thiokol propulsion · 2017. 5. 30. · 5 thiokol propulsion critical characteristics of cl-20 and...
TRANSCRIPT
ThiokolPropulsion
Scott Hamilton, ATK-Thiokol PropulsionKaren Burrows, Naval Surface Warfare Center – Indian Head Division
DISTRIBUTION STATEMENT A: Approved for public release; distribution is unlimited.
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Thiokol Propulsion
590N-02-0102Tue Aug 27 13:01:37 2002
0.005
0.010
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
0.065
0.070
0.075
0.080
0.085
0.090
0.095
Ab
sorb
ance
700 720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
170 mic ron
Epsi lon Po lymorph
9 8 % P u r e b y H P L C
590N-02-0102Tue Aug 27 13:01:37 2002
0.005
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0.015
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0.070
0.075
0.080
0.085
0.090
0.095
Ab
sorb
ance
700 720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
170 mic ron
Epsi lon Po lymorph
9 8 % P u r e b y H P L C
Background
• CL-20 is the most energetic conventionalexplosive available for military use inExplosives, Rocket, and Gun Propellants.
• Variability in production scale batches andthe cost of CL-20 limit wide acceptance ofCL-20 based energetic materials.
-Crystal agglomerates-Particle size distributions inconsistent-Lot-to-lot variability in sensitivity-TADF precursor expense
• CL-20 MANTECH Program implemented topositively impact:- CL-20 Reproducibility/Consistency- Crystal Quality and Sensitivity- Cost
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Thiokol Propulsion
CL-20 Prior to Mantech
590N-02-0102Tue Aug 27 13:01:37 2002
0.005
0.010
0.015
0.020
0.025
0.030
0.035
0.040
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0.055
0.060
0.065
0.070
0.075
0.080
0.085
0.090
0.095
Abs
orba
nce
700 720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
Distribution changed witheach crystallization batch
Epsilon Polymorph
98% Pure by HPLC
Agglomerated / Multicrystalline
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Thiokol Propulsion
CL-20 MANTECHCL-20 MANTECHGovernment/Industry TeamGovernment/Industry Team
NSWC/Indian Head DivisionNSWC/Indian Head Division
Project Management for Navy effortsCrystal Sensitivity EvaluationCrystallization Analytical Support
ATK-Thiokol PropulsionATK-Thiokol PropulsionNitration/Crystallization TechnologyCrystallization Process ControlScale-up & Transition to Production
NAWC-WD/China LakeCrystallization Technology
TACOM-ARDECTACOM-ARDECProject Management for Army EffortsNitration & Crystallization ModelingCL-20 Coating Studies
NAVAL AIR WARFARE CENTERWe apo ns Div is ion
SRI, IntlSRI, Intl..
Stevens Inst. TechStevens Inst. Tech
GeoCentersGeoCenters, Inc., Inc.
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Thiokol Propulsion
Navy Program Objectives
l Task 1 – Identify critical physical and chemical
characteristics of CL-20
l Task 2 – Evaluate alternative crystallization
techniques at the laboratory scale
l Task 3 – Evaluate crystal reproducibility, down select,
and transition process(es) to the pilot plant for full
scale production demonstration
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Thiokol Propulsion
Critical Characteristics of CL-20 andLaboratory Scale Crystallizationsl Database compiled for correlating CL-20 sensitivity with physical and
chemical properties
l Round Robin Testing- Many CL-20 samples (>50) submitted for visualassessment, testing and discussion
– Used controlled impact and friction testing
v NSWC-IH, NAWC-CL, ATK Thiokol, ARDEC, Aerojet, Bofors,SNPE submitted samples
v Testing at NSWC-IH, NAWC-CL, ARDEC, ATK Thiokol
Findings:
– Impact and friction showed little difference between samples
– Neat CL-20 is more sensitive than RDX/HMX standards despitedifferences in :
– Crystallization Method - Precursor Type
– Impurity Level - Visual differences (e.g., shape, crystallinity, etc.)
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Thiokol Propulsion
Round Robin Testing Samples
Highly purified CL-20TADF based CL-20
TADA based CL-20
Various crystallizationtechniques
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Thiokol Propulsion
Round Robin Testing ResultsNSWC Results: Sliding Friction NSWC Results: Sliding Friction vsvs Impact SensitivityImpact Sensitivity
0
50
100
150
200
250
300
350
0 2 4 6 8 10 12 14 16 18 20 22
Superfine PETN
RDX
HMX
Most impact and friction sensitive
CL-3CL-1, IHD 274, X991027
1696-73, 1697-53, M4 2000-01
PCL-74, PCL 74 (R)
CL-21696-47-1
1696-420174/2
IHD 174
AB
L S
lidin
g F
rict
ion
Sen
siti
vity
, lb
AB
L S
lidin
g F
rict
ion
Sen
siti
vity
, lb
(TIL
at
8 ft
/sec
)
Impact Sensitivity (50% Height), cm [ERL apparatus]
NSWC Results: Sliding Friction NSWC Results: Sliding Friction vsvs Impact SensitivityImpact Sensitivity
0
50
100
150
200
250
300
350
0 2 4 6 8 10 12 14 16 18 20 22
Superfine PETN
RDX
HMX
Most impact and friction sensitive
CL-3CL-1, IHD 274, X991027
1696-73, 1697-53, M4 2000-01
PCL-74, PCL 74 (R)
CL-21696-47-1
1696-420174/2
IHD 174
AB
L S
lidin
g F
rict
ion
Sen
siti
vity
, lb
AB
L S
lidin
g F
rict
ion
Sen
siti
vity
, lb
(TIL
at
8 ft
/sec
)
Impact Sensitivity (50% Height), cm [ERL apparatus]
NSWC-IH Round Robin Testing Results
Round Robin Testing Quantified the Sensitivity of CL-20
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Thiokol Propulsion
Crystallization Process Developmentl Applied methods learned on early crystallization processes
l Developed 2 reproducible processes on 100-gram scale
l Precipitation
l Evaporation
l Implemented Crystallization Process and Product Monitoringequipment using laser light-scattering technology
l Determined effects of temperature, stir rate, stirrer type, andseed quality/quantity on crystallization process
l Evaluated trends so that scale-up would go smoothly
Understanding the effects of crystallization variables is critical toensure product outcome during processing.
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Thiokol Propulsion
Real Time Crystallization Monitoring
Lab-scale Crystallizer Configuration
l Able to observe real time particle size distributionl Able to observe crystal growth characteristics within chosen
channel (particle size) groupingsl Watch fine and course particle behaviorl Observe average particle size over time
Benefit: Can apply corrective action during processing to render desired product characteristics.
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Thiokol Propulsion
Scale-up Process
l Developed methods on 100-gram scale
l Demonstrated reproducibility on 200 gram scale
l Observed crystal growth characteristics with LasentecInstrument (evaporative method)
l Scaled-up to the 50-gallon reactor
l Demonstrated that acceptable crystals could beproduced by precipitation and evaporative methods
l Scaled-up to the 500-gallon reactor
l Used processes developed on the lab scale and subscales
l Followed crystallization with Lasentec Instrument
l Demonstrated repeatability from batch-to-batch
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Thiokol Propulsion
500-Gallon Precipitation Crystallization Matrix
Lot Number
Batch Size (lbs)
Stir Rate (rpm)
Temp (deg F)
Seed Quantity
(lbs)
Seed Size (lot
2180150)
Starting Materials
Crystal Size
(microns) 590N-
02-0078 100 125 68 10 2 microns virgin 30
590N-02-0081
100 125 115 10 2 microns virgin 31
590N-02-0083
100 125 68 10 2 microns non-virgin 23
l Reduced original matrix due to time and expense issues
l Showed that process was stable at two different temperatureswith virgin materials
l Non-virgin materials produced somewhat smaller particles thanthe virgin counterparts
l Produced small particles without the need for grinding
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Thiokol Propulsion
Particle Size Distribution Comparison Chart for CL-20 590N-02-0077 06-20-02
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
16.00
18.00
704.
00
592.
0049
7.80
418.
60
352.
0029
6.00
248.
90
209.
3017
6.00
148.
00
124.
5010
4.70
88.0
0
74.0
062
.23
52.3
3
44.0
037
.00
31.1
1
26.1
6
22.0
018
.50
15.5
6
13.0
811
.08
9.25
7.78
6.54
5.50
4.63
3.89
3.27
2.75
2.31
1.95
1.64
1.38
1.16
0.97
0.82
0.69
Diameter (microns)
Per
cent
per
Cha
nnel
Unground 30 micron CL20
M590-02-0077 Dump sampleWed Jun 19 14:59:57 2002
-0.000
0.005
0.010
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
0.065
Ab
sorb
ance
720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
Lot 590N-02-0077
Epsilon Polymorph
29 Micron99.5% Pure by HPLC
99.5% Pure by HPLC
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Thiokol Propulsion
500-Gallon Evaporative Crystallization Matrix
l Monitored process by Rockwell trend software, LasentecInstrument and NMR.
l Evaluated effects of crystallization variables
l Stir rate – 95, 110, 125 rpms
l Temperature – 35, 45, 55 celcius
l Seed quality – 2 micron
l Stir time – 3, 10, 14 hours
l Demonstrated reproducibility at two different conditions
l 110 rpms and 55 deg C,
l 125 rpms and 60 deg C
l Recycled and virgin CL-20 was used
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Thiokol Propulsion
CL20 590N-02-0102
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
16.00
704.
0059
2.00
497.
8041
8.60
352.
0029
6.00
248.
9020
9.30
176.
0014
8.00
124.
5010
4.70
88.0
074
.00
62.2
352
.33
44.0
037
.00
31.1
126
.16
22.0
018
.50
15.5
613
.08
11.0
89.
257.
786.
545.
504.
633.
893.
272.
752.
311.
951.
641.
381.
160.
970.
820.
69
Diameter (microns)
Per
cen
t p
er C
han
nel
0.00
10.00
20.00
30.00
40.00
50.00
60.00
70.00
80.00
90.00
100.00
Cu
mu
lati
ve %
CL-20 Lot 590N-02-0102
590N-02-0102Tue Aug 27 13:01:37 2002
0.005
0.010
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
0.065
0.070
0.075
0.080
0.085
0.090
0.095
Ab
sorb
ance
700 720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
99.5% Pure by HPLC
224 micron
Epsilon Polymorph
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Thiokol Propulsion
CL20 590N-02-0103 Reactor
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
16.00
704.
0059
2.00
497.
8041
8.60
352.
0029
6.00
248.
9020
9.30
176.
0014
8.00
124.
5010
4.70
88.0
074
.00
62.2
352
.33
44.0
037
.00
31.1
126
.16
22.0
018
.50
15.5
613
.08
11.0
89.
257.
786.
545.
504.
633.
893.
272.
752.
311.
951.
641.
381.
160.
970.
820.
69
Diameter (microns)
Per
cen
t p
er C
han
nel
0.00
10.00
20.00
30.00
40.00
50.00
60.00
70.00
80.00
90.00
100.00
Cu
mu
lati
ve %
CL20 590N-02-0103 Reactor
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
16.00
704.
0059
2.00
497.
8041
8.60
352.
0029
6.00
248.
9020
9.30
176.
0014
8.00
124.
5010
4.70
88.0
074
.00
62.2
352
.33
44.0
037
.00
31.1
126
.16
22.0
018
.50
15.5
613
.08
11.0
89.
257.
786.
545.
504.
633.
893.
272.
752.
311.
951.
641.
381.
160.
970.
820.
69
Diameter (microns)
Per
cen
t p
er C
han
nel
0.00
10.00
20.00
30.00
40.00
50.00
60.00
70.00
80.00
90.00
100.00
Cu
mu
lati
ve %
CL-20 Lot 590N-02-0103
590N-02-0103 ReactorWed Aug 28 15:06:05 2002
-0.000
0.005
0.010
0.015
0.020
0.025
0.030
0.035
0.040
0.045
0.050
0.055
0.060
0.065
0.070
Ab
sorb
ance
720 740 760 780 800 820 840 860 880 900
Wavenumbers (cm-1)
99.5% Pure by HPLC
188 micron
Epsilon Polymorph
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Thiokol Propulsion
CL20 590N-02-0104 Dump
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
16.00
704.
0059
2.00
497.
8041
8.60
352.
0029
6.00
248.
9020
9.30
176.
0014
8.00
124.
5010
4.70
88.0
074
.00
62.2
352
.33
44.0
037
.00
31.1
126
.16
22.0
018
.50
15.5
613
.08
11.0
89.
257.
786.
545.
504.
633.
893.
272.
752.
311.
951.
641.
381.
160.
970.
820.
69
Diameter (microns)
Per
cen
t p
er C
han
nel
0.00
10.00
20.00
30.00
40.00
50.00
60.00
70.00
80.00
90.00
100.00
Cu
mu
lati
ve %
CL20 Lot 590N-02-0104
99.5% Pure by HPLC
196 micron
590N-02-0104 Dump SampleFri Aug 30 10:07:24 2002
0.014
0.016
0.018
0.020
0.022
0.024
0.026
0.028
0.030
0.032
0.034
0.036
0.038
0.040
0.042
0.044
0.046
0.048
0.050
0.052
0.054
0.056
0.058
0.060
0.062
0.064
0.066
0.068
0.070
Abs
orba
nce
700 720 740 760 780 800 820 840 860 880 900 Wavenumbers (cm-1)
Epsilon Polymorph
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Thiokol Propulsion
CL-20 Cost Reduction
Thiokol Propuls ion PO Box 707, M/S 230 Brigham City, UT 84302-0707 USA Tel: 1 435 863-2778 Fax: 1 435 863-8782 E-mail: [email protected]
November 18, 2002 3600-FY03-L141 NSWC - Indian Head Division 101 Strauss Ave. Indian Head, MD 20640-5035 Attention: Karen Burrows, Code 950 Subject: Projected Price Reduction for CL-20 Reference: Navy CL-20 Crystallization Mantech Contract No. N00174-99-C-0030. Dear Karen,
With the recent completion of the technical effort and formalizing of the final report, I have been able to review the entire trail of efforts that has been traversed under the CL-20 Crystallization Mantech contract. I am amazed at all of the different things that we have learned about CL-20 as we’ve pursued the two very different crystallization processes that were developed. There were many points along the trail when I would have sworn we would not be successful in bringing the two methods to the maturity that they currently have. We are truly fortunate that the processes are as robust as they appear to be. As part of this culminating effort, we have taken the opportunity to evaluate current costs for CL-20 manufacture. We have found that, with the incorporation of the new TADA precursor, the robust nitration process developed under the Army CL-20 Mantech contract, and the proven evaporative crystallization process established under the Navy contract, we can project some significant reductions in the price of CL-20. Although we have only processed the first production lot, converting 1000 kg of TADA to CL-20, we can foresee an immediate reduction in the price of CL-20 of $50 per pound, with possible further reductions that may be applied as we verify our cost projections while processing the second lot of material, which we should begin early next year. Of course, there are some underlying assumptions upon which this cost reduction projection is dependent. The principle assumptions are that the precursor price remains where it is at or below and that the annual CL-20 sales volume remains where it is at or above. The first assumption is probably dependent mostly on the second, but we are working with our supplier to obtain independent price reductions which we would pass along to our CL-20 customers. Also, with the many organizations currently evaluating CL-20 for defense as well as commercial applications, we do not expect a problem with the sales volume dropping in the near future. We have also identified other potential opportunities to save on CL-20 processing costs and we will be pursuing these as well. As processing of other materials such as TEX, TATB, DNAN, and MNA reach the pilot plant scale and processing in our M-590 facility we could foresee some processing synergies that could further reduce the price of processing CL-20.
Immediate $50/lb reduction in costattributable to:ü Lower cost precursor, TADAü TADA Nitration process
developed under Army Mantechü Optimized crystallization process
and SOTA process monitoringdeveloped underNavy Mantech
Further cuts to be determined aftercompletion of future production-scaleruns to fulfill orders.
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Thiokol Propulsion
Conclusions
l Sensitivity of CL-20 is similar to PETN
l TADA is acceptable for use a CL-20 precursor
l 30 micron CL-20 can be made reproduciblywithout grinding
l Large (>100 micron) unground CL-20 can bemade reproducibly
l Price of CL-20 reduced by $50/lb and furthercuts are anticipated
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Thiokol Propulsion
The Way Forward
CL-20 Is Ready for Transition andImplementation into DoD WeaponsCL-20 Is Ready for Transition andImplementation into DoD Weapons
üCL-20 can now be produced on the production scale(500 gallon) that is similar from lot-to-lot.
üAdvanced process monitoring technology is nowbeing utilized in the production of CL-20
- A window of acceptable operating conditions hasbeen established to ensure lot-to-lot consistency