:309px;">2ml, for liquid product</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Seals, Crimp Top</td>
			<td style="width:168px;">Chromatograghic Specialties Inc</td>
			<td style="width:111px;">C221150</td>
			<td style="width:309px;">11 mm, for use with GC vials</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">4 oz clear Boston round bottles</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">02-911-784</td>
			<td style="width:309px;">With PE cone lined caps, for use in feed system</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Sieve</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">6140269</td>
			<td style="width:309px;">Aperture 38 micron</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Sieve</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">6146265</td>
			<td style="width:309px;">Aperture 250 micron</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Shaker</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">MIN 2737-11</td>
			<td style="width:309px;">Minor-Meinzer 2 Sieve Shaker for catalyst screening</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">V20 Volumetric KF Titrator</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">5131025056</td>
			<td style="width:309px;">For water content analysis of the liquid product</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Hydranal Composite 5</td>
			<td style="width:168px;">Sigma-Aldrich</td>
			<td style="width:111px;">34805-1L-R</td>
			<td style="width:309px;">Reagent for Karl Fischer titration</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:231px;">Methanol (extremely low water grade)</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">A413-4</td>
			<td style="width:309px;">Mixed with toluene (40:60 w/w) for KF titration: also used to recover water in receiver</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Glass Wool</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">11-388</td>
			<td style="width:309px;">Placed inside the top of receiver outlet arm&#160;</td>
		</tr>
	</tbody>
</table>

laboratory production of biofuels and biochemicals from a rapeseed oil through catalytic cracking conversion

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil (HGO) for production of transportation fuels through a fluid catalytic cracking (FCC) route. Cracking experiments are performed with a fully automated reaction unit at a fixed weight hourly space velocity (WHSV) of 8 hr-1, 490-530 &#176;C, and catalyst/oil ratios of 4-12 g/g. When a feed is in contact with catalyst in the fluid-bed reactor, cracking takes place generating gaseous, liquid, and solid products. The vapor produced is condensed and collected in a liquid receiver at -15 &#176;C. The non-condensable effluent is first directed to a vessel and is sent, after homogenization, to an on-line gas chromatograph (GC) for refinery gas analysis. The coke deposited on the catalyst is determined in situ by burning the spent catalyst in air at high temperatures. Levels of CO2 are measured quantitatively via an infrared (IR) cell, and are converted to coke yield. Liquid samples in the receivers are analyzed by GC for simulated distillation to determine the amounts in different boiling ranges, i.e., IBP-221 &#176;C (gasoline), 221-343 &#176;C (light cycle oil), and 343 &#176;C+ (heavy cycle oil). Cracking of a feed containing canola oil generates water, which appears at the bottom of a liquid receiver and on its inner wall. Recovery of water on the wall is achieved through washing with methanol followed by Karl Fischer titration for water content. Basic results reported include conversion (the portion of the feed converted to gas and liquid product with a boiling point below 221 &#176;C, coke, and water, if present) and yields of dry gas (H2-C2's, CO, and CO2), liquefied petroleum gas (C3-C4), gasoline, light cycle oil, heavy cycle oil, coke, and water, if present.

The established protocol has been successfully applied to an oil blend of 15:85 volume ratio (i.e., 14.73:85.27 mass ratio) between canola oil and an SCO-derived HGO20. For practical reasons (cost, availability of canola oil, and possible challenges in commercial operation), the study was focused on feedstock containing 15 v% canola oil addition, although feeds with higher concentrations were also tried. The blend was catalytically cracked at 490-530 &#176;C and 8.0 hr...

Watch this Scientific Journal Video about Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion at JoVE.com

Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion

This paper presents an experimental method to produce biofuels and biochemicals from canola oil mixed with a fossil-based feed in the presence of a catalyst at mild temperatures. Gaseous, liquid, and solid products from a reaction unit are quantified and characterized. Conversion and individual product yields are calculated and reported.

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil ...

Research

JoVE Journal

Chemistry

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