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BEFORE SYNTHESIS 1:3 1:4 1:5

Mass of flask, g

Mass of boiling chips, g

1
Mass of PET, g

2
Mass of sodium acetate, g
3
Volume of 3-aminopropanol, mL 11.9 15.9 19.9

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + solids + boiling chips, g
Mass of BHPTA solids, g 0 0 0
Theoretical Yield, g
Percent Yield, %
1:3
PET sample clear, colorless solids
clear, colorless solids in clear
+ 3-amino-1-propanol
colorless solution

+ 0.5% w/w NaCH3COO clear, colorless solids in clear


colorless solution
clear, colorless solids in clear
Reflux at 0 hr
colorless solution
0.5 hr
1 hr
2 hrs
3 hrs
4 hrs
Product at Room T
+ cold dH2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHPTA recrystallization
Drying @ 80C
FINAL BHPTA
1:4 1:5
clear, colorless solids clear, colorless solids
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
BEFORE SYNTHESIS 1:3 1:4
Mass of flask, g 149.1865 167.4187

Mass of boiling chips, g 1.264 0.3693

1
Mass of PET, g 10.0257 10.0335

2
Mass of sodium acetate, g 0.0815 0.0815
3
Volume of 3-aminopropanol, mL 11.9 15.9

AFTER SYNTHESIS 1:3 1:4


Mass of flask + solids + boiling chips, g 172.8243 200.1928
Mass of BHPTA solids, g 22.3738 32.4048
Theoretical Yield, g

Percent Yield, %
01-March 2020
1:5 1:3
159.4859 PET sample clear, colorless solids
clear, colorless solids in clear
1.3346 + 3-amino-1-propanol
colorless solution

+ 0.5% w/w NaCH3COO clear, colorless solids in clear


10.0257
colorless solution
clear, colorless solids in clear
0.0966 Reflux at 0 hr
colorless solution
19.9 0.5 hr clear liquid with yellow tint
1 hr clear liquid with yellow tint
1:5 2 hrs clear liquid with yellow tint
191.5437 3 hrs clear liquid with yellow tint
30.7232 4 hrs clear liquid with yellow tint
Product at Room T white waxy solids
waxy solids undissolved in cold
+ cold dH2O
H2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHPTA recrystallization
Drying @ 80C
FINAL BHPTA
01-March 2020 01-March 2020
1:4 1:5
clear, colorless solids clear, colorless solids
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear liquid with yellow tint clear liquid with yellow tint
clear liquid with yellow tint clear liquid with yellow tint
clear liquid with yellow tint clear liquid with yellow tint
clear liquid with yellow tint clear liquid with yellow-orange tint
clear liquid with yellow tint clear liquid with yellow-orange tint
white waxy solids white waxy solids
waxy solids undissolved in cold
waxy solids undissolved in cold H 2O
H2O
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g

Mass of boiling chips, g

1
Mass of PET, g

2
Mass of sodium acetate, g

3
Volume of 3-aminopropanol, mL 11.90 15.90 19.90

AFTER SYNTHESIS 1:3 1:4 1:5

Mass of flask + solids + boiling chips, g 132.0172 131.9072 141.5602

Mass of BHPTA solids, g 132.0172 131.9072 141.5602

Theoretical Yield, g

Percent Yield, %
28-Feb-20
1:3
PET sample clear, colorless solids
clear, colorless solids in clear
+ 3-amino-1-propanol
colorless solution

+ 0.5% w/w NaCH3COO clear, colorless solids in clear


colorless solution
clear, colorless solids in clear
Reflux at 0 hr
colorless solution

clear liquid with yellowish tint


0.5 hr
+ some undissolved PET

1 hr clear liquid with yellowish tint

2 hrs clear liquid with yellowish tint

3 hrs clear liquid with yellowish tint

clear liquid with yellow-orange


4 hrs
tint
Product at Room T white waxy solids
waxy solids undissolved in cold
+ cold dH2O
H2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHPTA recrystallization
Drying @ 80C
FINAL BHPTA
28-Feb-20 28-Feb-20
1:4 1:5
clear, colorless solids clear, colorless solids
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution

clear liquid with yellowish tint +


clear liquid with yellowish tint
some undissolved PET

clear liquid with yellowish tint + clear liquid with yellowish tint
some undissolved PET

clear liquid with yellowish tint clear liquid with yellowish tint

clear liquid with yellowish tint clear liquid with yellowish tint

clear liquid with yellowish tint clear liquid with yellowish tint

white waxy solids white waxy solids


waxy solids undissolved in cold
waxy solids undissolved in cold H 2O
H2O
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g
Mass of boiling chips, g
1
Mass of PET, g
2
Mass of Zn(CH3COO)2•2H2O, g
3
Volume of 3-aminopropanol, mL 5.5 7.3 9.2

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + BHETA + boiling chips, g
Mass of BHETA solids, g
Theoretical Yield, g
Percent Yield, %
1:3
PET sample
+ PEG (400)
+ 0.5% w/w
Zn(CH3COO)2•2H2O

Reflux at 0 hr
0.5 hr
1 hr
2 hrs
3 hrs
4 hrs
Product at Room T
+ cold dH2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHETA recrystallization
Drying @ 80C
FINAL BHETA
1:4 1:5
BEFORE SYNTHESIS 1:3 1:4
Mass of flask, g 150.8229 147.6686

Mass of boiling chips, g 0.5046 0.4339

1
Mass of PET, g 1.0630 1.0084

2
Mass of Zn(CH3COO)2•2H2O, g 0.0856 0.0780

3
Volume of 3-aminopropanol, mL 5.5 7.3

AFTER SYNTHESIS 1:3 1:4


Mass of flask + BHETA + boiling chips, g 158.0896 159.3361
Mass of BHETA solids, g 6.76 11.23
Theoretical Yield, g
Percent Yield, %
1:5
145.6180 PET sample

0.7190 + PEG (400)

1.0084 + 0.5% w/w Zn(CH3COO)2•2H2O

0.0780 Reflux at 0 hr

9.2 0.5 hr

1 hr

1:5 2 hrs
158.412 3 hrs
12.08 4 hrs
Product at Room T
+ cold dH2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHETA recrystallization
Drying @ 80C
FINAL BHETA
1:3
clear, colorless solids
clear, colorless solids in clear colorless
solution
clear, colorless solids in clear colorless
solution
clear, colorless solids in clear colorless
solution

brown solution

caramelized / coffee brown solution

caramelized / coffee brown solution


caramelized / coffee brown solution
caramelized / coffee brown solution
1:4
clear, colorless solids

clear, colorless solids in clear colorless solution

clear, colorless solids in clear colorless solution

clear, colorless solids in clear colorless solution

cloudy solution with yellow tint; with some PET undissolved

cloudy solution with yellow tint; with some PET undissolved

cloudy yellow with some PET undissolved


cloudy yellow with some PET undissolved
cloudy yellow with some PET undissolved
01-March 2020
1:5
clear, colorless solids
clear, colorless solids in clear colorless
solution
clear, colorless solids in clear colorless
solution
clear, colorless solids in clear colorless
solution

cloudy orange solution

orange solution

orange solution
orange solution
orange solution
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g

Mass of boiling chips, g

1
Mass of PET, g

2
Mass of Zn(CH3COO)2•2H2O, g

3
Volume of 3-aminopropanol, mL 5.5 7.3 9.2

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + BHETA + boiling chips, g 119.2062 119.385 119.3397
Mass of BHETA solids, g 119.21 119.39 119.34
Theoretical Yield, g
Percent Yield, %
1:3
PET sample clear, colorless solids
clear, colorless solids in clear
+ PEG (400)
colorless solution
+ 0.5% w/w clear, colorless solids in clear
Zn(CH3COO)2•2H2O colorless solution
clear, colorless solids in clear
Reflux at 0 hr
colorless solution

0.5 hr

1 hr

2 hrs
3 hrs
4 hrs
Product at Room T
+ cold dH2O

Filtrate
Precipitate

Precipitate
+ dH2O for dissolution
Boiling for 30 minutes
Concentration
Chilling (ppt)

BHETA recrystallization
Drying @ 80C
FINAL BHETA
1:4 1:5
clear, colorless solids clear, colorless solids
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
clear, colorless solids in clear clear, colorless solids in clear colorless
colorless solution solution
cloudy white liquid with some
undissolved PET
cloudy yellow liquid with some
undissolved PET
BEFORE SYNTHESIS 1:3 1:3 R1 1:3 R3
Mass of container, g 12.4161 12.4011 12.3957
Mass of flask, g 232.1958 227.1354 222.7277
Mass of boiling chips, g 0.2758 0.5449 1.5261
3
Volume of caprolactone, mL 8.3 8.3 8.3

AFTER SYNTHESIS 1:3 1:3 R1 1:3 R3


Theoretical Yield, g #REF! #REF! #REF!
Percent Yield, %
1:4 R1 1:4 R2 1:5 R1 1:5 R2
- - - -
220.0565 229.9555 227.8578 232.2007
0.2352 0.2965 0.8069 0.2203
8.3 8.3 8.3 8.3

1:4 R1 1:4 R2 1:5 R1 1:5 R2


#REF! #REF! #REF! #REF!
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g
Mass of boiling chips, g
1
Mass of polyol, g
2
Volume of DBTDL, mL
3
Volume of caprolactone, mL

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + polyol + boiling chips, g
Mass of polyol solids, g
Theoretical Yield, g
Percent Yield, %
1:3
BHPTA
+ DBTDL
+ caprolactone
Reflux at 0 hr
0.5 hr
1 hr
2 hrs
3 hrs
4 hrs
Product at Room T
1:4 1:5
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g
Mass of boiling chips, g
1
Mass of polyol, g
2
Volume of DBTDL, mL
3
Volume of caprolactone, mL

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + polyol + boiling chips, g
Mass of polyol solids, g
Theoretical Yield, g
Percent Yield, %
1:3
BHPTA
+ DBTDL
+ caprolactone
Reflux at 0 hr
0.5 hr
1 hr
2 hrs
3 hrs
4 hrs
Product at Room T
1:4 1:5
BEFORE SYNTHESIS 1:3 1:4 1:5
Mass of flask, g
Mass of boiling chips, g
1
Mass of polyol, g
2
Volume of DBTDL, mL
3
Volume of caprolactone, mL

AFTER SYNTHESIS 1:3 1:4 1:5


Mass of flask + polyol + boiling chips, g
Mass of polyol solids, g
Theoretical Yield, g
Percent Yield, %
1:3
BHPTA
+ DBTDL
+ caprolactone
Reflux at 0 hr
0.5 hr
1 hr
2 hrs
3 hrs
4 hrs
Product at Room T
1:4 1:5

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