Computer Data Logged Pilot-Plant Reactors - American Chemical

Chapter 35

Computer Data Logged Pilot-Plant Reactors Design Philosophy and Use J . Bentley and S. L. Barker

Downloaded by UNIV OF CALIFORNIA SAN DIEGO on June 13, 2015 | http://pubs.acs.org Publication Date: August 29, 1989 | doi: 10.1021/bk-1989-0404.ch035

ICI Paints, Slough SL2 5DS, England The p i l o t plant stage i s v i t a l i n the scale-up of any new r e s i n process, and i n this paper we discuss the design philosophy of p i l o t plants and then describe two f u l l y instrumented and computer data logged reactors. Some i n d i c a t i o n i s given of the use of the extracted data for both modelling and scale up. Both controlled and data logged parameters are tabulated and an example of data extraction for heat balance i s illustrated. The p a i n t i n d u s t r y manufactures a l a r g e range o f polymer t y p e s i n c l u d i n g a c r y l i c , o i l m o d i f i e d a l k y d s , p o l y e s t e r s , m o d i f i e d epoxy r e s i n s and u r e t h a n e p o l y m e r s , i n s o l u t i o n and i n some cases i n d i s p e r s i o n , f o r a v a r i e t y o f a p p l i c a t i o n s . Many o f t h e p r e p a r a t i o n p r o c e s s e s a r e e x o t h e r m i c and can p r e s e n t a r i s k o f t h e r m a l runaway; another r i s k encountered i s t h a t o f g e l a t i o n . I n s c a l i n g up, o t h e r problems f r e q u e n t l y come t o l i g h t , such as unexpected r a t e s o f r e a c t i o n , temperature c o n t r o l d i f f i c u l t i e s , m i x i n g and f o u l i n g problems, and most troublesome l a c k o f p a r t i c l e s i z e c o n t r o l and 'grit formation i n dispersion r e s i n s . 1

Involvement o f a p i l o t p l a n t stage i s thus e s s e n t i a l i n the s c a l e - u p of any new polymer p r o c e s s . L a b o r a t o r y f a c i l i t i e s , though h i g h l y f l e x i b l e normally lack precise c o n t r o l or d e t a i l e d intrumentation; p l a n t f a c i l i t i e s , much l a r g e r i n s c a l e , w e l l i n s t r u m e n t e d and o f t e n d a t a l o g g e d , a r e geared t o p r o d u c i n g a s e t p r o d u c t range w i t h r e l a t i v e l y u n s k i l l e d labour. A w e l l equipped p i l o t f a c i l i t y c o n t a i n s a l l t h e p h y s i c a l elements o f p r o d u c t i o n equipment e n a b l i n g m i x i n g , heat t r a n s f e r and p a r t i c u l a r l y s a f e t y f a c t o r s t o be examined, and has q u a l i f i e d p e r s o n n e l w i t h a f l e x i b l e and e n q u i r i n g approach t o examine t h e p r o c e s s and observe and r e c o r d a t a l l s t a g e s . W i t h t h e i n t r o d u c t i o n o f more s o p h i s t i c a t e d p r o c e s s e s and the c o m p u t e r i s a t i o n o f l a r g e r s c a l e r e s i n p l a n t ( r e f . l ) the r o l e o f the p i l o t p l a n t has become even more c r u c i a l , s i n c e v e r y p r e c i s e d e f i n i t i o n o f p r o c e s s parameters can be e x p l o i t e d f o r enhanced p r o d u c t i v i t y and q u a l i t y . 0097-6156/89/0404-0454S06.00/0 ο 1989 American Chemical Society

In Computer Applications in Applied Polymer Science II; Provder, T.; ACS Symposium Series; American Chemical Society: Washington, DC, 1989.

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A d d i t i o n a l l y , our e x p e r i m e n t a l regime now i n c l u d e s e x t e n s i v e use of computer m o d e l l i n g of the p o l y m e r i s a t i o n p r o c e s s and we need t o e x t r a c t c h e m i c a l , t h e r m a l and e n g i n e e r i n g d a t a f o r model assembly, v e r i f i c a t i o n and f o r f i n a l p r o c e s s improvement. I n I C I a t Slough we have developed o u r own approach t o the c o n t r o l and d a t a a c q u i s i t i o n p r o c e s s used on o u r s e m i - t e c h n i c a l r e a c t o r s .


The P i l o t P l a n t and I t s R o l e The main r o l e o f p i l o t p l a n t i s i n t h e s c a l e - u p of polymer f o r m u l a t i o n s from l a b o r a t o r y t o f u l l s c a l e p r o d u c t i o n and t h e development o f new p r o c e s s e s and t e c h n i q u e s , i n c l u d i n g t r i a l s o f new equipment. The l a b o r a t o r y i s n o r m a l l y where t h e c h e m i s t r y of new p r o d u c t s and p r o c e s s e s i s i n v e s t i g a t e d and e s t a b l i s h e d . When s c a l e - u p i s contemplated, t h e use of commercial q u a l i t y m a t e r i a l s w i l l n o r m a l l y be i n v e s t i g a t e d , t e s t p r o c e d u r e s e s t a b l i s h e d and c e r t a i n p r o c e s s i n g t o l e r a n c e s examined. An e x p e r i e n c e d chemist can f r e q u e n t l y l e a r n much on t h e l a b o r a t o r y s c a l e t h a t w i l l i n d i c a t e l i k e l y s c a l e - u p b e h a v i o u r , b u t i t i s always prudent t o then go through the p i l o t stage b e f o r e embarking on f u l l s c a l e p r o d u c t i o n . C o m p u t e r - c o n t r o l l e d p l a n t can now make a l l o f the r e s i n s mentioned i n the i n t r o d u c t i o n above i n o u r own p l a n t s where we use a modular approach t o s o f t w a r e , g i v i n g g r e a t f l e x i b i l i t y i n p r o c e s s stage sequencing. A p a r t i c u l a r requirement f o r s o f t w a r e d e f i n i t i o n i s a complete u n d e r s t a n d i n g and c h a r a c t e r i s a t i o n of a l l p r o c e s s s t a g e s , and i n our own e x p e r i e n c e has n e c e s s i t a t e d c o n s i d e r a b l e e f f o r t , though t h e f i n a l b e n e f i t s i n p r o d u c t i v i t y , p r o d u c t q u a l i t y and c o n s i s t e n c y and s a f e t y have been c o n s i d e r a b l e . T h i s has been r e p o r t e d by o t h e r s ( r e f . 2 . ) . F o r new p r o d u c t s the n e c e s s a r y c h a r a c t e r i s a t i o n i s n o r m a l l y a c q u i r e d a t t h e p i l o t p l a n t s t a g e , and hence t h i s i s t h e v i t a l d a t a a c q u i s i t i o n p e r i o d i n s c a l e - u p . Thus f o r a s e m i - t e c h n i c a l p l a n t , even where p r o c e s s e s a r e s i m p l e and manning and s k i l l l e v e l s h i g h , t h e r e must be f u l l d a t a r e c o r d i n g and retrieval facilities. Normal methods (manual t a b u l a t i o n , c h a r t r e c o r d e r s ) can f r e q u e n t l y l a c k a u t h e n t i c i t y , permanence o r v e r y o f t e n t h e r e c o r d i n g of t h e r i g h t parameters. T h i s l a t t e r i s where we b e l i e v e our p i l o t r e a c t o r s t o have t h e c o r r e c t approach i n l o g g i n g a l l d a t a p o i n t throughout t h e b a t c h , r a t h e r than b e i n g s e l e c t i v e b e f o r e t h e event. The d a t a g a t h e r i n g a c t i v i t y i s t h e most v i t a l p a r t of t h e s c a l e - u p p r o c e s s and hence of t h e p i l o t p l a n t . When t h e f i r s t of our new p i l o t p l a n t s was designed we had t h e o p t i o n o f f u l l computer c o n t r o l . We d e c i d e d t o i n s t a l l s t a n d - a l o n e s o l i d s t a t e c o n t r o l l e r s and s a f e t y systems t o a l l o w t h e f u l l e s t o p e r a t i n g f l e x i b i l i t y and t h e b e s t p o s s i b l e d a t a r e t r i e v a l . The computers chosen f o r the l a t t e r have t h e c a p a b i l i t y when we w i s h t o c o n t r o l temperature, p r e s s u r e o r feeds u s i n g our own a l g o r i t h m s . For i n s t a l l a t i o n s now, the c h o i c e may be more d i f f i c u l t , i n t h a t p o w e r f u l computer c o n t r o l and l o g g i n g packages f o r t h i s type o f a p p l i c a t i o n a r e becoming a v a i l a b l e . E q u a l l y however, d i s c r e t e s o l i d s t a t e c o n t r o l l e r s a r e a l s o becoming v e r y s o p h i s t i c a t e d , w i t h m u l t i s t a g e programmable ramping and s e l f - t u n i n g now a v a i l a b l e .


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A g a i n s t h i g h l e v e l s o f computer c o n t r o l i s the p r e - b a t c h p r e p a r a t i o n time r e q u i r e d f o r s e q u e n c i n g , s o f t w a r e w r i t i n g and parameter s e t t i n g , the f u l l d e t a i l s o f t h e l a t t e r o f course o f t e n n o t a v a i l a b l e . T h i s a c t i v i t y i s a c c e p t a b l e as a p r e c u r s o r t o f u l l s c a l e p r o d u c t i o n b u t i s f e l t r e s t r i c t i v e and c o u l d i n h i b i t f l e x i b i l i t y i n a p i l o t p l a n t . The f i r s t p l a n t we designed was a c o m p l e t e l y new i n s t a l l a t i o n , h a v i n g a 2 5 0 - l i t r e i n d u c t i o n heated r e a c t o r w i t h a n c i l l a r y v e s s e l s f o r f e e d s , a t h i n n i n g / e m u l s i f y i n g v e s s e l and overheads f o r d i s t i l l a t i o n , c o n d e n s a t i o n and s e p a r a t i o n ( r e f . 3 ) . A v i e w o f t h i s p l a n t showing c o n t r o l room, r e a c t o r and t h i n n i n g v e s s e l i s g i v e n i n F i g u r e 1. We have now a l s o r e f u r b i s h e d a 120L w a t e r - j a c k e t t e d r e a c t o r , a g a i n equipped w i t h feed v e s s e l s , though w i t h fewer a n c i l l a r y f a c i l i t i e s , but w i t h t h e same l o g g i n g package and much more advanced c o n t r o l l e r s . Key

Requirements

A t t h e d e s i g n s t a g e , f a c t o r s we c o n s i d e r e d t o be paramount were: h e a t i n g and c o o l i n g demands, a c c u r a c y o f measurement and t h e c o n t r o l equipment, and d a t a l o g g i n g . Heating Cooling The 250L r e a c t o r makes b o t h h i g h and l o w temperature polymers i n s o l u t i o n and d i s p e r s i o n , i n c l u d i n g those t h a t are temperature s e n s i t i v e . A h i g h heat i n p u t was s p e c i f i e d f o r o p e r a t i n g e f f i c i e n c y , w i t h complementary e f f e c t i v e c o o l i n g by b o t h c o i l and condenser t o c a t e r f o r h i g h l y e x o t h e r m i c r e a c t i o n s ; tempered c o o l i n g was s p e c i f i e d f o r h i g h m e l t i n g p o i n t / c r y s t a l l i s i n g p r o d u c t s . E l e c t r i c a l i n d u c t i o n h e a t i n g was chosen, s i n c e i t l e n d s i t s e l f t o p r e c i s e c o n t r o l o f heat i n p u t . I t o p e r a t e s here over t h r e e zones, a l l o w i n g heat t o be d i s t r i b u t e d over t h e optimum h e a t i n g s u r f a c e w i t h good c o n t r o l o f w a l l t e m p e r a t u r e s . The w a t e r - j a c k e t t e d r e a c t o r r e t a i n e d i t s w a t e r c i r c u l a t i n g loop w i t h steam i n j e c t i o n f o r h e a t i n g and w a t e r feed f o r c o o l i n g ; t h e o n l y m o d i f i c a t i o n s were f o r heat b a l a n c e p u r p o s e s , as w i l l be d e s c r i b e d . A c c u r a c y A d e t a i l e d study o f o v e r a l l c h a r g i n g a c c u r a c y r e q u i r e m e n t s r e l a t e d t o t y p i c a l p r o d u c t s has been c a r r i e d out f o r o u r c o m p u t e r - c o n t r o l l e d p l a n t d e s i g n ; we used t h e d a t a f o r t h i s p l a n t , and r e l a t i n g p a r t i c u l a r l y t o f e e d i n g , we s p e c i f i e d i n one i n s t a n c e a l o a d c e l l r e s o l u t i o n o f 0.005% FSD (1:20,000), n e c e s s i t a t i n g h i g h e r than normal e x p e n d i t u r e on t h i s i t e m (and some d i s t r e s s t o t h e i n s t r u m e n t e n g i n e e r s ! ) , b u t now f u l l y j u s t i f i e d by t h e r e s u l t . S p e c i a l l y c o n s i d e r e d were items e s s e n t i a l t o heat b a l a n c e , i . e . t e m p e r a t u r e , f l o w and e l e c t r i c a l power measurement. The r e a c t o r c o n f i g u r a t i o n f o r heat b a l a n c e i s i l l u s t r a t e d i n F i g u r e 2. Batch temperature a c c u r a c y was c o n s i d e r e d s a t i s f a c t o r y a t ±0.5°C, a f t e r t a k i n g i n t o account t h e k i n e t i c f a c t o r s i n v o l v e d . Control A g a i n , c o n s i d e r i n g t h e k i n e t i c r a t e c o n s t a n t s and t h e c o n t r o l r e q u i r e m e n t s f o r p o l y m e r i s a t i o n r e a c t i o n s , a range o f c o n t r o l modes were s p e c i f i e d as summarised i n T a b l e I , w i t h ±1°C temperature c o n t r o l c o n s i d e r e d t i g h t enough, b u t w i t h u n u s u a l l y l a r g e r e g u l a t o r ranges. As t h e t a b l e shows, s o p h i s t i c a t e d ramping and s e l f - t u n i n g c o n t r o l l e r s have been f i t t e d t o t h e w a t e r - j a c k e t t e d r e a c t o r ; these have been p a r t i c u l a r l y s u c c e s s f u l .



Figure 1. M u l t i f u n c t i o n a l Reactor View showing c o n t r o l room, r e a c t o r (beneath o p e r a t o r ) and thinning vessel.


in

53

ft.

b

M H

W

in


τ

F i g u r e 2. M u l t i f u n c t i o n a l R e a c t o r L i n e Diagrams Showing s e n s o r s f i t t e d , p a r t i c u l a r l y f o r heat balance.

τ


Q 2 Q

C/3

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TABLE I .

459

P l a n t C o n t r o l l e d Items

Function

Control

F a c i l i t i e s , Comments

Temperature

Batch c o n t r o l

Induction heating (1) C o i l Cooling (1) Water j a c k e t , steam i n j e c t i o n heating (2) S e l f - t u n i n g , Cascade (2)

or or

Pressure

(1)

Temperature L i m i t Ramped change of s e t p o i n t Reflux Control (1) Tempered c o o l i n g (1) J a c k e t or Zone S e l e c t W a l l temp c o n t r o l (1)

w i t h temp.

Limiting

S t a t i c c o n t r o l or v e n t e d Ramped change of s e t p o i n t P r o f i l e change

Feed

Feed r a t e

Solvent Fractionating Column

R e t u r n temperature Head temperature

(1) (2)

(1) (1)

(2)

D i s t i l l e d pumpback

I n d u c t i o n heated g e n e r a l purpose p l a n t o n l y Water-jacketted reactor only

Data L o g g i n g A l l d a t a was t o be gathered from a l l i n s t r u m e n t s i n d i s c r i m i n a t e l y a t a s i n g l e b e a t , d i s p l a y e d d u r i n g the b a t c h and r e c o r d e d f o r s c r u t i n i t y post b a t c h . Items d a t a - l o g g e d are l i s t e d i n Table I I . The Data-Logging And A n a l y s i s System We s p e c i f i e d and wrote our own l o g g i n g and d a t a r e t r i e v a l packages. The equipment used i s the H e w l e t t - P a c k a r d HP3497A d i g i t a l v o l t m e t e r / d a t a a c q u i s i t i o n u n i t u s i n g HP9816S computers w i t h a s s o c i a t e d d i s k d r i v e s , p r i n t e r and p l o t t e r . A n a l y s i s i s c a r r i e d out u s i n g a H e w l e t t - P a c k a r d HP98581B computer. L o g g i n g The emphasis i s on g i v i n g the most u s e f u l d i s p l a y e d i n f o r m a t i o n , commensurate w i t h c a r r y i n g out the p r i m a r y l o g g i n g t a s k . The l o g g i n g computer e x p l o i t s a l l the f a c i l i t i e s , e s p e c i a l l y g r a p h i c s and the speed of the HP system, w i t h a chosen c a p a b i l i t y of p e r f o r m i n g a l l f u n c t i o n s up t o a speed of t e n times a minute (every six sees).


460


TABLE I I . R e a c t o r temperatures

Data Logged Items Batch Wall Vapour s t a c k D i s t i l l a t e return

Other temperatures

Coil/jacket

(1)

in/out

Condenser water i n / o u t

(1)

Reactor

(1)


Pressure Flow r a t e s Water, steam Speed, power

N i t r o g e n sparge

Weights

Stirrer

(1)

P l a t f o r m s f o r feeds Set p o i n t s & R e g u l a t o r

outputs Heating, c o o l i n g , feeds N i t r o g e n ( 1 ) , Vacuum (1) R e a c t o r e l e c t r i c a l heat i n p u t ( l ) C o i l / j a c k e t heat b a l a n c e Condenser heat e x t r a c t r a t e (1) R e a c t o r heat l o s s 80 (1) 30 (2)

Calculations

Total points (1) (2)

I n d u c t i o n - h e a t e d g e n e r a l purpose p l a n t o n l y Water-jacketted reactor only.

The l o g g i n g computer w i t h monochrome d i s p l a y c a r r i e s out t h e f o l l o w i n g tasks concurrently: a c q u i s i t i o n and c o n v e r s i o n t o e n g i n e e r i n g u n i t s o f 60 p l a n t items ( p o t e n t i a l l y 100). c a l c u l a t i o n o f up t o 18 v a l u e s d e r i v e d from t h e above ( t y p i c a l l y heat b a l a n c e ) p o s s i b i l i t y o f two c o n t r o l o u t p u t s t o p l a n t l o g g i n g t o 3h" d i s k o f b o t h p l a n t d a t a and c a l c u l a t i o n s g r a p h i c a l t r e n d i n g d i s p l a y o f t h e l a s t 240 r e a d i n g s o f any i n p u t " c o n t i n u o u s l y " updated d i s p l a y o f any s e l e c t e d i n p u t (1/10 second b e a t ) . message l o g g i n g s f o r f u t u r e graph a n n o t a t i o n The t a b u l a r d i s p l a y o f p l a n t items i s a r r a n g e d i n f o u r pages o f 20 i t e m s , grouped f o r l o g i c a l study o f p a r t i c u l a r types o f p r o c e s s . S e v e r a l a l t e r n a t i v e g r o u p i n g s can be c o n f i g u r e d t o c a t e r f o r s p e c i a l o p e r a t i o n a l needs.


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The lower h a l f o f t h e s c r e e n i s always a v a i l a b l e , t o show e i t h e r t h e l a s t and c u r r e n t messages b e i n g e n t e r e d o r a c o n t i n u o u s l y updated v a l u e of any chosen parameter when e x p e c t i n g r a p i d change o r t u n i n g or s t u d y i n g s i g n a l problems such as ' n o i s e . The graphed d i s p l a y can show 60, 120, 180 o r 240 l a s t time p o i n t s and t h e y a x i s s c a l e and span can be chosen a t w i l l , t o 'magnify changes. 1


1

The computer does n o t d i s p l a y alarms o r l i m i t v a l u e s and by i n t e n t i o n , t r i p s a r e independent. T h i r t y seconds i s t h e normal l o g g i n g i n t e r v a l as t h i s i s c a p a b l e of showing the d e t a i l o f t h e most abnormal change, e.g. runaway exotherm. However, i n t e r v a l s as c l o s e as s i x seconds a r e p o s s i b l e . L o g g i n g can be c o n t i n u o u s f o r up to 24 h o u r s , a l l o w i n g around 400,000 d a t a p o i n t s t o be r e c o r d e d p e r batch/disc. Messaging T h i s was f e l t t o be v a l u a b l e f o r our a p p l i c a t i o n t o mark p r o c e s s stage changes a c c u r a t e l y on t h e time a x i s ; a manual l o g i s s t i l l kept o f c h a r g e s , p r o c e s s s t e p s , t e s t r e s u l t s and comments, and though a t some stage these c o u l d be logged as t e x t f i l e s , t h i s i s n o t a c u r r e n t i n t e n t . Message e n t r y does n o t i n t e r r u p t t h e c o l l e c t i o n o f raw d a t a . Data A n a l y s i s F o r post a n a l y s i s the f o l l o w i n g t a s k s a r e a v a i l a b l e on the same o r another s i m i l a r computer:

-

s c r e e n o r hard copy m u l t i c o l o u r g r a p h i c a l p l o t o f any i t e m , w i t h c h o i c e of span o f range and time o v e r l a y of f u r t h e r parameter p l o t s on graph s t o r a g e o f graphs i n computer memory f o r " i n s t a n t " r e t r i e v a l e d i t i n g and s e l e c t i o n o f messages f o r d i s p l a y s u p e r i m p o s i t i o n o f messages on graph t a b u l a t i o n o f measured v a l u e s s t a t i s t i c a l a n a l y s i s of parameters i n t e g r a t i o n o f a r e a under c u r v e s u s e r d e f i n e d c a l c u l a t i o n s on t h e raw d a t a , e.g. r e v i s e d heat balance c a l c u l a t i o n s .

F i g u r e 3 shows an example o f g r a p h i c a l d i s p l a y of parameters w i t h s e l e c t e d messages added on a c o r r e c t t e m p o r a l a x i s . These f a c i l i t i e s a r e b e i n g added t o , as t h e need a r i s e s . I t was deemed e s s e n t i a l t h a t c h e m i s t s who might n o t be computer l i t e r a t e o r s p e c i a l l y t r a i n e d s h o u l d be a b l e t o use t h e i n t e r r o g a t i o n package i n a f a s t , easy and f l e x i b l e manner t o get the p r e c i s e i n f o r m a t i o n needed. The emphasis i s on u s e r f r i e n d l i n e s s , a much over-used term, but here e x e m p l i f i e d i n t h e f o l l o w i n g ways: r a p i d r e a d i n g i n o f complete b a t c h d a t a from d i s c s t o r a g e ( i n 60 seconds) a l l d a t a from one b a t c h i s p l a c e d i n computer memory i n a r r a y s i n RAM (1 meg b y t e r e q u i r e d ) f o r i n s t a n t a c c e s s easy c h o i c e o f s c a l e on g r a p h i c a l d i s p l a y s r a p i d p a i n t i n g of graphs on s c r e e n


In Computer Applications in Applied Polymer Science II; Provder, T.; ACS Symposium Series; American Chemical Society: Washington, DC, 1989. ^ -
Urethane Feed a l c o h o l i n t o i s o c y a n a t e over 2 hours A l l o w temperature t o r i s e t o 100°C, then h o l d a t 95°C Heat o f R e a c t i o n 9 K c a l s / m o l Heat o f R e a c t i o n T o t a l 10380 K c a l s Heat i n p u t by I n d u c t i o n Heater 1520 K c a l s


11900 K c a l s Heat Heat Heat Heat

up Charge from 20°C up Feed from 20°C up V e s s e l form 20°C removed by C o o l i n g C o i l

3270 3970 3320 1950

K K K K

cals cals cals cals

12510 K c a l s

F i g u r e 5 shows t h e c a l c u l a t e d heat i n p u t and c o o l i n g c o i l heat removal r a t e s i n KW, t h e l a t t e r c a l c u l a t e d from water f l o w and temperature d i f f e r e n t i a l by t h e computer when l o g g i n g . As i s t y p i c a l w i t h n o n - r e f l u x p r o c e s s e s , a c t u a l heat i s w i t h i n 5% o f t h a t expected from t h e t h e o r e t i c a l heat o f r e a c t i o n . F u t u r e Enhancements C o n s i d e r a b l e e f f o r t i s b e i n g spent r e f i n i n g the heat b a l a n c e f a c i l i t i e s , and e x t e n s i v e work i s now g o i n g i n t o t h e c h a r a c t e r i s i n g and m o d e l l i n g o f e x i s t i n g and f u t u r e polymers. O n - l i n e a n a l y s i s and p h y s i c a l p r o p e r t y measurements a r e now b e i n g i n s t a l l e d w h i c h , l i n k e d to p r e d i c t i v e s o f t w a r e w i l l extend our c o n t r o l s t r a t e g i e s t o a r e a s such as c o n t r o l l e d comonomer a d d i t i o n r a t e s t o c o n t r o l polymer s t r u c t u r e and c o n d e n s a t i o n polymer end p o i n t c o n t r o l . The computer package w i l l n o t need e x t e n s i o n t o h a n d l e t h e s e . Summary We have d e s c r i b e d two h i g h l y i n s t r u m e n t e d , d a t a - l o g g e d and v e r s a t i l e p i l o t r e a c t o r s which i n t e g r a t e i n t o a r i g o r o u s s c a l e - u p regime. T h i s i s n e c e s s i t a t e d by o u r h i g h l y complex p r o d u c t s and t h e p r e c i s e d e f i n i t i o n t h e c o m p u t e r - c o n t r o l l e d f u l l - s c a l e p l a n t can e x p l o i t . Our whole package i s in-house s p e c i f i e d and w r i t t e n , and w h i l e we are aware t h a t complete packages t o d a t a - l o g a r e now a v a i l a b l e , we f e e l c o n f i d e n t i n showing t h i s as an example of a h i g h t e c h n o l o g y s t a t e - o f - t h e - a r t system. Examples o f d a t a e x t r a c t e d f o r heat b a l a n c e , and comparison t o s i m p l e models can be demonstrated. F i n a l l y , i n l o g g i n g a l l p a r a m e t e r s , t h e a c q u i s i t i o n o f a growing a r c h i v e o f d a t a i s a v a l u a b l e and e x p l o i t e d a s s e t .



0 Mins: 0 Time: 11:41

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14

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kω

40 12:21

60 12:41

80 13:01

100 13:21

HEATER

CALCULATED

19BB

120 13:41

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BY

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INDUCTION

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CALCULATED

heatbal

4 F.b

F i g u r e 5. D i r e c t h e a t b a l a n c e element p l o t s f o r C r o s s l i n k e r Preparation. C a l c u l a t e d i n d u c t i o n h e a t e r i n p u t and c o o l i n g c o i l heat r e m o v a l r a t e s .

20 12:01

-X-LINKER

COOLING COIL

βΤΙβ'ΒχΒΙΙ


160 14:21

468


Literature Cited 1. · 3. 4. 2

The Chemical Engineer No. 388, May 1983, 85-87. Polymer Paint Colour Journal, November 30, 1983, 173, 786-790 Polymer Paint Colour Journal, May 14, 1986, 176, 366-367 Proceedings of Conference 'Technical for the Control and Prevention of Runaway Chemical Reaction Hazards', London Dec. 1987.


RECEIVED February 14, 1989


Computer Data Logged Pilot-Plant Reactors - American Chemical

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