Akzo Nobel Functional 

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Subject Process safety investigation PSI-3 of the preparation of 

PPR-001; 

Author G.B. Boerdijk

Date 2014-07-14

Document number STM 20140152

Project number 4001861

Customer AN FC OP

Project identification:

Project Name OP-Polymer Modification

Participants G.B. Boerdijk

Project Leader M. van der Schuur

Competence Team Leader H.J. Edelijn

Customer order reference -

Our order reference -

Laboratory notebook 4908

Safety testing & Modelling

Copies to M. van der Schuur

R.C.J. Millet

J. Nuysink

H.J. Edelijn

P. Dijkgraaf

B. Fischer

T. den Braber

P.M.M. Hoeijmakers

Safety Report

Drafted by

Name G.B. Boerdijk Date 2014-07-22

Function Safety Engineer Signature

Approved by

Name H.J. Edelijn Date 2014-07-22

Function Manager Safety Laboratory Signature
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 2

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Summary

Heat flow calorimeter experiments were carried out to investigate deviating conditions on 

the standard procedure for the production of PPR-001. This investigation is an extension of 

the investigations reported in PSI-2 (Ref 6.2). The following results were found:

The premix preparation in the HFC is tested with 30 minutes dosing time. The 10 minutes 

shown in the Batch Sequence Diagram (Appendix 7.1) is probably too short for a 

controllable reactor temperature (Treactor = 5°C).

Process carried out with Treactor + 10°C will give controllable heat production the premix 

preparation and in the peroxidation step.

Process carried out with 50% excess Premix will give controllable heat production the 

premix preparation and in the peroxidation step.

Process carried out with 50% excess H2O2-70% in the Premix will give controllable heat 

production the premix preparation and in the peroxidation step. More sulfite is needed for 

complete reduction of non-cyclic peroxide.

Process carried out with 50% excess H2SO4-84% in Premix preparation will give controllable 

heat production the premix preparation and in the peroxidation step. The maximum heat 

production and the total heat are both approx. 20% higher than in the standard recipe.

Process carried out with H2SO4-96% in Premix preparation shows strong deviating heat 

effect in both premix preparation and the peroxidation step. The premix heat production 

decreases to close to zero after dosing, but the peroxidation showed an increasing heat 

production starting half-way dosing. The maximum value is almost twice the standard value. 

After quenching, still some heat production is measured (4 W/kgfrm).
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Contents

1 Introduction 4

2 Sample data 4

3 Experimental 4

3.1 Process until post reaction of peroxidation at T+10°C. 4

3.2 Process carried out with 50% excess Premix. 7

3.3 Process carried out with 50% excess H2O2-70% in Premix preparation. 9

3.4 Process carried out with 50% excess H2SO4-84% in Premix preparation. 12

3.5 Process carried out with H2SO4-96% in Premix preparation. 14

4 Discussion 16

4.1 Process until post reaction of peroxidation at T+10°C. 16

4.1.1 Premix: 16

4.1.2 Peroxidation: 16

4.2 Process carried out with 50% excess Premix. 16

4.2.1 Premix: 16

4.2.2 Peroxidation: 17

4.3 Process carried out with 50% excess H2O2-70 in Premix preparation. 17

4.3.1 Premix: 17

4.3.2 Peroxidation and reduction: 17

4.4 Process carried out with 50% excess H2SO4-84% in Premix preparation. 17

4.4.1 Premix: 17

4.4.2 Peroxidation: 18

4.5 Process carried out with H2SO4-96% in Premix preparation. 18

4.5.1 Premix: 18

4.5.2 Peroxidation: 18

4.6 Overview Premix data 19

4.7 Overview Peroxidation data 19

5 Conclusions 20

6 References 20

7 Appendices 20

7.1 Batch Sequence Diagram PPR-001: T. den Braber: 19-02-2014. 20
Process Safety Investigation PSI-3 of the preparation of 

PPR-001;

STM 20140152

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

1 Introduction

For the development of 

a process safety investigation is needed. In this investigation, the thermal behaviour of 

deviations on the process steps has to be studied. The final process safety study: PSI-3,

according to the safety standards of AN Functional Chemicals (IERDPC-system). This work 

is additional to the tests done in the PSI-2 investigation (Ref 6.2).

2 Sample data

Table 2.1 Used chemicals.

substance quality supplier

3 Experimental

The following tests were done as final part of the process safety study of PPR-001, 

according to Batch Sequence Diagram in Appendix 7.1.

3.1
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; mi

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(financial) information, projections and other information in this report.

Table 3.1 Experimental data for premix preparation at 15°C Exp: BOY14084.

Reactor

Stirrer

Stirring speed

Glass

Glass, pitch blade turbine

880 rpm

Figure 3.1 HFC plot of premix preparation of PPR-001; Deviation: Treactor +10°C

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650

750

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130

150

-5.00 5.00 15.00 25.00 35.00 45.00 55.00 Dosed H2SO4-84 wt%( g) Heat production (W/kg frm; Total heat (KJ/kg frm)

Time (min)

HFC test of Premix preparation for "

prepared at 15°C; Deviation: Treactor + 10°C

T-Reactor

Heat production

Total heat

Dosed H2SO4-84 wt%

BOY14084

Charged:

414 g H2O2-70 wt%

Dosed:

469 g H2SO4-84 wt%

Dosing time: 

30 min 

63.4 W/kg frm

26.9 W/kg frm

78.4 kJ/kg frm

469 g sulfuric acid
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.2 Experimental data for peroxidation at 10°C Exp: BOY14085.

Reactor

Stirrer

Stirring speed

Glass

Glass, pitch blade turbine

880 rpm

Figure 3.2 HFC plot of PPR-001; peroxidation step. Deviation: Tr+10°C

0

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500

0

20

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60

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100

120

140

20 40 60 80 100 120 140 160 180 Total heat (kJ/kg frm); Dosed amount (g) Heat production (W/kg frm); Reactor temperature (°C)

Time (min)

HFC experiment of 

peroxidation at 10 °C; Deviation: T + 10°C

T-reactor

Heat production

Dosed amount

Total heat

file: BOY14085

Reactor : Glass 

Stirrer : Glass

Stirrer speed : 880 rpm

Charged: 

Spirdane D60 : 200.0 g

MEK : 143.0 g

MPK (>90%) : 73.4 g

Dosed premix : 294 g (32.8% H2O2; 44.6% H2SO4; 22.6% H2O)

dosing time : 60 min. frm1 = 710.4 g

220 kJ/kg frm1

q(max)=57.0 W/kg frm1

75 min: 4 W/kg

premix 294 g

peroxidation
Process Safety Investigation PSI-3 of the preparation of 

PPR-001;

STM 20140152

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Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

3.2 Process carried out with 50% excess Premix.

Table 3.3 Experimental data for premix preparation at 5°C Exp: BOY14078.

Figure 3.3 HFC plot of premix preparation of PPR-001; Standard premix preparation.

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750

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110

130

150

0.00 10.00 20.00 30.00 40.00 50.00 60.00 Dosed H2SO4-84 wt%( g) Heat production (W/kg frm; Total heat (KJ/kg frm)

Time (min)

HFC test of Premix preparation for

prepared at 5°C; standard recipe

T-Reactor

Heat production

Total heat

Dosed H2SO4-84 wt%

BOY14078

Charged:

414.0 g H2O2-70 wt%

Dosed:

468.0 g H2SO4-84 wt%

Dosing time:

30 min

67.8 W/kg frm

35.5 W/kg frm

1.9 W/kg frm

90.6 kJ/kg frm
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.4 Experimental data for peroxidation 0°C Exp: BOY14085.

Figure 3.4 HFC plot of PPR-001; peroxidation step. Deviation: 50% Excess premix.

0

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0

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60

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100

120

140

0 20 40 60 80 100 120 140 160 180 Total heat (kJ/kg frm); Dosed amount (g) Heat production (W/kg frm); Reactor temperature (°C)

Time (min)

HFC experiment of 

peroxidation at 0 °C; Deviation: 50% excess premix

T-reactor

Heat production

Dosed amount

Total heat

file: BOY14079

Reactor : Glass 

Stirrer : Glass

Stirrer speed : 880 rpm

Charged: 

Spirdane D60 : 200.0 g

MEK : 143.0 g

MPK (>90%) : 73.4 g

Dosed premix : 441 g (32.8% H2O2; 44.6% H2SO4; 22.6% H2O)

dosing time : 90 min. frm1 = 857.4 g

Quench : 84.1 g water frm2= 941.5 g

161 kJ/kg frm1

q(max)=57.3 W/kg frm1

75 min <2 W/kg

premix 441 g

quench

peroxidation
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

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Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

3.3 Process carried out with 50% excess H2O2-70% in Premix preparation.

Table 3.5 Experimental data for premix preparation at 5°C Exp: BOY14086.

Figure 3.5 HFC plot of premix preparation of PPR-001; Deviation: 50% excess H2O2.

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650

750

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110

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150

60.00 65.00 70.00 75.00 80.00 85.00 90.00 95.00 100.00 105.00 Dosed H2SO4-84 wt%( g) Heat production (W/kg frm; Total heat (KJ/kg frm)

Time (min)

HFC test of Premix preparation for 

prepared at 5°C; Deviation: 50% extra H2O2-70 wt% recipe

T-Reactor

Heat production

Total heat

Dosed H2SO4-84 wt%

BOY14086

Charged:

502.7 g H2O2-70 wt% (= 50% excess)

Dosed:

380.0 g H2SO4-84 wt%

Dosing time: 

30 min 

56.9 W/kg frm

33.3 W/kg frm

82.7 kJ/kg frm
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.6 Experimental data for peroxidation 0°C Exp: BOY14087.

Figure 3.6 HFC plot of PPR-001; peroxidation step. Deviation: 50% excess H2O2

0

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700

800

0

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55 75 95 115 135 155 175 Total heat (kJ/kg frm) Heat production (W/kg frm); Reactor temperature (°C); Dosed amount (g)

Time (min)

HFC experiment of 

peroxidation at 0 °C; Deviation: 50% excess H2O2in Premix

T-reactor

Heat production

Dosed amount

Total heat

q(max)=63.7 W/kg frm1

peroxidation

file: BOY14087

Reactor : Glass 

Stirrer : Glass

Stirrer speed : 880 rpm

Charged: 

Spirdane D60 : 200 g

MEK : 143 g

MPK (>90%) : 73.4 g

Dosed premix : 294.3 g (39.9% H2O2; 36.1% H2SO4; 24.0% H2O)

dosing time : 60 min. frm1 =711.6 g

ΔH = 241 kJ/kg

2.2 W/kg frm
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PPR-001; 

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.6 Experimental data for sulfite reduction Exp: BOY14087.

Figure 3.7 HFC plot of PPR-001; sulfite addition step. Deviation: 50% excess H2O2

It is observed that after these (excessive) additions, still linear peroxide is present. This

implies bad conversion to cyclic peroxide.

-1500

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0

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1000

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240 260 280 300 320 340 360 380 400 420 440 Dosed amounts (g) Heat production(W); Reactor temperature (°C); Dosed amount (g)

Time (min)

HFC experiment of 

sulfite reduction steps at 10°C and, 30°C; 

Deviation: 50% excess H2O2in Premix

T-reactor

Heat production

Buffer additions

Sulfite additions

file: BOY14087

Buffer additions at 10°C and 30°C : 156.1, 151.0 g 

Sulfite additions at 30°C : 125.0, 125.6, 76, 125.5 g 6.25 and 8.33 g/min

After these sulfite amounts, reduction was still not completed

baseline

baseline

84 W

84 W 79 W

69 W

17 W
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

3.4 Process carried out with 50% excess H2SO4-84% in Premix preparation.

Table 3.7 Experimental data for premix preparation at 5°C Exp: BOY14080.

Figure 3.8 HFC plot of premix preparation of PPR-001; Deviation: 50% excess H2SO4.

-50

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650

750

-10

10

30

50

70

90

110

130

150

20.00 30.00 40.00 50.00 60.00 70.00 80.00 Dosed H2SO4-84 wt%( g) Heat production (W/kg frm; Total heat (KJ/kg frm)

Time (min)

HFC test of Premix preparation for "

prepared at 5°C; Deviation: 50% extra H2SO4-84 wt%recipe

T-Reactor

Heat production

Total heat

Dosed H2SO4-84 wt%

BOY14080

Charged:

327.2 g H2O2-70 wt%

Dosed:

554.7 g H2SO4-84 wt% (183.9 g + 370.8 g)

Dosing time: increased

45 min (t_dosing + 50%) = standard dosing rate

55.4 W/kg frm

26.1 W/kg frm

<2 W/kg frm

97.0 kJ/kg frm

370.8 g

183.9 g
Process Safety Investigation PSI-3 of the preparation of 

PPR-001;

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.8 Experimental data for peroxidation at 0°C Exp: BOY14081.

Figure 3.9 HFC plot of PPR-001; peroxidation step. Deviation: 50% excess H2SO4.

0

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400

450

500

-10

10

30

50

70

90

110

130

40 60 80 100 120 140 160 180 200 Total heat (kJ/kg frm); Dosed amount (g) Heat production (W/kg frm); Reactor temperature (°C)

Time (min)

HFC experiment of 

peroxidation at 0 °C; Deviation: 50% excess H2SO4in Premix

T-reactor

Heat production

Dosed amount

Total heat

file: BOY14081

Reactor : Glass 

Stirrer : Glass

Stirrer speed : 880 rpm

Charged: 

Spirdane D60 : 200.0 g

MEK : 143.0 g

MPK (>90%) : 73.4 g

Dosed premix : 294 g (26.0% H2O2; 52.8% H2SO4; 21.2% H2O)

dosing time : 60 min. frm1 =710.4 g

263 kJ/kg frm1

q(max)=69.4 W/kg frm1

75 min 3.8 W/kg

premix 294 g

peroxidation
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

3.5 Process carried out with H2SO4-96% in Premix preparation.

Table 3.9 Experimental data for premix preparation at 5°C Exp: BOY14088.

Figure 3.10 HFC plot of premix preparation of PPR-001; Deviation: H2SO4-96%

0

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400

450

0

20

40

60

80

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120

140

160

180

200

40.00 50.00 60.00 70.00 80.00 90.00 100.00 110.00 120.00 Dosed H2SO4-96 wt%( g) Heat production (W/kg frm); Total heat (KJ/kg frm)

Time (min)

HFC test of Premix preparation for s 

prepared at 5°C; Deviation: H2SO4-96%

T-Reactor

Heat production

Total heat

Dosed H2SO4-84 wt%

BOY14088

Charged:

414 g H2O2-70 wt%

Dosed:

468 g H2SO4-96 wt%

Dosing time: 

30 min 

107 W/kg frm

3 W/kg frm

186 kJ/kg frm

468 g sulfuric acid

23.4 g/min

15.6 g/min

184 W/kg frm

pump control -failure reset:

max. pump rate -> pump stop -> programmed rate
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Table 3.10 Experimental data for peroxidation 0°C Exp: BOY14089.

Figure 3.11 HFC plot of PPR-001; peroxidation step. Deviation: H2SO4-96% in premix.

0

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500

0

20

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140

60 80 100 120 140 160 180 200 220 240 Total heat (kJ/kg frm); Dosed amount (g) Heat production (W/kg frm); Reactor temperature (°C)

Time (min)

HFC experiment of 

peroxidation at 0 °C; Deviation: H2SO4-96% in premix preparation

T-reactor

Heat production

Dosed amount

Total heat

file: BOY14089

Reactor : Glass 

Stirrer : Glass

Stirrer speed : 880 rpm

Charged: 

Spirdane D60 : 200.0 g

MEK : 143.0 g

MPK (>90%) : 73.4 g

Dosed premix : 294 g (32.9% H2O2; 50.9% H2SO4; 16.2% H2O)

384 kJ/kg frm1

q(max)= 109 W/kg frm1

75 min: 12 W/kg

premix 294 g

peroxidation

Quench: 84 g H2O
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

4 Discussion

In this investigation different deviations on the preparation process are tested.

The influence on heat production and runaway potential is studied.

4.1

Standard premix

ration 

data.
Process Safety Investigation PSI-3 of the preparation of 

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(financial) information, projections and other information in this report.

4.2.2
Process Safety Investigation PSI-3 of the preparation of 

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(financial) information, projections and other information in this report.

4.4.2
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(financial) information, projections and other information in this report.

5
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; )

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liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

5 Conclusions

5.1

6 References

6.1 Kamp, H.J.M.; Interim Research Report: Process safety investigation into the initiator D-129 

process in Isopar M (Trigonox 301; D-phase); 

Doc. code: ACRD 970-0632; Deventer July 23, 1997.

6.2 Boerdijk, G.B.; Safety Report: Process Safety Investigation PSI-2 of the preparation of 

PP-R-001; mixed cyclic peroxide of 2-Butanone and 2-Pentanone;

Doc. code: STM 20140017; Deventer, January 28, 2014.

6.3 Boerdijk G.B.; Test program for Process Safety Investigation stage: PSI-3 of peroxide 

process PP-R-001; mixed cyclic peroxide; Doc. code: STM 20140101; 

Deventer, May 12, 2014.

7 Appendices

7.1 Batch Sequence Diagram PPR-001: T. den Braber: 19-02-2014.
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 21

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.

Appendix 7.1

Batch Sequence Diagram PPR-001: T. den Braber: 19-02-2014.
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 22

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 23

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.
Process Safety Investigation PSI-3 of the preparation of 

PPR-001; 

STM 20140152

Although great care has been taken in drawing up the report, no rights can be derived from the contents thereof and Akzo Nobel Functional 24

Chemicals B.V. makes no warranties or representations as to its accuracy or completeness. Nor shall Akzo Nobel Functional Chemicals B.V. be 

liable for any loss or damages, including - without limitation - direct, indirect, special, consequential or incidental damages arising from reliance on 

(financial) information, projections and other information in this report.