298 94 307/02 Untersuchungen zum Stand der Umsetzung des ...

298 94 307/02 Untersuchungen zum Stand der Umsetzung des ... 298 94 307/02 Untersuchungen zum Stand der Umsetzung des ...

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Teil 3 Seite 6-13 tissue from the bone. The contents of the degreasing vessel are separated to give hard bone, sinew (soft bone) and liquids containing tallow and water. The hard bone is washed using hot water, to give a final moisture content of around 10 %. The sinew is pressed to remove fat and water before being dried with the hard bone to give a final moisture content of 14 %. Drying at 85 °C takes 45 minutes. The dried bone and sinew are sieved at 2 mm and 5 mm to give bone meal (< 2 mm fraction), intermediate bone pieces (2 - 5 mm fraction) and degreased gelatine bone/sinew (> 5 mm fraction). The tallow/water mix is separated using centrifuges to give purified tallow and process water. The liquids are maintained at a temperature of 85 °C for 30 minutes during separa- tion. Fine solids removed from the liquid during separation, together with fine solids from the pressing of the sinew are combined and dried to give a moisture content typically < 10 %. The product temperature achieved in the drier is around 110 °C for at least 45 minutes. Cyclones are used to remove the air and to separate the fines from the larger particles destined for the gelatine manufacture. Bone chips are graded by density, using a hydrocyclone, because higher density bones require more processing than low density bones, both to demineralise and to extract the gelatine. They are then dried in a band oven, with a starting air temperature of around 350 °C and an exit temperature of 150 °C. The chips are only in contact with the hot air for a short time and they are also cooled by the evaporation of the water, so their tem- perature will not normally exceed 85 ºC. The drying time varies from 20 – 60 minutes. The dried bones are then classified by size, using a densimetry table, comprising an in- clined screen with an upward air-draught on to which the bone chips are dropped. The amount of dried degreased bone chips obtained from 1 kg of bone is usually about 200 g. If hides or skins are used this pretreatment stage is not required. B Demineralisation/acidulation The demineralisation process is the removal of the inorganic component, which com- prises mainly natural phosphates and calcium carbonate. The defatted bones are placed in a strong hydrochloric or sulphuric acid solution at pH 1 - 2, where the tricalcium phos- phate is converted into the soluble monocalcium salt, which is run off in solution, for later conversion to dicalcium phosphate, soluble calcium chloride and carbon dioxide. The chemical reaction with hydrochloric acid is shown. Ca3(PO4)2 + 4 HCl -> Ca(H2PO4)2 + 2 CaCl2 CaCO3 + 2 HCl -> CaCl2 + H2O + CO2

Teil 3 Seite 6-14 For 1000 kg of degreased bone, containing 8 % water and having 63 % comprising 7 % CaCO3 and 56 % Ca3(PO4)2, approximately 7700 litres of 4 % HCl is required, for com- plete conversion. The solid “ossein” residue is used in the gelatine manufacture process. This process may take several days depending on the nature, size and density of the raw material. Several pits, e.g., six, sit in series, containing ossein, at various stages in the process. Fresh acid with a concentration of 3.5 % hydrochloric acid, is added to the pit containing the ossein which has been treated for longest, after about one day this acid is pumped to the pit containing the second oldest ossein, whilst the acid from this is pumped to the pit containing the third oldest ossein. The process continues by this batch counter-current action. In this way the “newest” liquor, with the highest acid concentration and lowest concentration of monocalcium salt is extracting the salt from the ossein with the lowest available yield and the “oldest” liquor, with the lowest acid concentration, i.e., about 0.5 %, is extracting the salt from the ossein which has most salt to give up. The process can be helped by air agitation. The process is illustrated in Figure 6.1 Each reactor tank in the process may typically contain a batch of 20 – 50 tonnes of bone chips, but smaller tanks may be used. The tank height may be about 7 metres and the diameter about 3.5 metres. New reactors are usually made from plastic coated steel. For a system with 4 reactor vessels of which every day one reactor is emptied and one is filled, 200 tonnes of degreased bone chips can be treated in four days, in 4 batches of 50 tonnes. To demineralise these approximately 1540000 litres of 4 % hydrochloric acid is required. When the efficiency of the process is approximately 90 %, this becomes ap- proximately 1710000 litres in four days or about 17800 litres/hour.

Teil 3 Seite 6-14<br />

For 1000 kg of degreased bone, containing 8 % water and having 63 % comprising 7 %<br />

CaCO3 and 56 % Ca3(PO4)2, approximately 7700 litres of 4 % HCl is required, for com-<br />

plete conversion.<br />

The solid “ossein” residue is used in the gelatine manufacture process. This process<br />

may take several days depending on the nature, size and density of the raw material.<br />

Several pits, e.g., six, sit in series, containing ossein, at various stages in the process.<br />

Fresh acid with a concentration of 3.5 % hydrochloric acid, is added to the pit containing<br />

the ossein which has been treated for longest, after about one day this acid is pumped to<br />

the pit containing the second ol<strong>des</strong>t ossein, whilst the acid from this is pumped to the pit<br />

containing the third ol<strong>des</strong>t ossein. The process continues by this batch counter-current<br />

action. In this way the “newest” liquor, with the highest acid concentration and lowest<br />

concentration of monocalcium salt is extracting the salt from the ossein with the lowest<br />

available yield and the “ol<strong>des</strong>t” liquor, with the lowest acid concentration, i.e., about 0.5 %,<br />

is extracting the salt from the ossein which has most salt to give up. The process can be<br />

helped by air agitation. The process is illustrated in Figure 6.1<br />

Each reactor tank in the process may typically contain a batch of 20 – 50 tonnes of bone<br />

chips, but smaller tanks may be used. The tank height may be about 7 metres and the<br />

diameter about 3.5 metres. New reactors are usually made from plastic coated steel. For<br />

a system with 4 reactor vessels of which every day one reactor is emptied and one is<br />

filled, 200 tonnes of degreased bone chips can be treated in four days, in 4 batches of<br />

50 tonnes. To demineralise these approximately 1540000 litres of 4 % hydrochloric acid<br />

is required. When the efficiency of the process is approximately 90 %, this becomes ap-<br />

proximately 1710000 litres in four days or about 17800 litres/hour.

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