5

. f

I D 0 -14486 Page 3-4

THE DETERMINATION OF EXCESSIVE EMULSIFICATION BY COALESCENCE BEHAVIOR MEASUREMENTS

by

0. W . P a r r e t t

Chemical Development Sect ion CPP Technical

PHILLIPS PETROLEUM COMPANY Atomic Energy Division Idaho F a l l s , Idaho

Contract AT( 10-1) -205

IDAHO OPERATIONS OFFICE U . S . Atomic Energy Commission

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document.

-+i ':7 .

i

"I, .- -I

ID0 -14486 Page 5-6

THE DETERMINATION OF EXCESSIVE EMULSIFICATION BY COALESCENCE BEHAVIOR MEASUREMENTS

0. W. P a r r e t t

A B S T R A C T

The development of a remotely operated device for determining the coalescence times of p lan t process streams suspected of containing sur fac tan ts such as s i l i c i c compounds and f i s s i o n product zirconium compounds i s described.

A general cor re la t ion between the coalescence t i m e s of p i l o t p l a n t ex t r ac t ion column aluminum n i t r a t e feeds and 3.25 percent t r i b u t y l phos- phate e x t r a c t a n t streams and the observations of column behavior of these streams i s demonstrated.

The appl ica t ion of t h e coalescence t e s t t o p lan t streams i s given.

Work done under Contract AT(10-1)-205 t o t h e U.S. Atomic Energy Commission,

THE DETERMINATION OF MCESSI-V'E EMULSIFICATION BY COALESCENCE BEHAVIOR MEASURmNTS

0. W. P a r r e t t

TABLE OF CONTENTS

ID0 -14486 Page 7

A . Laboratory Emuls i f ica t ion T e s t D O . . D ~ O D O . D ~ O ~ . D D . D O ~ ~ ~ ~ ~ ~ 10 B. Remote Apparatus f o r P l a n t Feed Tes t ing . . O O O . a O 13

A . Cor re l a t ion of Coalescence Behavior t o P i l o t P l an t Column Observations . . . ~ O . ~ D ~ ~ . ~ . O ~ ~ O O O . ~ ~ . ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 13

B. Coalescence Measurements of P l a n t Streams e e . .*. . 19

1. Coalescence Behavior of Untreated P lan t Streams D D s o 19 2. Coalescence Behavior of Gela t in Treated P lan t

Streams D . ~ ~ . . . O . O . D . . O ~ O . ~ O ~ ~ ~ ~ ~ ~ ~ * ~ . ~ ~ ~ . ~ . ~ ~ ~ ~ . ~ ~ ~ 20 3. Coalescence Behavior w i t h H i g h S i l i c o n Low

Zirconium P lan t Stream ............................. 20

V . CONCLUSIONS ...................................................... 20

V I . LITERATURE CITED .................................................. 22

1. CORRELATION OF PILOT PCLANT AND COALJ3SCENCE TEST DATA- D o - * 23 2. THE C3MFARISOni OF THX COALESCENCE BEHAVIOR OF FEEDS

AND RAFF'INATES. O . O O . . . . . ...* e . . . . . O . . O . . a a e e .. 25

ID0 -14486 Page 8

LIST OF FIGURES

LIST OF TABUS

1. THE CORRELATION OF DISPERSION-COALESCENCE MEASUREMENTS TO PILOT PLANT COLUMN OBSERVATIONS a - o e o L ) o p o D o o D o . . . e e 16

, --

ID0 -14486 Page 9

THE DETERMi'SJATION OF MCESSIYE EMULSIFICATION BY COALESCENCE BEHAiiIOR MEASUREMENTS

0 . W. P a r r e t t

I, SUMMARY

A s an a i d t o the successful processing of aluminum-uranium reac tor f u e l s containing surfactant-producing materials, it has been des i rab ie t o determine the emulsifying t rends of the feed streams p r i o r t o t h e i r e n t r y i n t o the ex t r ac t ion cycle with a laboratory measurement of t h e i r coalescence behavior. The coalescence behavior of these streams w a s determined by measuring t h e i r coalescing time and observing the appearance of t he emulsions formed by the surfactant-containing feeds and solvents , For t h i s purpose a remotely operated emulsion s t a b i l i t y ind ica to r w a s i n s t a l l e d i n the p lan t a n a l y t i c a l f a c i l i t i e s .

A co r re l a t ion was developed between ex t rac t ion column operab i l i t y i n the presence of sur fac tan ts and the coalescence behavior by the comparison of observations of the degree of emulsif icat ion experienced i n 97 p i l o t p l an t solvent ex t rac t ion experiments with a v a r i e t y of feed compositions and the corresponding laboratory coalescence behavior of t he end streams. I n these cold t e s t s , it w a s shown t h a t ex t rac t ion systems with equilibrium coalescence times of g rea t e r than 600 seconds were inoperable a t volume v e l o c i t i e s of 500 gal /hr f t , t h a t systems with coalescence t i m e s between 100 and 300 seconds were operable and systems with coalescence times i n the i n t e r v a l of 300 to 600 seconds were in f r e - quently observed and thus not r ead i ly cor re la tab le

2

Although determinations on p lan t samples were f requent ly confused by the appearance of a r e s idua l s t ab le f i l m (termed "spider web") a f t e r t r u e coalescence, general t rends of ex t r ac t ion column ope rab i l i t y were observed with the measuremen t s , It w a s concluded tha t these coalescenee time measurements of p lan t streams could be a valuable a i d i n pred ic t ing p l an t ex t r ac t ion column behavior w i t h surfactant-containing feeds .,

11, .L'NTRODUCTION

The highly surface-act ive feeds t h a t a r e produced i n the chemical reprocessing of s i l icon-containing alminum-uranium f u e l s have led t o e x t r a c t i o n column operat ing problems e

Plant column end stream analys is and column cont ro l instrumentation records have indicated varying degrees of flooding culminating i n forced processing r a t e reduction below ext rac t ion column volume v e l o c i t i e s of 300 gal /hr f t 2 t o regain column s t a b i l i t y . i n t e r f a c i a l crud was in fe r r ed but could not be observed.

The accumulation of excessive

IDO -14486 Page 10

These e r r a t i c operations have indicated the presence of surface-active mater ia l s i n the p lan t stream , such as s i l i c i c compounds o r f i s s i o n product zirconium compounds(ly the responsible sur fac tan t has necess i ta ted the development of an a n a l y t i c a l t o o l by which a quant i ta t ive measurement of t he excessive emulsive tendencies of t h e p l an t streams could be determined. L

However, the i n a b i l i t y t o i s o l a t e and analyze

I

It w a s found t h a t by co r re l a t ing the laboratory determined coalescence behavior of p i l o t p lan t streams with t h e i r a c t u a l column performance, the emulsifying t rends of these streams could be determined p r i o r t o t h e i r en t ry i n t o the ex t rac t ion cycle. The coalescence behaviors of these p i l o t p lan t streams w e e determined by a laboratory tes t t h a t w a s o r i g i n a l l y developed a t HanfordS2) ., These coalescence behavior determinations consis ted o f , (1) the coalescence time, o r the t i m e required f o r a l iqu id- l iqu id system, t h a t has been dispersed f o r a given length of t i m e , t o disengage; ( 2 ) the observations t h a t were made concerning the physical cha rac t e r i s t i c s of the emulsion and, ( 3 ) the proper t ies of any r e s idua l formation.

U t i l i z i n g the r e l a t ionsh ip between laboratory determined coalescence behavior and ex t r ac t ion column behavior, a study w a s made t o e s t a b l i s h the emulsifying t rends of p lan t ex t r ac t ion column feeds t o v h a t e preventat ive measures, such a s ge l a t in treatrnent(3) o r ac id a d d i t i o n 7 17

111. EQUIPMENT DESCRIPTION

A . Laboratory Emulsif icat ion T e s t

The coalescencebehavior of the process s t r e a m w a s observed by a standard t e s t with an emulsion s t a b i l i t y ind ica tor . This instrument w a s adapted f om the laboratory s ingle-s tage pulsed contactor developed a t

pers ion and coalescence times of a l iqu id- l iqu id system. T h i s t es t w a s o r i g i n a l l y made with an instrument consis t ing of a wire screen which,when mved i.n r ap id o s c i l l a t i o n across the l iqu id- l iqu id interface, produced a dispers ion which i s aqueous continuous i f the screen were p r e f e r e n t i a l l y aqueous-wetted o r organic continuous -if the screen were p r e f e r e n t i a l l y organic-wetted. A miniature pulse column i s created by replacing the screen with four small perforated plates,having holes 0,47 inches i n diameter and a3tached concentr ical ly t o a 0.0625 inch s t a i n l e s s s t e e l rod,spaced 0,25 inches apa r t . vesse i . With t h i s apparatus, (See Figure 1) it is possible t o measure with a 5 percent reproducib i l i ty the t i m e required f o r a complete dispers ion, t he coalescence time,and t o determine the e f f e c t of aging, temperature, and impuri t ies on these quan t i t i e s ,

HanfordC 27 which u t i l i z e d the v ib ra t iona l disengaging t e s t t o measure d i s -

A 25 m i l l i l i t e r graduated cyl inder i s used as the mixing

The dispers ion time i s defined as the time required f o r a dispers ion t o form from the in t e r f ace t o t he dispers ion l e v e l , the 23 m i l l i l i t e r mark on the graduated cyl inder . The c h a r a c t e r i s t i c s of the normal dispers ion a r e shown i n Figure 2, The coalescence time i s defined as the t i m e required f o r

Graduated Mixing Vessel

IDO- 14486 Page 11

Plunger Stor

NRTS 59-4046

FIGURE 1 - ENKLSION STABILITY INDICATOR from the laboratory single stage pulsed contactor.

T h i s instrument was adapted

IDO-14486 Page 12

Dispersion l e v e l

23 ml.

Coalescence l e v e l

15 ml

FIGURF: 2 - NORMAL DISPERSION This sample was dispersed i n 20 seconds. Dispersion time i s time required t o form an emulsion from t he in t e r f ace t o the d ispers ion l e v e l . (NRTS 59-4142)

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a d tspers ion t h a t has been formed by mixing f o r 30 seconds, t o disengage from t h e top of t he l i qu id , 25 m i l l i l i t e r mark, t o the disengaging l e v e l , t he 1-5 m i l l i l i t e r m a r k . The c h a r a c t e r i s t i c s of the normal coalescence are shown i n Figure 3.

B o Remote Apparatus f o r Plant Feed Test ing

A remote emulsion s t a b i l i t y ind ica tor was developed t o measure t h e d ispers ion times and coalescence t i m e s of highly rad ioac t ive streams p r i o r t o t h e i r en t ry i n t o t h e columns i n order t o p red ic t the tendencies of these p l an t streams t o form s t ab le emulsions i n t i m e t o take preventa- t i v e measures necessary t o insure the proper operat ion of the column,

The remote apparatus i s shown i n Figure 4, Basica l ly the remote instrument i s the same as the laboratory model with the following exceptions: i n p l an t sampling, an adaptat ion w a s needed t o t r a n s f e r t he feeds and

Fxtraztants f romthe sample b o t t l e s t o the mixing vesse l , A standard needle system w a s employed with one l i n e running t o the graduated mixing vesse l and another l i n e going t o the ex te rna l ly operated syringe v i a a t r a p , The a i r pressure provided by the syringe was used t o push the l i q u i d t o the mixing vessel . A platform was supplied t o raise and lower the sample b o t t l e s onto t h e needles, ac t ion pneumatic cy l inder , Less than one m i l l i l i t e r i s l e f t i n the sample b o t t l e s , mum, a wash system w a s u t i l i i e d cons is t ing of n i t r i c ac id , water, and acetone, i n t h a t o rder , I n t h i s way only one graduated cyl inder i s used and t h i s i s equipped with a drainage o u t l e t that i s valved by means of a pneumatically-operated pinchclamp, Separate syringes used for- the aqueous feed and , for the ex t rac t ion to prevenr; c ross contamination. The o s c i l l a t i o n i s provided. i n t h e same manner as the labora tory equipment 'except t he s top pos i t ion ing is obtalned by an a i r operated cy l inger ,

I n order t o handle the conical shaped sample b o t t l e s used

-

This platform system i s operated by a double

I n order t o keep the necessary manipulation t o a mini-

IV, RESULTS

A. Correlat ion of Coalescence Behavior t o P i l o t P lan t Column Observations

I n order t o determine the effect of e x i s t i n g su r fac t an t s upon the ex t r ac t ion process , it w a s necessary t o observe t h e columns during operat ion. Therefore, a series of experiments was designed t o simulate p l an t condi t ions. These p i l o t p l an t experiments(4) u t i l i z e d tLe continuous d i s so lu t ion of n a t u r a l uranium f u e l s t o provide p l an t - l i ke process streams. evaporation s t e p w a s included i n order t o simulate full-lscale blending of scrub e f f l u e n t and d isso lver e f f l u e n t . i n diameter, made up the ex t r ac t ion cycle which consis ted of ex t r ac t ion , scrub, and s t r i p columns. solvent c lean up

A head-end

Three g l a s s columns, two inches

Two mixer-set t lers were provided f o r extrackion

IDO- 14486 Page 14

Top of l i q u i d

25

Organic phase

Interface

Aqueous phase

11 ml

Dispersion level

23

Coalescence level

15

FIGURE 3 - N O W COALESCENCE The coalescence time was 100 seconds. emulsion to disengage from the top of the liquid to the coalescence level, 15 milliliter mark.

This sample was dispersed fo r 30 seconds. This is the time required for the

IDO-14486 Page 1 5

Plunger stop

Needle system sample t r a n s f e r

Wash system - nitric acid, water, acetone

Sample platform for- raising and lowering sample bot t 1 e s

Plunger

Pneumatic pinchclamp

NFX’S 59-3998

FIGURF: 4 - THE REMOTE ENULSION STABILITY INDICATOR

ID0 -14486 Page 16

The dispersion and coalescence times of samples of the feeds and ex t r ac t an t s were measured pe r iod ica l ly with the emulsion s t a b i l i t y i n d i - ca tor (See Figure 1) and the corresponding behavior of the system w a s observed i n the p i l o t p l an t g l a s s columns. t o be in sens i t i ve t o the observed emulsifying t rends of the column and were ignored; however, a d e f i n i t e re la t ionship was experienced using the coales- cence times. with excessive emulsif icat ion. when d is turbed as a r e s u l t of t he malfunction of t h e ex t r ac t ion column.

The d ispers ion times appeared

Only the extractiion column exhibi ted problems associated The other two columns were normal except

I n Table 1, the p i l o t p l an t column observations were cor re la ted with the coalescence times of eight consecutive samples. i n t e rp re t a t ion , t he p i l o t p l an t ex t r ac t ion column operat ion w a s considered bad i f t he column flooded

were g rea t e r than s i x inches of s t ab le , he4avy emulsion gathered a t the i n t e r - f ace ; and a l s o i f therewere l i t t l e or no organic coalescing i n the column. The coalescence times were considered bad i f they were grea te r than 600 seconds

For the purpose of

a t a volume ve loc i ty of 500 ga l /hr f t 2 ; if there

TABLE 1

This l i s t cons is t s of t he f i r s t 8 of 97 determinations

Equilibrium Coalescence Sample T i m e s Number (Seconds) P i l o t P lan t Column Observations

Standard 1 2 3 4 5 6 7 8

100 160 166

> 600 600

> 600 > 600 -200* 300 -1753 130

Column Good Column Good Very L i t t l e Organic Coalescing Emulsion Building Up Column Flooded Large llimounts of Heavy Emulsion Heavy Emulsion Column Good

* This i s the spider-,web e f f e c t as detected by the laboratory tes t , The main body of t he emulsion disengaged i n around 200 seconds. a spider.web-type f i lm w a s l e f t behind and remained s t ab le f o r g rea t e r than 600 seconds.

However,.

(See Figure 5)

+++ The complete t a b l e appears i n Appendix 1,

Organic phase

Interface

Aqueous phase

IDO-14486 Page 17

Dispersion level

23 ml

Coalescence level

15 ml

~ T S 59-3805

FIGURE 5 - SPIDER-WZB EFFECT This sample was dispersed for 30 seconds and then allowed to coalesce. in 200 seconds leaving a stable spider-web type film.

The main body of the dispersion disengaged

1 I D 0 -14486

Page 18

The samples of the feeds and ex t r ac t an t s t h a t were taken during the

A coalescence time of about 150 normal operat ion of the p i l o t p l an t columns (Samples 1, 2, and 8) gave coalescence times of about 150 seconds, seconds was considered normal when compared t o the 100-second coalescence time experienced with a standard feed which contained no surface ac t ive ma te r i a l s . The appearance of a tes t so lu t ion during normal coalescence can be seen i n Figure 3.

With samples 3, 4, and 5, t he column was observed t o have very l i t t l e organic coalescing and as a r e s u l t , emulsion began t o bu i ld up causing the

observation were grea te r than 600 seconds, amounts of heavy emulsion appeared a t t he in t e r f ace , The laboratory t e s t concurred with these observed c h a r a c t e r i s t i c s i n that the main body of the d ispers ion disengaged i n around, 200 seconds; however, a f i l m w a s l e f t behind and remained s t ab le f o r g rea t e r than 600 seconds, best be described as being s i m i l a r t o a spider web i n appearance. The spider web forms as the dispersed phases begin t o separate by the breaking of s m a l l bubles (See Figure 2) forming s t ab le l a r g e r ones which of ten continue t o grow i n t h i s manner u n t i l they have a t t a ined the diameter of the cyl inder . I n con t r a s t , normal coalescence i s character ized by the clean separat ion of the t w o phases (See Figure 3 ) . These films of l inked l a rge bubbles a t t a c h themselves tenaciously t o the opposite w a l l s of the mixing cylinder, sometimes making hor izonta l f i lms. appear t o f i l t e r or adsorb the p a r t i c u l a t e so l id s from the f a l l i n g aqueous phase. I n Figure 5, t h i s formation can be followed and the ind iv idua l s tages noted, A t t he upper levels of the organic phase, around the 23 m i l l i l i t e r mark, the e f f e c t appears as a s ingle f i lm s t r e t ch ing horizon- t a l l y from the cyl inder w a l l s . A t the lower ends of the organic phase, around the 1-5 m i l l i l i t e r mark, the e f f e c t i s s t i l l i n the smaller bubble s tage. The spider web i s e a s i l y broken with any physical contact , such as the addi t ion of aqueous so lu t ion o r manipulation of the mixing plunger. The a c t u a l i d e n t i f i c a t i o n of t h i s laboratory observed c h a r a c t e r i s t i c with the presence of heavy emulsion i n the column was not conclusive s ince heavy emulsion aggregation a l s o produced samples having extremely long coalescence t imes, g rea t e r than 600 seconds. web e f f e c t might be c h a r a c t e r i s t i c of boTderline cases and the in t e rp re - , t a t i o n as t o good o r bad column operation w a s d i f f i c u l t and not conclusive,

The coalescence behavior and the observed emulsifying t rends were compared i n 97 samples of p i l o t p l an t column feeds and ex t r ac t an t s and these comparisons are tabula ted i n Appendix 1, The t e s t concurred with the p i l o t p l an t column observations i n a l l but nine of t he 97 t r i a l s , a l l but one of the nine disagreements f i c a t i o n behavior while the column operation was observed t o be good,

- column t o flood. The coalescence times of samples taken during t h i s column With sample number 6, l a rge

This film can

I n t h i s manner they

Other samples ind ica ted t h a t t h i s spider

I n the t e s t predicted excessive emulsi-

These da ta showed t h a t the measurement of coalescence time of column end streams can be u t i l i z e d t o p red ic t major changes i n emulsif icat ion, However, the s e n s i t i v i t y of t he test i s such t h a t the in t e rp re t a t ion and evaluat ion of borderl ine cases, such as those possessing spider web e f f e c t s , would be d i f f i c u l t and subject t o e r r o r ,

,

B'. Coalescence Measurements of Plant Streams

The remote emulsion ind ica tor w a s employed t o measure t h e coalescence t i m e s o f p l a n t process streams t o determine t h e emulsifying tendencies of these feeds p r i o r t o t h e i r e n t r y i n t o the ex t rac t ion process, I n order t o obtain a standard, measurements were made with samples taken during t h e normal operat ion of the p lan t which produced feeds from t h e continuous d isso lu t ion of e n t i r e f u e l elements, These feeds contained s i l i c o n equivalent t o about 0 .4 percent by weight of t h e dissolved aluminum and 0.OOlM zirconium, Coalescence measurements were a l s o made on feeds of t h i s composition which had been gela-j;in t rea ted . I n order t o i s o l a t e t he responsible sur fac tan t and fur-cher evaluate g e l a t i n treatment a s p e c i a l p lan t experiment w a s designed which u t i l i z e d feed-s containing s i l i c o n equivalent t o 3.0 percent by weigh-$; of t h e dissolved aluminum and 0.OOOlM - zirconium.

1, Coalescence Behavior of Untreated P lan t Streams

The coalescence measurements of samples taken during normal operat ion o f t h e p lan t gave t h e spider web e f f e c t , These samples are described i n Table 2 , samples numbered 1, 2, and 3. These p l a n t streams contained s i l i c o n equivalent t o about Q,4 percent by weight of t h e dissolved aluminum and 0,OOlM zirconium. I n t h e coal.escence measurement the main body disengaged i n about 90 seconds but t he spicter web type f i lm remained s tab le f o r g r e a t e r than 600 seconds, by instrumentation t o be operat ing properly a t a moderate velume ve loc i ty .

The p l an t e>:traction column w a s determined

TABLE 2

COALESCENCE IQXSUREMENT OF P u i u STREAMS

Feed Description Specifi.c G e l a t i n Coal, Sample S i l i c o n Zirconium Aci d i t y Gravity TBP Dosage T i m e Number

COALESCENCE BEHAVIOR O F UNTREATED PLANT STFEAMS

Weight $I I!I M - g/ cc $ FFM See Remarks

1 0,4 0 0 001 0.6 1.27 3 0 3 none 7600-90 Spider Web 2 0-4 0 D 001 009 ~ 2 8 3.3 none 2600-90 Spider Web 3 0,4 0 0 001 008 1027 3 0 5 none 7600-90 Spider Web

COALESCENCE BEHAVIOR OF GELATIN-TREXTED PLANT STRWS

4 0.4 0 0 001 0~98 1029 3.0 100 7600-31 Spider Web 5 0 .4 0.001 0.49 i028 3 0 3 1.90 >600-35 Spider Web

COALESCENCE BEHAVIOR OF HIGH SILICON LOW ZIRCONIUM FEEDS

6 3 00 0 0001 1,46 1.27 3.3 none 7600 Sia-ble Emu 1 s ion

Fac ia l Crud

Emulsion

3.3 100 90 Some In t e r - P--- ---- 7 3.0 0 0 0001

8 3.0 0 0 0001 0.20 1029 3 * 3 none >600 Stable

9 3.0 0 0001 3.3 100 50 Clean ---- ----

IDO -14486 Page 20

2 Coalescence Behavior of Gelatin-Treated Plant Streams

These normal feeds were a l s o t r e a t e d w i t h g e l a t i n t o a l eve l of

Since samples of the g e l a t i n t r ea t ed feeds a r e 100 p a r t s per mi l l ion of feed , These samples a r e described i n Table 2 , samples numbered 4 and 5. unobtainable p r i o r t o t h e i r en t ry i n t o the ex t r ac t ion column, the r a f f i n a t e s corresponding t o these feeds were used i n the coalescence measurements, However, the coalescence times of p lan t feeds and t h a t of the corresponding p lan t r a f f i n a t e s compared s u f f i c i e n t l y t o determine major changes i n emul- s i f i c a t i o n (See Appendix 2 ) The coalescence measurement of these gelat in- t r e a t e d streams showed t h a t t he time required f o r the main body of the emulsion t o disengage was reduced grea t ly ; however, the spider web e f f e c t pe r s i s t ed .

3. Coalescence Behavior with High Silicon-Low Zirconium Plant Streams

I n a spec ia l p lan t experiment feeds were produced containing s i l i c o n equivalent t o about 300 percent by weigh% of the dissolved aluminum and 0.00OlM zirconium, Two samples of untreated feeds a r e described i n Table 2 , n b b e r e d 6 and 8, cence measurement of these untreated feeds giving coalescence times of grea te r than 600 seconds r a f f i n a t e s , samples numbered 7 and 9, produced clean separat ions i n 50 t o 90 seconds, There w a s small amounts of i n t e r f a c i a l crud present a t t he in t e r f ace of one sample but no spider web e f f e c t was experienced. P lan t operat ion was not attempted with the untreated feed but was successful with the g e l a t i n t r e a t e d mater ia l .

A very s t ab le emulsion resu l ted i n the coales-

However, t he corresponding ge la t in - t r ea t ed

V CONCLUSIONS

From these d a t a i twas concluded t h a t the measurement of coalescence times on p l an t column process streams can be u t i l i z e d t o pred ic t major changes i n emulsif icat ion such as were experienced i n the evaluat ion of t he g e l a t i n treatment. However, t he s e n s i t i v i t y of t he t e s t i s such t h a t t he i n t e r p r e t a t i o n and evaluat ion of borderl ine cases , such as those t e s t s possessing spider web e f f e c t s would be d i f f i c u l t and subject t o e r r o r .

ID0 -14486 Page 21

ACKNOWLEDGEMENT

The mechanical design and cons t ruc t ion of t h e remote t e s t i n g device was done by R, D o F l e t c h e r of t h e Hot Laboratory Equipment Development Group of CPP Technical and George Davis of t h e CPP Maintenance Group.

ID0 -14486 Page 22

VI. LITERATURE CITED

1. Cannon, R. D., Characteristics of Surfactants in Aluminum-Uranium Fuel Reprocessing Solutions, IDO-14489, March 26, 1959.

Hill, 0. F o , Classified Report, HW-26104, (1952). \

Newby, B. J., and Bernice E. Paige, A Gelatin-Filtration Headend for Fuel Reprocessing Solutions from Silicon-Containing Aluminum Alloys,

2*

3 .

IDO-14468, July 24, 1959.

4. Chamberlain, H., The Effect of AlSi in the Recovery of Uranium from Uranium Aluminum Alloys, IDO-14492

’

IDO-14486 Page 23

V I I . APPENDIX 1

CORRELATION OF PILOT PLANT ANDiCOALESCENCE TEST DATA

P i l o t P lan t R u n A

Sample Number

1 2 3 4 5 6 7 8 9

10 11 12 13 14 15 16 1-7 18 19 20 2 1 22 23 24 25 26 27 28 29 30 31. 32 33 34 35 36 37 38 39 40 41 42 43 44 45

Coalescence T i m e s ( see),

200 166

7 600 > 600 I 600 2 600

130 130 180 190 85 81

7 600

> 600 -142-* > 600 -142++ ) 600-150~ ) 600-165* 238 12 9 129 142 141 115 111 120 12 3 112 112 113 205 12 1 12 1 120 1-57 177 )600

? 600 600 -171* >600 -167* > 600 >600 ,600 - 1 7 ~ >600-170* ,600 -1 50*

---

Column Observation

Good

Good Good Good Good Good Good Bad(1)

Bad Bad/ 3 Bad( 2, Good Good Good Good Good Good Good Good Good Good Good Good Good Good Good Good Good Good Good d

Good J

Good r/

----

Bad Gootlyi Bad( l) Good J Good Goodd

Sample Coalescence Column Nuiber Times ( s e e ) Observation

46 47 48 49 50 51 52 53 5'; 55 56 57 58 59 60 61

1-73 182 1-79 ,600 -160* >600 - 170~. 7600 -180+ ,600 7600 116 130 126 125 12 5 122 12 5 12 5

Good Good

Bad Goofl-) Bad( 1) Bad(1) BadC2)(3) Bad(2i) Good Good Good Good Good Good Good Good

Column Operation Classi . f icat ion - Bad

(1) ( 2 ) Column flooded (3 ) (/) Dissagreement between t e s t and

(*) Spider web e f f e c t , Main body

>6 inches of i n t e r f a c i a l "crud"

L i t t l e or no organic coalescing

observed column observation

coalescence t i m e ,

( i'oniinueci )

IDO-14486 Page 24

CORRELATION OF PILOT ,PLANT AND COALESCENCE TEST DATA (cont )

P i l o t P l an t Run B P i l o t P l a n t Run C

Sample Number

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1.9 20 21 22 23 24 25

Coalescence T i m e s ( s e c )

156

174 151 15 5 155 14 6 218

---

7 600-215" )600-210*

1600 -221* >600-241*

248 297 267 272 266 280 267 300 240 243 2 52 246 265

co l m Observation

Good

Good Good Good Good Good

Bad Bad( 2,

----

;:ti 1 I : 1 Good Good Good Good Good Good Good Good Good Good Good Good Good

Sample Number

1 2 3 4 5 6 7 8 9 10 11 12

Coalescence T i m e s ( s e c )

> 600 - 113* 13 5 7600 7600 1.27 144

7 600 ,600 -230*

30 1

2600

Column Operation C l a s s i f i c a t i o n - Bad

(1) I 3 ) L i t t l e or no organic coa lesc ing (*) Spider-web e f f e c t . Main body coalescence time. ( 4

> 6 inches of i n t e r f a c i a 1 " c m d " 2) Colwnn flooded

Dissagreement between t e s t and observed column ope ra t ion

Column Observation

Bad( ')

Bad(3) Bad( Good

Bad(1)

Bad Goof5)

Bad Goofl)

Good Good Good

ID0 - 1448 6 Page 25

APPENDIX 2

THE COMPARISON OF THE COALESCENCE BEHAVIOR OF FEEDS AND RAFFINATES

Sample Number

3 4

b 7 8 9 10 11. 12 13 14 15 16 1-7 18 19 20 21 22

9 10 11

Feed Coalescence Times ( s e c )

p 600

7 600 7 600 7 600 300 255 300 16 5 160 156

7600

) 600 -150* ,600 -146* > 600-137* >600-141* 280

149

158

144

142

PLANT STREAMS

> 600 -88* >600 7600

R a f f i n a t e Coalescence Times ( see)

> 600 >600 -, 600 ,600 I 600 130 130 180 190 85 81

7 600 -142*

7 600 - 150* 7600-165* 238 129 129 142 14 1

> 600 442*

7 600 -73" >600 )600

(*) Spider web e f f e c t . Main body coalescence t ime.