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http://www.e-journals.net ISSN: 0973-4945; CODEN ECJHAO E-Journal of Chemistry Vol. 5, No.4, pp. 940-945, October 2008 Recovery of Glycerol from Spent Soap Lye By - Product of Soap Manufacture A.U. ISRAEL, I.B. OBOT* and J.E. ASUQUO Department of Chemistry, Faculty of Science, University of Uyo, P.M.B. 1017, Uyo, Nigeria. proffoime@yahoo.com Received 16 October 2007; Accepted 10 December 2007 Abstract: Three samples of spent lye from soap manufacturing companies namely Paterson Zochonis Ind
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    ISSN: 0973-4945;   CODEN ECJHAO   E-Journal of Chemistryhttp://www.e-journals.net Vol. 5, No.4, pp. 940-945, October 2008 Recovery of Glycerol from Spent Soap LyeBy - Product of Soap Manufacture A.U. ISRAEL, I.B. OBOT * and J.E. ASUQUODepartment of Chemistry,Faculty of Science, University of Uyo,P.M.B. 1017, Uyo, Nigeria.  proffoime@yahoo.com Received 16 October 2007; Accepted 10 December 2007 Abstract: Three samples of spent lye from soap manufacturing companies namelyPaterson Zochonis Industries (PZ), International Equitable Association (IEA),Kitchen Soap Industries (KSI) all in Aba, Abia State of Nigeria and onelaboratory simulated sample (SSL) were analyzed for the amount of glycerol andresidual salts. The amount of glycerol in all the samples increases in the orderbleached glycerin > crude glycerin > semi-crude glycerin > treated lye > spentsoap lye while the reverse is the order for the amount of residual salts. For theSSL, PZ, IEA and KSL samples, the percentage of recovered glycerol were91.00, 83.20, 82.80 and 81.40 while the residual salt content (%) were 9.80, 6.00,7.08 and 8.03 respectively. These values compare well with internationalstandards. The results show that the amount of the recovered glycerin andresidual salts depend on the quality of the spent lye and the technology employedin the recovery treatment used.  Keywords: Glycerol, Soap, Spent soap-lye, Recovered glycerin. Introduction Glycerol (propan-1, 2, 3-triol) is an important by-product of soap manufacture. It is founddissolved in the soap lye and as impurity in the crude soap when fats and oils are saponifiedby caustic soda 1-3 . The process of soap manufacture from fats and oil usually yield glycerolto about 10% of the value of the soap formed and because of its many uses, its recoveryis vital to the manufacturing cost analysis for any soap making venture. Unfortunatelymany small scale and medium scale soap producers usually discard the lye as a waste.Glycerol occurs in nature combined in the form of triglycerides (fats and oil) and is  941 I.B. OBOT et al.  obtained during saponification of these triglycerides 4 . This process was the onlymeans of producing commercial glycerol until 1949 when synthetic glycerol wasproduced as the compound recovered as by-product from the soap manufacture was notsufficient for the world consumptiom. Today glycerol is synthesized from propene by thealternate chlorination and hydroxylation process 5 . It is also obtained from fermentation of various sugars 6 .Some of the major industrial applications of glycerol include the manufacture of alkydresins and flexible polyurethane for the plastic industry. It is also an important ingredient incosmetics and adhesive manufacture. Many pharmaceutical preparations such as glycerol-phenol mixture which serves as bacteriological culture medium and glycerol derivatives( e.g . nitro glycerol) used as tranquilizers utilize glycerol.Glycerol residue has been reported to contain 20.2% glycerol, 6.6% fatty acids (assoap) and 64.3% salt 1 . Thus 91.1% of it is potentially useful. It is obviously advantageous,both environmentally and economically, to recover the glycerol in the waste (spent soaplye) for use.   The present work is aimed at practically exploiting these wastes materialsfrom soap industries as a potential alternative for the production of glycerol usingchemical methods. Experimental Spent soap lye which is a mixture of many compounds namely glycerol 6-16%, salt 10-12%,caustic soda 0.3-0.8%, total fatty matter 0.4% and water 39-40%. Others are organic andinorganic impurities such as resins, arsenic and arsenic compounds 7 , were obtained fromthree industries in Aba, Abia State in Nigeria. The industries include Paterson ZochonisIndustries (PZ), International Equitable Association (IEA), Kitchen Soap Industries (KSI)and the Laboratory Simulated Soap sample (SSL). Other reagents of Analytical grade fromBritish Drug House (BDH) were used as purchased in the analysis. Preparation of laboratory simulated soap sample (SSL) Palm oil (200 mL) was added to caustic soda (NaOH) slowly with constant stirring to obtaina smooth paste. The soap was grained with some quantity of brine which separated the soapmass from excess water containing glycerol, sodium hydroxide, salt and other impurities.This spent soap lye labeled sample SSL was preserved for analysis.   Treatment of spent soap lyes Spent soap lyes samples (200mL) (PZ, IEA, KSI, SSL) were first analysed for percentagecaustic soda, salt, glycerol, total fatty matter, other impurities and moisture by the methodof Igile 8 as described below. The left over liquor after soap manufacture (lye) was allowedto settle for 20minutes in each case after stirring with a rod. The clear phase was decantedfrom the sample and heated to 60 o C in a conical flask. Acid treatment was followed byaddition of dil. HCl (0.1 M) dropwisely until the pH was between 5.0-6.0. The sample waslater filtered into a conical flask. Sodium hydroxide solution (0.1 mL) was added with theaid of a pipette to the filtrate obtained above to raise the pH again to between 8.0-9.0. Thesample was filtered again and the filtrate was analyzed for percentage caustic soda, saltand glycerol. The semi-crude glycerin was obtained by evaporating the filtrate aboveunder vacuum pressure (80 mmHg). The resultant crude glycerin was for analyzed forpercentage salt, glycerin, moisture and impurities. Salt was recovered from the crudeglycerin by allowing the sample to stand for 4h after which the clear phase was decantedfor the salt.  Recovery of Glycerol from Spent Soap Lye 942  Bleaching of crude glycerin This was carried out using the method of Igile 10 . Crude glycerin with bleaching earth (3%)and 0.1% of H 2 SO 4 (10 mL) were introduced into a round bottomed flask. Heat wassupplied with continuous stirring for 30minutes under vacuum (120 mmHg) and 90 o C.Calcium carbonate (0.05%) was added to neutralize the content of the flask. The contentwas cooled to 70 o C and filtered. This is bleached glycerin and was analysed forpercentage glycerin, salt, moisture content and impurities. Bleached glycerin was furtherpurified by vacuum distillation in order to obtain purified glycerin with highconcentration. The distillate (purified glycerin) was collected and analyzed for percentageglycerin and salt.  Determination of salt content in the spent soap lye Untreated and treated soap lye sample (0.1 g) was weighed into a conical flask (250 mL)containing distilled water (100 mL). Methyl orange indicator (2-3 drops) was added to themixture. A drop of dilute nitric acid (0.1 M) was added to neutralize the sample. This wasfollowed by the addition of potassium dichromate (2 mL) as the sample colour changed toyellow. The sample content was titrated with silver nitrate solution (0.1 M). The end pointwas detected with a colour change from yellow to light brown. From the result obtained, thepercentage salt was calculated 8 . Percentage free caustic soda in lye 10 g of soap lye was weighed and diluted to 100mL with distilled water. Phenolphthaleinindicator (2-3) drops was added, the colour changed to pink. The same was neutralized byadding barium chloride (5 mL). The solution was titrated with hydrochloric acid (0.1 M) toobtain a colourless solution at the end point. The percentage caustic soda (NaOH) wasdetermined as volume of HCl (0.1 M) multiplied by conversion factor of 0.04% 10 . Percentage concentration of glycerol in crude glycerin 5.0g of the sample were taken into a conical flask and 50 mL of distilled water was added. Ablank (control sample) was set up with 50 mL water at the same time. Phenol red indicator(10 drops) was added to obtain yellow colour. 0.1M HCl (1.0 mL) was added to neutralizethe contents of the flask. The sample was left to stand for 20 minutes in a dark chamber. Thesample was then titrated with 0.1 M NaOH to pink colour as the end point taking the blank sample first.The concentration of glycerol was calculated as percentage of glycerol in the crudeglycerin using the titration value according to equation (1) as reported by 8 . 92.0  xW V V C  sbsa −= (1)where C a is the percentage concentration of glycerol, V s is the volume of 0.1 M NaOH addedto the sample, V b is the volume of 0.1M NaOH added to the blank and W s is the weight of sample.Percentage impurities in the sample were determined by pouring the whole sample intoa measuring cylinder and allowing it to settle for 1h. The percentage impurity was calculatedfrom the equation (2) as reported by Igile 8 .% Impurity = Level of impurity in cylinder X 100 (2)Total volume of sample  943 I.B. OBOT et al.   Results and Discussion Table 1 shows the estimated consumption of glycerin in various industries. Table 2 showsthe Glycerin Producers Association Standards for Glycerin recovery. Table 3 shows the   percentage concentrations of salt and glycerin and their standard deviations recovered fromSoap Lye for different samples (SSL, PZ, IEA and KSI), while Table 4 shows the standarddeviation for % salt and % glycerin for samples at different stages respectively. Table 1. Estimated consumption of glycerin in various industries 11   Industry Percentage useAlkyd resin 30.00Tobacco (humectants) 12.00Explosives 12.00Cellophane 11.20Cosmetics/Mouthwashes 5.10Pharmaceuticals 5.10Sealants, Lubricants 4.60Various intermediates for syntheticdyes, Lacquers, textiles20.00 Table 2. Glycerin Producers Association Standards for glycerin recovery 7 State of Recovery % Salt % GlycerinSpent soap lye 10-12 6-16Treated lye: Acid, (Alkaline) 11-13, (16-18) 5-7, (8-10)Semi-Crude Glycerin 19-22 30-45Crude Glycerin 8-10 80-84Bleached Crude Glycerin 6-9 85-91Purified Glycerin 9-10 92 Table 3. Percentage concentrations of salt and glycerin and their standard deviationsrecovered from soap lye for different samples (SSL, PZ, IEA and KSI)Samples SSL PZ IEA KSI% Salt % Gly. % Salt % Gly. % Salt % Gly. % Salt % Gly.Spent SoapLye9.30 15.00 9.59 7.31 10.50 5.48 9.48 7.29Treated Lye 17.00 10.00 9.75 7.95 12.90 6.15 9.04 7.08Semi CrudeGly.22.00 40.00 10.52 30.10 15.50 42.46 11.13 40.05CrudeGlycerin8.00 81.00 6.40 82.80 7.49 81.57 8.13 80.40BleachedGlycerin9.80 91.00 6.00 83.20 7.08 82.80 8.03 81.40StandardDeviation3.66 37.01 1.67 34.28 3.29 34.22 1.22 34.78From Table 3, the amount of percent glycerin (%) in all the samples increases in theorder: bleached > crude glycerin > semi-crude glycerin > spent lye > treated lyerespectively, while the reverse is the order for the amount of residual salts. The percentageof glycerin recovered for the various samples- SSL, PZ, IEA and KSI were 91.00, 83.20,82.80 and 81.40 respectively. These figures compare well with the standard value obtained
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