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BTEC Nationals

Edexcel level 3 BTEC National Certificate/Diploma

Applied Science (Laboratory and Industrial Science)
Applied Science (Medical Science)

Integrated Vocational Assignment

CASE STUDY 2- Johnson Matthey (Catalysts and Chemicals)

Unit 3: Workplace practices

This case study has been prepared by Mr. M. Hooper & Ms P. Hooper with the co-operation of Johnson Matthey (Catalysts and Chemicals) for the use of learners completing the IVA for the NQF Level 3 BTEC Nationals in Applied Science.

Prepared by M. Hooper & P. Hooper. March 2005

The following materials have been authorised for use by students in this context, by Johnson Matthey. Some data is not current, and some is adapted to give a working document to allow completion of the assignment,

To complete the assignment students must have access to detailed information about a company. This is often difficult to obtain, and the following information will provide exemplar material for the completion of the IVA.

The information is based on the British Company – Johnson Matthey, one of the leading speciality chemicals companies in the world specialising in Catalysts, Precious Metals and Speciality chemicals.
Johnson Matthey is a large multi-national company. There is a lot of information available on the various web-sites. The website reflect the divisional nature of the company. These notes will summarise the company structure, provide a guide to focus the students attention through the various divisions to the area of interest.

The full company’s website is: http://www.matthey.com Links can be followed to the 'Catalysts' division website at:

http://www.jmcatalysts.com

then, to the 'Process Catalysts and Technologies' (PCT) business unit at:

http://www.jmcatalysts.com/pct

and finally to the 'Precious metal catalysts and technologies' website at:

http://www.chemicals.matthey.com

Table of Contents

Introduction to the Company 6
Divisions 7
'Process Catalysts and Technologies' (PCT) 9
Products 9 Homogeneous Catalysts 9 Heterogeneous Catalysts 10
Company Structure 12
Financial Results 15
Standard operating procedures 15
Standard operating procedure – Laboratory Work 18
Standard operating procedure - Production 22
HAZOP 26
Typical cost structure per kilo of Homogeneous catalysts 27
Other Information - use the Website! 27
Practical Work 28
Separation of potassium nitrate and sand using a solvent (water) - comparison of three methods 28

Introduction to the Company

Johnson Matthey

Johnson Matthey is a speciality chemicals company focused on its core skills in catalysts, precious metals and speciality chemicals.
The group's principal activities are the manufacture of autocatalysts and pollution control systems, catalysts and components for fuel cells, pharmaceutical compounds, process catalysts and speciality chemicals; the refining, fabrication and marketing of precious metals; and the manufacture of colours and coatings for the glass and ceramics industries.

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The company comprises 4 divisions as above. This study will focus on the Catalysts division. The company has existed for over 150 years. It was founded by Percival Johnson and George Matthey around 1851. The company originally was based on the assaying precious metals i.e. determining the purity of the very expensive metals for the Bank of England. These metals include gold, silver, platinum, palladium, rhodium, iridium, osmium, and ruthenium; The last five are often referred to as the Platinum Group Metals (PGMs) and a frequently considered on their own as gold and silver are considered not expensive enough to be included!
The activities of the company have grown from the various uses that are found for the 'precious metals'. A quick summary of the divisions follows this idea.
Divisions

Catalysts

The precious metals are a subset of the chemicals known as the Transition Metals, which in various forms have been found to act as catalysts for chemical reactions i.e. the reactions are made faster or easier. Although precious metals are expensive they are often used because they enable some of the most complex reactions to take place. Johnson Matthey’s catalyst activities are split in to three key areas:

The 'Environmental Catalyst Technology' (ECT) business unit focuses on the ability of the precious metal catalysts to transform environmentally unfriendly gases (such as carbon monoxide and nitrogen oxides (Nox)) into safer gases. The major application of this in vehicle exhausts and this now represents the biggest use for precious metals outside their more familiar use in Jewellery.

The 'Process Catalysts and Technologies' (PCT) business unit focuses on precious metal catalysts in chemical 'processes'. This includes processes to make general chemicals for use in bulk process such as plastics manufacture; and also processes to make specific chemicals such as pharmaceutical drugs e.g. Viagra! This expertise in catalysis lead to the logical acquisition of the ex-ICI catalysts business called 'Synetix' in 2002. This means the expertise in catalysis now extends beyond the core precious metals into ‘base’ (i.e. cheaper) metals such as nickel, copper, iron, cobalt, and titanium. Another major part of the PCT business unit is the 'refining' of precious metals. Precious metals are by definition expensive; so old, used catalysts ('spent') are recycled in a process called refining. This involves purifying the metal by 'burning and smelting' away the main impurities such as carbon (e.g. charcoal) or silica (sand). The precious metals are then separated by a long chemical process involving selectively dissolving and re-precipitating the metals. This gives the customer their pure precious metal back, ready for re-uses to make new catalyst, or to be sold back to a bank!

The 'Fuel Cells' business represents a part of Johnson Matthey's investment into future technology. Fuel cells basically generate electricity from hydrogen and air directly in a very clean manner, and are therefore considered very ecologically friendly. The Fuel Cell has Platinum components, which provides a link to JM's core business. Also the possible concept of Fuel Cell vehicles removing the need for vehicle emission catalysts provides a driver for JM to be at the forefront of this exciting technology.

Precious Metals

This business unit focuses on the marketing and uses of the pure precious metals. Platinum and palladium can be 'metal-worked' just like other metals; so various products are made out of pure precious metals. For example, very thin metal wires and tubes can have uses in medical applications, as the precious metals are very inert and will not contaminate the patient. The metals are very resistant, so thin coating can be used to protect surfaces under extreme conditions such as 'casting' of glass. Another main use is in 'knitted' gauze. Thin wires of metal are knitted (on large machines just like wool) to make strong material (gauze) for use in large-scale oxidation process to make nitrates for fertilisers.

Pharmaceutical materials

This business unit was originally based on the discovery of the anti-cancer properties of two platinum-containing molecules, 'Cis-platin' and the newer 'Carbo-platin'. This lead JM into manufacture of pharmaceutical materials, and the business unit has expanded with various acquisitions. Pharma Services business (formerly PharmEco) provides contract research and development and small scale manufacturing services of pharmaceutical components. Johnson Matthey Pharmaceutical Materials - Ireland (formerly Cascade) is focused on the manufacture of prostaglandin’s and other complex molecules as active pharmaceutical ingredients for the pharmaceutical industry. Johnson Matthey Macfarlen Smith has a leading position in the manufacture of controlled substances, i.e. is the only UK company with a license to manufacture heroine for medical use!

Colours and Coatings

Traditionally companies such as 'Wedgwood' have produced tableware with beautiful shiny gold designs. This use of precious metals as decorative coatings led JM into the market for colours and coatings. In parallel with this development Johnson Matthey patented the original process for the screen-printing of metal containing inks. Though this process was originally developed for the production of printed circuit boards for the electronics industry, exactly the same process is used to create the pattern transfers, know as decals, which are used to put complex designs onto plates, providing yet another link to the tableware industry.

The division recently sold on of its component businesses which made pigments and dispersions for the paints and plastics industries, so the remaining businesses have been re-aligned into two operating units:
The Colour Technologies business now headquartered in the Netherlands, which reflects the huge decline in the UK tableware industry, manufactures black obscuration and silver conductive enamels for automotive glass. It also makes enamels and decorative precious metal products for other glass applications such as bottles and architectural glass as well as for the original tableware applications.
The Ceramics business, headquartered in Spain, manufactures colours, glazes and frits for the tile and sanitaryware industries, and includes the zircon business. Zircon is a naturally occurring sand, which when ground into a very find powder can be used as a whitener in clay and glazes. It also has an interesting crystal structure that allows it to “trap” other molecules to provide a highly stable substrate onto which coloured metal oxides can be grafted.

Process Catalysts and Technologies' (PCT)

The whole Johnson Matthey product portfolio would represent too large a field to study in this case study. It is therefore better to focus on one particular area of Johnson Matthey products: the Process catalysts and technologies, and within this area focussing on the precious metal catalysts. Details of this range of products can be found on the ‘process catalysts and technologies' website at: http://www.chemicals.matthey.com Then click on 'Catalyst Guide', which gives the two main groups of products: 'homogeneous catalysts' i.e. those that form a homogeneous mixture with the reactants - those that dissolve; and 'heterogeneous catalysts' i.e. those that are in a different phase to the reactants i.e. don't dissolve.

Products

There now follows a very brief overview of the main product areas:

Homogeneous Catalysts

These are precious metal compounds that will dissolve in the reaction mixture / solvent to catalyse a reaction or process to make the desired product. The advantage of this form of catalyst is that the mixing creates very high levels of activity as the active molecules are widely dispersed among the reactants, however the key disadvantage is that the catalyst them becomes mixed with the final product and is sometimes hard to extract. In some cases this removal is essential in order to create pure final product, in other cases it is simply desirable in order to reuse the catalyst or recycle it to recover the precious metals.

As can be seen on the 'Products' web page, under 'homogeneous catalysts' there are many different products available (>50), made from all the precious metals (Pd, Pt, Ir, Rh, Os, Ru). They have many applications in many industries. This study will focus on just 4 products and their general applications:

Palladium catalysts

Simple salts - Palladium Chloride, Palladium Acetate (Pd-111).
Complex compounds - Pd(PPh3)2Cl2 (Pd-100), Pd(dppf)Cl2 (Pd-107)

Palladium Chloride (PdCl2) and Palladium Acetate (Pd(OAc)2) are both used in industry as homogeneous catalysts. PdCl2 is made by reacting pure metallic Palladium with chlorine gas and hydrochloric acid. Pd(OAc)2 is made by dissolving pure metallic palladium in nitric acid, and adding acetic acid (vinegar!). Both products are brown/ orange solids. Details can be found on the website including the 'Materials Safety Data Sheet' (MSDS) which details safety information for handling, toxicity and transport (via 'MSDS search'). The newer Pd compounds such as Pd(PPh3)2Cl2 and Pd(dppf)Cl2 are part of the JM investment in new technology, and are subject to research and development work such as chemical process selection, process optimisation and production scale-up studies.
These compounds are used in both petrochemical (large scale) and pharmaceutical (more specialised) industries. They can be used to catalyse the formation of new carbon-carbon bonds to 'couple' two organic molecules together. This new area of chemistry is often referred to as 'coupling'.

Petrochemical industry:

Simple petrol derivatives such as ethene can be 'coupled' to make more complex (and valuable) compounds such as butene or butadiene. As the products are 'commodity' chemicals i.e. still quite cheap, there are strong financial pressures to minimise the costs, and therefore the precious metal catalysts is a major component to the process cost. Therefore the catalysts used are often the simple metal salts (such as PdCl2 or Pd(OAc)2) and often at low catalyst loading i.e. ~0.1% Pd with respect to reactants. So you would add 0.1% PdCl2 i.e. ~0.0001 mole of Pd for every mole of reactant.

Pharmaceutical industry:

Pharmaceutical drugs are often complex molecules that need selective process to make them. The products are, however, very valuable. Therefore, the catalysts used are often specialised and can be more complex. So in the 'coupling' chemistry, more complex versions of PdCl2 are developed. JM are world leaders in this technology, as can be seen on the website under 'New catalysts development for cross-coupling reactions'. The new catalysts involve adding a 'ligand' to the Pd, typically a phosphorus based compound (phosphine) such as triphenylphosphine (TPP) or bis(diphenylphosphino)ferrocene (dppf). This generates new products such as:
Trans-dichlorobis(triphenylphosphine)palladium(II) - Pd-100 (JM-code) and Dichloro(1,1-bis(diphenylphosphino)ferrocene) palladium(II) - Pd-107.
These products give the desired very high selectivity in the pharmaceutical applications, which justifies the higher cost (over PdCl2 or Pd(OAc)2). Also they are often used at higher loading (1-5% Pd).

Heterogeneous Catalysts

These are precious metals supported on a substance that will not dissolve in the reaction mixture/ solvent. Though these catalysts are generally less active that the homogeneous ones the fact that they are supported makes the recovery much easier as well as giving the option of controlling the reactants’ contact time with the catalytic material, offering greater control over the reaction.

As can be seen on the 'Products' web page, under 'heterogeneous catalysts' there are many different products available (>400), made from all the precious metals (Pd, Pt, Ir, Rh, Os, Ru) and various supports (carbon, alumina, silica, calcium carbonate). They have many applications in many industries, mostly based on hydrogenation i.e. the addition of hydrogen gas to an organic molecule, which is dissolved in a solvent. So the catalyst (solid) is helping a reactant (dissolved in a liquid) to react with a gas (hydrogen) i.e. three different chemical phases. This study will focus on one general application and the recommended catalysts for this application:

Hydrogenation of Aromatic Rings

Aromatic rings (e.g. benzene) can be found in many chemistries and industries from petrochemical applications (there are traces of benzene in petrol) to specialised industry e.g. pharmaceutical. Often it is desirable to change the aromatic ring (containing double bonds, 'unsaturated') to a cyclohexane ring (with no double bonds, 'saturated'). This is done by reaction with hydrogen gas, and is often best catalyzed by precious metal catalysts. Information on how to carry out this reaction can be found on the website under 'Catalyst Guide', 'Heterogeneous catalysts' (scroll to bottom of page), 'Hydrogenation of Aromatic Rings' and 'View recommended JM catalysts'. This gives you 4 recommended catalysts:

Catalyst Listing for Hydrogenation of Aromatic Rings
Recommended Heterogeneous Catalysts
1% Palladium on Alumina 1% Pd/ Al2O3
5% Platinum on Carbon 5% Pt/C
5% Rhodium on Carbon 5% Rh/C
5% Palladium on Carbon 5% Pd/C

The recommended catalysts involve three different metals (Pd, Pt, Rh) on two types of support (carbon, alumina). All these catalysts are made in broadly similar ways. A precious metal salt (e.g. PdCl2) is stirred in a solvent with the support (e.g. carbon). A reducing agent is then added (a chemical which turns the metal salt back to the pure metal i.e. from oxidation state +2 (salt) back to oxidation state 0 (pure metal) hence 'reducing the oxidation state from 2 to 0'). The catalyst is then filtered. These products are often stored, transported and used as 'wet' products (i.e. 50% water by weight) as the dry powders can by pyrophoric (i.e. so active that they ignite spontaneously in air!).
Each metal and support have different properties for the catalyst, so the combination of metal, support and manufacturing route can allow the customer to achieve the selective process to convert their reactants into the desired product. Again JM is constantly inventing new catalysts for specific processes, which involves research and development work such as chemical process selection, process optimisation and production scale-up studies.

Company Structure

As noted in the introduction, Johnson Matthey is a large multinational so it is beyond the scope of this case study to outline the whole reporting structure. However, the business unit 'PCT' will be highlighted with the top-down reporting structure in brief. A lot of this information is available in the Annual Report, and some is specifically authorised for use in this case study.

Johnson Matthey is a public limited company. This means it is own publicly by shareholders, is listed on the stock exchange and is in the FTSE-100 (one of the 100 largest public companies in the UK). It therefore has a board of directors who administer the company on behalf of the shareholders. This board includes 'Executive Directors' who are involved in the actual running of the company e.g. directors of the divisions; and 'Non-executive Directors' - experts from other companies who advise/ 'consult' on the best options for the shareholders.

Each division reports into the Board of Directors via the Executive Directors. So the 'Catalyst' division has three Executive Directors - Director (PCT), Director (ECT) and Director (Catalyst and Precious Metals), though this structure has recently changed when the Director Catalyst and Precious metals was appointed as Chief Executive Officer, on the retirement of the previous CEO. In the PCT business unit, there is a team of Senior Management including Division Finance Director, Vice President and General Manager (USA and Asia), Managing Director (UK and Europe), Vice President (Polymers, Chemicals and Edible Oils & Oleo chemicals - PCEO), Vice President (Ammonia, Methanol, Oil and Gas - AMOG) and Vice President (Research Chemicals).

Recently, after the acquisition of Synetix, the organisation structure of PCT has been changed to reflect the various markets that are being served by the business unit and the products groups produced in PCT. Within this market facing structure there twelve sub business units, three of which have been highlighted here: Catalysts and Chiral Technologies (CCT), Chemical Catalysts (Chem. Cat.) and Chemical Products and Refining Technologies (CPRT).
CCT this is a market-facing unit focusing on Pharmaceutical and Fine Chemical industries. Pharmaceutical includes companies such as Pfizer, Astra-Zeneca, Glaxo Smithkline and Merck Sharpe Dohme supplying medicines and pharmaceutical drugs. Fine Chemical includes suppliers of speciality chemicals (e.g. for use in plastics, herbicides or fertilisers) such as Syngenta, Aventis.
Chem. Cat. This business unit focuses on the larger scale petrochemical/ commodity chemical industry. Customers include petrochemical giants such as BP, Shell, Exxon and also chemical producers/ processes all around the world such as the OXO-process in Asia and the Far East.
CPRT. This unit focuses on the processing of the metals and catalysts, such as refining services, making metal salts, metal recovery options.

Each unit has their own management structure and teams. These include a Managing Director (MD) or Vice President (VP), Finance Director (FD), Commercial Director and Technology Director. The MD or VP and FD will co-ordinate the unit’s efforts. The commercial director is in charge of the customer facing aspects such as sales, administration, customer support, (logistics). The technology director co-ordinated the technology-push of the company, as Johnson Matthey is above all a 'technology lead' company - it aims to distinguish itself from the competition by continuous development and commercialisation of new technology, whilst promoting excellence in all other aspects of the company.

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Financial Results

Results summary for the year to 31 March, 2004,

Catalysts Division £ millions

Turnover 1142.7

Costs 1033.5

Operating Profit 109.2

Net Operating Assets 819.7

Number of Employees 4,120 people

----------------------------------------------------------------------------

Results for the Whole JM Group £ millions

Turnover 4492.9

Cost of Materials (3725.8)

Net Revenue 767.1

Other costs of sales (402.6)

Gross Profit 364.5

Distribution costs (83.2)
Administration costs (93.6)

Group Operating profit 187.7
--------------------------------------------------------------------------

Total Group Research and Development 54.5

Standard operating procedures

When a product or process is being developed in PCT, the first stage is laboratory development. There is a formal process for each project, involving project initiation (assessment of commercial potential, resources needed, timescale of the project). The research and development is then started at lab scale i.e. 2ml to 500ml scale experiments. This will involve selecting the best synthetic route, trailing and optimisation of the route for yield (how much product is made) and selectivity (how pure is the product that is made).
A formal risk assessment is carried out. This lists the operation procedure (method) and then assesses the risks involved with chemicals being used, many of which are now covered by the regulations know as COSHH (Chemicals Or Substances Hazardous to Health) and their interaction in the process (equipment, manual handling). Most equipment is standard and has been previously risk assessed, but any new equipment or process has to be separately risk assessed.
There now follow a standard Risk Assessment and COSHH for a lab process. It also includes a preliminary environmental impact assessment.

Standard operating procedure – Laboratory Work

|JOHNSON MATTHEY, CHEMICALS, MANAGEMENT SYSTEM |
| COSHH Assessment Form |Ref No. | |

|Dept: Catalyst Development |
|Location: Lab 1, Pro Tech building, Royston |
|Process Description: Preparation of Pd-XXX, |
|Solvent (500 ml) is stirred in a 1 litre r.b. flask with condenser under nitrogen. RRR (XXX g) and precious metal salt (XXX g) are added and washed in with more solvent (160 ml). The slurry is stirred and |
|heated to 80oC for 6 hours. It is cooled to room temperature and filtered. The product is dried in a vacuum oven and analysed. |
|Operating Procedure Ref: Based on previous preps by Jo Bloggs. |

Details of Substances

|Ref |Substance |Hazards |Dustiness/ |OEL |MEL? |Usage |MSDS Ref. |
| | |(R-phrases) |volatility |(mg/m3) |(Y / N) | | |
| | |

|Ref |Hazard Details |People affected |Existing Control Measures |S |L |RR | |Date Req. |
| | | | | | | |Action | |
|A, B,C,|Inhalation, skin contact |Lab 1 occupants |Gloves, safety glasses, lab coat, fume |3 |1 |3 |None. | |
|D | | |cupboard | | | | | |

Target Review Date: 29/4/09 Actual Review Date:

Assessment Leader: Jo Bloggs Assessment Team:

Signed: Date:

Further checks and tests
| |
|Are the Following Tests being Undertaken and Records being Maintained (as required)? |
| | | | | |
| |Yes |No |N/A | |
| | | | | |
|Ventilation inspection |( | | | |
|Weekly | | | | |
| | | | | |
|Statutory Ventilation Test |( | | | |
| | | | | |
|Workplace Monitoring | | |( | |
|( if yes please specify ) | | | | |
| | | | | |
|Health Surveillance | | |( | |
|( if yes please specify ) | | | | |
| | | | | |
|Respiratory Equipment | | |( | |
|( if yes please specify ) | | | | |
| | |
|Others | |
| | | |
|Remedial Actions Required, As Defined From This Assessment. |To Be Conducted By |Target Date |
| | | |
| | | |
|None | | |
| |
|JOHNSON MATTHEY, CHEMICALS, MANAGEMENT SYSTEM |
| |
|DEVELOPMENT |
|PRODUCT LIFE CYCLE REVIEW CHECKLIST |

Product/ process: Preparation of Pd-XXX

Assessed by: Jo Bloggs
Date: 29th April 2004
| |ISSUE | |
| | |RESPONSE |
| | |Notes |
|1 |What is the function of the product? | |
| | |Coupling catalyst |
|2 |What positive environmental benefits does the product have? Can these| |
| |be increased? |Enables reactions to take place at lower temperatures. No way to |
| | |increase benefit |
|3 |What negative environmental impacts does the product have? Can these | |
| |be reduced? |Contains palladium; no way to reduce impact |
|4 |Can the same function be done in a manner likely to cause less harm to| |
| |the environment? |No |
|5 |What raw materials are used? |Metal salt, RRR and solvent |
|6 |What is the environmental impact of these materials? | |
| | |CO2 emissions and aqueous effluent |
|7 |How can the environmental impact of these raw materials be reduced? | |
| | |No known way |
|8 |Is the product designed to minimise the energy and raw materials | |
| |required to make it? |Yes; the process has been optimised. |
|9 |What is the lifespan of the product? | |
| | |Not known |
|10 |Can the lifespan be extended easily? |No |
|11 |Can the product, components ,raw materials or the product at the end | |
| |of its life be reused/recovered? |It may be possible to recycle the solvent |
|12 |How can reuse/recycling be encouraged in the production process? | |
| | |Segregation of waste streams |
|13 |Could choice of raw material reduce impact during waste disposal? | |
| | |No |
|14 |Can packaging be reduced/reused? |No |
|15 |What wastes/emissions will be generated? | |
| | |Waste solvent |
|16 |What is the environmental impact of these wastes/emissions? Can these|Impact can be reduced by recycling and using as fuel. |
| |be reduced? | |
| |Solvent recycle will be investigated if process is scaled up. |
|ACTIONS TAKEN | |

Standard operating procedure - Production

Products can then be scaled up to full production. After safety trials at 5-litre scale, a process can then be performed at 20-100 litres in a pilot plant. The process can then be moved to full production scale. An example of a full-scale production process for a homogeneous catalyst is shown below:
| |
|JOHNSON MATTHEY |
|QUALITY SYSTEM DOCUMENT |
| |
|PROVISIONAL PRODUCTION PROCESS |
| |
|Product X |
|Product code : XXXXXX |
| |
|Batch size – 100 kg salt |

updated 3/05

Summary

Metal Salt is dissolved in solvent at 80oC and RRR slurried in solvent at rtp is added. The mixture is refluxed for 1 hours then cooled. The product is filtered off, washed (solvent) and dried. MX + RRR → M(RRR)X

Main Equipment Required

Production vessel 1,2
Nutsche Filter
Balance

IMPORTANT INFORMATION

Product

All liquors and solid waste should be retained for recovery of metal.

The product is an orange solid.

Product X is used as a catalyst for coupling reactions.

Safety testing has been carried out by performing the reaction on 5-litre scale first and pilot plant (100l).
Process yield

The yield should be 75 - 100 %, at 95% yield this would give 100kg salt. The rest of the metal is contained in the filtrate (which can be recycled into the next batch / campaign).

Health and Safety (general)

Eye protection as laid down by the Departmental Approved Safe Practice must be worn.
Gloves must be worn throughout the process (see 3.4).

Health and Safety (process specific)

The information on chemicals, given below, is a general summary. For more detailed facts refer to the relevant Material Safety Data Sheets.

Metal Salt is HARMFUL. It contains free acid and can damage skin and mucous membranes. Wear rubber gloves and appropriate eye protection when handling this material.

Solvent is HIGHLY FLAMMABLE (flash point 6°C) and TOXIC. The recommended UK exposure limits are short-term (10 min TWA value) 60ppm (105mg/m3) and long-term (8hr TWA value) 40ppm (70mg/m3). It should only be handled under extraction.

RRR is HARMFUL.

Product is UNKNOWN; treat as HARMFUL.

Gloves and appropriate eye protection must be worn at all times during processing.

Emissions relevant to Fine Chemicals EPA authorisations

Solvent is emitted at varying levels during the process. This must be removed using a scrubbed draft and the standard controls in the Plant.

Scrubbing requirements

Reaction run under scrubbed draft.

Effluent treatment

Product solvent filtrate may be reused in subsequent batches. Otherwise, the Product solvent filtrate can be transferred to the still, where it is distilled. The residue is absorbed on sawdust and sent for metal recovery.

Raw Materials

|Material |Code |Quantity |
|Metal salt |XXX |80kg |
|Solvent |XXX |1000 l (780kg) |
|RRR |XXX |20 kg |

The density of solvent is 0.786. This figure can also be used for the solvent filtrate.

Method - Process flow sheet

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Method details

1. Add 80 kg (salt) Metal slat to vessel 1 using Tornado helmet.

2. Vacuum cycle x3 under nitrogen. Leave under absorbed draft/ nitrogen.

3. Pump 550kg solvent into vessel 1 under nitrogen and stir.

4. Heat to XXoC.

5. Maintain at XXoC for 1 hour until all Metal salt dissolved.

6. Check and confirm all Metal salt has dissolved

7. Add the 20kg RRR to vessel 2 using Tornado helmet.

8. Vacuum cycle x3 under nitrogen. Leave under absorbed draft/ nitrogen.

9. Pump 75kg solvent into vessel 2 under nitrogen and stir.

10. Pump the RRR slurry from Vessel 2 into vessel 1 (slowly).

11. Pump 8kg solvent into vessel 2 under nitrogen and stir.

12. Pump the washings from Vessel 2 into vessel 1.

13. Heat Vessel 1 to XXoC and maintain for 1hrs.

14. Cool the mixture to less than XXoC.

15. Filter off the product on the Nutsche filter (under nitrogen)

16. Pump 10kg solvent into Vs 1. Wash onto product Nutsche filter.

17. Dry on Nutsche overnight at XXoC under vacuum with nitrogen bleed.

18. Analyse the Product for purity

TECHNICAL NOTES

The product is not air-sensitive.

Written by: Jo Bloggs 04/04

Updated Joanne Bloggs 03/05

Checked by:

Authorised by:................................................... Date: ................. Production

.................................................. Date: .................

Quality

HAZOP

The major Risk Assessment procedure for scale up pilot and full production is called a HAZOP (Hazardous Operations). In this process a team of experts will consider each operation step separately and ask a set of questions. These questions encourage the participants to consider all the possible scenarios that could occur and the associated hazards of those scenarios. In this way, the risks are identified and minimised. The team normally comprises the development chemist, a technician from the plant, an engineer and a production manager.

The guide words for the HAZOP are:

None, More of, Less Of, Part of, More than, Other.

For example, for a step of addition of a reagent the questions generated could be:
None - what if no reagent was added?
More of - what if more of the reagent was added than was desired?
Less of - what if less of the reagent was added than was desired?
Part of - what if only part of the reagent was added?
More than - what if something more than the reagent was added e.g. common impurities?
Other - what if something other than the reagent was added e.g. other common reagents that could be mistaken for the desired reagent?

Typical cost structure per kilo of homogeneous catalysts

% of Total cost Process costs: Metal Salt 5% Ligand 25% Works costs: Plant Maintenance 10% Payroll 10% Other 10%

Distribution 5% Research and Development 10% Indirect costs (including Sales, Admin) 25%

Total 100.0%

Other Information - use the Website!

Log on to the Johnson Matthey website site to look at:
1. Environmental, Health and Safety – under ‘Corporate Responsibility’
This will give; - Safety and health policy - Corporate Social Responsibility (CSR) Review 2003 or 2004 - Employment policies - Business Integrity and Ethics Policy Statement - Environment policy - ISO 14001
2. Check out ‘Careers’ for details on jobs and descriptions of types of jobs available.
3. Check out ‘Media’ for recent news at JM.
Practical Work

In developing process, there is always a degree of 'optimisation'. The practical assignment gives an example of one such situation that is common in the scale up of homogeneous catalysts. In this example, the valuable product you want is contaminated with an impurity. You manage to find a solvent that will dissolve your product but not the impurity. However, the solvent is expensive and you are worried over energy costs and environmental impact of the process you have to run. So you perform 3 experiments to try and determine which process is best in economic and environmental terms.
In the practical experiment, the 'valuable product' is potassium nitrate. This is a common salt - it has been around for a long time - formerly known as 'Salt-petre', it was one of the ingredients of gunpowder!! The impurity is sand (very insoluble!) and the solvent is water (yes its not very expensive in reality, but its safe and will dissolve potassium nitrate).

Some useful information:

Solubility of Potassium nitrate in water at various temperatures:

Temperature (oC) Solubility (grams per 100ml)

0 13.3 20 31.6 40 63.9 60 110.0 80 169.0

Separation of potassium nitrate and sand using a solvent (water) - comparison of three methods

1. SCOPE

The purpose of this experiment to find the best route to separate the desired product (potassium nitrate) from an impurity (sand). The best (optimised) route will be considered.

2. DEFINITIONS

2.1 Potassium nitrate, KNO3

3. PRINCIPLE

The desired product (potassium nitrate) is contaminated with an impurity (sand). The experiment will use the fact that potassium nitrate is soluble in water and sand is insoluble to separate the two components. Three different methods will be used. Method 1 will involve dissolving the potassium nitrate with water at room temperature (rtp), filtering off the sand and then evaporating off approx. 2/3 of the water at 100oC, cooling and filtering the salt. Method 2 will involve dissolving the potassium nitrate in water at 60oC, filtering off the sand whilst hot, cooling the solution to rtp and filtering off the salt. Method 3 will repeat method 2 but use the final water solution (mother liquor) obtained from method 2 in place of the fresh water. It will then be considered which method would be best to use in an industrial setting.
4. REAGENTS

4.1 Potassium nitrate / sand mix 1:1 ww (i.e. 1:1 ratio of each component by weight)

4.2 Water

5. APPARATUS

5.1 Thermometer

5.2 Buchner flask, Buchner funnel and filter paper

5.3 4-place analytical balance

5.4 Normal laboratory glassware

6. PROCEDURE

Method 1

6.1 Accurately weigh 120g of the potassium nitrate / sand mixture into a 250-ml beaker.

6.2 Add 150ml of distilled water (measure in a measuring cylinder).

6.3 Stir for 5 mins.

6.4 Filter the mixture through the filter paper/ Buchner funnel into a 250ml Buchner flask.

6.5 Transfer solution into a beaker and place on a hot plate/ stirrer, add a stirrer bar and heat slowly to boiling (~100oC). Boil until approx. 2/3rds (100ml) has evaporated.

6.6 Allow to cool to room temp, stirring every few minutes. Filter the resulting suspension.

6.7 Scrape the salt into a pre-weighed 50 ml beaker. Dry in an oven overnight. Weigh the beaker containing the dry salt. Record the amount of salt obtained.

Method 2

6.1 Accurately weigh 120g of the potassium nitrate / sand mixture into a 250-ml beaker.

6.2 Add 50ml of distilled water (measure in a measuring cylinder).

6.3 Place the beaker flask on a hot plate/ stirrer, add a stirrer bar and heat to between 58 oC and 62oC with stirring.

6.4 Filter the mixture whilst still hot (~60oC) through the filter paper/ Buchner funnel into a 250ml Buchner flask.

6.5 Allow to cool to room temp, stirring every few minutes. Filter the resulting suspension.

6.6 Scrape the salt into a pre-weighed 50 ml beaker. Dry in an oven overnight. Weigh the beaker containing the dry salt. Record the amount of salt obtained.

Method 3

6.1 Accurately weigh 120g of the potassium nitrate / sand mixture into a 250-ml beaker.

6.2 Add ~50ml of the final filtrate (mother liquor) from method 2

6.3 Place the beaker flask on a hot plate/ stirrer, add a stirrer bar and heat to between 58 oC and 62oC.

6.4 Filter the mixture whilst still hot (~60oC) through the filter paper/ Buchner funnel into a 250ml Buchner flask.

6.5 Allow to cool to room temp, stirring every few minutes. Filter the resulting suspension.

6.6 Scrape the salt into a pre-weighed 50 ml beaker. Dry in an oven overnight. Weigh the beaker containing the dry salt. Record the amount of salt obtained.

7. CALCULATION

The original mixture was 1:1 potassium nitrate:sand. So 120g of mixture would contain 60g of potassium nitrate. So the maximum amount of potassium nitrate you could have recovered is 60g. So if X is the amount of salt you recovered, the yield in % is: X x 100 60 This will give you a yield for each method.

8. Comparison and consideration

Key points to consider are: • Evolution of gas • Use of energy (heat) • Why not evaporate all the water? (consider a production scale vessel (plant)) • Recycle possibilities • Total amount of reagents (i.e. water) used

-----------------------

IVA CASE STUDY

Issued September 2005
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