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I. Studies on the Production of Oxalic Acid from Corn Stalks and Cobs; II

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I. Studies on the Production of Oxalic Acid from Corn Stalks and Cobs; II Iowa State University Capstones, Theses and Retrospective Theses and Dissertations Dissertations 1929 I. Studies on the production of oxalic acid from corn stalks and cobs; II. Studies on corn stalk cellulose Henry Albert Webber Iowa State College Follow this and additional works at: https://lib.dr.iastate.edu/rtd Part of the Chemical Engineering Commons Recommended Citation Webber, Henry Albert, "I. Studies on the production of oxalic acid from corn stalks and cobs; II. Studies on corn stalk cellulose" (1929). Retrospective Theses and Dissertations. 14695. https://lib.dr.iastate.edu/rtd/14695 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Retrospective Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. INFORMATION TO USERS This manuscript has been reproduced from the microfilm master. UMI films the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, while others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send UMI a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. Oversize materials (e.g., maps, drawings, charts) are reproduced by sectioning the original, beginning at the upper left-hand comer and continuing from left to right in equal sections with small overiaps. ProQuest Information and Learning 300 North Zeeb Road, Ann Arbor. Ml 48106-1346 USA 800-521-0600 NOTE TO USERS This reproduction is the best copy available. UMI' I. Si-iJDIBS or, SH3 P20I3CG2I0S 0? OXALIC AGID 5'202^ COEl S2ALES MD GOBS. II. SUfUDISS OS COBS C3LLUL0SE by Eenry Albert Webber A IThesis SabiEitted to the Graduate Faculty for the Degree of DOC?OH 0? rEILQSOPHY" Ka^or Subject: CbeEtioal Sngineerine ApproTed: Signature was redacted for privacy. Signature was redacted for privacy. Signature was redacted for privacy. Dean „ _ Iowa State College 192S UMl Number: DP14564 UMJ^ UMl Microform DP14564 Copyright 2006 by ProQuest Information and Learning Company. All rights reserved. This microfonn edition is protected against unauthorized copying under Title 17, United States Code. ProQuest Information and Learning Company 300 North Zeeb Road P.O. Box 1346 Ann Arbor, Ml 48106-1346 21BL3 0? G0S]?S!I2S !? ARiT X rage I. irrHODuaTioij 4 II. PHSYIOnS W02Z - QZIDATIOn -VliS ITITHIO AGI" S? III. i. Some factors InfluenciJig the Cyclio JSitric Acid 02d.dation Process 17 3. (Dreatineat of Com Cobs isith 30 to 70 Per Cent Hitric Aoid 91 1. Jhe Bffect of the Hitrie vcid Concen­ tration SI £• Sffect o'f Catalyst idded to Heaction ^^jLStlir e «a«as9aoa9es«es«as»9*ae*»«s»99c«9»9e 1G& 3. 3ffect of Various Cat^ilysts ^dded to the Piltrdte lii;:^ 4» Effect of Lei^th of Heatin^- Period in Presence of Catalyst 114 5. Stability of -^alic .»cid in Sitric Acid Solutions 115 6* Successivs 'xxeatsent of Corn Cobs vilth Increasing wtrezsgths of Nitric ^cid •*.•«••• iiS C. SJresitc-ent of Corn Cobs with 10 to £0 Per Cent Mtric Acid 1^5 Do Jorsation of Other ..Jlphatic icids •«••.••«••••• 132 3. Procedure to Obtain Ei.^h Yields of (ixalic T-tr oTTijtA AosT <r\aT TTT.'Str Tirrr?T:>Tr« Anrn !/• jrr.ii V J. Jc o v-ur.JL — rvaxsjij viAXii J-uj ly.-. MA ai ••••as JL«^ 71. 3Z?3HI]l^2HTAL ""OHZa A. Fusion with Sodiuai Hydroxide ••••••••••••••••«•• 153 B« Hecovery of the Sodiia^ Hydroxide •••••••••••e.-a 171 C. Ii'ethods of ^alysis •.•••••.•••••.•••».«••••••••• 176 711. - HJSIOJ: TIITd A'LKsiLI ETDROZa'DSS 179 PAH2 II I. irrTHODUOTION 164 II. TH^OHY - 2H5 C0HS1'I2U3I42 OSOUPS OF 'rHS LIG-i^> C3LIUL03SS •••••••••.•••••••••••.«•••.•••••.•.•.•••• 189 III. PH^OUS VVORS 129 x7. A-ti!rSI07 x'Hui COrtI? S'j.*^••••••..••••....•.•••••.• wOo 7. ISOLAxIOI 07- COHI ST^'JjZ C3LLTJL0S3 "vISH :iLZ.^.IS>-:: .... 231 1. Alkali-Insoluble Cellulose in Cornstalfcs ... E3£ 2. High Alpha-celliilose Pulps froD Soda Coolis . 233 3. I»l-jain Hefi'joVal at Low Pressiixe •..•••••..••» ci4S 4. Surzrrary 250 YI. ISOL^ilZIOS 0? COHII S2;iLZ C3I'UL0SE BY" CHIOHIIiii'IOL; •• 253 \ 3 3. (ij JD ^ Page !• •••«»•«•••«•••••••••••••••••••« 2o6 2« Discussion of iSesults 265 3* Sxuonary 271 4CKS07v13])&L'3:^S 274 LI?3HATtjH3 CITED 275 ? -i5T I ; s?aT)i3y OK 2Hi: ?B0i)ua2i0rT OF ax^iLia .iOiis I ?S(E: COHJ? 3:V -JZS COBS | I - iKTK0Dua:^i0tJ I The objoct of this research was to iiscert-:dn if it | is cosirnereially feasible to r inufacture oxalic j.cid fron; corn i i : I stalks -^d cobs. 2hi3 study is in accord with the r^eneral | trend of resG:^ch orirried on in the Cho-ical Bn^ineerin^ l;e- I piTtnert, low i States College, tf;lth the pnr^^ose in viou' of ! i7ori:iR : orofit ible by-products frOT the iE:rr;ense in-cunt of I ! •i-ricnltiir-il Wfistov- jrod-'ced .inR'a^lly in the I'liited Stites* ; : rno^so 7;\iGtes incr.;de corn eobs anl pcunut sr:olis, o-t ; I hulls, cottonseed hulls, v/hctit straw and sirrilar caterials. I I It hia beer, known for a Ion, tire that stroii^ nitric i I aciS. iirdcr the proper conditicns 7.111 oridi^je cext^ia t^pes of i • aliphatic hydroc^jrbons to o:K;ilic acid# th&:e t^-pes -xe I the aiifjriTS celluloses# If the oxid-.ition is continued too ; I Ion;- the rateri^l bein, treated eventually; i'oes to ccirbon I Sioxide^ carbon r onojdidG, ord ;;..tor« r'eiiior concentrations of nitric acid pro hj.ca virioiis cor. ;;ourids dependLn ; ur.on the stren.:t!- of tho. -icid -ir.d the duration of tre--iti.-.ont• idtric acid under these conditions e^:ercises a nitr-.itin.;, hydrolysia ,, and 0?:idi3in.- action. ;.ror: atic corpotirds. in £:€!?ierv;,li vrhon treated ivith stron"; nitric a:;xd for:: r-itro,[:cn con pounds. The corjnercial irrportanee of oxalic acid is probably best surrni-ixised by a short di.irest of an articlo by iHikpatrici: in Ohcsical :5a2d Ietallur^lcal "J^n^lneexing, July, ISi^o. Oxalic acid is one of the tost isiportant orj^ariic acids- Gonaui:ntion in the United States a-t the present tiiue is esti£r,ated at 6,000,000 to 8,0u0,000 pounds .mnuaLly. 2his consuciption de­ pends n;ore m>on the price at wliich it is available than upon essential uses for which there are no substitutes* about 50 per cent of donestic consunption is "by the liundries, which use it as 3n acicl rinse# Chcrrical uses, indudina the production of various oxalate salts, account for £0 per cent, tha dyeing and printin.i: of textiles xeq^jixe 15 yei cent -ind bieacuir^ oo.^- pounds 5 per cent. The rer^aininj 10 per cent is used for £.is- cellaneous purposes. ?he United States Tariff Q0!r?'--issi0n {35) in 1&£2 in connection '.Tith its invGSti.ration of oxalic acid irade the follovj in;: stat«-ent in re^'ird to the transportation and distribution of 03:alie acid; ""i'he chief r.aricets for or alio acid, vi?hich is Ij^r^ely handled by broiccrs and Jobbers, are in >;eiv York and Jhica^:,©. The frei ;ht x-.te fron; Ghic.ajo, one point of l anufactare, to lievi' Yori: City, is 56 i/E cents per 100 pounds axid fra:: liiajarii 7alis (another producinj center) to sq;? Yorii City is ^6 i/ii cents* 2he inland ocean freight frOD l-iottordarr (center of Dutch industry) is about 22 cents per 100 pounds w'hich is 34«3 cents less than the rate frorr Ghica.ro to irev/ Yoric, and 4.S cor.tg per 100 -'ounds less tfB.n the rate froE: MatTara Palis to the Jfew Yori: :/aiJcet. The price per pound of oxalic acid has varied in re­ cent years frOE 7 to 8 cents per pound in 1S14, through 70 cents per pound in 1916, then it steadily declined until from 1925 to 1925 it varied between 17 and 9 cents per pound, .^t present the quotations are 10 5/4 to 11 l/4 cents per pound." It is "believed that at present the onl^r domestic pro­ ducer of osalis acid is the "victor Chemical Gocipany of Chicago, Illinois* 'fheir product is -nade by the forn^ate n-.ethod which in general consists in passing carbon Doaozide over caustic soda under certain definite conditions oi" temperature and pres­ sure. tPhe process is carried on in twO stages, the first st comparatively lo?/ temperature and high pressure yields sodium formate. :^s the pressure is released and the temperature rais­ ed t"ffc siclecules of sodiuir. for*^ -ite unite to form sodiuin oxalate and hydrogen gas is evolved. She doisestic product at present is protected by a duty of 5 cents a pound. Siis is necessary in order to rneet strong soispetition fro-r forei^jn producers, Tsainly 'Germany and Holland, who also use the synthetic forrate process. Dor.estic production statistics are not av=,ilafcle but in 19E5, 3,559,275 po^inds of oxalic acid v;ere i^iported of v/hich 80 per cent can^e froE Jern^any.
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