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Liquefaction co-processing of coal shale oil at - Argonne National ...

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I<br />

Process Unit<br />

- 2 -<br />

EXPERIMENTAL<br />

Co<strong>processing</strong> experiments were carried out in a I-L<br />

<strong>co</strong>ntinuous-flow stirred tank reactor with a nominal capacity <strong>of</strong> 1 kg/h<br />

<strong>of</strong> slurry feed while product samples were <strong>co</strong>llected over I-h periods<br />

<strong>at</strong> steady st<strong>at</strong>e. For all the experimental runs reported in thls<br />

paper, the m<strong>at</strong>erial balances were within i5 wt X.<br />

purposes, all the d<strong>at</strong>a were normalized to 100% m<strong>at</strong>erial balance by<br />

proportioning the losses over each <strong>of</strong> the product fractions. Other<br />

details <strong>of</strong> the experimental unit are available elsewhere (2).<br />

Feedstocks<br />

For <strong>co</strong>mparison<br />

The analysis <strong>of</strong> Forestburq subbituminous C <strong>co</strong>al and Cold Lake<br />

vacuum bottoms (CLVB) is shown in Table 1. Additives or promoters<br />

were FeS04 or H2S or both. The HzS was obtained from M<strong>at</strong>heson and<br />

used as received. In experiments where H2S was used it was pumped as<br />

a liquid using a W<strong>at</strong>ers LC pump model 6000A.<br />

Product Yields<br />

RESULrS AND DISCUSSION<br />

Previous b<strong>at</strong>ch autoclave experiments indic<strong>at</strong>ed th<strong>at</strong> H2S is most<br />

effective <strong>at</strong> low tp moder<strong>at</strong>e severities in terms <strong>of</strong> improving product<br />

yields when <strong>co</strong>mpared to <strong>co</strong><strong>processing</strong> without any additive. AT<br />

moder<strong>at</strong>e-high severity, using the feedstocks reported in this<br />

paper,rel<strong>at</strong>ively high <strong>co</strong>ke form<strong>at</strong>ion was observed even in the presence<br />

<strong>of</strong> H2S. For this reason, the CSTR experiments which involved H2S only<br />

were performed <strong>at</strong> low to moder<strong>at</strong>e severities. For moder<strong>at</strong>e-high<br />

severity experiments, iron sulph<strong>at</strong>e was used to assure smooth process<br />

oper<strong>at</strong>ion and to prevent <strong>co</strong>ke form<strong>at</strong>ion. Attempts to perform<br />

<strong>co</strong><strong>processing</strong> experiments in the CSTR unit using CLVB and Forestburg<br />

<strong>co</strong>al without any c<strong>at</strong>alyst even <strong>at</strong> low severity resulted in <strong>co</strong>ke<br />

form<strong>at</strong>ion and plant shutdown. Thus, it is not possible to <strong>co</strong>mpare the<br />

results <strong>of</strong> experimental runs using H2S only with those using no<br />

additive or promoter as was done in the b<strong>at</strong>ch autoclave studies (15).<br />

The fact th<strong>at</strong> <strong>co</strong><strong>processing</strong> experiments <strong>co</strong>uld be performed in the CSTR<br />

with H2S and no other c<strong>at</strong>alyst <strong>at</strong> low and moder<strong>at</strong>e severities is<br />

significant and verifies earlier b<strong>at</strong>ch results which indic<strong>at</strong>ed th<strong>at</strong><br />

HpS prevents <strong>co</strong>ke form<strong>at</strong>ion under the <strong>co</strong>nditions employed (14-15).<br />

Table 2 <strong>co</strong>mpares <strong>co</strong><strong>processing</strong> results obtained in the presence <strong>of</strong><br />

HpS and iron sulph<strong>at</strong>e <strong>at</strong> two levels <strong>of</strong> severities. At both levels<br />

replacement <strong>of</strong> FeSO4 with H2S resulted in higher distill<strong>at</strong>e yield,<br />

pitch and <strong>co</strong>al <strong>co</strong>nversions. The results <strong>of</strong> b<strong>at</strong>ch studies indic<strong>at</strong>ed<br />

193

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