North Carolina State University is a landGrant university and a constituent institution of The University of North Carolina

Department of Wood and Paper Science

NC STATE UNIVERSITY

STANDARD OPERATING PROCEDURE (SOP) Parr Pressure Reactor

Location: 2226 Pulp and Paper Labs CAUTION Hot Temperature, High Pressure Sta !ar! Operati g Proce!ure
1) Determine which reactor should be used a. Use ONLY the hastelloy reactor for acid hydrolysis b. Either the hastelloy or the 316 stainless steel can be used for all other reactions ) !ut sam"le in the reaction #essel 3) !lace the ca" $with "ressure %au%e& thermocou"le& and #al#es) on the reaction #essel ') !lace the s"lit( rin% closures on the ca")reaction #essel *) +i%hten bolts with wrench 6) !lace the safety rin% on the bench surface ,) -it the reaction #essel in the safety rin% .) -lide safety rin% u" to co#er the s"lit( rin% closures /) !lace the safety rin% screw o#er the hole on the s"lit( rin% closure and ti%hten 10) 11) 1 ) 13) 1') 1hec2 bolts and screw to ensure that they are ti%htened 1onnect thermocou"le to controller& ma2in% sure the 3 and 4 line u" correctly on each "art $shown on thermocou"le) !lace the reaction #essel in the heatin% 5ac2et !ull u" sil#er 2nob on to" of blac2 motor to raise the stirrer 1enter the stirrer on the to" of the reaction #essel and lower

1*) 16) 1,) 1.) 1/) 0) 1) ) 3) ') *)

+urn on the !arr '.'3 controller dis"lay usin% the D6-!L7Y button !ush in the 8698 L6:6+ button on the bac2 of the controller to ma2e the hi%h limit li%ht turn off $a""ro;imately in the middle) +he control "anel should read the tem"erature inside the #essel $to" dis"lay) and the set"oint $bottom dis"lay) !ress the u" and down buttons to chan%e the tem"erature set"oint +urn on the heatin% 5ac2et by "ressin% the 8E7+E< button 4 u" for a hi%h heatin% rate and down for a low heatin% rate +urn on the stirrer usin% the :O+O< button 7d5ust the stirrin% s"eed if desired usin% the :O+O< control 2nob +he e;"eriment is now runnin% Once the e;"eriment is com"lete& turn off the heatin% 5ac2et usin% the 8E7+E< button !ull u" the sil#er 2nob to disconnect the stirrer <emo#e the reaction #essel from the heatin% 5ac2et to cool 4air cool& or "ut in a bath of cold water. =e careful not to %et water on the ca" or on the rin% closures Once the reaction #essel has cooled& remo#e the thermocou"le <emo#e the safety rin% by loosenin% the screws <emo#e the rin% closures by loosenin% the bolts <emo#e the ca" <emo#e sam"le +urn off controller usin% the D6-!L7Y button

6) ,) .) /) 30) 31)

C"ea i g Proce!ure
1) !lace a""ro;imately 1*0 mL of 10> w)# -odium 8ydro;ide in the reaction #essel ) !lace the ca" $with "ressure %au%e& thermocou"le& and #al#es) on the reaction #essel 3) !lace the s"lit( rin% closures on the ca")reaction #essel

') !lace the ca" $with "ressure %au%e& thermocou"le& and #al#es) on the reaction #essel *) !lace the s"lit( rin% closures on the ca")reaction #essel 6) +i%hten bolts with wrench ,) !lace the safety rin% on the bench surface .) -it the reaction #essel in the safety rin% /) -lide safety rin% u" to co#er the s"lit( rin% closures 10) 11) 1 ) 13) 1') 1*) 16) 1,) 1.) 1/) 3* 1 0) 1) ) 3) ') *) 6) +urn on the heatin% 5ac2et by "ressin% the 8E7+E< button 4 u" for a hi%h heatin% rate +urn on the stirrer usin% the :O+O< button 7fter reachin% 3* o 1& wait for 10 minutes 7fter the 10 minutes& turn off the heatin% 5ac2et usin% the 8E7+E< button !ull u" the sil#er 2nob to disconnect the stirrer <emo#e the safety rin% by loosenin% the screws <emo#e the rin% closures by loosenin% the bolts
o

!lace the safety rin% screw o#er the hole on the s"lit( rin% closure and ti%hten 1hec2 bolts and screw to ensure that they are ti%htened 1onnect thermocou"le to controller& ma2in% sure the 3 and 4 line u" correctly on each "art $shown on thermocou"le) !lace the reaction #essel in the heatin% 5ac2et !ull u" sil#er 2nob on to" of blac2 motor to raise the stirrer 1enter the stirrer on the to" of the reaction #essel and lower +urn on the !arr '.'3 controller dis"lay usin% the D6-!L7Y button !ush in the 8698 L6:6+ button on the bac2 of the controller to ma2e the hi%h limit li%ht turn off $a""ro;imately in the middle) +he control "anel should read the tem"erature inside the #essel $to" dis"lay) and the set"oint $bottom dis"lay) !ress the u" and down buttons to chan%e the tem"erature set"oint to

,) .) /) 30) 31) 3 ) 33) 3') 3*) 36) 3,) 3.) 3/) '0) '1) ' ) '3) '') ** 1 '*) '6) ',) '.) '/)
o

<emo#e the ca" <emo#e cleanin% solution !lace a""ro;imately 1*0 mL of 10> ?)@ -odium 8ydro;ide in the reaction #essel !lace the ca" $with "ressure %au%e& thermocou"le& and #al#es) on the reaction #essel !lace the s"lit( rin% closures on the ca")reaction #essel !lace the ca" $with "ressure %au%e& thermocou"le& and #al#es) on the reaction #essel !lace the s"lit( rin% closures on the ca")reaction #essel +i%hten bolts with wrench !lace the safety rin% on the bench surface -it the reaction #essel in the safety rin% -lide safety rin% u" to co#er the s"lit( rin% closures !lace the safety rin% screw o#er the hole on the s"lit( rin% closure and ti%hten 1hec2 bolts and screw to ensure that they are ti%htened 1onnect thermocou"le to controller& ma2in% sure the 3 and 4 line u" correctly on each "art $shown on thermocou"le) !lace the reaction #essel in the heatin% 5ac2et !ull u" sil#er 2nob on to" of blac2 motor to raise the stirrer 1enter the stirrer on the to" of the reaction #essel and lower !ress the u" and down buttons to chan%e the tem"erature set"oint to +urn on the heatin% 5ac2et by "ressin% the 8E7+E< button 4 u" for a hi%h heatin% rate +urn on the stirrer usin% the :O+O< button 7fter reachin% ** o 1& wait for 1* minutes 7fter the 1* minutes& turn off the heatin% 5ac2et usin% the 8E7+E< button !ull u" the sil#er 2nob to disconnect the stirrer

*0) *1) * ) *3) *') **)

<emo#e the safety rin% by loosenin% the screws <emo#e the rin% closures by loosenin% the bolts <emo#e the ca" <emo#e cleanin% solution <inse reaction #essel with deioniAed water and scrub with a brush& if necessary to remo#e the remainin% blac2 tar +urn off controller usin% the D6-!L7Y button