发明名称 Process for producing high-yield biodiesel applying high acidity triglycerides with generation of glycerin 90% free of salts
摘要 Process for producing high-yield biodiesel applying high acidity triglycerides with generation of glycerin 90% free of salts starting from fatty lower cost fatty material allied with an esterification and innovative extraction process that generates a further value, more specifically for the production of biodiesel.
申请公布号 US9090845(B2) 申请公布日期 2015.07.28
申请号 US201313748281 申请日期 2013.01.23
申请人 GLYCEROSOLUTION QUIMICA LTDA 发明人 Nishiama Hiromu;Cazzolato Silvio Antonio;Santos Silva Matheus Marchi dos
分类号 C10L1/18;C11C3/04;C10L1/02;C11C3/10 主分类号 C10L1/18
代理机构 Stites & Harbison, PLLC. 代理人 Schulman, Esq. B. Aaron;Stites & Harbison, PLLC.
主权项 1. A process for producing high-yield biodiesel applying high acidity triglycerides with generation of glycerin 90% free of salts, the process comprising the steps of: (a) providing an esterified material with an acidity index of about 30 mgKOH/g; (b) adding methanol at a ratio of from 20% to 40% mass/mass and a catalyst MW at a ratio of from 0.1% to 0.5% mass/mass to the esterified material at a temperature ranging from 45° C to 65° C, providing a mixture of esterified material and methanol; stirring the mixture of esterified material and methanol until the acidity index reaches a value less than 2 mgKOH/g; for a period of time from 60 minutes to 240 minutes; (c) stopping the stirring for 30 minutes, allowing for the mixture of esterified material and methanol to separate, wherein a first upper layer is dark and is predominantly composed of methanol, water and coloring agents; and a first lower layer is light brown and primarily esterified fatty material and solubilized methanol; (d) transesterificating the first lower layer, wherein methanol is added to the mixture of esterified fatty material and methanol, providing a mixture of esterified fatty material and methanol with added methanol to correct the esterified methanol ratio to 15% mass/mass; heating the mixture of esterified material and methanol with added methanol to a temperature of from 50° C. to 60° C.; adding sodium methylate; providing a mixture of esterified material and methanol with added methanol and sodium methylate; and containing the mixture of esterified material and methanol with added methanol and sodium methylate in a stirring and heating container until a mixed glycerin reaches a value lower than 0.25% mass/mass; (e) stopping the stirring for 30 minutes, allowing for the mixture of esterified material and methanol with added methanol and sodium methylate to separate, wherein a second upper layer is of biodiesel with 98% conversion and a second lower layer is of crude glycerin, from 50% to 65% glycerol, containing free methanol, fatty material selected from the group consisting of: soaps, esters, glycerides, moisture and mixtures thereof; distilling the second lower layer to remove the free methanol; (f) treating the crude glycerin originating from steps (b) to (e); (g) adding fatty acid to the second upper layer mixture of esterified material and methanol with added methanol and sodium methylate, with an acidity index ranging from 80 mgKOH/g to 210 mgKOH/g, at a temperature ranging from of 60° C. to 95° C. already being stirred; and adding the crude glycerin, stirring and maintaining the same reaction conditions for 30 minutes; (h) stopping the stirring for 30 minutes, allowing for the second upper layer mixture of esterified material and methanol with added methanol and sodium methylate and fatty acid and crude glycerin to separate, wherein a third upper layer of the second upper layer mixture of terified material and methanol with added methanol and sodium methylate and fatty acid and crude glycerin is fatty material containing soap, ester, glycerides, and residual glycerol; and a third lower layer is glycerin about 95% glycerol, containing residue soap and moisture, the glycerol content depending on the water content and residue free methanol in the crude glycerin; (i) the third upper layer undergoing a split of soap so that all the fatty acid is recovered, by using an a first additive solution to reduce the effect of sulfuric acid on the formation of sulfonates and other agents that confers color to the recovered fatty layer; (j) adding the third upper layer to a stirring and heating container at a temperature ranging from 50° C. to at 80° C.; and then adding a second additive solution containing a non-ionic surfactant at 1% and at room temperature; and slowly adding sulfuric acid 98%, hydrolyzing the soap, and (k) stopping the stirring for 30 minutes at a temperature of 80° C., allowing for the third upper layer of the mixture of esterified material and methanol with added methanol and sodium methylate and fatty acid and crude glycerin to separate, wherein a fourth upper layer is fatty acid and ester with a moisture of about 1% mass/mass; and a fourth lower layer is water, additive, glycerin, sulfates and sulfonate compounds which are sent to effluent treatment.
地址 São Paulo-SP BR