U.S. patent number 3,644,732 [Application Number 04/872,205] was granted by the patent office on 1972-02-22 for crystallizers.
Invention is credited to Reuel Shinnar.
United States Patent |
3,644,732 |
Shinnar |
February 22, 1972 |
CRYSTALLIZERS
Abstract
The invention relates to improvements in crystallizers and more
particularly, to the elutriation of the mix in a crystallization
vessel, and measurement of the particle size distribution in the
elutriated sample to obtain a control signal for controlling the
parameters associated with the crystallization process.
Inventors: |
Shinnar; Reuel (Great Neck
Estates, NY) |
Family
ID: |
25359064 |
Appl.
No.: |
04/872,205 |
Filed: |
October 29, 1969 |
Current U.S.
Class: |
250/394; 250/304;
250/575; 356/335 |
Current CPC
Class: |
G01N
23/12 (20130101) |
Current International
Class: |
G01N
23/12 (20060101); G01N 23/02 (20060101); G01n
023/12 () |
Field of
Search: |
;250/43.5D,83.3D,218
;356/102,208 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Lawrence; James W.
Assistant Examiner: Willis; Davis L.
Claims
What is claimed as new and desired to be secured by Letters Patent
of the United States is:
1. Crystallization apparatus including a vessel, means for
introducing a mix to said vessel and means for retrieving a product
from said vessel; and further including first means for circulating
a portion of said mix from said vessel through monitor means and
back to said vessel, said monitor means including a radiation
source and a first radiation detector and a second radiation
detector and a first passage for said mix pervious to the rays of
said radiation source disposed intermediate said radiation source
and said first radiation detector and adapted to provide a first
signal at said radiation detector representative of the mix passing
therebetween, and second means for circulating a portion of said
mix through a filter and through a second passage for said mix
pervious to the rays of said radiation source disposed intermediate
said radiation source and said second radiation detector and
adapted to provide a second signal at said second radiation
detector, means for comparing said first and second signals to
develop a third signal, and means responsive to said third signal
for controlling selected parameters associated with said
vessel.
2. Crystallization apparatus as defined in claim 1 and wherein said
radiation source develops gamma rays and said radiation detectors
are responsive to gamma rays.
3. Crystallization apparatus as defined in claim 1 and wherein said
radiation source is a light source and said radiation detectors are
responsive to rays generated from said light source.
4. Crystallization apparatus as defined in claim 1 and wherein said
means for circulating a portion of said mix from said vessel
through said monitor means and back to said vessel includes an
elutriation leg between the vessel and said monitor means to
provide a flow of the mix first through said elutriation leg and
thence through said monitor means.
5. Crystallization apparatus as defined in claim 4 and wherein the
elutriation leg comprises a conical member.
6. Crystallization apparatus as defined in claim 1 and wherein said
filter comprises a fines trap.
7. Crystallization apparatus including a vessel, means for
introducing a mix to said vessel and means for retrieving a product
from said vessel; and further including means for monitoring the
mix in said vessel, said monitoring means including means for
elutriating a portion of the mix from said vessel, means for
splitting said portion of said mix into a first portion and a
second portion, means for passing said first portion through a
filter and thence through a passage intermediate a radiation source
and a radiation detector to develop a signal representative of the
state of said first portion of said mix after it has passed through
said filter, means for passing said second portion of said mix
intermediate a second radiation source and a second radiation
detector to develop a signal representative of said mix derived
directly from said vessel, means for comparing said two signals to
obtain a control signal; means for recombining the two portions of
said mix, pump means for receiving said recombined portions and
discharging the same to a fines trap; a controller for controlling
said pump, and means responsive to said control signal in said
controller to control said pump in a predetermined manner.
8. Crystallization apparatus as defined in claim 7 and wherein said
radiation sources respectively each develop gamma rays, and said
radiation detectors respectively are each responsive to gamma
rays.
9. Crystallization apparatus as defined in claim 7 and wherein said
radiation source is a light source and said radiation detector is
responsive to rays generated from said light source.
10. Crystallization apparatus as defined in claim 7 and wherein
said means for elutriating a portion of said mix from said vessel
comprises an elutriation leg.
11. Crystallization apparatus as defined in claim 10 and wherein
the elutriation leg comprises a conical member.
12. Crystallization apparatus including a vessel, means for
introducing a mix to said vessel and means for retrieving a product
from said vessel; and further including means for monitoring the
mix in said vessel, said monitoring means including means for
elutriating a portion of the mix from said vessel, means for
splitting said portion of said mix into a first portion and a
second portion, means for passing said first portion through a
filter and thence through a passage intermediate a radiation source
and a radiation detector to develop a signal representative of the
state of said first portion of said mix after it has passed through
said filter, means for passing said second portion of said mix
intermediate a second radiation source and a second radiation
detector to develop a signal representative of said mix derived
directly from said vessel, means for comparing said two signals to
obtain a control signal; means for recombining the two portions of
said mix, pump means for receiving said recombined portions and
discharging the same to said vessel; a controller for controlling
said pump, and means responsive to said control signal in said
controller to control said pump in a predetermined manner.
13. Crystallization apparatus as defined in claim 12 and wherein
said radiation sources respectively each develop gamma rays, and
said radiation detectors respectively are each responsive to gamma
rays.
14. Crystallization apparatus as defined in claim 12 and wherein
said radiation source is a light source and said radiation detector
is responsive to rays generated from said light source.
15. Crystallization apparatus as defined in claim 12 and wherein
said means for elutriating a portion of said mix from said vessel
comprises an elutriation leg.
16. Crystallization apparatus as defined in claim 15 and wherein
the elutriation leg comprises a conical member.
Description
BACKGROUND OF THE INVENTION
This invention relates to improvements in crystallizers, and more
particularly to apparatus for improving the control and stability
of crystallizers.
Close control of particle size is, in many cases, hard to achieve
by manual control and completely automatic control schemes are not
as yet in common use.
The major difficulty encountered in controlling crystallizers, is
the inherent time lag between the moment crystal nuclei are formed
and the time these newly formed crystal nuclei reach a significant
size, such that their total mass and surface area significantly
affect the properties of the crystal mix. Thus, for example, if the
supersaturation increases, the nucleation rate increases. After the
nuclei have grown, their increased surface reduces the
supersaturation thereby counteracting the initial upset. Due to the
time lag involved between cause and effect, the system tends to
overreact and the amount and size of the crystals tend to exhibit
self-induced cyclic behavior which makes control even more
difficult.
I have determined that as a prerequisite for any successful control
of a crystallizer it is necessary to find a method to determine,
promptly, any changes in the nucleation rate.
In one aspect of my invention, I elutriate the crystal magma and
measure the properties of the elutriated fraction, containing only
the small particles. This can be done either continuously or by
periodic sampling. In crystallizers equipped with a fines trap,
such an elutriation device is present. The feed to the fines trap
primarily contains small crystals and the number and size of the
crystals entering the fines trap gives a good indication of the
most recent conditions of nucleation in the crystallizer. In other
types of crystallizers, a small stream may be withdrawn through a
standard elutriation device and the properties of the elutriated
solution containing the small particles may be measured proximate
the top of the elutriation device.
Monitoring of the total number of particles in the system is
accomplished either by attenuation or scattering of radiation
through the dispersion.
Attenuation is approximately proportional to the total surface area
of the particles, and as the maximum size of the particles is
limited by the elutriation device, the degree of attenuation is
indicative of the number of small crystals present in the
dispersion. By making this maximum size small as compared to the
average crystal size, the time span in which a newly created
nucleus affects the measuring device is small and I therefore
provide a method for early detection of changes in the nucleation
rate as discussed previously.
When light is used as the measuring device, attenuation by colored
impurities may introduce numerous errors. These errors can be
avoided by comparing the signal from the crystal mix to a signal
obtained from a similar light source passing through a continuously
filtered solution from the same crystallizer.
The number of small particles in the elutriated stream obtained by
any of the above methods may then be utilized to control any of the
independent parameters affecting the operation of the crystallizer,
such as feed rate, flow of cooling water, vacuum in the evaporator,
and the like. The correct set point of a controller for controlling
any such parameter responsive to the signal from the elutriated
stream can be found from a measurement of the particle size
distribution and should be periodically readjusted for such
measurements. Where a continuous measurement of the product
particle size is available (such as is obtained by weighing the
product streams leaving the sieves), then this measurement may be
used to periodically or continuously adjust the set point of the
utilized controller.
If a crystallizer is equipped with a fines trap, the control may be
substantially improved by using the signal from the particle
density measurement in the elutriated stream which, in this case,
is the stream entering the fines trap, to control the flow through
the fines trap itself. This will give a rapid response direct
control on the most important variable in the operation of the
crystallizer, namely the number of new particles formed. This
direct continuous control of the flow through the fines trap by a
measurement of the number of particles entering the fines trap,
forms an important part of this invention.
Although efforts have in the past been expended in an effort to
improve yield, it has been found that much of the difficulty with
crystallizer yield persists despite attempts to rigidly control
temperature and material inputs.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide apparatus for
rapidly analyzing the particle size of material mix in a
crystallizer and to generate a signal dependent thereon, which
signal is utilized to provide corrective action to restore the
material mix to an optimum desired condition.
It is a further object of the invention to detect changes in the
nucleation rate at an early stage.
It is still another object of the invention to provide a more
efficient control system for crystallizers utilizing a fines
trap.
It is another object of the invention to provide improved apparatus
for use in crystallization, which apparatus will provide greater
yield of the desired product with a lesser requirement for operator
surveillance.
It is a further object of the invention to provide improved
crystallizer apparatus which is economical to manufacture, requires
a minimum of maintenance and surveillance.
BRIEF DESCRIPTION OF THE DRAWINGS
Further objects and advantages of the present invention will be
obvious to those skilled in the art, when resor is had to the
following specification and the drawings, wherein:
FIG. 1 is a view, partially in section, of a crystallizer
incorporating one embodiment of the invention.
FIG. 1a is a view of a monitor or measuring device utilized with
the embodiment of the invention shown in FIG. 1 of the drawing.
FIG. 2 is a view, partially in section, of a crystallizer
incorporating a second embodiment of the invention.
FIG. 2a is a view of a comparator utilized with the embodiment of
the invention shown in FIG. 2 of the drawing.
FIG. 2b is a block diagram of an elutriation monitoring device
utilized to control the pump as shown in FIG. 2 of the drawing.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawing, wherein like reference numerals refer to
similar elements in the two embodiments shown, a vessel 12 is
provided with a feeding conduit 14 and a product retrieval conduit
16. A stirrer 18, which may be driven in a manner well known in the
art is disposed in vessel 12.
An elutriation leg 20 extends from a port 22 in a lower portion of
the vessel 12 to an input port 24 of monitoring or measuring device
26. An output port 28 of monitoring or measuring device 26 is
connected by means of conduit 30 to an input port 32a of a pump 32,
and output port 32b of pump 30 is connected by a conduit 34 to a
port 36 in the upper reaches of vessel 12.
The elutriation leg 20 is formed of either a vertical or inclined
pipe or conduit or an inverted cone in which the flow velocity is
such that all large particles fall faster than the upward velocity
materially reducing the passage of particles above a predetermined
size through the output side of the elutriator.
Monitoring or measuring device 26 comprises a transparent conduit
member 38 intermediate a radiation source 40 and a radiation
detector 42.
In operation, a mix is introduced into vessel 12 through conduit
14. The mix is subjected to stirring by means of stirrer 18 and is
heated by means not shown, but well known in the art. In order to
obtain an indication of the nature of the new particle generation
in the mix, a portion of the mix is elutriated under the action of
pump 32 through elutriation leg 20, measuring or monitoring device
26, the pump itself and back into vessel 12 through conduit 34. In
the loop described, the fine or smaller crystals flow through the
loop, with the larger crystals returning to the vessel through
gravitational action.
The state of the mix as it relates to the number of small particles
is obtained by means of the measuring or monitoring device. A
radiation source 40, which may radiate gamma rays or other suitable
rays, such as a light source, X-rays and the like, is caused to
direct its rays through the mix confined but flowing through the
transparent tube 38. Radiation detector 42 is positioned relative
to the transparent tube or conduit 38 so as to measure the
radiation transmitted therethrough. The output of radiation
detector 42, being a function of the transmissivity of the mix
contained or flowing through the loop, the output of the radiation
detector may be utilized to control one of the parameters which
influences the mix makeup in the vessel. For example, the output of
radiation detector 42 could be utilized to control a heating or
cooling circuit associated with vessel 12, or feed rate or mix of
source materials being fed into vessel 12.
Although no details are herein incorporated with respect to the
control which may be exercised by the output signal from radiation
detector 42, such control circuits are well known in the art, and
require no experimentation in order to obtain the results
desired.
In the embodiment disclosed in FIG. 2, it will be seen that
applicable reference numerals have been applied to elements which
are common to both embodiments. Within vessel 12, there is disposed
a baffle 50, which is arranged to form an elutriating passage with
the wall of vessel 12 to permit the mix within vessel 12 to be
drawn off through port 52 into a monitoring or measuring device 54.
The mix is drawn through device 54 by means of pump 56. The
measuring device 54 is connected to vessel 12 by means of a conduit
53 and to pump 56 by means of a conduit 55. The mix is returned to
vessel 12 after passage through a fines trap 58, which is connected
to pump 56 through a conduit 57 and to vessel 12 by means of a
conduit 59. The details of a fines trap are well known in the art,
and the details thereof are not set forth herein.
The measuring or monitoring device 54, which is more fully shown in
FIG. 2a comprises two paths, 60 and 62 respectively. Path 60
includes a filter 66 which is connected to conduit 53 at its input
by means of a conduit 74. The output of filter 66 is permitted to
enter a transparent tube or conduit 70 by means of a conduit 68.
The other end of transparent tube 70 is connected to conduit 55 by
means of a conduit 72.
Path 62 of the measuring or monitoring device 54 includes a conduit
74 which connects conduit 53 to a transparent tube or conduit 76,
which conduit 76 is substantially similar to conduit 70. The other
extremity of transparent tube or conduit 76 is connected directly
to conduit 55 by means of a conduit 78.
Each conduit or transparent tube 70 and 76 is disposed between a
radiation source and a radiation detector respectively. Tube 70 is
disposed between radiation source 80 and radiation detector 82, and
tube 76 is disposed between radiation source 84 and radiation
detector 86.
In operation, a mix is elutriated through tube or conduit 53 and
split between paths 60 and 62. The mix flowing through path 60 is
caused to flow through filter 66 wherein the suspended particles
are removed and the filtered solution is permitted to flow through
transparent tube 70 and subjected to radiation source 80 and
radiation detector 82. The radiation passing between the radiation
source 80 and radiation detector is determined by the state of the
solution passing through transparent tube 70. An output signal
representative of the radiation transmissivity is obtained at
terminals C and D respectively.
The mix flowing through path 62 is permitted to flow directly
through transparent tube 76 and to conduit 55, and is also
subjected to radiation passing between radiation source 84 and
radiation detector 86. Again the radiation passing between
radiation source 84 and radiation detector 86 is determined by the
state of the particle mix on the elutriation suspension. An output
signal representative of the mix leaving the elutriation section 50
is obtained at terminals A and B respectively.
The signals appearing at terminals A and B, and C and D
respectively are connected to a comparator circuit, such as is well
known in the art, and a difference signal is developed. This
difference signal is a function of the variation of the mix from
the desired mix and may be utilized to control the parameters of
the system to bring the crystallizer back to or closer to the
desired steady state conditions.
One form of control is shown in FIG. 2 and in FIG. 2b, wherein the
signal from comparator 88 is fed to a controller 90 which controls
the rate of flow generated by pump 56. The difference signal is
also available to control other parameters of the system such as
mix makeup, temperature and the like.
Although I have shown only certain preferred features of the
invention by way of illustration, many modifications and changes
will occur to those skilled in the art. For example I have made
reference to the use of a radiation detector and source based on
gamma ray radiation, and obviously without limitation X-rays or
light rays may provide the radiation source which when associated
with the companion detector will produce the signal or difference
signal contemplated by the invention. It is to be understood,
therefore, that the appended claims are intended to cover all such
changes and modifications as fall within the true spirit and scope
of my invention.
* * * * *