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lAttached horex>rith are tlae minutes of the Terari~caSteering Cv=ltttec . held Su1 y ' 2 1 x 1 . 9 6 9 ,

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- 1

Presents R.

.V . CroninR . E . Brouillard (Chairman)0 . H . TouseyP . E . GeiserMurray Senkus

. K . W . ' .Kirby (Secretazy . ) .. ' . o~

Guests : W C . Black ,. . . ; . .

. C . M . m W i d m e r. . . ~ . . . .

D . O . Tackaberry ~P . B . Nelson

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U S O F J U L Y 2 M I N T E 1 . r 1 9 6 9

TECHNICAL STEERING COMMITTEE `

Mr . Tackaberry reviewed the project to date indicatingthat the product suffered from def-iciencies such as poor color andflavor stability .on heating and/or On storage . A review meeting washeld on June 24 with Winston-Salem Product Development~people at whichtime plans were laid for resolution .o f .the problems .

1 . Review of Current Sta,tus'

2 . Plans

it was noted that at this point we do not'have a processwhich will'produce a .satisfactory product and that additional investigativework will be necessary . To . obtain raw material for this further work,it was decided to re-start the isomerization pilot plant and to retainquantities of product from various points in the process (i .e ., beforeand after isomerization, after the carboxylic acid resin treatment, etc . )Recent laboratory work has indicated that the use of a granular carboncolumn, especially if operated at a low (2 .5) pH, is much more effectivethan the previously used .powdered column so its use following thecarboxylic acid resin treatment will be investigated during the pilotplant series . If a satisfactory carbon column operation is achievedduring these runs, it is planned also .to give the product the standardpilot plantn ion exchange .resin treatment, etc . It is hoped that it willbe possible to obtain useful performance data on both the carbon andion exchange columns . ,

The retained samples will be-used for stud'ies'on :mono-bed and mixed-bed ion exchange resin systems, additionaltreatments, studies on bleaching with sulfurous acid, the use

ion exchange resins, etc .

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'While the carbon requirements as indicated by lab work will ~e somewhat higher than for our present syrup production, m the economics '

variouscarbonof sulfite

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-2-

will offset thi .s to a degree and the overall economics may not besubstantially changed .

effected by the use of granular carbon (as compared with powdered carbon

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will serve to resolve this difference .

In the work performed recently in Cedar Rapids and in Winston-Salem, a degree of confusion has resulted from the two groups usingdifferent substandard syrups as the base material for their clean-up

studies . The Winston-Salem group used the 1800 lb . batch produced inMarch, while the Cedar Rapids work was performed on the subsequently,produced May batch . This was caused by a difference of opinion on thevalidity of the use of optical rotation as a measure of purity orsuitability of a hydrolysate as a feed for the isomerization unit . It, ,is hoped that additional data can be obtained in this program which

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work is approximately six weeks, and the earliest a product could beexpected would .be the end of theJyear . This is considered optimisticand does not account for equipment delivery delays and carbon column

The-time estimated for the conducting of the laboratory

Salem is being prepared .~ .

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leader . A complete detailed report of the work done to date in Winston-Mr . Black has been designated as the coordinating project

Mr . Cronin questioned whether now is the time that we shouldinquire of Clinton to see .what licensing terms they may want for their

: - , p r o c e s s . According to Mr . Tousey, Corn Products and Staley are alsoready to go on such a product,and products of this nature are obviously

. ready to move in the market .

Mr . Geiser suggested that when a run is made we shouldu

and we should also request, A DorrclQne . - : S t a r . c h , . . . -arrange it so that no "run-around" starch is present in the feed tanks~

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aa3ustments wnicn may be necessary .

3 . Winston-Salem Activity

Thesuperior to, theterminated .

1 1

- dlcoholic isomerization process has not been foundaqueous alkaline process and work on this has been

Calcium hydroxide has been suggested as a base for-alkalineisomerization . This has been evaluated and the process appears to be

,more complicated .because of the clean-up necessary, and this work hasalso been terminated

. ,- -- - - - ---- ork on the enzymatic isomerase system con. Dr . Senkus; indicated that the cost analysis will begin on August 1 on data whichwill be presented to Mr . Sawyer . The process to date as conducted ina 30 gallon fermenter proceeds for 65 hours . At the end of this time,eriough cells are obtained to invert 3,00 gallons of 95-97 D .E . syrup at30% solids . This-inversion is conducted in 24-hours for a total requiredtime of about 90hours . Using this process, a fructose level of about40-42% is obtained . LThe process is conducted at approximately pH 7 .2using glucose,as a growth medium for the, cells ~ w . , ~ .They f ind that they getten times faster conversion b2 .sed on glucose'than on xylos The CornProducts patent describing an enzyme which conducts isomerization works

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equally on xylose and glucose . Thus, it wo: our product a glucose isomerase rather than

as used .in the procedure are re-usable, butre-us~e,,~ Clean-up studies remain to be done and may be as involved asClion reportedly found in their enzymatic process . It would appearthat the enzyme as produced could be made by a commercial manufacturerunder our direction .

. Total Sugar

1 . Market Introduction

2 . Pendex

3 . Commercial Development Activity

4 . Plant Start-UpConstruction is on

planned for a run sometime,inschedule aSeptember .

Aggressive promotion ofCelutab continues, although we areshort of product at the present time . We have reports of certain problemsincluding hardening of tablets on storage, and it would appear that ananhydrous product would be required to do a broad job in the .tableting-----field . We continue to hear good reports of the product . Mr . Touseyindicated that it is .not necessarily a large market initially and thathe estimates approximately 3 to 5 million pounds sales in 1970

. Packagingsize and description has been determined .

appear that we can call MO"somerase b Zb2 whole ce]ls~'.~

ficiency drops off on

The question remains concerning the marketing and manufacturdof Pendex . We still have, the possibility of a contract with Sunlinefor their tableting needs . Additionally, Green & Green is interestedat any time in a product that would be blended with sucrose for thegrocery market, particularly in the Buffalo and Chicago area . Thisproduct would possibly claim a slight premium over dextrose price .

Activity is still continuing in the fat absorption, and colorand spice absorption areas . All of these fields are being promoted at15~/lb . A recent'indibation is that Lipton's would be very interestedin a sizable amount of product for use in dry mix soups for the purposeof holding the fat .

`breakthrough has been made in the technology of flavor orincorporation at Winston-Salem and it would appear that a bulk consumersuch as a baker may be able to use such a product . The market is notexpected to be large, but it would be profitable . RJR Foods would-initially bevery interested in the product .

in~wtial plant start-up is

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' C . Total Sucrose

We have approximately 70 lbs . of spray-crystallized sucroseavailable as supplied by the Japanese . Our total effort will'be withDean Kanig at Columbia University in tableting evaluation . Initially,it would appear that sucrose would overcome some of the possibledeficiencies of Celutab . It has extremely low moistur'e, is relativelynon-hygroscopic and is unreactive with amine compounds . Our initialattempts at'making tablets at, the University of Iowa looked very good .We would expect such a product to have'a premium price at approximately25~/lb .

~ D . Fructose

We currently have .approximately .100 lbs . of dried pure fructoseand 100 lbs . of 70% syrup on hand . We are doing nothing with these forcommercial evaluation until the economics of the process are satisfactoryThe estimated price of 32~ .as suggested in a recent evaluation is too

high for this product . Eventual use may not involve use of pure fructoseas such but rather in blends with corn syrup : ,

called dextrose via .current processes . It was indicated that Dr . Lartigueof Winston-Salem'is of the opinion that on saccharification procedures

, . .. We are at this time at the s ame po3 .nt as we were at our lastmeeting . It does not appear possible to make a product that can be

" approximately 98 to 98 . 5 D .E . is the maximum obtainable with about 2%other saccharides present whether using either the Rhizopus or Aspergillusorganisms .

product is considered patentable and is now under consideration . As datacontinue to be developed at Winston-Salem, it is to be given to Mr .Sawyer for his economic evaluation . ~ We are currently refining our process using the Komai continuous

,pressure cooker to get as high a D .E . as practical . it'is consideredthat either carbon or a Boehringer type column could'be used to yieldpure dextrose from such a mixture . The process for such a high D .E :

ideal to have a process which would allow us to introduce dextrose atthe same time,we introduce Total Sugar on the market .

It was noted that for proper market introduction, it would be

. Dry Milling

to the-pilot plant scale .

Mr . Nelson reviewed the process as developed in the laboratoryindicating that we now have'a process workable on a laboratory scale andthat the next step is to get an economic evaluation before proceeding

Current work was done on Alabama meal which is a commerciallyavailable degermed partially dehulled corn product available in the

czir,d,ohydrate in the wet milling, process .

United States using a process very similar to that of Miag . Using sucha product, .we can get yields of 88-90%,carbohydrate versus about 95%

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I Three key points have been instrumental to the development o f,the process . These ar e

1 . Pressure cooking the product to get compl e'te dispersion ofthe carbohydrate and the protein material, but cooking without exces ssteam

2 . After t he cooking, the product is sac chari fied in th epresence of an amount of calcium ion somewhat larger than necessar yfor the heat st abilizat ion of the enzyme

3 . Lowagitat ion or none at al l is very i mportant during theconversion as this allows very much improved filtration . Cean-up o fthe pr oduct .has i nvolved usi ng ground granular . carbon at a rat e ofabout 5-7% . Comparabl e dat a f or Confex usi ng the i dentical .processresults i n a carbon dosageof about 4 .8% . This suggest s t hat th eprocess as devel oped i s not si gnificantly more demanding as r egardscl ean-up procedures t hant he one used for some of our current product s .

In our plant, we do not use 4 .8%but actual ly use ab out 1% . This workmerel y shows t he r el at ive .relat ionship of the t wo processes . Theproduct as produced has f iltration rates i n a l ab test of 5-20secondsdepending on the point of measurementwhichcasfies i ts f iltrat ionas "rel atively easy .' .' The syrup appears t o have a sat isfactory fl avor ~

, and the carbohydrate yield on an unwashed filter cake is about 95%, an dafter washing, is abo ut 96%

Work has been done to determine if the meal as received shouldbe pre-washed to lower t he protein in the fi ltrate . Work i n t hi sdirection indicated that the protein in the filtrate was lower, but notsi gnificantly. Additionally, also, we did not determne that-the D E .was any higher so the process of pre-washing does not appear necessary .

The only plus factor,from pre-washing was an indicated slightly highe r

yield ..

Oher work has sho wn t hat a pre-coat filter would not benecessar y i n such a-process- and it would be a_dvisabl e t o use co ntinuou s- -- - ---

nzyme addition . Certai nlyt he i on -exchange capaci ty necessar y woul dbe increased because the ash content would be higher in the product thanin our present conventional syrups ;

Recently certain new approaches have been evaluated . Theseinclude the use'of the NSK continuous pressure cooker for preparingthe initial hydrated medium . Holdup tinle'and--temperature may beimportant vari ables i n the use of this cooker . It appears t hat we d o

.get higher protein in the fi lter cake . Additional ly, we do not get as

much st aining wth iodine usi ng t his pr ocess . The protein is higher i n.the fi ltered materi al also . Additionally, we fi nd that the D E . increase

fast er af ter t his t ype of cooking, and it would appear that we couldmake syr ups of al most any t ype abov e 23 D .E . wth such a .process . Th emaximum D .E . iridicated obtainable is about 98 .5 .

. The si gnificance of this work is t hat it would appear that fo ra corn syrup or sugar plant one could avoid the steeping tanks and the

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centrifuges, etc .'of the conventional wet milling operation and insteaduse a process involving only,syrup production and clean-up . Additionally,it would appear that if ground corn would be satisfactory as a starting

, p r o d u c t , t h e p r o c e s s b e c o m e s e v e n s i m p l e r - o n l y g r i n d i n g , h y d r a t i o n ,

.thinning, saccharification, filtration and clean-up of the syrup .

It was decided to proceed and complete the work using wholeground corn and .that the economics should be determined before proceed-ing to the pilot plant . It was suggested that experiments should bedone .with .de-oiling of the cake prior to drying .

G . Malto-Dextrines. .

. ~~ :_ _Pilot studies are under way on these and also for corn syrup

solids . It uias suggested that we could make a 20 D .E . syrup with noretrogradation properties and if such a product co~ . i l d f i n d a m a r k e t,would be very likely competitive with high D . E . malto-dextrines suchas MOR-REX which is finding a very-good market . The product would bea syrup .

It appears that our possible production of a malto-dextrinewould not involve enough volume for s .-spray tower and that the cornsyrup solids market should be worked into this process to allow theeconomics to be favorable ..

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This project has been terminated .

Ransburg

B . Klopman Mills

Klopman .Mills continues to find our Sutro-Penford Gum blendsto besatisfactory products and are tentatively planning on convertinga newly acquired plant to'the use of this particular product . It wasindicated that we may soon have an order for 100,000 lbs . of thisproduct .' It is entirely possible that this may not be a continuingtype product, but once a plant was started on such a product, it couldin time be switched over to Penford Size which is currently being usedsuccessfully for sizing polyester/cotton blends .

Attempts are being made to obtain weaving~efficiency data toadd substance and validity to a'patent application .

A blend of polyvinyl alcohol and oxidized carboxymethyl l st archeswas evaluated at Gulf States this past week . The run was successful inthat no separation of the components was apparent during the run . .However, no paper evaluation has been done as yet .

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only alternative that we have to the chemical conversion process .

7 1

. Chemical and Enzyme Conversion

Dr . Brouillard indicated that we were ready for mill trialswith a continuous process for enzyme conversion at up to the 20% solids.level at any time . This process overcomes the principal_deficiency of ourpresent cookers (i .e ., viscosity limitations) and it appears to be the

Penford Gum in improving the Gurly porosity and some wax pick results

Laboratory evaluation would suggest its use in PMaPermsurfacie'sizing . Ouz data indicates that the product is not as effective as

a r e a l s o i n f e r i o r .

markets .

E . Benzyl Starch

A new development with Champion Paper in addition to our expectedcommitment soon to Owens-Corning would indicatethat by January 1970, wewould be expected to make about 100,000 lbs . per month . Growth in threeyears could be up to 6-8 million pounds for the domestic and foreign

scrubber columns as well as possibly hooded dryers and washing filters. _

Benzyl chloride handling equipment requires use of either nickel, lead,or glass . The latter is least desirable because of possible pin holes .These are suggested even with stabilized material which according toMonsanto is currently stabilized with 0 .35% propylene oxide .

Mr . Tousey evidenced'caution at offering something we couldn'tdeliver, but Mr . Geiser has indicated a current,annual capacity ofabout 3 million pounds . Inquiries are being made for bulk handling ofbenzyl chloride in our plant and for installation of sealed tanks with

A major laboratory effort is under way to study improved methodsof preparation of benzyl starch . These will be refined and supplied toWinston-Salem for use in the preparation of pilot scale batches to allowexpanded cooking and use studies in Cedar Rapids as well as an optimumprocess for plant operation . Pilot plant batches will be prepared atseveral levels of substitution .

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Dr . Senkus indicated that a theory had evolved on the mechanismof benzyl substitution of the starch which involves .the hydrolysis ofbenzyl chloride to benzyl alcohol which subsequently acts as a couplingagent for the benzylgroup for addition to the starch .

Wor'k haspryceededon making a starch with a low ash conductivityfor Owens-Corning b adding ammonium phosphate to the starch . Owens-Corning has been contacted regarding changes in their test procedurenecessary to validly evaluate starch containing the dry-blended phosphates

filtrate from a reaction should include a check of dermatitis and other-skin irritations s'ince we had several reports of this during the

Mr . Geiser requested that any studies that are done on the

preparation of the plant batch a year and a half ago.

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A. High'Amylose Starcha , . , , . . . . .

One mill ~rial has been completed successfu . l ] .y at Mason AuMagenheimer in New York which showed excellent results and qave

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products comparable to those obtained with Staley's high amylose

. ' Miscellaneous Activity

product . The starch used was a blend of 1 part of high amylose and2 parts of acid modified corn starch . Mr . Tousey indicated thatalthough this was successful another test should be set up under thesame conditions at another location .

It"was considered that other market areas are limited andthat the textile market for high amylose btarch appeared to be small .

Apparently ; theseed fox next year has already been ordered .However, no commitment has .been made for planting as yet . It wassuggested that Staley'did not plant a crop of high amylose corn for1969 .

. Waxy Maize Starch

- , W e c u r r e n t l y h a v e p r e p a r e d l a b o r a t o r y m a t c h e s - f o r a l l c u r r e n t '

products of significance on the market today . We expect to pilot theseas soon as the starch is available from our current harvest and fieldtrials will be conducted as soon as possible .

It appears that Chun K,~ng may be a possible place for .experimentation since they consume about 2 million pounds of Waxy . .

Maize base products a year . Very likely we coulde become a supplierof approximately half of this'derivative Waxy Maize business .

Eldib

Dr . Senkus will consider the new proposal-and notify Mr : Eldibnur conr l _ u s i _ o n s . : . ,

p op ~ o s e l heymou rof Indiana for solubleCompan a starch/iron complex t o r e p 7 . a c ea product they now use was considered . The product would be of pilot

scale volume and'command a price of $5`or more per pound . Dr . Kirbywill transmit the summary of the'request to Dr . Senkus for his action .

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