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Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory CL-175097-4 Seite 1 von 21 Please use a separate questionnaire for each product. The information which you provide in this questionnaire is the basis for the planning and preparation of your trials. We therefore ask you to fill the questionnaire in as conscientiously and completely as possible. If insufficient space is provided, please use additional sheets. BCT - PROJECT N° CUSTOMER REFERENCE N° COMPANY NAME CONTACT PERSON DEPARTMENT STREET CITY/POST CODE COUNTRY TELEPHONE FAX E-MAIL © BUSS ChemTech AG, 2006 Made by: R. Schaffner Issue Date: 29.07.2005

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Page 1: Questionnaire for trials for Gas / Liquid Reactions in the ...  · Web viewThe information which you provide in this questionnaire is the basis for the planning and preparation of

Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory

CL-175097-4Seite 1 von 14

Please use a separate questionnaire for each product.

The information which you provide in this questionnaire is the basis for the planning and preparation of your trials. We therefore ask you to fill the questionnaire in as conscientiously and completely as possible. If insufficient space is provided, please use additional sheets.

BCT - PROJECT N°      

CUSTOMER REFERENCE N°      

COMPANY NAME      

CONTACT PERSON      

DEPARTMENT      

STREET      

CITY/POST CODE      

COUNTRY      

TELEPHONE      

FAX      

E-MAIL      

© BUSS ChemTech AG, 2006Made by: R. Schaffner

Issue Date: 29.07.2005 Filed by: QM

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1. CHEMISTRY

1.1 Reaction equation

     

1.2. Side reactions

Possible side reactions:

1)      

2)      

3)      

Measures to be taken for the suppression of these reactions:

1)      

2)      

3)      

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2. PRODUCT DATA /SAFETY INFORMATION

2.1. Product data

2.1.1. Starting materials, additives, products and by-products

Please list your starting materials, additives, products and by-products:

starting material or product 1:      

starting material or product 2:      

starting material or product 3:      

starting material or product 4:      

starting material or product 5:      

starting material or product 6:      

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starting material / product 1 2 3 4 5 6

chemical formula                                    

molecular weight (g/mol)                                    

melting point ( °C)                                    

boiling point (°C)                                    

density (ambient conditions) (kg/m³)                                    

density (reaktion conditions) (kg/m³)                                    

specific heat cp (ambient conditions) (kJ/kgK)                                    

specific heat cp (reaction conditions) (kJ/kgK)                                    

latent heat of evaporation (kJ/kg)                                    

viskosity (ambient conditions) (cP)                                    

viskosity (reaction conditions) (cP)                                    

reaction enthalpy (kJ/mol)                                    

thermal conductivity (ambient conditions) (W/mK)                                    

thermal conductivity (reaction conditions) (W/mK)                                    

decomposition temperature (°C)                                    

vapour pressure (ambient conditions) (bar)                                    

vapour pressure (reaction conditions) (bar)                                    

Please add curves of vapour pressure, density, viskosity etc. as a funktion of temperature, if available

© BUSS ChemTech AG, 2006Made by: R. Schaffner

Issue Date: 29.07.2005 Filed by: QM

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2.1.2. Reaction mixtureDensity (ambient cond.)       (kg/m3)

Density (reaction cond.)       (kg/m3)

Viscosity (ambient cond.)       (cP)

Viscosity (reaction cond.)       (cP)

Vapour pressure (ambient cond.)       (bar)

Vapour pressure (reaction cond.)       (bar)

Reaction enthalpy       (kJ/mol)

Thermal stability: At which temperature does the thermal decomposition of the reaction mixture start?:       (°C)

2.2 Safety data for the starting materials, additives, products and by-products

1 2 3 4 5 6

Flash point (°C)                                    

Self ignition temperature (°C)                                    

Lower explosion limit (%vol)                                    

MAK-value                                    

UN-N°                                    

Poison classification                                    

Is contact with water dangerous(yes/no)

                                   

Melting point (°C)                                    

Boiling point (°C)                                    

Safety sheet N°                                    

Transport classification                                    

Are any special precautions to be taken for the safety and protection of human beings or the enviroment?

     

All products made in the trials and all unused starting material are best returned to the customer for disposal. To which address should they be dispatched?

     

© BUSS ChemTech AG, 2006Made by: R. Schaffner

Issue Date: 29.07.2005 Filed by: QM

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3. CUSTOMER'S experience

3.1. Experience from laboratory or pilot plant work

What influence does the temperature have on the course of the reaction?

     

What influence does the pressure have on the course of the reaction?

     

What different kind of catalysts have been investigated?

     

What influence does the catalyst type have on the course of the reaction?

     

What influence does an increase of the catalyst concentration have on the courseof the reaction?

     

What influence does the starting material concentration have on the course of the reaction?

     

What kind of solvents have been investigated?

     

What influence does the solvent have on the course of the reaction?

     

What influence does the stirrer speed have on the course of the reaction?

     

(Please add graphs showing the observed influences if available)

What kind of equipment has been used for the laboratory investigations?Please name the type of the equipment or illustrate it with a diagram.

     

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3.2. Experience from production

Please describe the standard operating procedure:

Charge composition:      

Starting material 1 :       (wt%/total charge)

Starting material 2 :       (wt%/total charge)

Starting material 3 :       (wt%/total charge)

Starting material 4 :       (wt%/total charge)

Additive :       (wt%/total charge)

Solvent component 1 :       (wt%/total charge)

Solvent component 2 :       (wt%/total charge)

Catalyst type :       (wt% dry/starting material)

Catalyst supplier :      

Reaction pressure :      (bar)Reaction temperature :       (°C)

Reaction time :       (min)

Conversion :       (%)

Selectivity :       (%)

What kind of equipment has been used to achieve the above mentioned results? Please name the type or add a process diagram.

Stirred tank type :      

Working volume :       (m3)

Maximal operating pressure :       (bar)

Maximal operating temperature :       (°C)

Stirring rate :       (1/min)

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How does the equipment have to be cleaned after the trials?

     

What are the requirements for the material of construction? Please name the appropriate materials of construction.

     

What kind of additional actions or precautions have to be taken to influence the course of the reaction positively?

     

Is there a possibility of crystallisation of intermediates or products below a certain temperature?

no

yes(please give crystallisation temperature and describetype of crystals):      [°C]

     

What impurities or substances that are known to be a catalyst poison or can act as such are there in the reaction mixture or in the starting materials and additives?

     

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4. BUSS-CT PILOT PLANT TESTS

4.1. Objectives

4.1.1. Aim of the trials

Please list the goals you would like to achieve:

actual target

Yield             (%)

Selectivity             (%)

Reaction time             (min)

Catalyst amount             (wt% dry/starting material)

Re-use of the catalyst             (N° of recycles)

Starting material concentration             (wt%/total charge)

Which of the above mentioned parameters are critical for the economy of the process?

     

4.1.2. Product requirements:

Please add the specifications you would like to achieve:

     

4.2. Performance of trials

4.2.1. Working procedure

Please give the chronological order of the required working procedure. What effect does a deviation from this given procedure cause?

     

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4.2.2. Charge

Starting material 1 :       (wt%/total weight)

Starting material 2 :       (wt%/total weight)

Starting material 3 :       (wt%/total weight)

Starting material 4 :       (wt%/total weight)

Additives :       (wt%/total weight)

Solvent component 1 :       (wt%/total weight)

Solvent component 2 :       (wt%/total weight)

Catalyst :       (wt%/starting material)

4.2.3. Catalyst details

Type :      

Supplier :      

In what form will the catalyst be delivered?

powder

humid e.g. Pt/C : % H20 content :      

Raney-Nickel in H2O

other forms

in case of Ra-Ni:

are there any special instructions for weighing out the catalyst?

     

4.2.4. Reaction conditions

Pressure :       (bar)

Temperature :       (°C)

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4.2.5. Further information

Which of the following pump seal flushing liquids are preferable for your product?

paraffin oil

water/glycerine mixture

Is the starting material dissolved or is it a slurry?

If a slurry, how many wt% of the total reaction mixture are not dissolved?

      (wt%)

Does the starting material dissolve as the reaction proceeds?

     

Pre-treatment:What steps are required before the reaction?

     

Post-treatment:Is a work-up of the product after the reaction and catalyst filtration necessary or desired?

     

4.3. Analyses

Which substances are analyzed using a.) physical determinations :      

b.) chemical determinations :      

Please add the required analytical methods. Please use the forms in the appendix if possible.

So that we can reproduce, your analyses before trials begin, please let us have the reference substances, column(s) and chromatograms 4 weeks before the start of the trials at the latest.

To reach an optimal and efficient utilisation of the laboratory equipment it is usually advisable for an analytical specialist to come to BCT to advise our laboratory staff on the details of the procedures to be used.

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APPENDIX

1. Gas chromatography

1.1. Column

Supplier :      

Type/Support :      

Length :       (m)

Diameter :       (mm)

1.2. GC-Method

Start-Temperature-Oven :       (°C)

End-Temperature-Oven :       (°C)

Initial-Time :       (min)

Rise of temperature :       (°C/min)

End-Time :       (min)

Detector :       (°C)

Injector :       (°C)

1.3. Sample preparation

Solvent :      

Concentration :      

Injection volume :       (ul)

Sample preparation (please describe the preparation exactly):

1.4. Integration method: Area %

Internal Standard method

External Standard method

1.5. Customer's equipment

Supplier :      

Equipment type :      

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2. HPLC2.1. Column

Supplier :      

Type :      

Support :      

Particle size :       (um)

Diameter :       (mm)

Length :       (mm)

2.2. Conditions

Wavelength :       (nm)

Flow :       (ml/min)

Range :       (AUFS)

Pressure :       (bar)

Column temperature :       (°C)

Method Pump A Pump B

isocratic            

gradient            

Gradient program

Time       Initial (min)

Flow      

%A      

%B      

2.3 Sample preparation

Solvent      

Concentration      

Injection volume       (ul)

Sample preparation (Please describe the preparation exactly):

     

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2.4. Integration method:

Area %      

Internal Standard method

External Standard method

2.5. Customers equipment

Supplier :      

Type :      

3. IR/UV

3.1. Conditions

Cell thickness :       (mm)

Concentration :      

Wavelength :       (nm)

Reference solution :      

3.2. Sample preparation

Sovent :      

Concentration :      

Sample preparation :      

(please describe the preparation exactly)

     

3.3. Customer's Equipment

Supplier :      

Type :      

Appendix

Summary of the analytical capabilities of the BCT laboratory (see FF-477339-0)

Please complete this Questionnaire formand send it to: or contact us please by:BUSS ChemTech AG Fax: +41 61 82 56 737Hohenrainstrasse 10 Phone: +41 61 82 56 668CH-4133 Pratteln1, Switzerland e-mail: [email protected] site address of Buss ChemTech AG: www.buss-ct.com