Document v1QvqqOr3Vp00a6w3p8aRrXv8

E. X. DU PORT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT NEWPORT PLANT1 s e r ia l n o . k n -67-15 copy vi3lM4A*cJLJL. jT 0 fWs)n\J!^C4j^ NEWPORT PLANT PIGMENT COLORS RESEARCH REPORT SUBJECT: FLASH DISTILLATION - ENGINEERING DEVELOPMENT BLUE B BREACHING STUDY - GREEN G BREACHING STUDY PERIOD COVERED: JUKE 1966 - FEBRUARY,1967 DATE: 3/24/6? SERIAL MO. 0 - 6 7 - 1 5 E, I* DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT KN-67-I5 DISTRIBUTION: Copy No, / .1. Research Numerical Pile 2 Research Office Pile M. Hunt/E. Gonick W. S. Struve/A, A, Brizzolara 5. J, H. Cooper/B.H, Perkins/H.R. Linton/P.F. Ehrich 6, W, J, McClure/R. A, Hageman/H. Arnoul/O.C. Pile 7. P, J. Monahan (Vital Records) 8. E, L, Rodowskas/W, A. Jenkins 9. G, M. Loughran ..10 R. M. Salemi/P. N..Odell/Q.C. Pile 11 R. H. Wetzel .12 J. W. MInnich/S, E. Bakes 13. H. H. Gyorgy .14. J, F. Maurer 15- N.R. Levins - Louviers 16. C. E, Rick 17. W, E, Miller 18. Research Pile - Colors - Newport 19. Extra ,20 Extra .21 Extra .22 Extra 23. Extra NEWPORT PIANT PIGMENT COLORS RESEARCH REPORT SUBJECT: PLASH DISTILLATION - ENGINEERING DEVELOPMENT BLUE B BREACHING STUDY - GREEN G BREACHING STUDY PERIOD COVERED; JUNE 1966 - FEBRUARY 1967 SUBMITTED BY: D. H. EASTHAM APPROVED BY: J. W. DATE SUBMITTED: 7/25/67 DATE RELEASED: 8/24/67 ABSTRACT The theory and development of a continuous flash steam distillation process is described. A brief study of pertinent variables was made to demonstrate feasibility of flash distillation process for QDCB removal from Green G and Blue B pigment slurries. Effects of temperature.* hold time and ODCB/Pigment ratio on quality were also determined. Blue B products were also evaluated in soft vinyl. DUP050027564 TABLE OP CONTENTS X. INTRODUCTION II. CONCLUSIONS XXI. SUMMARY XV. DISCUSSION A, THEORY B. HEATING REQUIREMENT 1. STEAM FOR ODCB REMOVAL 2. ODCB VAPORIZATION STEAMREQUIREMENT 3. SUMMARY OF STEAMREQUIREMENT C, SEMI-WORKS TESTING D. CYCLONE B. ODCB REMOVAL EFFICIENCY -BLUE B F. SYSTEM OPERABILITY 0. SYSTEM PRESSURE DROP Ho ANALYSIS OF ODCB REMOVAL- BLUE B 1, OTHER USES 3. QUALITY - BLUE B K. QUALITY - GREEN G V. TABLES AND FIGURES FIGURES 1-12 TABLES 1-4 PAGE 1 1 1 1 2 2 3 3 3 4 4 4 4 4-5 5 5 5-6 7-18 19-22 DUP050027565 I. INTRODUCTION A continuous steam distillation process has "been designed and tested on semi-works scale to remove o-diehlorobenzene (ODCB) from pigment slurries, A description of the process, laboratory results and data on demonstrated performance on green and blue products are included, A brief study was made on the effects of significant variables in the breaching of green and blue products. II. CONCLUSIONS 1. The flash distillation process is an effective, repro ducible method for removing ODCB from pigment slurries, 2. By controlling pigment-solvent contact time and tempera ture, a green or blue product of standard strength with a significantly darker, more transparent masstone can be produced, 3. The flash distillation process can be incorporated to remove other water immiscible solvents from a waterpigment dispersion, 4. Flash distillation will make possible a reduction in distillation cycle of about 50$ as compared to batch distillation. III. SUMMARY A steam distillation process was developed to effectively remove ODCB from pigment slurries. The process is carried out continuously and under conditions that dp not produce foam which is currently a frequent serious operating problem. The equipment required is relatively simple5 a steam Jet eductor provides a "pump" as well as high efficiency con tactor for steam and slurry coupled with a cyclone separator to separate the solvent-free slurry from the vapors. The contacting is done in the absence of air which prevents the formation of foam which occasionally causes serious operating problems in the plant. The process produced green and blue products of standard strength with a much darker, more trans parent masstone. The rapid continuous removal of solvent makes relatively close control possible of solvent-pigment contact time. This led to a study of other pertinent vari ables affecting breaching, ODCB/Pigment ratio and temperature. IV. DISCUSSION A. Theory Flash distillation incorporates the same steam distillation principle on a continuous basis that is currently used on batch basis. To determine operating parameters we have the following. DUP050027566 -2- 17. DISCUSSION (Cont'd) A. Theory (Coat'd) % % ( JL~ BS) w { PB ) % Mass flow rate of carrier vapor (steam), lb./hr. % Mass flow rate of material in vapor (ODCB), lb./hr. % Molecular weight of carrier (steam), 18 mb Molecular weight of material (ODCB), 147 p Total pressure, 760 mm % Partial pressure of material, assumed to he 0.9 x vap. press., 63 mm Hg NS Vaporization efficiency, assume unity WA n 18 (iy <W7) 760 - 1 0*9(63) WA 1.52 lb. Steam WB IFTTOF" B, Heating Requirement Typical Breaching Slurry Composition Gallons Lh. Moles iSihkJ Water "Stayhelite,f ODCB CPC NaOH 1,082 12* 46.5 96 2.5(50#) 1,239 9,050 91 507 1,200 32(50#) 10,870 503 3.45 0.4 98 0.7 *Solid - estimated. 1. Steam for OPCB Bemoval 1.52 (507) 770 Lh. Heating Requirement Heat 10,870 lb. slurry from 60F. Assume Gp = 1 BTU/Lb. F. Q = MCpAT Q = (10,870) (1) (210-60) Q * (10,870) (1) (150) Q 1,630,000 BTU to 210F. DUP050027567 -3- IV. DISCUSSION (Coat'd) B. Heating Requirement (Cent *d) I* Steam for ODCB Removal (Cont'd) Qlb. * 1,630,000 BTU 10,870 lb. Slurry Qib,. 150 m________ * Lb. Slurry (Lb, Steam) (10,870 Lbs, slurry) (150 BTU/Lb. Slurry) ('5trBTIF~) (1^239 ^1. Slurry ) 1.345 Lb. Steam Oallon blurry"' Total Heating Steam = (1,239 gal.) (1,345 Lb. Steam ) _ Gal ."Slurry) l,66l Lb, Steam 2. ODCB Vaporization Steam Requirement Latent Heat of Vaporization ODCB * 140 BTU/lb. - DG 14.1A ^Vap. 140 BTU/Lb. ODCB 0.14^ Lb. Steam W$~BTWLX> . Steam Lb...Sd CB"' %ot, = (507)(0.143) = 72.5 DU. Steam 3. Summary of Steam Requirement Lb. Steam Heating ODCB `Vaporization Distillation 1,661 73 770 Total 2,504 Lb. Add 15# for heat loss 1.15 (2504) 2,880 Lb, Steam 2,88o Lb, Steam _ 2.33 Lb. Steam 1,239 Gal. Slurry Gal. Slurry C, Semi-Works Testing A semi-works scale unit as shown in Pigure 1 was assembled. Test results indicated a steam requirement of about twice theoretical is required to achieve satis factory removal of ODCB. A steam to slurry ratio of 5 lb. steam per gallon of slurry is recommended for design purposes. DUP050027568 -4- IV. DISCUSSION- (Cont'd) D. Cyclone A cyclone was provided to separate the ODCB-free slurry from the vapor stream* Design of semi-works still cyclone was not entirely in accordance with Design standard DG2.2D "because required pipe size was unavailable* Lab cyclone reentrained slurry at exit vapor velocities (Section dimension e of DG2.2D) of 10 ft./sec. If cyclone had been fabricated as outlined in DG2.2D, exit velocity would have been 4 ft./sec. and no re-entrainment would have occurred. Slurry/steara ratio at cyclone corresponds to 5-6 gal./I,000 ft3. A special spray separator with a conical bottom in accordance with DG2.2D is recommended. E. ODGB Removal Efficiency - Blue B Tests were conducted under various operating condi tions to determine optimum for removal of ODCB. Steam to feed ratio was found to be the most effective variable. Below a -ratio of 4 lb. steam/gal. slurry, the percentage removal of ODCB begins to fall off rapidly with slurry at room, temperature. The effect of velocity has some influence, higher velocity-better removal, but the effect is much less significant than steam to feed ratio. At higher slurry temperatures, a lower steam ratio can be tolerated, F* System Operability In all cases, the semi-works still operated well. Host problems experienced were associated with the steam supply and not the still operation. The exclu sion of air apparently prevents the formation of foam which was at no time evident in any of the tests* G. System Pressure Drop Estimating pressure drop in a system containing two phases is difficult and in most cases accurate only to within + 30$, Provisions were made to measure pressure drop under design conditions in semi-works. Results are shown in Figure 2. The pressure drop in the steamslurry transfer pipe is expected to be 8.8 Ib./sq.in./ 100 ft, pipe at proposed design conditions of 50 ft./ sec. velocity. H. Analysis of ODCB Removal - Blue B To determine the effectiveness of ODCB removal, the material processed was placed in a flask and vigorously distilled in the lab. The vapors were condensed and the volume of ODCB remaining measured. By material balance DUP050027569 M IV, DISCUSSION (Cont'd) H. Analysis of ODCB Removal - Blue B (Cont'd) the percentage removal was calculated. This does not take into account the ODCB that cannot be removed by distillation, I, other Uses Considerable effort has been put forth to improve quality of dispersion milled blue products. Some thought has been voiced that extended contact with perclene in the plant extraction tank was causing crystal growth. If this is the case, a flash still can also be used to heat the wetted blue mill powder (ground alum and CPC mixture) and remove the perclene rapidly. Several tests were conducted that indicated a standard product could be made in this fashion. J, Quality - Blue B The effect of breaching variables was studied using the still as a tool to rapidly remove the ODCB. Effects of temperature, breaching time and ODCB/Pigment ratio were studied and are shown in Figures 3-8 and Table 3A significant improvement in masstpne can be achieved by reducing the ODCB-Pigment contact time. The effect of these variables is also shown on 5-15 cut soft vinyl in Table 3* K. Quality - Green 0 The development of a flash distillation process made possible close control of solvent contact time by rapid removal of ODCB, A series of tests were conducted to determine the effect of ODCB/Pigment ratio, solvent contact time and temperature on tinctorial properties of Green G as the process would relate to plant scale flash distillation. Two levels of solvent were used at various contact times and temperatures. The Solvent/Pigment ratios studied were 1.2 (current plant standard) and 0.5. No significant difference was noted in quality by rubout between the two levels. The results are shown in Figures $-12. Figures 1 and 2 show the temperature as the most effective variable affecting strength and masstone over the levels of ODCB examined. The solvent concentration does serve to reduce the time and tempera ture somewhat but not to a major degree. Hence, the lower solvent concentration is more desirable since it can be removed at a higher rate in a continuous dis tillation and would be an advantage in cycle time. DUP050027570 6- - IV. DISCUSSION (Cont'd) K, Quality - Green G (Cont *d) Figures 11 and 12 show the effect of contact time. Figure IX shows a gradual decline in masstone darkness and transparency of about 10 points over a period of 3 hours while the tinting strength was not affected. Figure 4 shows the effect at a higher level of ODCB and again shows similar behavior. One additional test was conducted at the higher ODCB level which showed strength and desirable masstone properties can be attained by holding at room temperature for about 4 hours. The flash still can be utilized to produce a pro duct of standard strength with a significantly darker, more transparent masstone because of close control of solvent-pigment contact time. 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DUP050027582 ffl'S *S tf u gfj s 2S * -i pi g o5 a -O g Kox- * 9SUMB Hp -19- 0 a0 mo 05 g CoOs oins o#orl ID OS <inn mC4F*S coos ions doss oiss tn mcu cou tiHt cu OH h co rHl st to to i-f4" Wi~3 in iHn oA * o * o o * o ** o 9 o a9 oo -*p5 O* *oCH) x0,)!, H *! Oic_no**mrOo *doco*l\c*Ou *titno*4icno S*in!y irntictcnu Occuo 4>>i| si saP>8|f?:d> ,f*| COpi: Hf IS 3 o9 O9 in9 US .*S* -4* co ts cu in *4 .* OS tn !S s ib cu to os W Ol H ctu- ciun cou O C-- CU H H CU i 0 fll -P *rtf os .4- 0C0O CO 4- *i si H rl 'H CU a!" CSS H CO 10 H HI H CU CHU H jst H CO co ri CM H <h | CO -*C3U cCoO 4- vicnoo IS* VCOU s ' r*5 uo HI CCCOOO in .'fr*** H to Q H cu s sOsJf S3 H CU CO 4- in VO IS 00 c\ o jsd H ttao S Oi *s o ot<3a) Oo 5 cu pc; 45 DUP050027584 -20 TABLE 2 Theoretical Steam Requirement for ODCB Steam Distillation TC VP M.w Hfe 50 60 TO 75 80 85 90 95 100* 105 110 9* 150 230 300 360 ^20 520 625 760 900 1,100 ^-Design Bf11:J.i# VP ODCB .mm. 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