HYDROPHOBIC SYNTHESIS METHOD OF DEEP EUTECTIC SOLVENTS FROM VEGETABLE OIL REFINERY WASTE FOR DEGUMMING CRUDE PALM OIL

Abstract

This invention concerns Hydrophobic Deep Eutectic Solvents (DES) from vegetable oil refinery waste as raw material for Degumming Crude Palm Oil (CPO). This invention aims to reduce phosphorus content in CPO and process SBE waste into value-added products. This synthesis includes oil extraction from SBE waste, fatty acid extraction from extracted oil using NADES solvent, hydrophobic DES synthesis, and DES application in CPO degumming.

Description

Hydrophobic DKEP Eutectic Solvents (DES) from Refinery Waste VEGETABLE OIL AND ITS APPLICATION IN DEGUMMING CRUDE PAIM OIL Invention Engineering Field The present invention concerns Hydrophobic Deep Futectic Solvents (DES) from Vegetable Oil Refinery Waste and Its Application in Degumming CPO. More specifically, the present invention relates to the utilization of SBE (Spent Bleaching Earth) waste to produce DES which used in refining palm oil, with the aim of reducing phosphorus levels and increase the efficiency of the degumming process. Background of the Invention This invention has been known and used to overcome environmental problems caused by SBE waste from palm oil industry. SBE is the largest waste that produced by the palm oil refinery and oleochemical industries, which has the characteristics of being flammable and corrosive, as well as contains high oil. Technological inventions related to SBE have also been disclosed as contained in the patent PID201906686 Date February 9, 2021 with the title 'Soil Waste Processing Technology' Bioprocess Bleaching Earth (SBE) as a bleaching agent Mixture of Bio-Organic Fertilizer, Planting Media, and Soil Enhancer,' wherein a method for obtaining bio-organic fertilizer is disclosed, planting media, and soil restoration based on bleaching soil waste (Spent Bleaching Earth, SBE) from coconut oil industry waste palm oil. The invention still has shortcomings in terms of efficiency and environmental friendliness. Other inventions as disclosed in patents S00202112276 Number 2022 / SID / 00277 dated January 24, 2022 with Title 'Deep Eutectic Solvent (DES)' Based on Potassium Carbonate and Glycerol as Production Catalyst Biodiesel,' which discloses the process of producing eutectic fluid. in (DES) from pure commercial potassium carbonate and glycerol. This process has drawbacks in terms of raw materials and complexity of the synthesis process. However, the above mentioned inventions are still has weaknesses and limitations, among others is inefficiency in the use of raw materials, the impact environment is still high, as well as complexity in the process synthesis and application. Furthermore, the proposed invention is intended to overcome the problems stated above by means of utilizing SBE waste to synthesize hydrophobic DES which more efficient and environmentally friendly, and apply it to CPO degumming process to reduce phosphorus content. Brief Description of the Invention The main objective of this invention is to overcome pre-existing problems especially in Hydrophobic Deep Futectic Solvents (DES) from Vegetable Oil Refinery Waste And its application in CPO degumming, where a deep hydrophobic Futectic Solvents (DES) from Vegetable Oil Refinery Waste and The application in CPO degumming according to this invention consists of from (a) SBE waste, (b) DES synthesis from menthol and fatty acids, and (c) DES application in the degumming process, which is characterized by the use of Hydrophobic DES with a certain molar ratio is effective in reducing phosphorus levels in CPO. Another objective of this invention is to reduce the impact environment from SBE waste and increase purification efficiency palm oil. This Hydrophobic DES synthesis process also provides a safer and more sustainable solution compared to conventional methods, as well as producing value-added products from industrial waste. Other goals and benefits as well a more complete understanding of the following invention as preferred embodiment and will be explained with reference to in the accompanying pictures. Short Description of Image Figure 1 is a perspective view of the Hydrophobic Deep Futectic Solvents (DES) from Vegetable Oil Refinery Waste and Its application to CPO degumming in accordance with the present invention. Figure 2 is a block diagram of the oil extraction process from SBE waste. Figure 3 is a flow diagram of the synthesis process of Hydrophobic DES. Figure 4 is a perspective view of the application. Hydrophobic DES in CPO degumming process. Figure 5 is a graph of the FTIR test results data from Hydrophobic DES. Synthesized. 1:1 ratio (Black), 2:1 ratio (Red), 3:1 ratio (Blue) Complete Description of the Invention This invention will be fully described with reference to to the accompanying figures. Referring to Figure 1, which shows a complete detailed image of Hydrophobic Deep Futectic Solvents (DES) from Vegetable Oil Refinery Waste And its application in CPO degumming, which consists of several the stages are: 1) 100 grams of solid SBE waste was extracted using Soxhletation method using n-Hexane solvent as much as 500 mL. 11) The extracted oil is processed using the distillation method to separate the solvent. i11i) Hydrophobic DES synthesis is carried out by mixing acid fat extracted with menthol crystals in molar ratio 1:1, 2:1, and 3:1. Referring to Figure 2, the process is described in full. Oil extraction from SBE waste. Solid SBEK waste as much as 100 grams were extracted using the Soxhletation method using n-Hexane solvent as much as 500 mL. The soxhletation process is complete if the solvent that is condensed and collected in the Soxhlet tube is already clear. The result of extracting the mixture of oil and n-Hexane in distillation to separate oil from solvent. After the process / distillation is complete, the oil obtained is reheated above hot plate at 70”C for 15 minutes to re-evaporate residual solvent in the oil. Referring to Figure 3, the process is described in full. Hydrophobic DES synthesis. Hydrophobic DES preparation is carried out by mixing the extracted fatty acids as HBD with menthol crystals as HBA with molar ratios of 1:1, 2:1, and 3:1. The mixture homogenized with a magnetic stirrer at a rotating speed 500 rpm for a mole ratio of 1:1 for 1 hour 30 minutes, 600 rpm for 2:1 ratio for 3 hours 30 minutes, and 700 rpm for 3:1 ratio for 5 hours 30 minutes. All three variations are operated at the temperature which is kept constant at 50t1”Cc. Referring to Figure 4, the application of Hydrophobic DES is described in CPO degumming process. The degumming process was carried out on 150 mL of CPO. which is preheated at a temperature of 80”C for 60 minutes. The water degumming method is carried out by adding as much water as 208 into the heated CPO. Then, the mixture heated again at a temperature of 90”C for 20 minutes at a speed of stirring at 250 rpm. After cooling to room temperature, The mixture was centrifuged at 3000 rpm for 20 minutes. CPO from water degumming is used in the acid degumming method. with the addition of Hydrophobic DES with a variation of 0.385, 0.68: and 0.98 volumes. This mixture is then heated to temperature 60”C for 30 minutes with a stirring speed of 250 rpm. The content phosphorus in CPO from water degumming and acid degumming then analyzed. After the degumming process, the sugar content test was carried out phosphorus in CPO, water degumming, and acid degumming samples The results data are presented in Table 1. Table 1. Data on Phosphorus Content in Samples Percentage Types of Phosphorus Content Ratios Hydrophobic HDES sample (mg / 3 g) DES (SS) Initial CPO — — 1, 64348 Water — — degumming 0, 15712 Acid 1:1 0.3 0.65652 degumming 1:1 0.6 0.53482 1:1 0.9 0.39061 Acid 2:1 0.3 0.41875 degumming 2:1 0.6 0.58899 2:1 0.9 0.28298 Acid 3:1 0.3 0.57914 degumming 3:1 0.6 0.44689 3:1 0.9 0.44337 Determination of phosphorus levels is carried out using a spectrophotometer. UV-Vis at a wavelength of 650 nm. The phosphorus content in CPO was measured in the linear concentration range of 0-0.1 mg phosphorus with a coefficient correlation (R) of 0.99767. Based on the research results, the process Water degumming can reduce phosphorus levels by 538, while the acid degumming process with various HDES ratio variations and the percentage is able to reduce phosphorus levels which range from 60- 108. The most optimal reduction in phosphorus levels is 82$ with the use of Hydrophobic DES at a ratio of 2:1 and the percentage 0.98. With the obtained data, it can be concluded that CPO degumming process using DES hydrophobic solvent with ratios of 1:1, 2:1, and 3:1 were successfully carried out. Referring to Figure 5, it explains how to carry out the test. FTIR for DES Hydrophobicity Characterization. FTIR data from the synthesis Hydrophobic DES consisting of menthol as HBA (Hydrogen Bond) Acceptor) and fatty acids as HBD (Hydrogen Bond Donor) with ratios l:1, 2:1, and 3:1 show some characteristic bands that significant. At a 1:1 ratio, the main band appears at 3313.27 cm” (OH group), 2925.42 cm'' and 2868.36 cm! (CH group), and 1635.81 cm! (CO group). The ratio 2:1 shows a band similar to a slight shift in the OH band to 3316.44 cm" and in the OH band CO becomes 1636.45 cm'!. At a ratio of 3:1, the OH band shifts more continue to 3319.54 cm, and the CO band appears at 1636.50 cm!- Frequency shifts indicating hydrogen bond interactions between DES components. Hydrogen bond interactions between menthol and fatty acids seen from the changes in intensity and shifts of the OH and CO bands. At a ratio of l:1, the intensity of the OH band is lower compared to ratios of 2:1 and 3:1, indicating increased hydrogen interactions with increasing menthol ratio. Frequency shift in the CO band from 1635.81 cm' at a ratio of 1:1 to 1636.45 cm'! at a ratio of 2:1 and 1636.50 cm! at a ratio of 3:1 indicates the formation of hydrogen bonds which is stronger with increasing menthol ratio. Changes band intensity at various mixture ratios indicates the effect increase or decrease of certain components to stability eutectic solvent. At a ratio of 3:1, the intensity of the CO band is higher, shows stronger hydrogen bonding interactions and better stability compared to 1:1 and 2:1 ratios. From the description above it is clear that the results of this invention can benefits the palm oil industry because it is practical and efficiently reduce phosphorus levels in CPO using solvents which is safer and more sustainable. This invention is truly presents a very practical improvement especially on Hydrophobic Deep FEutectic Solvents (DES) from Refinery Waste Vegetable Oil and Its Application in CPO Degumming.

Claims

Ll. A method of synthesis of Hydrophobic Deep Futectic Solvents (HDES) from vegetable oil refinery waste consists of several stages, namely: i) Oil extraction from Spent Bleaching Earth (SBE) waste using the soxhletation method with n-Hexane solvent, where 100 grams of SBE waste was extracted using 500 mL of n-Hexane. until the solvent is clear, followed by distillation to separate oil from solvent. ii) Extraction of fatty acids from SBE waste oil using Natural Deep Futectic Solvents (NADES) solvents, with mixing SBE and NADES waste oil at a mass ratio 2:1, homogenized at t43”c for 3 hours, and centrifuged at 2000 rpm for 20 minutes. iii) Synthesis of HDES by mixing fatty acids as Hydrogen Bond Donor (HBD) with menthol crystals as Hydrogen Bond Acceptor (HBA) at molar ratios :l, 211, and 3:1, homogenized at different speeds and times according to the ratio, namely 500 rpm for 1 hour 30 minutes for a ratio of l:1l, 600 rpm for 3 hours 30 minutes for a 2:1 ratio, and 700 rpm for 5 30 hours for a 3:1 ratio, at a constant temperature of 50t1”Cc.

2. HDES according to claim 1, characterized in that the density in the range of 0.927-0.946 g / cm?', viscosity in the range of 14.1986- 25.4203 cP, and pH in the range of 4.06-6.07, where the density tends to decrease, viscosity decreases, and pH decreases with time. with increasing molar ratio of crystalline menthol to fatty acids.

3. HDES according to claim 1, wherein the best HDES ratio for The application of degumming Crude Palm Oil (CPO) is a molar ratio of 2:1 between fatty acids and menthol crystals, which showed a decrease phosphorus content of 828 at a percentage of HDES usage of 0.96 volume.