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Copyright ©, Green INSTRUCT 2016 - THIS DOCUMENT IS UNCONTROLLED WHEN PRINTED

Project Title:

“Green Integrated Structural Elements for Retrofitting and New Construction of

Buildings”

Deliverable No 7.1

Deliverable Title Polymer recovery report

Work Package and Task Number

Work Package 7 Task 7.1

Participants: 1- UBRUN 2- CID 3- LEITAT 4- NTUA 5- CETRI 6-

EXERGY 7- ALCN 8- STRESS 9- UAVR 10- ARTIA 11- NRGIA 12- COLL 13- COOLH 14- ACCIO

Sign off Name Date Approved

Originator CID 30/03/2018

Work Package leader UBRUN 30/03/2018

Tech Lead NTUA 30/03/2018

Coordinator UBRUN 30/03/2018

1 Enter a cross (X) in the appropriate cell.

Dissemination Level 1

PU Public

PP Restricted to other programme participants (including the Commission Services)

HORIZON 2020 SPECIFIC PROGRAMME: Nanotechnologies, Advanced

Materials, Advanced Manufacturing and Processing, and Biotechnology

THEME: [EEB-04-2016]

GRANT AGREEMENT NO: 723825

Ref. Ares(2018)1754260 - 31/03/2018

Green INSTRUC - Contract No: 723825 EEB-04-2016


DISCLAIMER

This document contains the description of the Green INSTRUCT project findings, work and

products. Certain parts of it might be under partner Intellectual Property Right (IPR) rules.

Therefore, prior to using its content please contact the consortium coordinator for approval. E-

mail: [email protected] .

Should you feel that this document harms in any way the IPR held by you as a person or as a

representative of an entity, please do notify us immediately.

The authors of this document have taken all available measures in order for its content to be

accurate, consistent and lawful. However, neither the project consortium as a whole nor the

individual partners that implicitly or explicitly participated in the creation and publication of this

document hold any sort of responsibility that might occur as a result of using its content.

This document has been produced with the assistance of the European Union. The content of

this document is the sole responsibility of the Green INSTRUCT consortium and can in no way

be taken to reflect the views of the European Union.

RE Restricted to a group specified by the consortium (including the Commission Services)

CO Confidential, only for members of the consortium (including the Commission Services) X

mailto:[email protected]



Table of Contents 1 Project Summary ............................................................................................................................... 4

2 Glossary of Terms .............................................................................................................................. 5

Definitions .................................................................................................................................. 5

Additional Definitions ................................................................................................................ 5

3 Introduction and Description of Work ............................................................................................... 6

4 Recovery of PU foam CDW ................................................................................................................ 7

5 PU foam CDW as lubricant for extrusion processes. ....................................................................... 15

6 Acknowledgment ............................................................................................................................. 19



1 Project Summary

The Green INSTRUCT project will develop a prefabricated modular structural building block that

is superior to conventional precast reinforced concrete panels by virtue of its reduced weight,

improved acoustic and thermal performance and multiple functionalities. The Green INSTRUCT

block consists of over 70% of CDW in weight.

The Green INSTRUCT project will:

(i) achieve sustainability and cost savings through CDW sourced materials and C2C;

(ii) develop efficient, robust, eco-friendly and replicable processes;

(iii) enable novel cost efficient products and new supply chains;

(iv) develop a building block that renders refurbished or new buildings safe and energy

efficient; and

(v) safeguard a comfortable, healthy and productive environment.

They can be achieved by defining the structural, thermal and acoustic performance of our final

product to be competitive to similar products in the market. The types and sources of CDW are

carefully identified, selected and processed while the supply chain from the sources,

processing, fabrication units to assembly site of the whole modular panel will be optimized.

The project is guided by a holistic view through building information modelling and optimal

overall performance. This includes considering the life cycle analysis, weight, structural

performance, thermal and acoustic insulation, connectivity among modular panels and other

structural/non-structural components as well as the compatibility of different internal parts of the

each modular panel and integration with building information modelling. In order to homogenize

the production process, all individual elements, except the PU insulation layer which will be

fabricated by a moulding process, are fabricated by extrusion which is a proven cost effective,

reliable, scalable and high yield manufacturing technique. The concept, viability and

performance of developed modular panels will be verified and demonstrated in two field trials in

test cells.



2 Glossary of Terms

Acronym Meaning

EC European Commission

EU European Union

CDW Construction and Demolition Waste

PU Polyurethane

C2C Cradle – to - cradle

BIM Building information modelling

MOC Magnesium Oxychloride Cement

LCA Life-Cycle Analysis

TGA Thermogravimetric analysis

DSC Differential scanning calorimetry

FTIR Infrared spectroscopy

Definitions

Words beginning with a capital letter shall have the meaning defined either herein or in the

Rules or in the Grant Agreement related to the Project.

Additional Definitions

Project: Project refers to the Green INSTRUCT project funded from the European Union’s

Horizon 2020 research and innovation programme under Grant Agreement 723825.



3 Introduction and Description of Work

The following document presents the work developed for Polymer recovery and processing, in

the frame of Work Package 7, Task 7.1, within the Project Description of Work. Polymer refers

here to the Polyurethane (PU) foams which appear among the typical components of

construction and demolition wastes.

Two different sub-tasks are related to this point:

Task 7.1.1: PU coming from Construction and Demolition wastes will be used (recycled) as a

material for the insulating layer in the new Panel design. In principle, it was envisaged the

development of the new insulating layers mainly based on PU foam CDW, in such a way that

most of the used material was recycled PU foam, meeting the requirements of the project (70%

of recycled materials in the final Green Instruct Panel). But, in case that insulating layers made

totally (or in high percentages) of PU foam CDW had not enough quality (mechanical resistance

or insulating performance), and taking into account that insulating performance is a very

important goal, and the contribution of PU foam layer to the total weight of the panel is small, it

was considered the development of this insulating layers from pristine PU foams. There, the PU

foam CDW will be included as filler, at ratios lower than 70%.

So, the work in this sub task 7.1.1 deals with the recovery of PU foam CDW blocks, and

treatments to convert them into a homogeneous powder to be used in the described application.

Task 7.1.2: PU foam as lubricating component in the geopolymer and MOC extrusion process.

Here, a second application is envisaged for the powder of PU foam CDW. This polymeric

material could be recycled and re-used as lubricating agent for the extrusion processes of other

materials intended in the Green INSTRUCT Panel: geopolymers and magnesium oxychloride

cements (MOC).

Other polymers are currently used for that purpose, and the work in this subtask has been

focused on the characterization of the PU foam CDW and the treatments applied to make it

closer to the currently used lubricants.



4 Recovery of PU foam CDW

Recycled PU foam was obtained from sandwich panels.

The samples employed in this project came from the deconstruction and renovation of the roof

panels. Also, this kind of materials could be found in sandwich panel producers, as an industry

waste.

Products obtained from rigid foam waste can be a substitute for original products such as:

- insulation panels used in industrial construction;

- internal insulation of heating pipes;

- acoustic insulation in sound-absorbing screens;

- insulation panels in refrigeration equipment.

Typically, rigid foam of this kind is crushed to a fraction depending on the method of reuse.

In our case, the recovery procedure was as follows:

1- disassembly of roof panels;

2- extracting the core from PU foam by removing the metal layers;

3- fragmenting the PU foam boards into smaller pieces;

4- Milling the smaller pieces into powder.

For grinding, standard grinder for polymers was used, with modification, i.e. better material

pressure to the grinding wheel, to obtain a finer fraction of the material. Power of this machine

is 7 kW.

During the demolition of sandwich elements, different types of foams can be found. The

panels differ in the density of the foam and thus the weight and degree of isolation and

saturation.

Usually, the apparent density of PU foams ranges between 30 and 200 kg/m3. But in most

cases, it falls about 30-40 kg/m3.

NRGIA recovered and sent samples of PU foam from CDW to CID, both in the forms of row

blocks and powder.



Figure 1 – Blocks of PU foam from CDW.

Shipments were done under these references:

#01/01/03/2017/CIDETC/FOAM/CDW# (powder, 0.6 kg)

#02/15/03/2017/CIDETC/FOAM/CDW# (blocks, 1.2 kg)

#22/07/2017/CIDETEC/PUFOAM/# (powder, 6 kg)



In order to characterize this material, micrography, thermal gravimetric analysis, Fourier

transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC) and test of

solubility were performed.

OPTICAL MICROSCOPY.

Microscopy images were obtained from an Optical Microscope LEICA DM4000M. Objectives

with 5x, 10x, 20x and 50x magnification power. Eyepiece 10x magnification power. Images were

registered by a digital camera LEICA DFC 420C, 5M pixel resolution.

Figure 2 – Optical microscope.

Samples of this PU foam from CDW powder showed small fragments of a branched structure,

being those fragments 50 – 300 microns in size, the average of which was close to 150 microns.



Figure 3 – Micrography of PU foam powder from CDW.

THERMOGRAVIMETRIC ANALYSIS

Thermogravimetric measurements were carried out using a thermobalance TA Instruments

Q500. Heating rate from 0.1 to 100 ºC/min. Weight sensibility: 0.1 microgram. Weight accuracy:

0.01%. Isothermal temperature measurement accuracy: 0.1ºC.

Figure 4 – Thermogravimetric analysis device

The material, subjected to TGA analysis, lost a small percentage of weight bellow 200 ºC (7%,

probably due to humidity). Main loss began over 200 ºC, dropping to 100% of decomposition at

575 ºC. It could be deduced from this analysis that this polymer is not thermally stable above

200 ºC.



Figure 5 – TGA analysis of PU foam from CDW

FOURIER TRANSFORM INFRARED (FTIR) SPECROSCOPY

FTIR measurements were carried out using a Fourier Transform IR spectrophotometer (Jasco

4100 LE). The FTIR spectra were obtained in the wavenumber range from 350 to 7800 cm−1

repeated for 32 scans. Samples are measured in ATR mode by direct contact in the measuring

window.

5.113%

5.504%

170.61°C

180.70°C

6.388% 199.87°C

-0.2

0.0

0.2

0.4

0.6

De

riv.

We

igh

t (%

/°C

)

-20

0

20

40

60

80

100

120

We

igh

t (%

)

0 200 400 600 800 1000

Temperature (°C)

Sample: PU FOAM polvo 10-03-17Size: 2.1200 mgMethod: LiS_5ºC_min_400

TGAFile: C:...\PU FOAM polvo 10_03_17_air.001

Run Date: 10-Apr-2017 10:10Instrument: TGA Q500 V20.13 Build 39

Universal V4.5A TA Instruments



Figure 6 – Infrared spectroscopy (FTIR) device.

FTIR measurements confirmed that this material consists of polyurethane.

Figure 7 – FTIR spectroscopy of PU foam CDW

*01/01 /03/2017 /CIDET E C/FOAM/CDW

0,6

0,7

0,8

0,9

T

Po lyether u rethane, PP O+MBI, pyrol .

0,2

0,4

0,6

0,8

T

Po ly(N-1,4-phenylene hydroquinone bis (2 -oxazoli don-4-ylm ethyl) e ther

0,2

0,4

0,6

0,8

T

1000 1500 2000 2500 3000 3500 4000

cm -1



DIFFERENTIAL SCANNING CALORIMETRY (DSC)

Differential scanning calorimetry was performed with the TA Instruments DISCOVERY DSC25

AUTO device in a range of temperature from -80 ºC to 725 ºC, and using a heating rate of 20

ºC/min.

Figure 8 – Differential scanning calorimetry (DSC) device.

DSC analysis showed the glass transition temperature (Tg) of PU foam from CDW was about

59-61 ºC.

Figure 9 – Differential scanning calorimetry of PU foam CDW.

PU FOAM NRGY

Exo Down

Midpoint type: Half height Midpoint: 58.66 °C




SOLUBILITY TEST.

Some pieces of PU foam from CDW (blocks) were put in different solvents to observe their

behaviour in such media (no interaction, swelling, solution,..). After being 14-32 days in contact

with these solvents (ethanol, acetone, ethyl acetate, chloroform, diethyl ether, hexane,

tetrahydrofurane, dimethylformamide) the solid pieces of PU foam remained completely

undissolved, meaning that this material is not affected by solvents. This behaviour conformed

with the characteristic of typical crosslinked (or thermoset) polymers.

Figure 10 - Pieces of PU foam CDW (blocks) in different solvents, at t=0.



Figure 11- Pieces of PU foam from CDW (blocks) in different solvents, at t=14-32 days.

5 PU foam CDW as lubricant for extrusion processes.

One of the envisaged applications for PU foams (coming from construction and demolition

wastes, CDW), as stated in the Green INSTRUCT Project, is to act as co-extrusion agents

(lubricants) for the process of extrusion of geopolymers and magnesium Oxychoride cements

(MOC), which are among the intended materials for the Green INSTRUCT panel development.

Common polymers used for those applications are, for example, hydroxyethyl methyl cellulose,

methylcellulose, hydroxypropyl methylcellulose (that are, alkyl and hydroxi-alkyl derivatives of

cellulose), Carboxymethyl Hydroxypropyl Cellulose (CMC) powder and Polymer Polyacrylamide

(PAM).

The role to be played by these additives in the extrusion process is to modify the rheology of

geopolymer and MOC paste so that it is more cohesive, better water retaining and better plastic

behaviour, etc.

The PU foams from CDW taken under consideration in the Project are polyurethane polymers,

so their composition is in principle quite different from that of the celluloses and polyacrylamides.

Hence, a detailed examination of similarities and differences between those two families of

materials should be done, in order to identify convenient features for making the PU foams from

CDW a possible alternative to commonly used polymers for lubricant of extrusion process.

One of the main and most common features of these additives is the water solubility, which

allows to use them as water solutions. This is not valid for PU foams, since they are insoluble

polymers. When taking into consideration their potential use as co-extruders for the geopolymer

or the MOC extrusion process, it will be very important to have the PU foam as finely divided as

possible, in order to achieve the highest admixture homogeneity.



An approach could be go through a modification of the chemical structure of the PU foam in

order to make it closer to that of the currently lubricant polymers used. Following this idea, a

controlled thermal degradation of the PU foam CDW has been tried. This kind of treatment could

break a part of the covalent bonds in the molecular structure, making the PU polymer less

crosslinked, and hence closer to the linear macromolecules that constitute the currently used

lubricants.

In the first attempt, a sample of PU foam from CDW was treated in an oven at 180 ºC for 2

hours. The material was completely burned, meaning that milder conditions are need for the

controlled thermal degradation. After testing at several temperatures and times, it was found

that a treatment at 150 ºC for 1h should be enough to promote some changes in the molecular

structure while avoiding the material to be burned.

The treated PU foam from CDW was characterized by TGA, DSC and FTIR.

TGAs showed that the thermal stability of the PU foam CDW fails at temperatures above 150

°C. At 200 °C, a 3% loss of weight can be measured. This value reached 6% in the case of

original PU foam CDW (not thermally treated) and could account for the humidity content.

Figure 12 - TGA of PU foam CDW thermally degraded (150 ºC, 1h.)

DSCs showed a thermal transition point around 52 °C – 60 °C in both original and thermally

degraded PU foam CDWs.

1.246%4.031%

34.98%

59.46%

551.26°C

300.07°C

208.95°C

-0.2

0.0

0.2

0.4

0.6

0.8

Deriv. W

eig

ht (%

/°C

)

-20

0

20

40

60

80

100

120

We

igh

t (%

)

0 200 400 600 800 1000

Temperature (°C)

Sample: PU FOAM pirolisis 1h 150CSize: 1.5430 mgMethod: RampComment: 400 gr para enviar

TGAFile: PU FOAM NRGY 1h 150C enviar 400gr.001

Run Date: 12-Dec-2017 09:05Instrument: TGA Q500 V20.13 Build 39

Universal V4.5A TA Instruments



Figure 13 - Two DSC scans of PU foam CDW thermally degraded (150 ºC, 1h.)

FTIR showed some characteristic absorption peaks of polyurethanes. After controlled thermal

degradation, peak at 1220 cm-1, corresponding to C-N bonds, suffered a decrease of intensity

relative to the peaks at 1700 cm-1 (C=O bond of polyurethane) and 1515 cm-1, 1410 cm-1 (C-H

bonds). This meant that the treatment led to the breaking of such bonds in some extension.

PU FOAM NRGY pirol150C 1h envio 400gr

Exo Down





Figure 14 - Top: FTIR of PU foam CDW; Below: FTIR de PU foam from CDW after thermal treatment (150 °C, 1h).

Samples (300 g) of:

a) PU foam CDW powder.

b) PU foam CDW powder, treated by controlled thermal degradation (1h at 150 °C).

were sent to UBRUN, to be tested as lubricants for the geopolymer and MOCs extrusion

processes.

*02/15 /03/2017 /CIDET E C/FOAM/CDW

0,65

0,70

0,75

0,80

0,85

0,90

0,95T

**

0,6

0,7

0,8

0,9

1,0

1,1

1,2

1,3

T

500 1000 1500 2000 2500 3000 3500 4000

cm -1



6 Acknowledgment

This project has received funding from the

European Union’s Horizon 2020 research and

innovation programme under grant agreement No

723825.

Disclaimer

The Horizon 2020 project has been made possible by a financial contribution by the European

Commission under Horizon 2020 research and innovation programme. The publication as

provided reflects only the author’s view. Every effort has been made to ensure complete and

accurate information concerning this document. However, the author(s) and members of the

consortium cannot be held legally responsible for any mistake in printing or faulty instructions.

The authors and consortium members reserve the right not to be responsible for the topicality,

correctness, completeness or quality of the information provided. Liability claims regarding

damage caused by the use of any information provided, including any kind of information that

is incomplete or incorrect, will therefore be rejected. The information contained in this document

is based on the author’s experience and on information received from the project partners.

2020 s p : nanotechnologies, advanced materials ......exergy 7- alcn 8- stress 9- uavr 10- artia 11-...

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