WP4: Evaluation of catalyst activity and stability
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WP4: Evaluation of catalyst activity and stability. Slide 1. Workpackage:. WP4. Evaluation of catalyst activity and stability. Presenter:. MTEC - Angkhana Jaroenworaluck. Collaborating teams:. UoB / URJC UCL / UoR, MTEC / SIRIM / VAST-ICT. WP4: Tasks & Teams. Slide 2.

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Slide 1

WP4: Evaluation of catalyst activity and stability

Slide 1

Workpackage:

WP4. Evaluation of catalyst activity and stability

Presenter:

MTEC - Angkhana Jaroenworaluck

Collaborating teams:

UoB / URJC

UCL / UoR,

MTEC / SIRIM / VAST-ICT


Slide 1

WP4: Tasks & Teams

Slide 2


Slide 1

WP4: Objectives

Slide 3

1. Core/shell nanostructure

materials

2. New photocatalyst types

Tested photocatalysts

to be further characterised

to maximise results

WP2

WP5

New materials to increase

visible light activity

Kinetic and Mechanism Studies

WP4

TiO2 photocatalysts

deposited on

various type of supports

Test key parameters

for the reactor design

WP3

WP6

Improving TiO2 based systems

Reactor design, evaluation

& scale up

Standardization for Photocatalyst reactions


Slide 1

Deliveries

Slide 4

Due

No.

Description

D4.1

M9

Report on the optimum design of a test reactor for the project

Performance of new generation of photo-catalysts

D4.2

M42

M42

Industry effluent degradation performance

D4.3


Slide 1

Milestones

Slide 5

M12-18

Milestone

Milestone name

Expected

Means of verification

Standardised reactor constructed in

all sites working on WP4.2 and 4.3.

Screening reactor

operational

MS14

M12

Initial kinetic analysis doped and

non-doped TiO2 powders

MS15

Kinetic profiles available

M18


Outline

Outline

Task 4.1. Standardisation of Test Conditions

1.- Preliminary design of the photoreactor

2.- Proposed reactor design

6


Slide 1

Task 4.1. Standardisation of Test Conditions

1.- Preliminary design of the photoreactor

  • Objective: simple reactor to test different catalysts at equal conditions at the different research locations.

  • The conditions that should be equal, as previously discussed, are: temperature, pH, oxygen supply, indicator concentration and light intensity.

  • To measure the pH, oxygen, and temperature there should be 3 access points for sensors.

  • To be able to control the temperature the reactor should have a cooling/heating jacket.

  • To ensure an equal light intensity the distance between the source and the catalyst and the height of water should be fixed.


Slide 1

Task 4.1. Standardisation of Test Conditions

1.- Preliminary design of the photoreactor

Basic Design I


Slide 1

Task 4.1. Standardisation of Test Conditions

1.- Preliminary design of the photoreactor

Basic Design I

The light source will be placed on top of the reactor vessel and integrated with the required access points and sample point

To ensure a fixed distance between the light source and the catalyst a frame to hold the immobilized catalyst.


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

Reactor Design Considerations

FLUID DYNAMICS AND HEAT TRANSFER:

Perfectly mixed conditions should be ensured to:

- Discard external mass transport effects  Reaction kinetics control.

- Homogeneous composition in the withdrawal of samples.

- Isothermal conditions.

Proposals:

- Magnetic stirring at the bottom.

- Air bubbling to improve mixing.

- Position of the catalyst inside the liquid at a height around 2/3.

- Diameter of the catalyst 1/2 of the reactor diameter.

- Cooling jacket to keep temperature constant (bad for wall reflectivity)


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

Reactor Design Considerations

RADIATION TRANSFER:

Homogeneous irradiation of the catalyst  Homogenous reaction rate.

Low LEDs-catalyst distance  Higher radiation flux (especially for non-reflective walls)

Low LEDs-catalyst distance  Risk of wetting the LEDs circuits.

Proposals:

- Air chamber above the liquid surface required for air equilibrium.

- Highly reflective walls to increase radiation flux and to improve homogeneity.

- Optimal distribution of the LED sources to improve homogeneity.


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

Reactor Design Considerations

CHEMICAL REACTION KINETICS:

Constant dissolved O2 concentration: Simplifies kinetics and avoids measurement.

Nearly constant reaction volume: (withdrawn samples < 10% total volume).

Relatively short reaction time:

- Reduces heating problems.

- Reduces stripping of chemicals to the gas phase.

- Low conversion < 10%  Initial reaction rate conditions, intermediates effects can be discarded in the kinetics.

Proposals:

- Relatively high reaction volume

- Sampling below <10% of the total reaction volume.

- Conversion around 10% optimal for getting significant data above the experiment error of the analytical method keeping initial reaction rate conditions.


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

Proposed Reactor Dimensions

Reactor diameter: D_R = 80 mm

Liquid height:H_L = 50 mm

Sample volume:V_S = 2.5 mL

Sample number (máx):N_S = 10

Catalyst diameter:D_C = 40 mm (1/2 of the reactor)

Catalyst height:H_C = 30 mm above bottom, 20 mm below surface.

LEDs height:H_LED = 80 mm (50 mm from catalyst, 30 mm air)

Reaction volume V_L = 250 mL

Max volume V_Smax = 25 mL

Min H_L = 45 mm (DH_L 10%)


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design


Slide 1

Task 4.1. Standardisation of Test Conditions

  • Number, dimensions and arrangement of the LED.

LEDs Circuit Preliminary Design

Possibility of switching off some LEDs to modify irradiation flux


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

LED Circuit

Reactor Vessel


Slide 1

Task 4.1. Standardisation of Test Conditions

2.- Proposed Reactor Design

Cover / Catalyst Frame

Openings

LEDs Circuit position

Catalyst Holder


Slide 1

Slide 18

Standardization bodies on photocatalyst materials

(CEN vs ISO)


Slide 1

CEN

Slide 19

CEN: European committee for standardization

CEN/TC386-(Photocatalysis) established in 11/2008

WG3: Water purification

WG6: Light source

WG8: Microbiological effects

Secretariat: AFBOR (France)

Chairman: Dr. Pascal KALUZNY (France)

Source: http://www.cen.eu and http://www.dri.mmu.ac.uk


Slide 1

Slide 20

00386001

Project reference: FprCEN/TS16599

Title: Photocatalysis-Irradiation conditions for testing photocatalytic properties of semiconducting materials and the measurement of these conditions

Candidate citation in OJEU* :No (-)

Current status: Under Approval

DAV: 2013-12

(*) OJEU-Official Journal of the European Union

Source: http://www.cen.eu


Slide 1

ISO

Slide 21

ISO: International organization for standardization

ISO/TC206-Fine Ceramics established in 1992 with JISC as secretariat

Secretariat: Dr. Shuji Sakaguchi (AIST, Japan)

Chairman: Dr. Tai-Kyu Lee (Nanopac Co., Korea)

(WG37: Test methods for photocatalytic materials)

Convenor: Dr. Koji TAKEUCHI (AIST, Japan)

Source: http://www.iso.org


Slide 1

Published standards-1

Slide 22

ISO/TC206: Photocatalyst materials / water purification/ anti-bacteria /

light source

ISO 10676:2010

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Test method for water purification performance of semiconducting photocatalytic materials by measurement of forming ability of active oxygen.

Abstract

ISO 10676:2010 describes a test method covering photocatalytic materials formed on, or attached to, another material surface for the purpose of decomposing, and thus eliminating, the pollutants in water, using photocatalytic performance.

This test method is applicable to photocatalytic materials under UV irradiation, and not under visible light irradiation.

Source: http://www.iso.org


Slide 1

Published standards-2

Slide 23

ISO 10677:2011

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Ultraviolet light sourcefor testing semiconducting photocatalytic materials.

Abstract

ISO 10677:2011 describes an ultraviolet (UV) light source and specifies a method of measuring the radiation intensity which is used in testing the performance of semiconducting photocatalytic materials in a laboratory.

Source: http://www.iso.org


Slide 1

Published standards-3

Slide 24

ISO 10678:2010

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Determination of photocatalytic activity of surfacesin an aqueous medium by degradation of methylene blue.

Abstract

ISO 10678:2010 specifies a method for the determination of the photocatalytic activity of surfaces by degradation of the dye molecule methylene blue (MB) in aqueous solution using artificial ultraviolet (UV) radiation, and characterizes the ability of photoactive surfaces to degrade dissolved organic molecules on ultraviolet radiation.

The test method specified is also applicable to evaluation of the specific photocatalytic self-cleaning activity of surfaces covered with respective coatings.

This method is not applicable to characterizing the photoactivity of surfaces on visible illumination, regarding direct soiling, degradation of gaseous molecules and the determination of antimicrobial photoactivity of surfaces.

Source: http://www.iso.org


Slide 1

Published standards-4

Slide 25

ISO 13125:2013

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Test method for antifungal activity of semiconducting photocatalytic materials.

Abstract

ISO 13125:2013 specifies a test method covering the determination of the antifungal activity of materials that contain a photocatalyst or have photocatalytic films on their surface, by counting the number of pre-incubated fungal spores that survive exposure to ultraviolet (UV-A) light.

ISO 13125:2013 provides for the assessment of different kinds on materials used in various applications, such as construction materials in flat coating, sheet, board or plate form, etc. Powder, granular, fibrous or porous photocatalytic materials are not included.

Values expressed in ISO 13125:2013 are in accordance with the International System of Units (SI).

Source: http://www.iso.org


Slide 1

Published standards-5

Slide 26

ISO 27447:2009

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Test method for antibacterial activity of semiconducting photocatalytic materials.

Abstract

ISO 27447:2009 specifies a test method for the determination of the antibacterial activity of materials that contain a photocatalyst or have photocatalytic films on the surface, by measuring the enumeration of bacteria under irradiation of ultraviolet light.

ISO 27447:2009 is intended for use with different kinds of semiconducting photocatalytic materials used in construction materials, in flat sheet, board, plate shape or textiles that are the basic forms of materials for various applications. It does not include powder, granular or porous photocatalytic materials.

This test method is usually applicable to photocatalytic materials produced for an antibacterial effect. Other types of performance of photocatalytic materials, i.e. decomposition of water contaminants, self-cleaning, antifogging and air purification, are not determined by this method.

The values expressed in ISO 27447:2009 are in accordance with the International System of Units (SI).

Source: http://www.iso.org


Slide 1

Standards under development

Slide 27

ISO/FDIS 14605

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Light source for testing semiconducting photocatalytic materials used under indoor lighting environment.

ISO/DIS 17094

Fine ceramics (advanced ceramics, advanced technical ceramics) -- Test method for antibacterial activity of semiconducting photocatalytic materials under indoor lighting environment.

Source: http://www.iso.org


Slide 1

New proposal for water purification

Slide 28

Standards to be proposed:

Test method for environment purification

performance of photocatalyst and applied

materials by dissolved oxygen consumption (Temperary)

Proposed by:

Dr. Koji TAKEUCHI (AIST, Japan)

Dr. Tsutomu HIRAKAWA (AIST, Japan)

Target dates of proposal and issue of the standards:

JIS: Proposal FY 2012 Issued FY 2013

ISO: Proposal FY 2012 Issued FY 2017

Source: from Dr. Takeuchi (AIST, JAPAN), page 18 of 23souran_hyoujyunkiban.pdf


Slide 1

MB degradation test of P25 TiO2

Slide 29

Light source

Light off - 24 h

filtration

Light on -150 min

filtration

MB concentration: 4 ppm

UVA intensity: 50 W/m2


Slide 1

Future plans

Slide 30

Make a simple reactor (closed system) of LED light source from UOB.

Set test conditions: Light on-off, P25 TiO2 / MB concentrations / LED intensities.

Compare reaction rate from all reactors used.

Change catalyst types for the same test conditions.

(started from powder type to pellets and 3D-porous TiO2 catalysts)

5. Draft scientific papers to be published. (if possible)


Slide 1

Slide 31

Thank You


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