Document Kz6vKvBmk7eaqXGRQvEZmZn8x
V I. 60 No. 7
joccab ao(7) 24S-274 (1*77)
-7-
July 1977
BOUND COPIES OF PAPERS PRESENTED
LIMITED NUMBER AVAILABLE
See insert for details
&
5iin^e
PREPRINTS
OURNA IL &
OLOUR
HEMISTS'
SSOCIATION
Vinyl chloride mention in coatings formed from solutions C. M. Hansen
Measurement and use of surface tension data in film-forming polymers F. Ewane-Ebala and H. P. Schreiber
The microanalysis of copper oxide based marine antifouling paints in
the scanning electron microscope
/j, j g,rtj
Non-eonventional anticorrosive primers for steel D. E A. Williams-Wynn
OCCA-30 EXHIBITION INVITATIONS TO EXHIBIT DESPATCHED
Details on page 270
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2M> c. m. Hansen jocca
him vinyl chloride copolymer mentioned above1. Polymer* with lower glass transition temperatures can be expected to retain less solvent (or monomer) became of greater internal mobility. Polyivinyl chloride) (PVCI) is ^nerally plasticised or modified by copolymerisatioo to allow its use in a solution coating. Such coatings can be expected to retain leas solvent or monomer then rigid poly(vinyl chloride), for example.
It might alio be noted that the mathematics of diffusion predict a dependence of solvent loss on the square of the film thickness. This means that if a drying film is compared with one of twice its film thickness (at longer times), the thicker film will require four times as long to reach the tame level of solvent (or monomer) content as the thinner film. Thus thicker films can inherently be expected to retain more solvent or monomer than thinner films. These relations have alto been confirmed experimently in the experiments mentioned above.
Estimates of vinyl chloride logs during thn flret phaea
M f. W
The first phase evaporation phenomena are closely related to what in the chemical engineering literature is termed "differen tial distillation" (distilling solvents in a batch process, for example). The polymer may influence the process to tome degree, as will the activity coefficients for the mixtures involved. In a first approximation, however, these will not be con sidered.
The differential distillation process is described by McCabe and Smith*. In the simplest case, mathematical relations are derived for estimating the compositional change* in the liquid film as a function of material evaporated.
The equation concerned is:
where:
Ng - amount of ff(VCM) present at a given stage in the evaporation process
Np, -- amount of B originally present
NA -- amount of A present at a given stage in the evaporation process
NAt -- amount of A originally prerent
V " relative volatility of B to A
The relative volatility can be estimated by a simple ratio of the evaporation rates, but this value is dm available for vinyl chloride. In the example below the relative volatility was, therefore, estimated by a ratio of(be vapour pressures tt room temperature''1,
v,*(r)........................
Example: Assuming a typical lacquer formulation having the following composition:
Vinyl copolymer 23g
Methyl ethyl ketone 73g
Vinyl chloride monomer variable
The above mentioned experiments with VYHH have demon strated that the end of the first phase is assodated with a solvere composition of about 0.2| sohunt/x VYHH*. Thus, the first phere represents a reduction of the volatile content of (hie lacquer (rare
3e/g VYHH to 1/13 at (his value before entering into the reoond phase. 'BA at MX is approximately 2630/71.3 - 37.06 from equation 2.
Substituting there values into equation I greet:
Nrctt (ip.s-.wNycm
Thus it it dear that theoretically these should be essentially no VCM remaining at the end of the first stage of the evaporation
For the sake of including all factors, the data on solvent retention for VYHH cited above indicate that a further reduction of the advent and/or monomer content present et the start of the diffusion controlled phase will occur to the extent of a factor somewhat greater than two within a reasonable time (hours). Should the temperature be increased above room temperature, the mobility of the polymer chain regments will be increased with an accompanying increase in the diffusion coefficients of the so)vent/monomer molecules. A greater reduction in the amount of retained volatile material will retult.
Experimental
aft. -n
The analyse* for VCM were carried out using a garchromato graph. For liquid samples with a large VCM content the solvent or lacquer solution was injected directly into the gas chromatograph. When the VCM content was small, the analysis was done by the head space method**11. Here the principle is to place the sample in a suitable container, such that a gaseous sample can be removed with a syringe through a membrane without otherwise disturbing the contents. The volatile contents establish an equilibrium in the container and a calibration of the VCM signal by the method of addition allows analysis of the VCM content in the sample itself.
Experimental rauHi fihai
A commercially available lacquer with the composition described in the example above was used for there studies. This lacquer was found to have 16ppm VCM based on the nonvolatile portion of the formulation. Films were made in Petri dishes. These were made at an exaggerated film thicknesses of 140 to 180 microns. After 66 hours of drying st room temperature (according to the film thickness squared role this corresponds to 1.6 minutes for the normal film thidnrew of 3 microns for this product) no measurable (< Ippm) VCM could be detected in the film.
It might also be noted that measurable VCM could not be found in film* applied in the manner the product ie customarily used k in a film thickness of 3 microns on aluminium foil.
Experimental values for
were determined by adding
dOOOppm VCM to methyl ethyl ketone (MEK) and following
the concentration of VCM as a function of the per cent MEK
evaporated. Figure 1 shows a gaa chromatogram of the
VCM/MEK mixture after 4 per cent MEK and 48 per cent
VCM are evaporated. Collected results from similar analyses
are riiown in Figure 2.
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Rf roncM
j. Hansen. C. M.. Doctoral Dmenion `The "Three Dtmrftsional Solubility PiimkIo and Solvent Diffusion Coefficient , Danish Technical Press, Copenhagen, 1967.
: Hanien. C. M,, lad- Eat- Chrm. Prod. Mrs. Dee., 1970,9.282. i Doolittle. A. K. "The Technology of Solvents and Plasticixers",
John WUry ond Sons, Mr.. New York, I9S4. 4 Hansen, C. M.. Licentiat Dissertion. `The Free Volume
Interpretation of the Drying of Lacquer Films". Technical Llmr. of Denmark, Copenhagen, 1964, (Fig. 3,3). * See ref. I. Chanter S.
11 CM. HANSEN JOCCA
6. McCabe, W. L. and Smith, J. C, "Unit operations of Chemical Engineering", McGrow Hill, New York, 1956, p. 674-8
7. Berena, A. R.. 168th National Am. Chcm. Soc. Meeting, Atlantic City. September 9-13,1974. Divof Polymer Chemistry. Polymer Preprma, 1974, IS: X 197-202.
8. Steichen, R. J.. Analytical Chemistry, 1976,4g: 9. 1398-1402.
9. Personal communication with cand. pharm. Vagn Agftrd, Jydsk Teknolotisk Initiiut, Aarhus. Denmark.
10. Purcell, J. E. A Giordano, B D., "The Gas Chromatographic Analysts of Vinyl Chloride", Perkm-Elmer Publication Nr. GCD-43, January 1975.
11. Vitenberg, A. G., Chromatofrayhia, 1974, 7; 10, 610-619.
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13
DEPARTMENT OF THE INTERIOR
(BUREAU OF RECLAMATION)
Request for copies of Deportment of tho Interior specifications should bo directed to Commissioner's Office, Building 53, Oenver, Colorado 80202
VR 3
VINYI Of SIN PAINT: Auf 14, I9h4 UNION CARBIDE Formutetfen ,i' m Usui* bam L lit vmyi resins VMCM and VVHH.
FORMULA SUGGESTION VP 3010 Maintenance Primer Finish*
FORMULA BAKELlTE Vinyl Resin VMCM BAKELlTE Vinyl Resin VYHH
fLEXOL PlestlcUer OOP Pigment (II Asbestine 3X Methyl tspbuty) Ketone 7 Nltropropen* Toluene
Parts By Weight u.) 4.9 9.0 19.0 9.9 16.1 16.2 32.9
100.0
(DWhll# System - Tltenium Dioxide, rutile. non-chelklnf. Red System Synthetic Rad Iron Oxide. Blscfc System - Synthetic Blech Iron Oxide. Aluminum System - Aluminum Powder, 9.9 pert* rather then 19,0 parts.
PROCEDURE l. Dissolve resins Into the solvent system. 9. Charts all Ingredients** and resin solution Into pebble mill and
(rind lor 94 hours. 'except In aluminum system
For best adhesion of primers to bere steel. It Is haipfuf to add 14% of 95% phosphoric acid, baaed on the weight of vinyl mein VMCH, to the primer formulation.
VR 6
VINYL RESIN PAINT; July 6 I960 UNION CARBIDE Formulation VP 3O01 using BAKELlTE vinyl resins VMCM In prime coat. vyhm m body coat and VYHH and VYNS In sail coat.
FORMULA SUGGESTION VP-3001 Maintenance System
FORMULA BAKELlTE Vinyl Resin VMCH BAKELlTE Vinyl Resin VYHH BAKELlTE Vinyl Resin VYNS FLEXOL Ptesticiter 10-10 TiOi, rutile, non*chelklne Cirbon Sleek Synthetic Red Iren Oxide Aluminum Powder (1) Methyl isobuiyl Ketone 2 Nltropropen# Toluene
Pttato* MM 1U0
--
-- 1XO 1U0 1.00 --
--
10.50 16.50 uxo
100IX
Part* by Weight
Rad Rady Caat
" Rady
Caat
--
13.00
-- 15.00
----
140
uo
-- 1040 -- 140
1MD
-
** --
1740
nxn
flXO
1040 10.00 1040
10040
10040
aaf CaM
-- 1147 0.77
140 -- -- -- (1) 1040 1046 1040
10040
0) "Alcoa" 40 luuiitm - 15 ib* to b* addad to 1 cation of .olution toe uaa. Fot boat adbtakm of primara to bara itoel. It la Helpful to add to% of 5 pHoephorie acid. baaad on tha walght of vinyl
ra.ln VMCH, to tha prlmar formulation.
PROCEDURE I. Dliiolva ratlna In aolvont ayatom. J. Chart* all Inyudlanti** and raaln aolutton to pebbto mill amt grind nr 1* Hour*.
'anc.pt In aluminum ayatom
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030634
ACTIVITY COEFFICIENTS OF . Solvent Components IN . ,, PVC WMtttfSU* _____
Vie. stall assent ital iW .ptlgisgy. came. sf. ft&iw&j,
coefficient'* beino^ JtaffecewL--fW_ IJ5 vn tkt.
--1S_
tta lar^t Silt of PVC rt*\n TnoltCvsllS. _ TV'i J'iU _tff_tct
is best ireotttA b^ ita riorr Hwy^in* _e<^uAtlfty ^--
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___________
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* CftvnOonCntl k enl^.
_____
N : toiel rvutnbtr of components------------------------------------------
Subscript p refers to rts*n*_. ______________________ __
AC.h,* fret encr^f f mWVn^
Wt Viave etasen to neglect. tVift trvttalp'jtf.
.....
since tbe bwblk of eVt solvent Vs. t*\v<.fcne_,,tnl__^\ene .o-'ta.
we would e>pitt a Uo ctataVp^ of mixing..-Alsovie .uonVA-.
expect our components .to ^cv'votc _poiiivi\>(-A jito.\vty _
.............................. ....... ....................
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--
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<*) RT ------------- RT
where U; i* tV* fltcblviV.'j coeffiticnb. o"T_ov>'\p**\jin4_ V ^rtWkwc___
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iW ^*rtu\-_ia\jA__C*CAM.J-eet_JtA*r^
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R i iVt toi constant anA "T to the absaWhc ten Y<.rat>>Y_i.
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activity coefficient ok`"tn b>j t^wot'On
___________________
_______ ________________
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BATCH DR'tlNC EQUATION VllTU 1 VMmus via rioftvuuccius, eqh
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APPENDIX__ II CALCULATION OF ^S0LV, STEP (1)
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APPENDIX I 11 CALCULATION OF ^$0LV STEP <2)
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