EXPERT APPRAISAL OF SOVIET PAPER ENTITLED "ACOUSTIC COAGULATION OF VAPOR CONTAINING FLUORINE COMPOUNDS", BY M L VARLAMOV AND COLLABORATORS (WHICH EXPERIMENTS WITH ULTRA SONICS)

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP80T00246A019600280001-4
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 21
• Document Creation Date: December 23, 2016
• Document Release Date: August 1, 2013
• Sequence Number: 1
• Publication Date: January 3, 1963
• Content Type: REPORT

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INFORMATION REPORT AsNFORMATIO+4 REPORT
CENTRAL INTELLIGENCE AGENCY
ts."s inforrnotIon effecyng tire Notion& Oefena ot tie jnoed Starer ii dim tie""R.0,,9 of the ESPonaget Lows. Tole
IR. U.S.0 Secs 793 and 79S the ironsmimon or revelation of wh,On ii nov trainer to on unoutlorred Lietss'n b'bb'b"d by low.
C -N-F -I -3) -1 -A
COUNTRY USSR
REPORT
SUBJECT Expert Appraisal of Soviet Piper Entitled DATE DISTR.
"Acoustic Coagulation of Vapor Containing
Fluorine Compounds", by M L Varlamov NO. PAGES 2
and Collaborators (6: 0,r c
s- i. REFERENCES
DATE OF
INFO.
PLACE &
DATE ACO
3 Jen 63
THIS IS UNEVALUATED INFORMATION
a translation of an
limagub44allied article in Russian entitled, in English, "Acoustic Coagulation
of Vapor Containing Fluorine Compounds" by M L Varlamov, Ye L Krichevskaya,
A A Ennan, LMKozakova and G A Manakin, Chair of Technology and Automation
of Chemical Processes of the Odessa Polytechneal Institute
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2. This work deals with laboratory scale experiments for the precipitation of
fluorine effluents from the exhaust gases of a superphospgraflUlat0r..
e rluorine effluents were present both as aeIiVaPOr5. The flow
rate treated in a standing waves tube averaged one CFM. The sound source
was a modified Hartman whistle previously developed by the authors (see
Use of Ultrasound in the Investigation of Matter, Proceed of OPT, 1960)
for suinFic acid coagulation with ultrasonics. The emission frequency was
16.5 KC and an average intensity level of 153-155 decibels was reached in
the agglomeration pipe despite the use of a diaphragm in front of the
generator. It was found that sound waves increase the precipitation yield
from between 42-69 percent (without irradiation) up to 80-95 percent. The
fluorine content oscillated between 0.6 and 4.5 gr/m3 values which in general
correspond to a very good load for sonic processing. As expected collection
efficiency went up with increasing particles concentration and humidity (15
to 120 g/0). The best contact time averaged 3-4 seconds as expected from
literature data.
3. Direct experimentation conducted with the exhaust gases of a superphosphate
granulator demonstrated that with a three second contact ti inc the precipitation
yield reaches 87 percent when dealing with an inlet fluorine content as low as
0.18 gr/m3. In other words, the exhaust gases contained only 0.025 gr/m3
which is a safe exit concentration according to Public Health Standards. The
authors will continue this work with the idea to later develop an industr
gas cleaner.
C-0-N-F-I-D-E-N-T-I-A-L
'STATE
I ARMY
I INAVY lAift
1 I '8'
I IAEc
GROUP 1
(abided from avtonlic
dewavadiag vul
docluslAcatlea
I I
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INFORMATION REPORT INFORMATION REPORT
CONTROLLED NO DISSEM ABROAD NO FOREIGN DISSEM
DISSEM: The dissemination of this document is limited to civilian employees and active duty military personnel within the intelligence conaponents
of the USIB member agencies. and to those senior ofticiahr of the member agencies relic TWA act upon the information. However unless specifically controlled
is accordance with paragraph 11 of DCID 1/7. it may be released to those components of the departments and agencies of the U. S. Government directly
participating in the production of National Intelligence. 1T SHALL NOT BE DISSEMINATED TO CONTRACTORS. It shall not be disseminated to organiso.
tions or p111,0120?1, 131Chldhlq consultants, under a contractual relationship to the ELS. Government without the written permission of the originator.
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NO VAC Atinvr
C-O-N-F-I-D-B-N-T-I-A-L
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the weak point of this investigation lies in the power
requirements of the sound sources (which are not mentioned). Feasibility
of the technique has been clearly established, but the bottleneck for future
extrapolation will be the development of a high power economical sound source.
-end-
C-0-N-F-I-D-E-N-T-I-A-L
NO DIGGER ABROAD NO FOREIGN DISSEM
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Acoustic Coa ulation of Vapor
Containing Fluorine Compounds
By
1,1, L. Varlamov, Ye, L. Krichevskaya,
A. A. Ennan, L. M. Kozakova and
G. A. Manakin
Chair of Technology and Automation of
Chemical Processes of the Odessa Poly-
technical Institute
In the production of simple and granulated super-
phosphate there is a precipitation of fluorine compounds
which are not completely trapped by the usual absorption
devices. The exhaust gases of these Processes contain 0.1
to 2.0 g/m3 of fluorine /1-37 , which is considerably in
excess of the permissible health safety norms. Therefore,
a need arises to devise new methods of fine purification
of gases from fluorine compounds.
During the production of simple superphosphate,flu-
orine precitpitates from the reaction chambers and mixers,
mostly in the form of SiF4; further interaction with water
causes the formation of 1I2SiF6 and silica gel /4/. The for-
*) First Report.
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FiLtion of a film of silica gel on the surface of droplets
of the absorbing liquid impedes the
fluorine compounds /5/.
In simple superphosphate the
further
absorption
of
fluorine is in the form
of fluosilicic acid and salts containing fluorine. The mil-
librium of pressure of vapors on fluorine compounds depends
not only on the temperature and concentration of H2Si26,
but also on the content of free Phosphorous acid in the li-
quid phase of superphosphate ZU.
During granulation of superphosphate preciPitation
of fluorine takes place mainly in the drying Process, with
10 to 20 percent of the fluorine introduced with the simple
superphosphate being transformed into the gaseous phase A/.
According to the data of one of the investigations
conducted at a superphosphate plant by us, no more than
1/3 of the fluorine is trapped in the absoprtiou turret
and gas pipes out of this amount; the discharge of fluo-
rine into the atmosphere constitutes tens of kilograms per
hour.
In the drying drums precipitation of fluorine takes
place at increased temperatures. Subsequent decrease of
temperature causes water vapor to condense, accompanied
by the formation of a stable and slowly settling vapor.
According to bibliographical data 5, 61, and our own
!observations, it contains the major portion of fluorine
2
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1Tompounds which are present in exhaust gases. The pressurel
of vapor of fluorine compounds on diluted solutions of
H2SiF6 is insignificant; therefore on reachinga state of
equilibrium; most of the fluorine is transformed into the
liquid phase of the aerosol. Thus, at temperatures between
50 and 7000, gas in a state of equilibrium contains only
0.02 to 0.04 g/m3 fluorine. /7/. :he remaining quantity
should be in the form of vapor. The transition into the li-
quid phase takes place fairly rapidly on account of the
large specific surface of the aerosol.
Thus, the task of removal of fluorine is reduced to
devising methods of fine purification from exhaust gases
and vapor containing H2SiF6 and other fluorine compounds.
A number of investigations were dedicated to prob-
lems of absorption of fluorine compounds by water or by
weak fluosilicic acid in nozzle and bubbling apparatus
TA
Lo-1V. The use of Venturi tubes and other high-intensity
apparatus makes possible a considerable increase of the
rate of absorption of fluorine compounds; however, it is
difficult to solve t172e problem of complete purification
of gases by these methods, because fluorine is mostly pre-
sent in the form of vapor which is poorly retained in ab-
sorption apparatus.
Fine purification of gases from vapor containing
fuorine compounds can be accomplished either by electro- I
3
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73.1ters 1g, or by the mtho of acoustic coagu1ation.1
A marked increase of collIsions of particles of the aero-
sol takes place as a result of the effect of a powerful so-
nic field. The vapor rapidly consolidates, and can then be
easily removed by regular dust extractors or other mecha-
nical precipitators D5-217. Acoustic coagulation success-
fully occurs at frequencies of 1 to 25 cps ad an intensity
of 0.1 to 1.0 W/cm2.
Powerful sonic fields in gaseous media are produced
by gas-jet generators: static and dynamic sirens. The me-
thod of acoustic coagulation is -articularly important in
these instances, where it is necessary to accomplish a fine
purification of gases from finely-dispersed aerosols.
The purpose of this work is to investigate the acou-
stic coagulation of vapor containing fluorine compounds,
and to study the possibility of using this method of puri-
fying the exhaust gases of superphosphate production from
fluorine.
Experimental Part
Method of investigat10-1. The first stage of this
work was to investigate acoustic coagulation under labo-
ratory conditions. The initial aerosol was obtained by
mixing water vapor with tetrafluoride of hydrogen, which
precipitates under the action of concentrated sulfuric
IL!.pid into a mixture of equal ;volume of silica sand and
?4
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7ommercial fluosilioate of natrium. Before the experiment 1
the gas was diluted with air in a gas meter to a concentr-
ation of the order of 0.1 to 1.0 g/m3, which is close to
manufacturing conditions. 1-:ineral oil of low viscosity was
used as sealing liquid. Uater vapor was obtained by mixing
het air saturated with steam with cooler air. Temperature
stability in the gas mixture at the input of the sonic
tube was provided by a thermoregulator. For a sonic gene-
rator we used an improved gas-jet generator GS-2 of the
Hartman whistle type, employed by us in investigating the
acoustic coagulation of sulfuric acid vapor /22_7.
The second stage was the investigatitn of acoustic
coagulation of fluorine-containing vapor directly from the
exhaust gases of the granulated superphosphate department.
A diagram of the apparatus is shown in Fig. 1. The
investigated gas was pumped from the exhaust pine 1 by
vacuum pump 2 and transferred to sonic treatment tube 3
which has a diameter of 45 mm and a length of 960 mm. Zie
front end of the tube, tightened with a rubber diaphragm,
joined the sleeve of-z:the gas-jet generator 4. The amount
of Gas passing through the sonic treatment tube was mea-
sured by rheometer 5. Part of the gas was removed for ana-
lysis by means of suction apparatus 6 and 7, both before,
and after sonic treatment. The fluorine was absorbed with
'distilled water in a system of four Drexel jars 8 and 9. i
5
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1-17:-Jart of the gas was withdra.:a into a continuous ultra= C:71
roscope 10, be means of which we calculated the number of
particles in a unit of volume before and after acoustic
coagulation. The condensate which accumulated in the sonic
treatment tube in droplets was removed through tap 11. The
temperature was measured by thermometers 12. Air was pumped
into the sonic generator under 1Dressure of 2 kg/cm2 by com-
pressor 13 through oil separator 14 and receptacle 15. The
frequency of sound was measured by means of oscillograph
B0-7 to which tension was transferred from a titanate-ba-
rium probe, which served as receiver of sound, and gene-
rator of electric oscillations ZG-0. The parity of fre-
quencies was derived from Lissajcus figures observed on
the screen of the oscillogrfaph. Sound intensity was deter-
mined with the help of a titanate-barium probe, connected
to the amplifier and cathode voltameter.
The selection of method of analysis of gases for
fluorine content is of essence L.3-257. In the control of
production of superphospahte and in scientific research
the most widespread method is to absorb fluorine in water
with subsequent titration of the absorbing liquid with al-
kali according to two indicators. The alkalimetric method
was used by us in the first series of laboratory tests
in working with pure gases. This method is not suitable for
1 analysis of plant exhaust gases, since along *....th fluorine i
6
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r--
1 compounds, water absorbs suparphosp ate dust containing S1
phosphorus acid and SO2 and 002 from combustion gases.
Therefore, analysis by the alkalimetric method gives re-
sults which are several times overstated.
In our investigation we used the colorimetric me-
thod based on the alizarin-zirconium reaction t6-2q7. It
IS based on a weak pink coloring of the alizarin-zirconium
complex in the presence of small cuantities of fluorine.
Colorimetric analysis was conducted with chemically pure
solution of NaP by the standard scale method. Control-ana-
lyses were conducted in the central laboratory of the Od-
essa Superphosphate lant and in the analytical labora-
tory of the NIUIF by the method of low-temperature remo-
val of fluorine with subsequent titration by a solution
of thorium nitrate.
The humidity content of the gas was determined by
means of absorption with calcium chloride and phosphorous
anhydride. During the laboratory experiments splashes and
large particles of vapor were deposited in. traps. Under
manufacturing conditions the content of splashes and va-
por was determined by trapping them with absorbent cotton.
The control of the process of acoustic coagulation
was also conducted by means of microphotoPraPhy.
7
1
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Fig, 1. Diagram of a-device for the investi-
gation.of acoustic coagulation of vapor con-
taining fluorine compounds from exhaust gases
of the superphosphate granulation department.
- exhaust pipe; 2 - vacuum pump; 3 - sonic treat-
ment tube; sonic generator; 5 - rheometer; 6, 7 suc-
on apparatus;,My 9 - Drmel jars ; 10 - continuous
ultramicroscope; 11 - condensate tap; 12 - thermometers;
13 - compressor; 14 - oil separator; 15 - receptacle;
16 - wires to titanate-barium probe.
8
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Fig. 2. Sonic pressure along the
axis
of the sonic treatment tube.
Fig. 3. Effect of duration of sonic
treatment on degree of purification
of gases from fluorine.
Fig. 4. Effect of initial concentration
of fluorine on degree of purification.
9
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Results of Experiments
In order to determine the nature of the sonic field
we took a -number of measurements of the intensity of sound
along the axis of the sonic treatment tube. The results are
shown in Fig. 2. Due to the echo from the rear end part of
the tube, a system of vertical waves is established in the
tube. In the front part (up to 60 mm) the sonic field is
distorted by conditions at the
intake
and by the presence
of a nozzle for removal of the gas. The maximum sonic :ores-
sure is observed at a distance of 190 to 235 mm from the
diaphragm; further damping
is insignificant. The mean
of the tube corresponds to
decibels.
We determined the effect on acoustic ooag-ulation
under laboratory conditions of the following: duration of
sonic treatment, humidity content and initial concentra-
tion of fluorine at temperatures of 50, 55 and 60?C. The
humidity content wascontrolled by changing the ratio bet-
ween the expenditure of hot and cold humidified air.
In Fig. 32 we cite data of the relation between
the degree of purification of gases from fluorine and the
duration of sonic treatment, with humidity being constant
of oscillations along the tube
sonic pressure along the axis
the
level of
intensity of 155
1 (at a 1.2perature of 5500 and the ratio between cold and_j
10
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Vc
[Tot air = 10. The initial. concentration of fluorin;-1
was 0.6 - 1.7 g/M3. As can be soon from Fig. 3, the dura-
tion of the order of 4-5 seconds is sufficient for acoustic
coagulation of vapor, ensur
(1.
degree of purification
from fluorine between 75 and 78 'pe_.-oent without additional
mechanical precipitators. Further ex-oosure of vapor to the
sonic field provides an insignificant increase of the de-
gree of purification. Analogous curvos were obtained by us
earlier for vapor of sulfuric acid ./.1/.
Shown in Pig. 4 are data on the relation between
the degree of purification and the initial concentration
of fluorine. Experiments were made without sonic treatment
and with sonic treatment of 3
to 4 seconds duration. In
the area under investigation (0.6 to 4.5 gA13 ) purification
is more comPlete with an increase of the concentration of
fluorine. Without sonic treatment the precipitation of
fluorine is 42 to 69 percent; with sonic treatment the
degree of purification increased to 80-95 percent, depen-
ding on the humidity of the gas.
The degree ofxipurification substantially changes
with an increase of the weight concentration of vapor and
steam. In Fig. 5 data are shown on the relation between the
degree of purification and general humidity content of the
gas. An increase of the latter from 15 to 120 g/m3 causes
Ian increase of the concentration of vapor and an increase 1
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the separation of fluorine from 75 to 95 Percent.
Fig. 5. Effect of the general humidity
content on the degree of purification from
fluorine.
A - degree of purification (%), 3 - humidity
content (g/m3).
Fig. 6. Effect of duration of sonic
treatment on the degree of purification
from fluorine of the exhaust gases of the
superphosphate granulation ,:7.)artment.
A - degree of purification (), B - duration
of sonic treatment (sec).
Thus, laboratory experiments have shown that it
is possible to use the method of acoustic coagulation
to purify industrial gases from fluorine compounds.
?";; 2
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Conentation
,of fluone in
"gas (g/2))
EL:genditure -LJ ?. ... L.) . ., Initial
of gas (1/m1n) of sonic '
treatment
(sec)
Without Sonic Ti-eatment
Degree
Final (DJ. Du-
rification
(`A
0.040 0.036 10.00
?Olio-wins sonic treatment at a frequency
of 16.5 cps
ean
13
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The results of the secend etags of investigation:-]
of acoustic coagulation of fluorine cez.pounds, conducted
with exhaust gases of the suPerphosphate granulation d
partment are shown in the Table. It follows from the data
of the Table that for practical Purposes the duration of
sonic treatment of the order of 3 seconds is sufficie_1-?
this causes a precipitation of 87 pecent of the fluorine
contained in the gas. At a mean concentration of fluorine
of 0.18 g/m3 following sonic treatment of 3 seconds shows
a remainder of 0.023 g/m3 which is below the recomended
health norm (0.03 g/m3). The relation between the degree
of purification of cases and duration of sonic treatment
is shown. in
It should be noted that at the industrial depart-
ment of superphosphate granulation acoustic coagulation
occurred more completely than with gases of laboratory
equipment. This can apparently be explained by the higher
humidity content of the gas, as well as by the presence
of center of condensation (specks of dust) which facili-
tate the formation ofvapor.
In some experiments, along with the determination
of degree of purification, we also made analyses of the
cendensate from the sonic treatment tube. The fluorine
content in the condensate varied from 0.7 to 8.5 g/l,
Idepending on the initial concentration of fluorine in
- 14 -
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r7he gas.
Determination of the number of particles in a unit
of volume and their distribution according to size was
made by means of a continuous ultramicroscope and micro-
photography.
Conclusions
1. In laboratory investigation of acoustic coagu-
lation of vapor containing fluorine compounds (at the
level of the intensity of sound of the order of 153 to
155 decibels and frequency of 16.5 cps) it was found that
the action of sound increases the degree of purification
from between 42 and 69 Percent (without sound treatment)
to between 80 and 93 percent.
2. The completeness of purification depends in
large measure on the concentration of vapor in the gas.
An increase of the total humidity content from 15 to 120
g/m3 causes an increase of the degree of purification from
73 to 93 percent. -;:ith a constant humidity content the
degree of purificatL= increases with the increase of the
initial concentration of fluorine in the gas and duration
of sonic treatment.
3. Investigations wore conducted of acoustic coagu-
lation of vapor containing fluorine compounds from e:zhaust
!lases of the superphosphate granulation department. It
_____ 15
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rTas found that with sonic treatment of 3 seconds duration i
there is a Precipitation of 37 --Jercent of fluorine contai-
ned in exhaust gases. -Jith an initial concentration of
fluorine of 0.18 g/m3, its content, following acoustic
coagulation, Is reduced to a magnitude of the order of
0.025 g/m3, i.e., below the recommended health norm.
4. The cited results were obtained in the sonic
treatment tube alone, without additional mechqnical pre-
cipitators. 12 the latter are used, the decree of preci-
pitation of fluorine compounds will be even higher.
BIBLIOGRAPHY
r._
/1/ I. Li. Boguslavskiy and L. D. Kiosse, Soobshcheniya
o na chno-tekhnicheskikh rabotakh 11'11112 (Reports of Scien-
tific-Engineering Works of the Scientific Research Institute
of Fertilizers and Insectifuges), 2, 54 (1957).
/2,7 H. Sh. Safiullin, Khim Prom. (Chemical Industry)
6, 77 (1959).
t$/ G. K. Shilin, Sbornik annotatsiy
tel'skikh rabot NIIOGAZ za 1956-1957
tations of Scientific Research Wo7ks
search Institute of Gas Purification
tation for the Years 1956/1957).
A/ K. E. Lunde, Ind.Eng.Chem. 50, 3, 293 (1958).
nauchno-issledova-
ggo(Symposium of An7a0-
of the Scientific Re-
for Industry and Sani-
2-57 A. L. Whynes, Inst. Chem, Eng. Graduates & Students
Section, Feb. 19 (1954).
/67 A. I. Shereshevskiy, L. S. Goritskiy and L. K.
Pot apova, Soobshcheniya o nauchno-tehhnicheskikh rabotakh
NIUIP, 2, 26 (1957).
17/ V. V. Illarionov, T. I. Sokolova, S. Z. Kulagina I
1,5
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T--
and 1. G. Knyazeva, Soobshohoniya 0 mauchno-tekhnicheskikhi
rabotakh NIUIF, 2, 48 (1957).
/8/ I. H. Boguslavskiy, V. LI amm and V. I. Matrozoy,
Soobsheheniya o nauchno-issledovatcl'skikh rabotakh NIUI2,
6-7, 13 (1958).
/9/ I. M. Boguslavshiy and V,
t10/ Ya. V. Shyartsshteyn and V. . Eamm, 55.
ibid., 410
- n-
1-117 V? . I. Matrozov and V. H.
Eamm, ibid., 102.
11.?./ V? . I. Matrozov, V. H. EamL1 and G. H. Yusoya, ibid.
108.
7137 I? . Y. Boguslavskiy and V. M. Earn., Soobshcheniye
o nauchno-tekhmicheskikh rabotakh NIUIr, 2, 49 (1957).
107 I. Zaring and G. Popoya, Zh2kH (Zhurual 2rikiad-
noy Xhimii - Journal of Applied Chemistry), 14,866 (1936).
LW L. Bergman Ul'trazyuk (Ultrasonics) 1956.
/16_7 A? . E. Crauford, Ul'trazyukoyaya tekhnika (Ultra-
sonic Engineering) 1956.
[IV E? , T. Rueter and R. H. Bolt, Sonic Technicues
for Use of Sound and Ultrasound Engineering and Science,
N.Y. (1955).
/18/ Ye. L. Hednikov, Primeneniye ul'traakustiki k
issledolianiyu veshchestva (Use of Ultrasound in investi-
gation of Hatter) OK, 3 (1956).
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