Che5700 Batching and MixingBatch feed always involves mixing, objective: - high uniformity, high reliability (more judgment (experience) rather science)

Before mixing: action of feeding; next few graphs showing some common equipments, goal: good powder flowability.

Most ideal state of mixing: random homogeneous mixture RHM

Bulk Solid TransportChe5700 One way to avoid funnel flow: reduce friction from walls Mass flow first in, first out, good results;Funnel flow first in, last out (rat holing); not desirable

Properties of Mass of ParticlesChe5700 Pressure is not the same in all directions: one applied pressure will create some pressures in other directions, but always smaller; related to particle shape and packing; define K = normal pressure/applied pressureShear applied at surface will be transmitted through a static mass of particlesDensity of mass will varyBefore flow, mass of particles will increase its volume first (dilation)When angular solids are piled up on a flat surface, there will be an angle of repose; (free flowing solids: this angle is between 15 and 30o)

Angle of FrictionAngle of storage tank and angle of friction of particle whether particle can free flow, i.e. mass flow or funnel flow;

Arching: state when particle can not flow at all

Common experience: flow of powder decrease if size of flow unit > 15% of opening size

Cohesive & Noncohesive SolidsNon-cohesive solids (free flowing): K 0.35 0.6Cohesiveness: often sensitive to moistureChe5700

Angle of friction: influenced by particle size, shape, or even water content, it often increase cohesive force between particles increase angle of friction more difficult to free flowAbrasion: another possible problem with ceramic particles during transportation

Powder MixingChe5700 More art than science;Can never achieve perfect mixing like that in fluid phase;Complete mixing: often refers to specific structure, not attainable from a random process; Characterization of mixture: I.e. degree of homogeneity - (1) a statistical problem; (2) sample size (scale of scrutiny) consideration need to be proper, too large or too small: little value; e.g. sintering after mixing then consider diffusion distance during sintering, choose appropriate size for samplingcan be considered as single sample within that size.

Scale of SegregationThe length, area or volume of the largest region of each component in the mixture is referred to scale of segregation of that component In a liquid solution: minimum scale of segregation size of largest molecules In a particle system: largest particle size

Completely random vs completely dispersed Degree of segregation larger in the former caseSampling size: e.g. adding carotene into powder milk (1/1000), how should we sampling?

Degree of Mixednessp,q true fractions; x measured fraction Che5700 Use statistical numbers as index of degree of mixing, to discuss uniformity of sample, to compare different mixing equipment and operation conditions.Statistically, bimodal distribution for mixtures, often use Gaussian or Poisson distribution as examplesE.g. A, B equivalent , except color different, then

Mixing IndicesChe5700 * Sampling analysis: Standard deviation s (s2 = variance) ; where o = standard deviation of original segregated mixture; r = standard deviation of ultimate completely random mixture; s = standard deviation of current sample; N = number of analyzed samples; n = particle number in sample

More IndicesChe5700 For example:Rose M = 1 s/o; (unmixed 0 mixed 1- 1/n1/2)Lacey M = (o2 s2)/(o2 - r2) (from 0 1)Kramer M = (o s)/(o - r) (from 0 1)Hixon-Tenney-Harvey index: if x > p D1 = (1-x)/(1-p) x < p D2 = x/p x = p D3 = 1 average degree of mixing Da = (N1 D1 + N2 D2 + N3 D3)/N ( x = value of some component in sample, p= expected value)

For different material and different size, use this equnation to calculate RHMvariance;C1, C2 = fractional concentration of each componentMs = mass of samplefw sum of product of the weight fraction f of particles in each size class and the mean particle weight W in the class (could it be f * w; not fw)

Mixing AnalysisChe5700 Previous mixing index to evaluate mixing process or effect of parameters, try to minimize error in sampling and analysis. Macro-scale mixing: by chemical analysis, phase analysis, etc.; Micro-scale mixing: observation by microscopy techniqueE.g. use M index: to study time effect, determine optimal condition; indicating de-mixing behavior; mixing by relative movement of particles: convection, shear, diffusion (three mechanisms). Different equipment provide different mechanisms.Inverse of mixing segregation (percolation of fines, trajectory segregation, rise of coarse upon vibration)

Important ParametersChe5700 Mixing effect affected by: type of equipment energy input flowability and composition of sampe (size, shape, density, surface characteristics)

For complete description of mixing, one need: sample variance (intensity of segregation) scale of segregation (to micro-scale) long range structure

Microscale and Macroscale Mixedness Microscale analysis provide information on microscale mixedness Macroscale mixedness can be analyzed by many technqiues (chemical or physical) Sampling and analysis error should be kept to a minimum uncertainty in the standard deviation (s) become low when a large number of samples are taken

Taken from JS Reed, 2nd ed.

Taken from JS Reed, 1995 Commercial mixers: usually with two or more mixing elements to produce: high shear mixing in a local region & low shear bulk mixing

One example of two mixing elements

To avoid vortex, we may add baffles

Turbulence and cavitation for diffusion (micro-scale mixing)

Mechanism in Horizontal Drum MixerChe5700 Path of circulation: particle move with rotating cylinder, mixing only if change in path of particlesRadial mixing: due to mixing in the gravity direction (drop to a void); velocity gradient important;Radial de-mixing: core formation, small and heavy particles gradually go to bottomAxial mixing: diffusion modeAxial de-mixing: band formation, effect from mixer walls;

Change drum mixer into cone shape, beneficial to mixing; (taken from JS Reed, 1995) cement mixer!

Rate ProcessChe5700 dM/dt = A (1-M) B (where is segregation potential; M = 1 - 2) unmixing processIn principle: B effect from equipment; - effect from particle characteristics

Equipment used in mixing of viscous paste (Taken from JS Reed, 1995); (a) helical mixer; (c) double planetary mixerSigma blade mixer

JS Reed, 1995

Extent of reaction depend on degree of mixing and uniformity

Aeration BlendingChe5700 Or named fluidized blending, for mixing of different particles. Some advantages: can obtain uniform mixtures, even different in density can be precisely controlled, energy cost/unit weight sample lower easy to operate and maintain large capacity fast and easy loading; many different methods for feeding (e.g. pneumatic, mechanical, gravity) Can use other gases, in addition to air

Dispersion of Powder into LiquidChe5700 Steps involved: adhesion (a b), immersion (b c) and spreading (c d); Work involved with each step (equilibrium consideration):Wa = SL (LV + SV) = -LV (cos +1) negative for any Wi = 4SL - 4LV =-4LV cos < 90o, negative valueWs = (SL + LV) - SV = -LV (cos -1) positive value, at=0o, this number is zeroIn summary: work must be done to obtain spreading

Contact AngleChe5700 cos = (SV - SL) /LVWetting implies contact angle < 90o

Macroscale Mixing and Microscale MixingChe5700 Mixing of viscous slurry with a single impeller: difficult to achieve both ** macrocsale mixing high pumping capacity ** microscale mixing turbulence

Look at two parameters, Re & P (power requirement) ** Re = N s (dia.)2/ . turbulence ** P/Re = CD N2 (dia.)3 . Pumping capacity CD: drag coefficient; For high viscosity, same power, but need large Re (microscale mixing) need small size propeller, or increase velocity; yet for small propeller, non-uniformity occur (macroscale mixing)

Mixing and EMI Performance* ABS + Ni powder or fiber mixing (Barbender mixer or dry mixing) composite for EMI measurements

Dry mixing produced better shielding effect than Barbender mixer (in terms of low threshold value)

(a) Barbender mixer (powder; 20%); (b) dry mixing (powder 7%); (c) dry mixing (filament, 7%)Barbender mixer produced perfect mixing, not necessary good for EMI purposes; dry mixing produced macro-scale uniformity, not micro-scale uniformity

Correlation between percent measureable (electrical resistance) of composite of various samplesElectrical resistance measurement by 4 point probe