paperChain project - Circular case 4 - Emil Thalen (RISE Processum) & Erik Thalen (SEKAB)

This project has received funding from the European Union’s Horizon 2020 research and innovation Programme under grant agreement N° 730305
CC4: FROM FIBRE REJECTS TO ETHANOL AND CHEMICAL DERIVATIVES.

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Valorisation of fibre sludge waste generated by the pulp industry
as secondary raw materials for the production of ethanol
derivatives for the chemical industry (e.g. paints, pharmaceuticals,
agriculture and plastics)

Domsjö Fabriker Biorefinery – From log to bale
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DD-wash
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Fibre sludge - Challenges
• Side product from screening during pulping
process
• Consists of uncooked or partially cooked fibre
• High moisture content
• Low energy content
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Circular Case 4, Chemical Sector
activities
• Ethanol production from fiber rejects
• Ethyl chloride from ethanol
• Chlor-alkali process
• Wood based cellulose for cellulose ether production
• Evaluation of wood based cellulose in Bermocoll® production
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Ethanol Fermentation, PFD

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Hydrolysis/Fermentation of Fiber Rejects

Ethyl Chloride production
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Ethyl Chloride Pilot Plant
• Construction of pilot plant.
• Programming of control system
• Risk assessment
• Successful trials for production of ethyl chloride
• Some process optimization made
• Flow rate
• Ratio of HCl:Ethanol
• Temperature
• Distillation trials
• Catalyst evaluation
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Synthesis of ethyl chloride, PFD
Simplified process diagram
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P&ID

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Summary of trial runs
𝐻𝐶𝑙 + 𝐸𝑡ℎ𝑎𝑛𝑜𝑙
!"#"$%&#'()"#
𝐸𝑡ℎ𝑦𝑙 𝑐ℎ𝑙𝑜𝑟𝑖𝑑𝑒 + 𝑊𝑎𝑡𝑒𝑟 (+𝐷𝑖𝑒𝑡ℎ𝑦𝑙 𝑒𝑡ℎ𝑒𝑟)
Diethyl ether is undesirable but small amounts acceptable
Focus has been on reaction and not distillation.
Work started with specialized catalyst
Commercial catalyst proven successful
High conversion 91 % of ethanol and selectivity of 98 % achieved with commercially available catalyst.

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Chlor-alkali process
• Concentrated HCl in solution is to expensive
• HCl supply for ethyl chloride production could be
achieved using different technologies
• Dry HCl may be produced using a chlor-alkali
process via combustion of Cl2 and H2
• Membrane based chlor-alkali fully mature
technique
• Theoretical at this point in the project
• May be one of the keys to long term profitability
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Pulp for cellulose ethers
First stage – Pilot scale investigation
• Pilot scale test run at MoRe Research
• Investigate suitability of Domsjö pulp in cellulose ether trials
- pilot testing at Nouryon
• Full scale trials at Domsjö Fabriker, 7 cooks in total
• Different conditions used in the consecutive cooks
Pulp viscosity is important for cellulose ethers. Other variables that are also important to follow are
brightness, kappa number, and hemicelluloses.
Photo 1. Wood Chips from pilot cooking trial

Cellulose Ether Production
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Nouryon pilot plant
Cellulose grinding
Reaction
Neutralization of
surplus lye
De-watering
Centrifugation
Wet-grinding Drying
Dry-grinding
Sieving Product
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Evaluation of Aditya Birla cellulose at
Nouryon pilot plant
• Trials has been done with Aditya Birla cellulose at Nouryon pilot plant
• Product is evaluated dissolved in a water solution at 1% concentration of the cellulose ether
Results:
Conclusion:
Aditya Birla cellulose need to be improved further, with regards to gel content (insolubles). Viscosity (cP) and transparency are
borderline properties that needs to monitored carefully.
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Summary
• Ethanol production
• Knot rejects and fines (fiber rejects) successfully hydrolysed to a monomeric sugar stream
• Sugar stream fermented to ethanol
• Ethyl Chloride production
• Demonstration rig constructed
• Safety assessment performed
• Multiple test runs at different feed rates and molar ratios of HCl/EtOH
• Different catalysts evaluated
• Multiple 24 h test runs to test stability of process
• Cellulose for cellulose ether production
• Pilot scale trials to evaluate conditions to be used in scaling up
• Seven full scale trials performed to evaluate new cooking conditions
• Samples for analysis and production tests from full scale tests
• Bermocoll pilot production
• Wood based cellulose used for Bermocoll production
• Evaluation of the produced Bermcoll
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Business case
Core issues
1. We have a company that is looking for a solution to use a residual
product from the pulp production in a good way. Domsjö Fabriker
2. We have a company that wants to expand its product portfolio with
sustainable chemicals. Sekab BioFuels & Chemicals
3. We have a company that wants to increase the proportion of sustainable
raw materials in its production of cellulose derivatives. Nouryon
The Paperchain project has provided an opportunity to analyze the core
issues the companies had in this case and see how the circular economy
can be developed within the industrial area in Domsjö. Coordination of
this work has been handled by RISE Processum.

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Overall mass balance for business case

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Dissolving pulp
Within the project, the possibilities have been investigated of using the quality
of viscose pulp that Domsjö Fabriker manufactures as a raw material for
Nouryon. It has been found that this is possible from technical point of view if
certain adjustments are made in the manufacturing process. However, this
entails costs which mean that at present the raw material from Domsjö
Fabriker becomes too expensive compared with the existing raw material flow
to Nouryon.

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Enzymatic hydrolysis
Hydrolyzing residues in the form of wood chips is a well-known process. On the
other hand, using fiber reject had not previously been tested before the
Paperchain project. During the project, it has been investigated what such a
process should look like and what process data it has.

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Ethyl chloride production
A relatively extensive effort has been made to evaluate suitable processes,
including raw materials, catalyst and process equipment, in order to be
able to produce ethyl chloride from bio-based residues, fiber reject, from
Aditya Birla's pulp mill.
The evaluations were made in a pilot built at RISE Processum. The results
from the tests have shown that from a process engineering point of view it
should be possible to produce ethyl chloride from dry HCl and bio-based
ethanol from fiber reject in a full-scale plant.

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Electrolysis Plant
The raw material for the production of ethyl chloride is ethanol and HCL. At a
relatively early stage of the project, it was found that the use of hydrochloric
acid, HCl dissolved in water, as a raw material for the production of ethyl
chloride is not a good solution from both a technical and economic point of
view. The water contributes to high energy consumption in the process
The project evaluated different ways of accessing dry HCl as a raw material.
The answer was that in order to get a good solution, an electrolysis plant must
be built where salt (sodium chloride) is the raw material. The finesse of this
process is also that sodium hydroxide is formed as a by-product, which both
Aditya Birla and Nouryon need in their processes.

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1
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1. Fiber reject
2. Enzymatic hydrolysis/Ethanol plant
(Existing ethanol plant, can be supplemented with
enzymatic hydrolysis.)
3. Harbour
(Salt deliveries to a new electrolysis plant.)
4. Electrolysis plant
(Existing building. Today unused and where a new
electrolysis plant could be built.)
5. Ethyl chloride production
(Existing production of ethanol derivatives that can
be supplemented with a process for ethyl chloride
production.)
6. Cellulose ethers production
(Existing plant)
Overview of a potential full scale implementation of CC-4

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Conclusions
- During the project, business opportunities connected to circular economy
were discovered that did not exist in our minds before the project began.
- The realization that an electrolysis plant would be needed for the production
of dry HCl as a raw material for the production of ethyl chloride gave the
advantage of the by-product sodium hydroxide which would also improve
the circular economy in Domsjö industrial area.
- Nourion's need for ethyl chloride for its operations may be somewhat small in
order to obtain financial viability in a full-scale project. However, there is the
possibility of expanding a full-scale project to also produce methyl chloride
from methanol and HCl in the same plants. This would in principle mean that
the capacity for HCl production would have to be doubled and both ethyl
chloride and methyl chloride could be produced in the same plant. This
would significantly increase the opportunities for financial sustainability in a
full-scale project.

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Conclusions
- A full-scale project described here would also receive benefits from a
logistics point of view (safety and environmental point of view). Transport of
dangerous goods, ethyl chloride and perhaps also methyl chloride, by rail to
Nouryon in the Domsjö industrial area would be replaced by salt being
transported by boat to the same place. The volume of transports of sodium
hydroxide by truck to the industrial area would also be reduced.
- As the need for ethyl chloride is limited in the global market, there is a major
issue to be resolved before a full-scale project can be started. Is Nouryon
prepared to commit to buy its need for ethyl chloride, and perhaps also
methyl chloride, from new chemical plants in the Domsjö industrial area?

paperChain project - Circular case 4 - Emil Thalen (RISE Processum) & Erik Thalen (SEKAB)

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paperChain project - Circular case 4 - Emil Thalen (RISE Processum) & Erik Thalen (SEKAB)