FIELD: chemistry.
SUBSTANCE: invention relates to an integrated method of producing jatropha methyl ester (JME) and by-products from encapsulated seeds of jatropha containing 1.06% of free fatty acids (FFA), said method comprising the steps of: (i) mechanically removing the shells of the jatropha seeds in a shell-removal machine to obtain jatropha shells and jatropha seeds; (ii) squeezing out jatropha oil, obtaining jatropha oil cake containing 4-6% nitrogen and waste oil sludge from the jatropha seeds obtained at step (i), using an oil press; (iii) neutralising jatropha oil obtained at step (ii) with a base; (iv) transesterifying one part of neutralised jatropha oil obtained at step (iii) with an alcohol and a base with stirring for 10-20 minutes and separating the crude glycerol layer GL1 and crude jatropha methyl ester (JME); (v) washing crude JME obtained at step (iv) three times with the pure glycerol layer to separate three impure glycerol layers GL2, GL3 and GL4 containing methanol and KOH to obtain glycerol-washed JME (JME-G3W); (vi) purifying JME-G3W obtained at step (v) to remove alkali metal impurities; (vii) treating part of remaining neutralised oil obtained at step (iii) with glycerol layers GL5 (GL1+GL2+GL3) obtained at steps (iv) and (v) to obtain JME and glycerol layer GL6; (viii) separating JME and glycerol layer GL6 obtained at step (vii); (ix) treating glycerol layer GL6 obtained at step (viii) with remaining part of neutralised oil for removing methanol to obtain JME and glycerol layer GL7; (x) separating JME and glycerol layer GL7 obtained at step (ix); (xi) using glycerol layer GL7 as obtained at step (x) directly for the production of polyhydroxyalkanoates (PHAs) or for the neutralisation of alkali with sulphuric acid to obtain pure glycerol and still bottom GL8; (xii) combining JME-G3W obtained at step (vi) and JME obtained at steps (viii) and (x) to obtain combined methyl ester; and (xiii) transesterifying combined methyl ester obtained at step (xii) with methanolic KOH to obtain pure jatropha methyl ester (biodiesel) having total glycerol content of 0.088% and free glycerol of 0.005%. The invention also relates to an integrated method of producing JME and byproducts from jatropha seeds, the method including steps of: a) carrying out said steps (i) and (ii); b) briquetting the jatropha shells obtained at step (i) in a briquetting machine with the addition of waste oil sludge obtained at step (ii) to obtain jatropha briquettes with density of 1.05-1.10 g/cm3 as a by-product; c) hydrolysing jatropha oil cake having 4-6% nitrogen obtained at step (ii) with H3PO4, H2SO4 to obtain jatropha oil cake hydrolysate (JOCH) as a by-product; and d) carrying out steps (iii)-(xiii).
EFFECT: invention provides a simpler and more energy-efficient method of producing fatty acid methyl ester (biodiesel) which is integrated with beneficial recycling of by-products such as seed shells, deoiled cake and crude glycerol stream.
13 cl, 7 dwg, 7 tbl, 13 ex
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Authors
Dates
2014-09-20—Published
2010-03-29—Filed