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Safety analysis for DFC process

Dust DSC Analysis


Sr. No. Sample Detail Explosive Powder Resistivity MIE
DSC
1st Endotherm 79°C

2nd Endotherm 109°C

Specific Powder
Violent Resistivity:
1 MNG explosion- > 1 X1012 Ohm- 200 mJ
St 2H m
Resistive Exotherm 170°C

1st Endotherm 128°C

Specific Powder
Mild Resistivity:
2 MNMTI explosion > 1 X109 Ohm-m 4 mJ
St 1H Moderately Exotherm 149°C
Conductive

3 Wet MNMTI With solvant NA NA NA NA

Endotherm 101°C

4 Reaction mass Step-01. NA NA NA

Exotherm 186°C

1st Exotherm 168°C

5 Reaction mass Step-02. NA NA NA


5 Reaction mass Step-02. NA NA NA
2nd Exotherm 215°C

1st Exotherm 161°C

6 Reaction mass Step-03. NA NA NA

2nd Exotherm 280°C

Endotherm 90°C
Residue after Distillation
7 NA NA NA
(Step-01)
Exotherm 182°C

Molten mass after


8 Distillation NA NA NA Exotherm 154°C
(Step-02)

Residue received after


9 distillation of STEP-03 NA NA NA NA
Filtrate ML -01

Endotherm 164°C

Violent Specific Powder


explosion- Resistivity: > 1 X1012
10 Dry CTZ
Ohm-m
19 mJ
St 2H Resistive
Violent Specific Powder
explosion- Resistivity: > 1 X1012
10 Dry CTZ
Ohm-m
19 mJ
St 2H Resistive

Exotherm 190°C

Milled Tebu
その他 1.2mJ
DSC Analysis Fall Hammer Operating
Flash point
Peak Enthalpy Severity Test temperature
84°C 40 J/g

139°C 95 J/g

MNG having 5%
And 10% N.A 50 deg C
Moisture Test is
negative
205°C 997 J/g High

134°C 120 J/g

Negative NA 60 deg C
215°C 2228 J/g High

NA NA NA Negative NA 40 deg C

112°C 18 J/g NA NA

60 deg C

221°C 170 J/g Medium NA NA

196°C 17 J/g Low NA NA

80 degC
80 degC
257°C 89 J/g Low NA NA

239°C 456 J/g High NA NA

60 deg C

310°C 44 J/g low NA NA

110°C 13 J/g NA NA
60 deg C
223°C 332 J/g Medium NA NA

243°C 583 J/g High NA NA 80 degC

Residue sample is
thick & non stirrable.
NA NA NA NA So Flash Point analysis
is not possible

173°C 118 J/g

Negative NA 90 deg C
Negative NA 90 deg C

229°C 1473 J/g High


Observation/Findings Precautions required

1. Mild endotherm at 79 and 109 deg C.


2. At 170 deg C, exotherm of 997 J/gm is very 1. Process conditions well below decomposition
severe. temperature of 170 deg C.
3. MNG has severe dust explosion hazard and 2. Earthing bonding, conductive surface, anti static
falls in ST2H. bags/clothes essential.
3. Avoid use of plastic, non conductive tools/tackles for
4. Low MIE. handling.
5. Material is resistive. 4. Innertisation required.
6. Material is not impact sensitive. 5. Equipments to be grounded properly.
7. In laboratory, solid MNG was charged in glass 6. All flameproof electricals required and avoid source
vessel from elevation and found to generate of ignition.
very small amount of dust.

1. Mild endotherm at 128 deg C. 1. Process conditions well below decomposition


2. At 149 deg C, exotherm of 2227 J/gm is very temperature of 149 deg C.
severe. 2. As MIE is very low, stringent precautions against
3. MNMTI has moderate dust explosion hazard static ignition required.
and falls in ST1H. 3. Earthing bonding, conductive surface, anti static
4. Very low MIE. bags/clothes essential.
5. Material is moderate conductive. 3. Avoid use of plastic, non conductive tools/tackles for
6. Material is not impact sensitive. handling.
4. Innertisation required.
5. Equipments to be grounded properly.
6. All flameproof electricals required and avoid source
of ignition.
7. To avoid drying and dry powder handling.
8. To provide double earthing to piping and
equipments.

1. Earting, bonding, conductivity required.


1. Slurry contains MNMTI, DMF and traces of 2. Proper grounding of all eqiupments.
Toluene. 3. Avoid use of plastic, non conductive tools/tackles.
4. Innertisation in reaction vessel required.

1. Earting, bonding, conductivity required.


1. Operating condition well below 112 deg C. 2. Proper grounding of all eqiupments.
2. Reaciton mass contains Toluene solvent. 3. Avoid use of plastic, non conductive tools/tackles.
4. Innertisation in reaction vessel required.

1. Earting, bonding, conductivity required.


1. Operating condition well below 196 deg C. 2. Proper grounding of all eqiupments.
2. Reation mass contains DMF, Toluene 3. Avoid use of plastic, non conductive tools/tackles.
solvents. 4. Innertisation in reaction vessel required.
1. Earting, bonding, conductivity required.
1. Operating condition well below 196 deg C. 2. Proper grounding of all eqiupments.
2. Reation mass contains DMF, Toluene 3. Avoid use of plastic, non conductive tools/tackles.
solvents. 4. Innertisation in reaction vessel required.

1. Earting, bonding, conductivity required.


1. Operating condition well below 239 deg C. 2. Proper grounding of all eqiupments.
2. Reation mass contains Methanol solvent. 3. Avoid use of plastic, non conductive tools/tackles.
4. Innertisation in reaction vessel required.

1. Earting, bonding, conductivity required.


1. Operating condition below 182 deg C. 2. Proper grounding of all eqiupments.
2. Residue contains traces of Toluene solvent. 3. Avoid use of plastic, non conductive tools/tackles.
4. Innertisation in reaction vessel required.

1. Earting, bonding, conductivity required.


1. Operating condition below 154 deg C. 2. Proper grounding of all eqiupments.
2. Molten mass contains DMF. 3. Avoid use of plastic, non conductive tools/tackles.
4. Innertisation in reaction vessel required.

Analysis of "as such" and neutralized sample


under progress.

1. Process conditions well below decomposition


temperature of 173 deg C.
1. Mild endotherm at 173 deg C. 2. As MIE is very low, stringent precautions against
2. At 190 deg C, exotherm of 2227 J/gm is very static ignition required.
severe. 3. Earthing bonding, conductive surface, anti static
3. CTZ has severe dust explosion hazard and bags/clothes essential.
falls in ST2H 3. Avoid use of plastic, non conductive tools/tackles for
handling.
4. Very low MIE. 4. Innertisation required.
5. Material is moderate conductive. 5. Equipments to be grounded properly.
6. Material is not impact sensitive. 6. All flameproof electricals required and avoid source
of ignition.
7. To provide double earthing to piping and
equipments.
1. Process conditions well below decomposition
temperature of 173 deg C.
1. Mild endotherm at 173 deg C. 2. As MIE is very low, stringent precautions against
2. At 190 deg C, exotherm of 2227 J/gm is very static ignition required.
severe. 3. Earthing bonding, conductive surface, anti static
3. CTZ has severe dust explosion hazard and bags/clothes essential.
falls in ST2H 3. Avoid use of plastic, non conductive tools/tackles for
handling.
4. Very low MIE. 4. Innertisation required.
5. Material is moderate conductive. 5. Equipments to be grounded properly.
6. Material is not impact sensitive. 6. All flameproof electricals required and avoid source
of ignition.
7. To provide double earthing to piping and
equipments.
Comment
ENGINEERING CONTROLS
MNG is requested to measure
Drop hummer test again.
And check the scorched part or
burned part.
And measure IMO test.

1. Metal SS-316 Charging Hopper provided And confirm with Cibatech


2. Charging Hopper & Vessel RB-801 Earthing Bonding 「Not likely to be impact
2. N2 provision in Hopper & Vessel RB-801
3. Flameproof Electricals provided i.e Agitator Motor, RTD sensitive」or not.
Sensor
4. Charging of MNG in vessel thorugh Bag
5. All Connected Flanges & Piping Earthing

1. Anstistatic Filter Cloth provision in Dom Filter MNMTI is required to handle


2. N2 provision in Dom Filter under nitrogen blanket or in the
3. Doble Electrical Earthing & Bonding of Dom filter & condition with water Wet.
connected piping (This step is to dissolve MNMTI
4. MNMTI will be kept in wet form (only filtration, no Drying with DMF instead of removing as
consider) solid.)
5. Wet MNMTI will be Kept in DOM Filter, DMF will be
circulated in Dom Filter to dissolve MNMTI in DMF to avoid
Scrapping.

1. Dom Filter, MNMTI+DMF Slurry Tank & Vessel is provided


earthing, bonding & Grounding
2. All connected piping earthing, bonding
3. Circulation Pump Flame Proof Motor

The heat source temperature is


1. RB-801 Rxn. Vessel is provided earthing, bonding & required to be lower than TMRAD
Grounding
2. All connected piping earthing, bonding at 24 hour.
3. TMRAD 24 Hrs. is 124 °C & Provision of Utility is Hot
Water Temp.@ 60 °C in RB-801.
4. Flame proof electricals used i.e Agitator Motor, RTD
5. N2 provision in RB-801

1. R-802 Rxn. Vessel is provided earthing, bonding &


Grounding
2. All connected piping earthing, bonding
3. TMRAD 24 Hrs. is 156 °C & Provision of Utility is Hot
Water Temp.@ 60 °C in R-802.
4. Flame proof electricals used. i.e Agotator Motor, RTD
5. N2 provision in R-802
1. R-802 Rxn. Vessel is provided earthing, bonding &
Grounding
2. All connected piping earthing, bonding
3. TMRAD 24 Hrs. is 156 °C & Provision of Utility is Hot
Water Temp.@ 60 °C in R-802.
4. Flame proof electricals used. i.e Agotator Motor, RTD
5. N2 provision in R-802

1.R-802 Rxn. Vessel is provided earthing, bonding &


Grounding
2. All connected piping earthing, bonding
3. TMRAD 24 Hrs. is 83 °C & Provision of Utility is Hot Water
Temp.@ 60 °C.
4. Flame proof electricals used i.e Agotator Motor, RTD
5. N2 provision in R-802

1. RB-801 Vessel is earthing, bonding & Grounding


2. All connected piping earthing, bonding
3. N2 Provision in RB-801 Distillation vessel
4. Flame proof electricals used i.e Motor. RTD
5. Residue will be collected in Drum

It is required to measure ARC and


1. ATFE, Concentrated mass collection Vessel & Feed Tank is heat source temp. is below TMRAD
provided earthing, bonding & Grounding at 24 hour.
2. All connected piping earthing, bonding
3. TMRAD 24 Hrs. is °C & Provision of Utility is Hot Water
Temp.@ 60 °C in ATFE & Molten mass Collection Vessel.
4. Flame proof electricals used i.e Agotator Motor, RTD
5. N2 Provision in R-803 Molten Mass Coll. vessel

To measure the flash point


reference to below procedure.
(ASTM D3278-1982: Standard
Test Methods for Flash Point of
Liquids by Setaflash Close-d-Cup
Apparatus)
If no methylalcohol is in the
residue, not be required.

In the test of SCC (IMO burning


test), it was confirmed that there
was no reaction propagation
1. N2 provision in ANFD & Dust Filter property under nitrogen.
2. Antistatic Cloth in Dust Filter
3. Flame Proof Electricals used Agitator Motor, RTD, FLP
Panel of ANFD
4. ANFD & connected equipments earthing, bonding &
grounding
5. Utility Hot Water Temp. is 60 °C
6. Double Earthing, Bonding of Electricals to ANFD &
connecting equipments + Piping
7. For Scrapping of Dry CTZ from ANFD Conductive Scoop/
Tackles will be used
8. Dry CTZ will be collected in Fiber Bord Drum having
metalic strip which will be connected to crocodile earthing
was no reaction propagation
1. N2 provision in ANFD & Dust Filter property under nitrogen.
2. Antistatic Cloth in Dust Filter
3. Flame Proof Electricals used Agitator Motor, RTD, FLP
Panel of ANFD
4. ANFD & connected equipments earthing, bonding &
grounding
5. Utility Hot Water Temp. is 60 °C
6. Double Earthing, Bonding of Electricals to ANFD &
connecting equipments + Piping
7. For Scrapping of Dry CTZ from ANFD Conductive Scoop/
Tackles will be used
8. Dry CTZ will be collected in Fiber Bord Drum having
metalic strip which will be connected to crocodile earthing

In the case the MIE is below 3mJ ,


it is rquired Nitrogen blanket.
it is requested to control particle
size so that energy becomes more
than 3 mJ.
To cotrol the particle size by
condition of jet mil.

to measure Kst, and design proper


raputre disk and proper venting
place/direction based on NFPA68.
(Standard on explosion
protection)
SCC
in Japanese
1. 住友化学では昇温速度
10℃/minのSC-DSC測定にお
いて、発熱検知温度とプロ
セス最高温度(熱源)との温
度余裕(安全率)として100℃
を考慮しています。安全率
を満たさない場合に、ARC
断熱試験を追試しています

2. Drop hummer testの内容
が住化にて実施している内
容と異なります。試験機関
に一般論として「Not likely
to be impact sensitive」の結
論であれば粉砕操作上の危
険性は低いと考えてよいか
確認ください。
1.住友化学では3mJ(MIKE3
法)を窒素置換実施の目安と
しています。
2.Wet品での取り扱いを徹
底してください。

ARC取得品については、
「TMRAD at 24 hour」が熱
源温度よりも低いことを確
認してください。
ARCを取得し、「TMRAD at
24 hour」が熱源温度よりも
低いことを確認してくださ
い。

固体の引火点測定方法も存
在するため、データ取得を
検討ください。(ASTM
D3278-1982: Standard Test
Methods for Flash Point of
Liquids by Setaflash Close-d-
Cup Apparatus参照)
メタノールが存在しない、
あるいは開放作業が無いの
であれば引火点の評価不要
です。

過去の住化での試験(IMO
燃速試験)では、窒素雰囲
気(酸欠雰囲気)下にて反応
伝播性はないことが確認さ
れています。
気(酸欠雰囲気)下にて反応
伝播性はないことが確認さ
れています。

粉砕後の粒径を現状よりも
大きめに調製し、着火感度
を低く(MIEを大きく)できな
いか検討してください。
爆発放散設備の開口面積に
ついて、NFPA68を基に適切
か確認してください。
Reaction mass
STEP-01.
The material starts decomposing at 147.5 °C.
2. Overall Heat of Reation (ΔH) is 143.8 J/g.
3. Temperature for TMRAD 8 hours (Time for maximum rate under adiabatic codition at 8 hou
is approximately 130 °C.
4. Temperature for TMRAD 24 hours (Time for maximum rate under adiabatic codition at 24 h
is approximately 124 °C.
5. Maximum Pressure reached during exothermic decomposition is 28 bar.
6. At 30°C, Residual Pressure is 11 bar.

Reaction mass
STEP-02
1. The material starts decomposing at 166.5 °C.
2. Overall Heat of Reation (ΔH) is 645.7 J/g.
3. Temperature for TMRAD 8 hours (Time for maximum rate under adiabatic codition at 8 hou
is approximately 162 °C.
4. Temperature for TMRAD 24 hours (Time for maximum rate under adiabatic codition at 24 h
is approximately 156 °C.
5. Maximum Pressure reached during exothermic decomposition is 119 bar.
6. At 30°C, Residual Pressure is 21 bar.

Reaction mass
STEP-03
The material starts decomposing at 126.1 °C.
2. Overall Heat of Reation (ΔH) is 346.98 J/g.
3. Temperature for TMRAD 8 hours (Time for maximum rate under adiabatic codition at 8 hou
is approximately 105 °C.
4. Temperature for TMRAD 24 hours (Time for maximum rate under adiabatic codition at 24 h
is approximately 83 °C.
5. Maximum Pressure reached during exothermic decomposition is 47 bar.
6. At 30°C, Residual Pressure is 7 bar.
adiabatic codition at 8 hours)

r adiabatic codition at 24 hours)

adiabatic codition at 8 hours)

r adiabatic codition at 24 hours)

adiabatic codition at 8 hours)

r adiabatic codition at 24 hours)

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