Engineering topics

Sudol, E. D.

Publications and source records attributed to Sudol, E. D..

10 records

NASA NTRS1988

The first products made in space: Monodisperse latex particles

The preparation of large particle size 3 to 30 micrometer monodisperse latexes in space confirmed that original rationale unequivocally. The flight polymerizations formed negligible amounts of coagulum as compared to increasing amounts for the ground-based polymerizations. The number of offsize large particles in the flight latexes was smaller than in the ground-based latexes. The particle size distribution broadened and more larger offsize particles were formed when the polymerizations of the partially converted STS-4 latexes were completed on Earth. Polymerization in space also showed other unanticipated advantages. The flight latexes had narrower particle size distributions than the ground-based latexes. The particles of the flight latexes were more perfect spheres than those of the ground-based latexes. The superior uniformity of the flight latexes was confirmed by the National Bureau of Standards acceptance of the 10 micrometer STS-6 latex and the 30 micrometer STS-11 latexes as Standard Reference Materials, the first products made in space for sale on Earth. The polymerization rates in space were the same as those on Earth within experimental error. Further development of the ground-based polymerization recipes gave monodisperse particles as large as 100 micrometer with tolerable levels of coagulum, but their uniformity was significantly poorer than the flight latexes. Careful control of the polymerization parameters gave uniform nonspherical particles: symmetrical and asymmetrical doublets, ellipsoids, egg-shaped, ice cream cone-shaped, and popcorn-shaped particles.

Vanderhoff, J. W.↗

NASA NTRS1987

The first products made in space - Monodisperse latex particles

Monodisperse latex particles developed by seeded emulsion polymerization on various Space Shuttle flights are analyzed. The flight hardware was composed of a monodisperse latex reactor and a support electronics package, and the particles were examined by optical microscopy and TEM. Data on the particle size distributions, larger and smaller off-size particles, and conversion-time curves for the particles are examined and compared to ground-based results. It is observed that the ground-based polymerizations have more coagulum than the flight polymerizations; the flight latex particles have narrower size distributions than the ground particles; and the number of off-size larger particles in the flight particles is smaller than in the ground data.

Vanderhoff, J. W.↗

NASA NTRS1986

Development and testing of a space-flight dilatometer/reactor

A stainless-steel piston cylinder dilatometer (volume about 100 cu cm), designed for use in microgravity, was tested and modified for the purpose of obtaining the polymerization kinetics of monodisperse polystyrene latexes, as well as the latexes themselves. A low-speed, oscillatory agitation (10 rpm, 30 deg of arc/per cycle) and redesigned stir paddle were selected for the low shear requirements of the microgravity experiments. Conversion histories accurate to within 2 percent were obtained after apparatus modification and procedural changes were implemented.

Sudol, E. D.↗

NASA NTRS1986

Making Latex Microspheres in Space

Equipment yields larger, more uniform particles. Two NASA reports describe first commercial product to be manufactured in space. Product monodisperse latex, suspension of spherical particles of essentially same diameter. Carried aboard Space Shuttle on its orbital missions, monodisperse latex reactor (MLR) produces spheres of much larger size than possible on Earth. Mircospheres 30 micrometers in diameter produced, whereas 5 micrometers is limit for Earthbound reactors. Microspheres as large as 100 micrometers scheduled for production in MLR.

Kornfeld, D. M.↗

NASA NTRS1986

Preparation of large-particle-size monodisperse latexes in space

Results are reported of latex sphere polymerization experiments performed on two flights of the Columbia and three flights of the Challenger. The trials were carried out because polymerization of the spheres in space avoids coagulation, nucleation of a new crop of particles, and excessive stirring requirements, and allows growth of spheres larger than 4 microns diam. The Monodisperse Latex Reactor (MLR) held four stirred 100 cc sealed stainless steel cylindrical containers. The mixtures were monitored for the conversion times, volume decreases as spheres formed and the mixture temperature. The spheres were grown from 0.19 micron seeds. Details of the flight preparation efforts are outlined. In flights which did not experience mechanical malfunctions spheres 3-30 microns diam were grown that had noticeably lower size variations than did the ground-based control particles. The 10 micron diam spheres grown on STS-6 were accepted as standard reference material by the NBS and became the first products made in space to be commercially sold on earth; the 30 micron spheres also became NBS standards. The experiments confirmed all projected benefits of producing the spheres in space, as well as provided the opportunity to grow more larger offsize spheres by finishing the growths on earth.

Vanderhoff, J. W.↗

NASA NTRS1986

Kinetics of successive seeding of monodisperse polystyrene latexes. I - Initiation via potassium persulfate. II - Azo initiators with and without inhibitors

The polymerization kinetics of monodisperse polystyrene latexes with diameters of 1 micron are studied. The monodisperse latexes were prepared by the successive seeding method using 1 mM K2S2O8 with an 8 percent emulsifier surface coverage and 0.5 mM K2S2O8 with a 4 percent emulsifier surface coverage, and the kinetics were measured in a piston/cylinder dialometer. The data reveal that the polymerization rate decreases with increasing particle size; and the surface charge decreases with increasing particle size. The effects of initiators (AIBN and AMBN) and inhibitors (NH24SCN, NaNO2, and hydroquinone) on the product monodispersity and polymerization kinetics of latexes with diameters greater than 1 micron are investigated in a second experiment. It is observed that hydroquinone combined with AMBN are most effective in reducing nucleation without causing flocculation. It is noted that the kinetic transition from emulsion to bulk is complete for a particle size exceeding 1 micron in which the polymerization rate is independent of the particle size.

Sudol, E. D.↗

NASA NTRS1984

Preparation of large-particle-size monodisperse latexes in space: The STS-3, STS-4, and STS-7 mission results

Large-particle-size monodisperse latexes were prepared on four STS missions of the space shuttles Columbia and Challenger using flight hardware comprising four automated 100 cm(3) polymerization reactors. Seven polymerizations carried out on the March 1982 STS-3 mission of the Columbia, and the April 1983 STS-6 and June 1983 STS-7 missions of the Challenger, gave monodisperse latexes of 5 to 18 micron diameter with narrower particle size distributions than the corresponding ground-based control polymerizations. The rates of polymerization in microgravity were the same as on Earth. The results of these experiments are reviewed, and the prospects of the development of a space production process are discussed.

Vanderhoff, J. W.↗

NASA NTRS1984

Production of large-particle-size monodisperse latexes

The research program achieved two objectives: (1) it has refined and extended the experimental techniques for preparing monodisperse latexes in quantity on the ground up to a particle diameter of 10 microns; and (2) it has demonstrated that a microgravity environment can be used to grow monodisperse latexes to larger sizes, where the limitations in size have yet to be defined. The experimental development of the monodisperse latex reactor (MLR) and the seeded emulsion polymerizations carried out in the laboratory prototype of the flight hardware, as a function of the operational parameters is discussed. The emphasis is directed towards the measurement, interpretation, and modeling of the kinetics of seeded emulsion polymerization and successive seeded emulsion polymerization. The recipe development of seeded emulsion polymerization as a function of particle size is discussed. The equilibrium swelling of latex particles with monomers was investigated both theoretically and experimentally. Extensive studies are reported on both the type and concentration of initiators, surfactants, and inhibitors, which eventually led to the development of the flight recipes. The experimental results of the flight experiments are discussed, as well as the experimental development of inhibition of seeded emulsion polymerization in terms of time of inhibition and the effect of inhibitors on the kinetics of polymerization.

Vanderhoff, J. W.↗

NASA NTRS1984

Preparation of large-particle-size monodisperse latexes in space - Polymerization kinetics and process development

Monodisperse polystyrene latexes are prepared by seeded emulsion polymerization; however, sizes larger than 2 microns are difficult to prepare because of the creaming and settling of the particles and their sensitivity to mechanical shear. Preparation in space would obviate the creaming and settling, and allow agitation just sufficient for good heat transfer and mixing. Three polymerizations yielding 3-5 micron size particles were carried out successfully on the third flight of the 'Columbia' launched Mar. 22, 1982; however, four polymerizations yielding sizes up to 10 microns on the fourth flight launched June 27, 1982 were incomplete owing to apparatus malfunction. The results of these polymerizations and the prospects of developing a preparative space process are reviewed.

Vanderhoff, J. W.↗

NASA NTRS1982

Preparation of large-particle-size monodisperse polystyrene latexes in microgravity

Three large-particle-size monodisperse latexes (3.44, 4.08, and 4.98 micron diameter) were prepared in an automated four-reactor apparatus on the third orbital mission of the 'Columbia' begun on March 22. Comparison with ground-based controls showed that the 4.98 micron-size flight sample was the more uniform; the uniformity at the other two sizes was about the same. The rates of polymerization in microgravity and on earth were the same within experimental error, demonstrating that radical-initiated vinyl addition polymerizations are unaffected by the weightless environment.

Vanderhoff, J. W.↗