FAIR-CT96-3130 Production of environmentally-friendly surfactants from agricultural coproducts of large-scale farming: agrisurfactants

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Agricultural Residues : Agriculture : Detergents : FAIR Area 1.2 - Green Chemicals and Polymers Chain

	Proposal No:	FAIR-CT96-3130
	Date Prepared:	May 1999
	Source:	Second Progress Meeting Report

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Second Progress Meeting Report

The report of the meeting held in Malle (Belgium) on the 3rd of April 1998 was agreed by each participant.

During this meeting held at Santomera and organised by Riverbend, each participant described the work carried out for the last six months, and the points concerning the setting-up of the pilot plant process, the design of the screw press, the comparison between demineralisation by ion-exchange and electrodialysis, the improvement of the chemistry process at the pilot scale, the evaluation of the functional properties of the surfactants as well as the macroeconomic evaluation flows modelisation and investment appraisal has been discussed in details.

Opening and welcome

Mr Cremades general manager of Riverbend España welcomed the participants. Mr Andreu (technical manager) gave a short introduction on structure of Riverbend, the markets they are involved in, and their crucial issues of citrus peels (60 000 tons a year).
Philippe Mathaly welcomed the participants and thanked Riverbend for organising the meeting.

General remarks

All participants were asked to send their intermediate reports in due time. Reports could not be compiled before the meeting. It was remembered that the project was at the mid-term and that it was the opportunity to evaluate the work of all of us according to what was expected in the technical annex.
Each partner was asked to supply their individual cost statements in order to submit them to the EC.

Progress report

Riverbend (Juan Antonio Andreu) reported on:
The trials they done at Riverbend aimed at comparing the behaviour of the fresh citrus peels as compared to the frozen peels. They shown that the grinding of citrus peels played an important role allowing to work at a higher dry matter, and then decreasing the amount of water to be evaporated further. This treatment seemed to be also efficient regarding the enzymatic hydrolysis of the pectin. They reduce the hydrolysis time from 10 hours to 6 hours. They confirmed the demineralisation steps already optimised by A.R.D on frozen citrus peels. They shown that the elution of the galacturinic acid on the anionic resin could be performed with only l,2 BV of ammonia at 1,5%. They obtained also very pure products (more than 80 % of galacturonic acid on Dry matter) when eluting the resin with ammonia.
They shown that it should certainly be possible to simplify the head of the process by replacing the decanting and centrifugation by one filter-press step. In that case we will save time, energy and overall water. Nevertheless the flow rate are low, the cakes seem to be difficult to built, and we have to compare the economic advantage of this technology as compare to the in place technology.

A.R.D (Philippe Mathaly) reported on:
The comparison between Demineralisation by ion-exchange and by electrodialysis. The life time of the resins was assessed by repeating feeding and washing cycles on the resins. Results showed that one can run 10 feeding cycles on the resins (with a regeneration step between each cycle) without modifying the behaviour of the resins (capacity to retain ions from hydrolysed juices). Nevertheless, we shown that a decontamination cycle (NaOH 4%) was required after 10 feeding cycles in order to release some specific sites of the resin which could not be regenerated by sulphuric acid. This specific sites are completely saturated after 6 passages on the resin, then the ion retention capacity of the resin does not change as quickly as the six first passes. The complete cycles of regeneration-decontamination was optimised and Validated at the pilot plant scale (columns of 200 litres capacity).
Electrodialysis was also studied. The advantage of using this technology as compare to ion-exchange is that in that case regeneration is not needed and as a consequence, no effluents are generated. We studied the behaviour of the membranes after several passes of products (capacity of separating ions and fouling index).
Results showed that membranes did not fouled up according to time, after a small washing cycle membranes recovered their fahradic yield (capacity to separate ions through the membrane). Nevertheless, we shown that it was absolutely necessary to maintain the ionic strength in the brine compartment by a constant dilution in order to avoid a decreasing of the performances of the electrodialyser due to the increasing of the ionic strength.
Flow rates of the product through the membranes were quite interesting, as we reach around 1301/h/m2, for a 80 % demineralisation yield.
Nevertheless we shown that it was not possible to demineralize more than 80 % of the products by electrodialysis, nor declorize them, which is a serious disadvantage of the technology.

A.R.D (Jean Noël Bertho) reported on:
The optimisation of the glycoxidation reaction. Several trials have been performed at the pilot plant level. Corrosion problems were discovered and worked out by using enamelled reactors, teflon pipes and a titanium heat exchanger.
Butyl glycosides synthesis was optimised at the pilot plant level as well as the transglycosylation. It was difficult to maintain a regular temperature during transglycosylation mainly due to a bad sizing of the butyl alcohol condenser. A new one has been bought, it will be tested soon.
The sizing of the thin layer evaporator has been done in collaboration with industrial manufacturers. Preliminary trials have been performed on industrial devices, they shown that they were not problem of viscosity, evaporation could be realised in one stage, necessary vacuum is about 4 mbars and temperature requirement is about 200°C. Such device is being installed in our facilities in order to optimise this unit operation.

ATLAS-STORD (Mr Steinar Jacobsen) reported on:
Press tests in AMSE (lab. piston press) of acidified sugar beet pulps, acidified wheat straw, and acidified wheat bran. These preliminary tests were needed in order to design as well as possible the new set of spindles for the pilot plant screw-press.
The results show that wheat bran can be pressed at moderate pressure, but as high content of dry solids in the press liquid than straw (4%). Sugar beet pulps did not give so optimistic results, neither regarding press liquid nor presscake content of dry solid when using a non optimised design of screw.
Products were confirmed to be able to be pressed on a twin screw press. The new set of spindles was designed according to these trials, and sent to A.R.D for pilot plant trials.

Ecover (Mr Malaisse) reported on:
The evaluation of functional properties of new samples send by A.R.D with different combinations of carbon chain lengths . Physical and chemical parameters were screened, Performance and foam behaviour along the established test protocols. No problems cause to pH differences anymore.
It was decided to continue with about a dozen combinations, and to make a final choice only at he finish of the project. Differences between the samples were small, as the variations of carbon chains were small as well. The results of the tests were discussed within the scientific team and laid out for discussion new Sapromat device for ultimate degradation testing was delivered. Several tests cycles were run.

Faculty of Gembloux (Mss Druand) reported on:
The research of the supply side (raw material, transformation industry). Production of beet, bran, and citrus in the EC (areas, average yield, coproduct production, current prices) were discussed in order to define the most interesting areas for raw materials production as well as for erecting a production plant. The environmental weight of these raw materials and the availability of natural fatty alcohols were also considered. The sociological aspects will have to be studied at later date when the localisation of the plant has been decided. Flow modelisations of the fractionation of wheat brans process has been studied as well as the chemical part.

Financial Budget

It was asked the partners to supply the coordinator with a cost statement for the first year.

Focus on the Six Next Months:

It was decided to plan several weeks for pressing trials in A.R.D facilities with the new set of spindles designed by Atlas-Stord. These trials will be realised in January.

It is necessary to continue to supply Ecover with different surfactant samples (different chain length, as well as a range of anionic surfactants), in order to start the formulation trials in January. Moreover biodegradability and ecotoxicologic tests must start also in January.

All the costs (devices, steam, electricity, raw material, etc.) must be supplied to Gembloux before the end of the year. This will allow to start the study of the investment of a plant having 3 thousand tons capacity on one hand, and 50 thousand tons capacity on the other hand. In that way it has been planned to supply Gembloux with the most up to date flow-sheet of each process before the end of December, including the number of people expected to be necessary for running the plant.

Riverbend has planned to continuos working on pressing with Atlas-Stord, as well as focus is attention on the valorisation of the citrus peel process co-products.

The coordinator thanked the participants for coming and Riverbend España for the good organization.

The next meeting has been scheduled on April 9th, it will be held at the Faculty of Gembloux.