Polyol polyether+NCO Isupur PDF

Ref.
Ares(2016)6711556 - 30/11/2016
INSPUR project
Quality control protocols
WP2
D 2.5
Development of a document about the specific control protocols for a reliable

and stable quality of INSPUR bi-components resins, with a focus on the validation
of the features of INSPUR components, considering humidity, OH/-NCO ratio, and
final viscosity. Report (PU).
Issue Date
November 30th 2016 – M9
Type
R – Report
Dissemination Level: PU
Leader
IMA
This project is implemented through the HORIZON 2020 SME Instrument, Phase-2 (GA 711591)
1
Quality control protocols
Table of contents
Quality control protocols ............................................................................................................. 2

Table of contents ........................................................................................................................................... 2
D 2.5, Quality control protocols ................................................................................................... 3
Executive summary........................................................................................................................................ 3
INSPUR Quality control protocols, introduction............................................................................................ 4
Quality assurance for the bi-components PU ............................................................................................... 6
State of art and prior knowledge in PU resins QC ......................................................................................... 7
Flow diagram for PU resins production ......................................................................................................... 8
INSPUR: QC Parameters and variable............................................................................................................ 9
Humidity Control ....................................................................................................................................... 9
Viscosity ....................................................................................................................................................... 11
Density ......................................................................................................................................................... 11
Flow diagram for 2K PU production ............................................................................................................ 12
Current applications status ......................................................................................................................... 13
Raw materials .......................................................................................................................................... 13
Future developments .................................................................................................................................. 14
Achieved results and conclusions ................................................................................................................ 15
Used experimental protocols for the [Acat], (Biso) and pigments QC ........................................................... 17
QC Method 1, determination of the polyester polyols pH ...................................................................... 17
QC Method 2, determination of the polyether polyols pH ..................................................................... 18
QC Method 3, determination of the pigment pastes water content using Karl Fischer titration and ADP
611 evaporator ........................................................................................................................................ 19
QC Method 4, determination of the polyols and glicole water content using the Karl Fisher titration . 20
QC Method 5, INSPUR / bi-component system density determination .................................................. 21
QC Method 6, determining the reticulation of INSPUR made products ................................................. 22
QC Method 7, Brookfield viscosity determination in bi-components systems ....................................... 24
QC Method 8, determination of free isocyanate in urethane pre-polymers .......................................... 25
QC Method 8, kinetic determination of a bi-component system (INSPUR) ............................................ 27
2
D 2.5, Quality control protocols
Executive summary
The utilization of innovative products demands the identification of the main critical issues
that derive by the application of a new technology.
The main objective of this task is to identify all the necessary controls that have to be
performed on both the two INSPUR components, in order to ensure optimal results and
considering the bi-component mixtures production process until their final application.
The quality controls mainly concern the raw materials used for the bi-components
formulation, these are followed by the controls performed on the polyols and isocyanates
formulated components until the final verification of the film reticulation during the
application phase.
After obtaining the polyurethane film, it is then possible to proceed with the final control
phase. This concerns the evaluation of the demanded physical – chemical resistance
features (light, washing, solvents, flexions…) directly on the film; these parameters must
complain with the identified standard for each article application.
3
INSPUR Quality control protocols, introduction
To obtain optimal results using INSPUR products, it is fundamental to ensure the lowest
humidity content for the polyols mixture [Apol]. The presence of water during the two
components mixing phase will indeed determine a reaction among the isocyanate group
of (Biso) component and water thus determining the consequent withdrawal of the
isocyanate group viability from the polyol part [Apol].
Following, the reaction that occurs among the isocyanate group and the hydroxyl group
of the glycols [Apol] component:
R-NCO + R’OH → R-NHCO-OR’
A possible presence of water, subtracts although the viable isocyanate groups from the
reaction thus provoking the release of gas that causes bubbles in the film.
R-NCO + H2O → R-NHCO-OH → R-NH2 + CO2↑
In order to avoid this effect, we have therefore focused our efforts on the evaluation of
the humidity parameters by accurately assessing the used raw materials quality (polyols
and glycols) and by issuing the two components manufacturing process within confined
anhydrous conditions (under a constant N2 flow).
Another parameter, that results fundamental to assess, is the occurrence of a complete

reticulation between the two components; first of all, it is necessary to calculate the ratio
between the two components (NCO/OH=1) according the % of effective reactive group.
During the utilization phase, it is relevant that these amounts being correctly dosed.
A complete film reticulation is instead necessary to ensure the production of a desired

polymer with the demanded chemical-physical features and thus assuring the
reproducibility of the finished product.
4
Therefore, we provided to setup a reticulation control methodology based on FT-IR
spectrophotometry. This test can be performed at the end of the reticulation phase to
evaluate the possible presence of isocyanate groups directly on the film.
The absence of peak indicates a complete reticulation.
5
Quality assurance for the bi-components PU
Critical issues during the production phase
The main problem that arises during the production and manipulation of the two INSPUR
components is the avoidance of any contact from the atmospheric humidity.
After the verification of the water content in the raw materials, that must be below the
0.05%, it is necessary to ensure a production system under controlled conditions (under a
constant N2 flow). This is necessary to avoid the absorption of further external humidity.
At the end of the production process and after the final humidity control, the product
should to be packed into “two 2 caps drums”, to avoid any further absorption of external
humidity.
6
State of art and prior knowledge in PU resins QC
The quality control for the solvent based PU resins production requires the initial inspection
of raw materials input, the process analysis and the control of finished products.
In details the following controls are performed on the raw materials:
- Polyol resins (humidity and pH)

- Glycols and extenders (humidity)
- Solvents (Humidity and GC-MS to evaluate purity)
Process control:
During the production phase, and before the extension phase, the isocyanate group
inside the prepolymer is analysed while the control of reached viscosity is performed
before the closing of the reaction.
The reaction closing phase is further monitored through the control of residual -NCO peak
with FT-IR spectrophotometer.
On the finished product, it will be then evaluated:
- The aspect
- Viscosity
- Hazen colour
- Dry residue
A resin sample will be also left for 48 hours at 60°C to simulate an accelerated ageing and
in order to verify its stability. At the end of the ageing in stove, the values of viscosity and
hazens are reported; both of values have not to move above the +/- 10% compared to
the sample value.
Following a flow diagram of QC system.
7
Flow diagram for PU resins production
Diagram 1 Flow diagram of PU resins production.
8
INSPUR: QC Parameters and variable
Humidity Control
A Component:
The control phase for both raw materials and formulated polyols mixtures is aimed at
verifying that the overall water amount does not exceed the threshold of 0.05%.
The respect of this specification, that is required by the used raw materials (polyols and
glycols), and the production phase within a closed system, permits although to ensure the
respect of this parameter in the finished product (0.05%).
Pigmented pastes:
For what concerns the pigments dispersed in a polyol nature vehicle, it is not possible to
respect the limit established for the [Apol] component due the humidity already present
into the pigment powder.
Despite the precautions, to minimize the humidity absorption during the pigment
dispersions phases, the final pigmented paste shows however a humidity value higher
than the awaited one.
Since this value can affect both reaction kinetics and the complete reticulation of the 2
INSPUR components, different tests have been issued to establish the percentage (%) of
the maximum acceptable humidity. The humidity threshold, that is necessary to avoid
issues on products during the application phase, is the 0.3%.
The addiction of coloured paste to the formulation is usually around 15% (maximum 30%)
and it does not significantly affect the overall humidity amount [Apol] + pigment + (BIso).
To measure the pigmentary paste humidity, it has been required the improvement of the
current system. The polyols and glycols humidity determination must be performed by
using the Karl Fischer coulometric test and by dosing directly into the titrating jar the
sample to test.
9
This is not possible for the pigments due to the difficulty of solubilizing them in a Karl Fisher
jar, and due to the possible interference of substances present in the pigments solutions
(E.g. Oxides) with the Karl Fisher experimental protocol; these can indeed compromise the
analysis results. On purpose, it has been necessary to acquire an evaporator that allow to
dry the samples by heating.
The humidity is then conveyed directly to the colorimetric reaction jar via an anhydrous
vehicle gas to permit the quantification.
It has been indeed developed a new methodology that permits to identify the best
options of temperature and humidity stripping for the different pigment pastes.
B Component:
Since the -NCO group reacts with humidity it is fundamental that the isocyanate mixture is
produced within a closed system and under strictly controlled conditions.
At the end of the reaction, an experimental measure of the free -NCO will be issued to
understand the exact amount of reactive group within the sample; this have not to move
from the 3%(+/1) awaited value.
10
Viscosity
A, B components
During the tuning of the formulations, the viscosity is a parameter that should be
accounted since the both 2 components require a low viscosity to be correctly dosed into
the production plant. The viscosity must then stay below the 6.000 cps at 25°C.
During the control phase, the value is measured using a Brookfield viscometer.
Density
A, B components
The density value is measured with an aerometer to provide an information feedback to

the user. This value will support the user in setting up the volumetric dosing of the two
INSPUR components.
Pigmentary pastes
For the coloured pastes, due to their high viscosity, the density is directly measured by
weighting a known material volume.
Since viscosity is a temperature depending parameter, a density curve has been derived
to support the user during the manufacturing phase. Temperatures above 30°C are
however not taken in account. This because the temperature greater than 30°C can
affect the overall reaction kinetics and the reaction speed will be consequently
excessively high (the optimal operative condition is 25°C).
11
Flow diagram for 2K PU production
Diagram 2 Flow diagram of 2K PU resins production.
12
Current applications status
The Quality Control system provides the analysis of the raw materials, of [Apol] and (Biso)
components and the verification of the correct reaction between the two components.
Raw materials
Polyols resins
polyether, polyester and polycarbonate
- % of humidity (Karl Fisher coulometric method)

- PH
- Glycols
- % of humidity
A Component [Apol]
- % of humidity
- Viscosity
- Density
B Component (Biso)
- Analysis of free -NCO

- Viscosity
- Density
- [Apol] + (Biso) mixture
To evaluate the effective reticulation, it will be performed a laboratory testing to verify the
correct catalysts dosing, the reticulation will be tested by checking on the reticulated film
and the possible presence of free -NCO groups through the FT-IR spectrophotometer.
13
Future developments
It has been planned by IMA to implement the polyol control phase by experimentally
measuring the amount of free -OH on the sample.
The polyols resins are already provided with a related certificate of analysis that calculates
the ratio among the two components, in the future it is however planned to issue an
additional laboratory measurement as a further verification mean.
At the moment, 2 different methodologies are available, one for the polyols polyether and
the other one for polyol polyesters.
For what concerns the experimental measure of polyols [Apol], and in case of a mixed
nature (polyester / polyether) mixture, at the state of art it is not yet possible to determine
the OH value of the mixture since the available methodologies do not consider the
presence of polyols of different natures.
In this case, a theoretical calculation should be performed on the production recipe.
14
Achieved results and conclusions
a) The controls provided during the different tuning phases of the two components,
and during the manufacturing of 2 bi-component resins, permitted to achieve the
planned project objectives concerning the development of industrial QC protocols.
In detail, the threshold limit of (<0.05%), as maximum amount of water content, has
been reached thank to the use of selected raw materials with a high-quality
standard and by pursuing a correct manipulation practice during their utilization.
Further progresses can be however achieved for what concerns the water content
within the coloured pastes. The use of pigments with a low humidity content will be
investigated and the pigmental dispersion conditions will be further improved.
In this way, it can be possible to lower the threshold for the maximum amount of
humidity that is currently established as the 0.3%.
b) During the tuning of both [Apol] and (Biso) components, the viscosity had to be
further accounted; this results fundamental for a good industrial application of the
product.
The raw materials have been indeed chosen also considering this parameter, and
they must not to exceed the amount of 6.000 cps at 25°C. This value has been
established as the maximum threshold for an optimal plant operability during the
production phase using INSPUR.
This has however further limited the possibility to formulate few products which the
final features were of optimal quality in terms of physical-chemical performances,
however, due to a viscosity largely higher than 6.000 cps, this implies a very
complex industrial handling.
Therefore, the formulations now respect this parameter.
15
c) The -NCO/-OH ratio between the two components must be ensured by correctly
mixing the reactive groups of the two components and by providing a correct
dosing during the mixing phase.
Furthermore, in order to ensure the complete reaction between the 2 components,
it is necessary that the quantity of catalyst is present in sufficient amount.
Therefore, during the tuning of the two components, many tests have been
performed to establish the optimal amount of the catalysts, further considering that
the reticulation should be completely reached and that the reaction kinetics have
to be not too fast in order to maintain the mixture pot-life without reducing it.
The amount of dosed catalyst must be correctly dosed to obtain the optimal
compromise among the mixture reticulation and half-life.
Concluding, we can consider that during this months a reliable QC control system for the
manufacturing process of 2 bi-components resins has been tuned also providing the
control of the correct reaction after the mixing phase.
The INSPUR manufacturing QC system will be further improved considering as priority the
analysis of -OH group in polyol polyether and polyester/polycarbonates.
Considering this, it will be tried to setup a methodology that will permit to measure these
parameters in polyols mixtures of different chemical nature.
16
Used experimental protocols for the [Acat], (Biso) and pigments QC
QC Method 1, determination of the polyester polyols pH
DETERMINATION OF THE POLYESTER POLYOLS pH
PURPOSE To evaluate the pH of the polyester polyols
EQUIPMENT - pH meter (to be calibrated daily with normalized buffer solutions)

- Electromagnetic stirrer
- Beaker 50 [ml]
- Beaker 250 [ml]
- Normal laboratory equipment.
REAGENTS - Bidistilled water

- Isopropyl alcohol R.P.
- Acetone R.P.
- NaOH 0.001 [N]
- HCl 0.001 [N]
PROCEDURE 1. Carefully wash the electrodes of the pH meter with distilled water
and dry with soft absorbent paper;
2. Pour into a 250 [ml] clean and dry beaker:
50 [ml] of isopropyl alcohol
50 [ml] of acetone
60 [ml] of bidistilled water
3. Operate the agitation of the pHmeter, heat up to 40 [° C] and
possibly correct the pH with NaOH or HCl 0.001 [N] until you
reach pH 7.0 ± 0.1;
4. Add 27 [g] of polyol, previously melted, to the mixture under
stirring (if necessary heat on a electromagnetic hotplate);
5. The reading of the pH must be performed when the variation is
less than 0.05 pH units / min.
NOTE: this procedure must be repeated twice; if the difference

among the various determinations is greater than 0.2 pH unit,
perform another series of determinations until a correlation of the
values within these limits is reached. Immediately after the test, the
electrodes must be washed thoroughly.
EXPRESSION OF THE Calculate the arithmetic mean of the two values obtained and round
RESULT to the first decimal figure.
TEST REPORT The test report must contain:

- all the elements necessary for the complete identification of the
sample
- The pH value, expressed in pH units
- The reference to the test method below
17
QC Method 2, determination of the polyether polyols pH
DETERMINATION OF THE POLYETHER POLYOLS pH
PURPOSE To evaluate the pH of polyether polyols
EQUIPMENT - pH meter (to be calibrated daily with normalized buffer solutions)

- Beaker 100 [ml]
- Syringe 10 [ml]
- Normal laboratory equipment.
REAGENTS - Bi-distilled water

- Isopropyl alcohol RP (to be mixed together in the ratio 10:6 v/v)
- NaOH 0.001 [N]
- HCl 0.001 [N]
PROCEDURE 1. Wash the electrodes of the pHmeter with distilled water and dry
with soft absorbent paper;
2. Calibrate the electrode with buffer solutions at pH 4.00 and pH
7.02;
3. Pour into a dry and clean beaker of 100 [ml]:
50 ml] mixture of isopropyl alcohol / distilled water (10: 6 v /v)
4. Immerse the electrode, operate the agitation of the pHmeter, and
correct if necessary the pH with NaOH or HCl 0.001 [N] to reach
pH 7.0 ± 0.05. Do not make back-adjustments.
5. Add 10 [g] of polyol to the mixture under constant agitation (if
necessary heat on an electromagnetic hotplate);
6. The reading of the pH must be performed when the variation is
less than 0.05 pH units / min.
NOTE: This procedure must be repeated twice; if the difference

between the various determinations is greater than 0.2 pH unit,
perform another series of determinations up to reach a correlation of
the values within these limits. Immediately after the test, the
electrodes must be washed thoroughly.
EXPRESSION OF THE Calculate the arithmetic mean of the two values obtained and round
RESULT at the second decimal figure.

- All the elements necessary for the complete identification of the
sample
- The pH value, expressed in pH units
- The reference to the test method below.
18
QC Method 3, determination of the pigment pastes water content using Karl Fischer
titration and ADP 611 evaporator
DETERMINATION OF THE PIGMENT PASTES WATER CONTENT USING KARL FISCHER

TITRATION and ADP 611 EVAPORATOR
PURPOSE To determine the water content of the pigment pastes used in the bi-
components system.
EQUIPMENT - ADP 611 evaporator

- KEM coulometer
- 5 [ml] syringe
- Analytical balance, 0,1 [mg] precision
- Aluminium foil
- Normal laboratory equipment
REAGENTS - Hydranal Coulomat Oil

- Hydranal Coulomat GC
PROCEDURE 1. Prepare the titration cell by adding the Hydranal Coulomat Oil
into the cathodic compartment and 1 vial of Hydranal Coulomat
GC into the anodic compartment
2. Turn on the ADP 611 evaporator and start the pre-titration
3. During the pre-titration position on the sample loading cell a
correctly cut aluminium foil
4. When the evaporator is in BACK PURGE mode, load 1 [gr] of
sample on the cell
5. Start the measurement
EXPRESSION OF THE The percentage value is provided directly by the automatic titrator.
RESULT

sample
- The water contents, expressed in % percentage
19
QC Method 4, determination of the polyols and glicole water content using the Karl
Fisher titration
DETERMINATION OF THE POLYOLS AND GLICOLE WATER CONTENT USING THE

KARL FISCHER TITRATION
PURPOSE To determine the water content inside the polyols part of a bi-
component system
EQUIPMENT - KEM coulometer

- 5 [ml] syringe
- Analytical balance, 0,1 [mg] precision
REAGENTS - Hydranal Coulomat Oil

- Hydranal Coulomat GC
PROCEDURE 1. Prepare the titration cell by adding the Hydranal Coulomat Oil
into the cathodic compartment and 1 vial of Hydranal Coulomat
GC into the anodic compartment
2. Condition the syringe
3. Weight about 1 [ml] of product with the syringe
4. Wait 1 minute
5. Introduce the product into the cathodic compartment of titration
the cell
6. Follow the instructions provided by the automatic titrator
EXPRESSION OF THE The percentage value is provided directly by the automatic titrator.
RESULT

sample
- The water contents, expressed in % percentage
20
QC Method 5, INSPUR / bi-component system density determination
INSPUR / BI COMPONENT SYSTEMS DENSITY DETERMINATION
PURPOSE To determine density of the isocyanates and polyol parts
EQUIPMENT - Constant weight aerometer

- 1000 [ml] cylinder provided with a conditioning chamber
REAGENTS None
PROCEDURE 1. Pour about 300 [ml] of product inside the cylinder

2. Connect the cylinder to a thermostatically-controlled water bath
3. Set the thermostatically-controlled water bath to the density
measurement temperature
4. Immerge the densitometer and check the sample temperature
from the cylinder
5. Read the density value on the graduated scale
EXPRESSION OF THE Calculate the arithmetic average of the two obtained values and
RESULT round the obtained numbers to the third decimal

sample
- Density value, expressed as Kg/l
21
QC Method 6, determining the reticulation of INSPUR made products
DETERMINING THE RETICULATION OF INSPUR MADE PRODUCTS
PURPOSE To determine the reticulation of INSPUR bi-components systems
EQUIPMENT - Film reticulation oven

- Spreading frame
- Release paper
- Spatula / knife
- 4 blades impeller and stirrer
- Graduated cylinder for bi-component weight and mixing
- FT-IR spectrophotometer
REAGENTS - Polyols and isocyanates component of the INSPUR resin
PROCEDURE 1. Weight in a small jar the amount of polyol part, determined by the
using ratio. The overall amount of the two compounds must be at
least 50 [gr]
2. Weight in the same jar of 1. the isocyanate part, that is
determined by the using ratio
3. Shake the bicomponent using a stirrer at 350 rpm/min for 50 sec
4. Spread 0.1 [mm] of mixture using the spreading frame
5. Reticulate the bi-components using the oven according the
specific temperatures and times of the formulation
6. Measure the initial transmittance data at 2260cm-1 using the FT-
IR spectrophotometer in different sample zones. Proceed as
follow:
 Clean the ATR ground plan
 Issue the background reading
 Position the film on the ATR ground plan and acquire the
spectrum
 Verify that the baseline falls at 100% of transmittance
 Evaluate the possible presence of an absorbance peak at
2260-2270 cm-1, typic of -NCO functional group: if present
read the % transmittance value
 If the value results ≥ 98.5%, we can suppose a correct
reticulation
 If the value results < 98.5%, the film is not completely
reticulated and is not compliant
 In case of a good reticulation, repeat the same measure in
the following days to monitor the residual peak decreasing
time
 It is advised the acquisition of IR spectrum from different
zones of the sample.
EXPRESSION OF THE It is the transmittance percentage value red by the FT-IT instrument
RESULT and the -NCO peak annihilation time
22
sample
- The initial transmittance percentage measured at 2260 cm-1
23
QC Method 7, Brookfield viscosity determination in bi-components systems
BROOKFIELD VISCOSITY DETERMINATION IN BI-COMPONENTS SYTEMS
PURPOSE To determine density of a viscose fluid, evaluating its resistance

against the rotation of a predefined impeller.
EQUIPMENT - Brookfield Viscometer mod. RV/DV II PLUS, 18 speeds, 6

spindles
- Thermostatically-controlled water bath at 25±1[°C]
- 300 [ml] sealed glass jar
- Thermometer
REAGENTS None
PROCEDURE 1. Pour into the 300 [ml] jar about 200 [g] of the sample to examine
2. Close the jar and submerge it into the thermostatically-controlled
water bath for the amount of time necessary to reach the test
temperature (25°C)
3. Put the instrument on the ground
4. Immerse the spindle in the sample to examine and perform the
test at the desired rotation speed
5. The test ends when the instrument output is stable
EXPRESSION OF THE It is the instrumental value and is expressed as mPa·s

RESULT

sample
- Apparent viscosity in mPa·s
24
QC Method 8, determination of free isocyanate in urethane pre-polymers
DETERMINATION OF FREE ISOCYANATE IN URETANTE PRE-POLYMERS
PURPOSE To determine the contents of free-isocyanates in pre-polymer or in

isocyanates monomers throughout the HCl [1N] retro-titration
EQUIPMENT - Automatic titrator Crison Compact V

- 250 [ml] Schott Flasks
- Electromagnetic stirrer anchors
- Analytical balance with 0.1 [mg] of precision
REAGENTS - HCl [1N]

- Toluene, ACS
- Isopropyl alcohol, ACS
- N-Butylbutan-1-amine [2N] in Toluene, ACS
- Bromocresol green marker
- Tris(hydroxymethyl)aminomethane ACS (TRIS), volumetric
standard
PROCEDURE 1. Prepare 3 X 250 [ml] Schott flasks

2. Pour 40 [ml] of toluene into each of the 3 flasks and put a
magnetic anchor for each
3. Weight for each flask the prepolymer sample according this
formula:
Sample to weight [g] = 80 / (% of theoretical free NCO)
4. Shake flask with the magnetic stirrer until the complete sample
solubilisation
5. Add 25 [ml] of N-Butylbutan-1-amine and wait 15 minutes
6. Add 50 [ml] of Isopropyl alcohol
7. Add 0.8 [ml] of Bromocresol green
8. Titrate samples with HCl [1N] until the equivalence point
9. Issue 3 blank tests using the same procedure but without
prepolymer sample
EXPRESSION OF THE Free isocyanate is expressed as percentage of the following formula:

RESULT
(V  Vc ) N  F  42,02
%NCO  b 100
M  1000
Vb = HCl volume [ml], used for blank test

Vc = HCl volume [ml], used for sample test
N = HCl normality [e1/l]
42.02 = -NCO group equivalent weight
M = sample mass [g] of the sample
25
(V  Vc ) N  42,02
% NCO  b  200
M  1000

sample
- Free isocyanate, expressed as percentage
26
QC Method 8, kinetic determination of a bi-component system (INSPUR)
KINETIC DETERMINATION OF A BI-COMPONENT SYSTEM (INSPUR)
PURPOSE To determine the peculiar kinetics of a bi-component INSPUR

system, or the system viscosity behaviour (Vx) in function of time (t),
and temperature (T) after the two components mixing.
EQUIPMENT - Brookfield Viscometer mod. RV/DV II PLUS, 18 speeds, 6

spindles
- Thermostatically-controlled water bath at 25±1[°C]
- 300 [ml] sealed glass jar
- Thermocouple
- 4 blades impeller and stirrer
REAGENTS - Polyols and isocyanates component of the INSPUR resin
PROCEDURE 1. Heat the two components in a thermostatically-controlled bath at

25 [°C] (or starting temperature)
2. Weight in a glass jar the amount of polyols, determined by the
utilization ratio, ensuring that the total amount considering the
polyols and isocyanates parts is at least 200 [gr]
3. Weight in the glass jar containing the polyol part the isocyanates
components using 60 [ml] syringes
4. Shaken the polyol part at 350 rpm/min for 10 seconds, max
5. Start the chronometer and isocyanate part to shaking jar
6. Shaken the two components for a maximum of 45 seconds
7. Measure the viscosity (Spindle 6, speed 5) and the temperature in
function of time, report the obtained value on the proper template
8. Arrived at 100,000 [cPs] of viscosity we can consider the test
finished; quickly remove the spindle and thermocouple from
measuring jar
EXPRESSION OF THE They are viscosity values (expressed as [cPs]) measured by the
RESULT viscometer and temperature (expressed as [°C]) measured by
thermocouple.

sample
- Viscosity curve in function of time
27

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Ref.

Development of a document about the specific control protocols for a reliable

November 30th 2016 – M9

Quality control protocols ............................................................................................................. 2

R-NCO + R’OH → R-NHCO-OR’

R-NCO + H2O → R-NHCO-OH → R-NH2 + CO2↑

Another parameter, that results fundamental to assess, is the occurrence of a complete

A complete film reticulation is instead necessary to ensure the production of a desired

The absence of peak indicates a complete reticulation.

Critical issues during the production phase

In details the following controls are performed on the raw materials:

- Polyol resins (humidity and pH)

On the finished product, it will be then evaluated:

Following a flow diagram of QC system.

Diagram 1 Flow diagram of PU resins production.

The density value is measured with an aerometer to provide an information feedback to

Diagram 2 Flow diagram of 2K PU resins production.

- % of humidity (Karl Fisher coulometric method)

- Analysis of free -NCO

Therefore, the formulations now respect this parameter.

QC Method 1, determination of the polyester polyols pH

DETERMINATION OF THE POLYESTER POLYOLS pH

PURPOSE To evaluate the pH of the polyester polyols

EQUIPMENT - pH meter (to be calibrated daily with normalized buffer solutions)

REAGENTS - Bidistilled water

NOTE: this procedure must be repeated twice; if the difference

TEST REPORT The test report must contain:

DETERMINATION OF THE POLYETHER POLYOLS pH

PURPOSE To evaluate the pH of polyether polyols

EQUIPMENT - pH meter (to be calibrated daily with normalized buffer solutions)

REAGENTS - Bi-distilled water

NOTE: This procedure must be repeated twice; if the difference

TEST REPORT The test report must contain:

DETERMINATION OF THE PIGMENT PASTES WATER CONTENT USING KARL FISCHER

EQUIPMENT - ADP 611 evaporator

REAGENTS - Hydranal Coulomat Oil

TEST REPORT The test report must contain:

DETERMINATION OF THE POLYOLS AND GLICOLE WATER CONTENT USING THE

EQUIPMENT - KEM coulometer

REAGENTS - Hydranal Coulomat Oil

TEST REPORT The test report must contain:

INSPUR / BI COMPONENT SYSTEMS DENSITY DETERMINATION

PURPOSE To determine density of the isocyanates and polyol parts

EQUIPMENT - Constant weight aerometer

PROCEDURE 1. Pour about 300 [ml] of product inside the cylinder

TEST REPORT The test report must contain:

DETERMINING THE RETICULATION OF INSPUR MADE PRODUCTS

PURPOSE To determine the reticulation of INSPUR bi-components systems

EQUIPMENT - Film reticulation oven

REAGENTS - Polyols and isocyanates component of the INSPUR resin

BROOKFIELD VISCOSITY DETERMINATION IN BI-COMPONENTS SYTEMS

PURPOSE To determine density of a viscose fluid, evaluating its resistance

EQUIPMENT - Brookfield Viscometer mod. RV/DV II PLUS, 18 speeds, 6

EXPRESSION OF THE It is the instrumental value and is expressed as mPa·s

TEST REPORT The test report must contain:

DETERMINATION OF FREE ISOCYANATE IN URETANTE PRE-POLYMERS

PURPOSE To determine the contents of free-isocyanates in pre-polymer or in

EQUIPMENT - Automatic titrator Crison Compact V

REAGENTS - HCl [1N]

PROCEDURE 1. Prepare 3 X 250 [ml] Schott flasks

Sample to weight [g] = 80 / (% of theoretical free NCO)

EXPRESSION OF THE Free isocyanate is expressed as percentage of the following formula:

Vb = HCl volume [ml], used for blank test