Method of extraction of natural wax

Abstract

Method for producing wax from raw palm material comprising the steps of: (a) heat treating separated palm leaflets in a liquid, (b) drying the leaflets, (c) beating the leaflets, and (d) separating the wax from the residual material in (c). The heat treatment may comprise heating to 80-100oC, preferably boiling, for 30 minutes to 6 hours. The liquid may be water or a solution, preferably an alkaline solution including surfactants and / or acidic buffers. The leaflets may be dried until the moisture level is below 15% and may be beat using a rotating beating blade. The leaves may be chopped, pulverised or ground after beating. The wax may be separated by manual screening, centrifugal air or flotation separation. The method may include step (e) of purifying the wax from the residual vegetable matter, preferably melting the wax or dissolving in a solvent. Step (e) may comprise adding the melted wax or solution to adsorbents, such as activated carbon, silica gel or activated clay, or filtering the solution through paper, cloth or membrane via centrifugation. The method may include a bleach step after steps (d) and / or (e) and may include an initial step of separating palm leaflets from palm fronds.

Description

Field of the Invention This invention relates to a method of extraction of fibres and wax and more particularly, but not exclusively, the invention relates to extraction of textile fibres and surface wax from palm leaflets, such as textile fibres and wax from date palms. Background Date palms are mainly cultivated in the Middle East and North African regions. Typically, global harvests exceed 1 million hectares. The estimated annual byproducts of pruning of date palms globally are around 5 million tons (air dry weight), in the form of frond and fruit stalks, leaflets and leaf sheath. These are often treated as agricultural waste. Previous attempts to extract fibres from date palm leaflets were limited to milling them into small particles or manually slitting them into long strands with no attempt to remove the non-cellulosic impurities. These tended to be used traditionally in manufacture of fibre fill for cushioning. As for the wax extraction, the majority of the palm wax extracted are from the Brazilian carnauba palm and only one published research article investigated the extraction of date palm leaflet wax using a complex supercritical carbon dioxide extraction method. Some of these are described in the documents mentioned below. Prior Art International patent application WO2023007223A1 (NAMA WOMEN ADVANCEMENT ESTAB) discloses a method of fibre extraction from palm, using a biological degumming process employed to loosen the date palm leaves structure. The degumming process comprises the steps of retting in warm using a biological enzyme (Laccase). The degumming temperature is from 25°C to 60°C and the degumming treatment time is from 2h to 24h. The degumming process is followed by manual combing process and then the leaves are dried at room temperature. United States patent application US 11370953B2 (SAUDI ARABIAN OIL CO) discloses a method of preparation of date tree waste-based lost circulation material (LCM). The date tree waste LCM may include fibres from the date tree waste produced from processing date trees in the production of date fruits. The date tree waste may include fibres from one or more of the following: date tree trunks, date tree rachis, date tree leaflets, date tree panicles, and date tree roots. The date tree waste LCM may include fibres having lengths in the range of 5 millimeters (5 mm) to 15 mm, diameters in the range of 0.5 mm to 0.8 mm and having an aspect ratio range of 6 to 30. Japanese patent application JP2020532607A (tfC'^ 7j tf7’> JU —) discloses a method of making of date palm fibre blend lost circulation material (LCM) comprising a ternary blend of fibres made from date palm. Date palm fibre mixed LCM comprises date palm fibre made from date palm trunks, date palm leaves and leaf stem fibres made from date palm leaves and leaf stems, and date palm inflorescence fibres made from date palm inflorescences. The LCM comprises a mixture of 30% by weight date stem fibre, 30% by weight date palm leaf and leaf stem fibre, and 40% by weight date inflorescence fibre. International patent application WO2012108860A1 (BROWN LAURENCE B) discloses a method of making dental implement made from palm leaflet, the dental implement usable as dental floss that can be manipulated while held in one hand includes an elongate body cut from dried palm leaflet. A dental implement in accordance with the present invention preferably consists only of dried palm leaflet. A leaflet is dried, and the dried leaflet is cut to the desired length and width to form the dental implement. International patent application WO2020139088A1 (SULTAN QABOOS UNIV) Preparation of high performance fibre from natural fibre (date palm) a method for preparation of high performance fibre from natural fibre (date palm), the method includes separating raw fibres from the natural fibre source and dewaxing the separated raw fibres with an alcoholic solution of ethanol and water for a predetermined time at a first predetermined temperature. The method further includes sterilizing the dewaxed fibres with an acidified salt solution at a second predetermined temperature and alkalizing the sterilized fibres with an alkali solution at a third predetermined temperature to generate the high-performance fibres. In a paper by Karima Al Bulushi, Thomas M. Attard, Michael North, Andrew J. Hunt, 2018 entitled “Optimisation and economic evaluation of the supercritical carbon dioxide extraction of waxes from waste date palm (Phoenix dactylifera) leaves”. Journal of Cleaner Production, Volume 186, Pages 988-996. None of the above techniques were capable of extracting long textile grade fibres from date palm leaflets or were able to extract surface wax. An object of the present invention is to valorize large quantities of agricultural residues generated by palm, particularly date palm plantations and to extract long textile fibres from the leaflets and to extract the surface wax. Summary of the Invention According to a first aspect of the invneiton there is provided a method for producing wax from raw palm material comprising the step of: a) heat treating the separated palm leaflets in a liquid; b) drying the leaflets; c) beating the leaflets; d) separating wax from the remaining residual material from c). In some embodiments step a) comprises treating in the liquid between 80°C to 100°C. Optionally step a) comprises boiling of the liquid. The duration of the heat treatment is typically from 30 minutes to 6 hours, preferably 1 to 5 hours. The liquid may be water or a chemical solution. Optionally the solution is an alkaline solution and / or includes surfactants, and / or acidic buffers. In some embodiments step b) is performed until the moisture level drops below 15%. In some embodiments step c) comprises passing the dry leaflets against a rotating beating blade. In some embodiments following step c), an additional step of chopping pulverizing, or grinding the dried leaves. In some embodiments step d) is performed by at least one of: manual screening, centrifugal air or flotation separation. In some embodiments step e) is applied after d) and includes purifying the wax from the residual vegetable matter. Preferably step e) includes heating the crude wax over its melting point; optionally with stirring. Optionally step e) comprises dissolving and heating the wax in a solvent, optionally with stirring. Preferably the solvent is from the group comprising: xylene, toluene, alkanes, alkaline hydrogen peroxide, ethyl acetate, acetone, benzene, naphthas, alcohols or any other non-polar organic solvent chemical or vegetable-based solvent. In some embodiments including the step in step e), preferably any one or more of: active carbon, silica gel, activated clay and adsorbents are added to the melted wax or wax solvent mixture. Optionally included in step e) is the step of filtration by passing the wax solution through paper, cloth, or membrane or by centrifugation. In some embodiments a bleach step may be applied after step d) and / or e). Some embodiments include an initial step of separating palm leaflets from palm fronds. Embodiments of the invention will now be described by way of example only and with refence to the Figures in which: Brief Description of the Drawings Figure 1 Process flow diagram for extraction of textile fibres and surface wax from palm leaflets; Figure 2 Leaflet fibres morphology before (left) and after degumming (right); Figure 3 Palm leaflet fibres after scraping; Figure 4 Palm leaflet fibres after degumming; and Figure 5 Resulting wax extracted from date palm leaflet. Detailed Description of Preferred Embodiments of the Invention Methodology for Fibre Extraction The method is shown diagrammatically as a series of steps in Figure 1. Referring to Figure 1, there is shown a process flow diagram for extraction of textile fibres and surface wax from palm leaflets. Initial Preparation The leaflets are separated from the date palm fronds either manually by hand, knife, or by using a mechanized system with blades to peel off the leaflets, which are then collected for further processing. Pre-Soaking Fresh green leaflets may be used directly for fibre extraction; however, pre-soaking may enhance the quality of the extracted fibres. Whereas, for dry leaflets they must be presoaked in water from 1-5 days at room temperature or they might be boiled between 80°C to 100 °C to shorten the pre-soaking time and also to enable the extraction of the surface wax. Scraping Palm leaflets are then scraped to remove the non-fibrous surface layer and facilitate the fibre extraction. The scraping action can be performed using a reciprocating blunt scraper along the length of the leaflets. It can also be performed using a rotating drum (decorticator) with multiple blunt scraping blades rotating against a stationary beater. In this case the leaflets are fed into the clearance 0.1 to 0.4 mm between the rotating scraping blades and the stationary beater, in one or multiple strokes from one or both ends. It is important that the scraping is performed while the leaflets are still moist. Brushing After scraping, the extracted fibres can be then brushed for further refinement and to remove residual surface impurities. Brushing is performed by a rotating drum with multiple blunt blades or short metal combs, in which the fibres are held from one end and fed into the clearance between the rotating drum and a flat metal surface, in one or multiple strokes from one or both ends. Degumming The degumming is an optional step used to further remove intra and inter fibre bundles gum and fibrillate the bundles into smaller bundles and / or individual fibrils with less than 25pm diameter. This can be achieved by using an enzyme degumming process or chemical degumming process or a combination of both. In the enzyme degumming process, the fibres are boiled at 80 °C in 0.1 M sodium phosphate buffer pH 2:3 for at least one hour. After boiling, the fibres may be soaked for 24 hours in the sodium phosphate buffer at room temperature. The fibres are thoroughly rinsed with tap water after removing the fibres from the phosphate buffer. Afterwards, the fibres are soaked for 6 hours in an acid pectinase enzyme solution, 4 g pectinase powder / 100 g dry fibres, in a treatment solution ratio of 1:20, with enzyme activity 30,000 U / g at pH 4 and 50 °C while maintaining continuous agitation, for removing the pectin. Then the fibres are soaked in an enzyme solution of laccase and acid xylanase using 4 g enzyme powder / 100 g dry fibres, in a treatment solution ratio of 1:20, with laccase activity 2,000 U / g and xylanase activity 100,000 U / g, at pH 4.8 for 10 hours with continuous agitation at 50 °C for first 2 hours, then raised to 60 °C for the remaining 8 hours, for removing the lignin and hemicellulose. The enzyme treatment can also be conducted in an enzyme mix containing all 3 enzymes; pectinase, laccase, and xylanase. After completing the enzyme treatment, the fibres are scoured in an alkaline solution of 2% including soda ash, sodium hydroxide, potassium hydroxide, or lye concentrate at temperature 80 °C for 2 hours. In any of the previous steps the treatment may include surfactant such as Triton X-100 and / or chelating agent such as Ethylenediaminetetraacetic acid (EDTA). After the scouring process, the fibres are beaten using rotary serrated rollers, steel or wooden mallet or any combination thereof. Finally, the fibres are neutralized in a solution of 5% acetic acid for 30 mins at room temperature, then rinsed with tap water. In the chemical degumming process, the fibres are boiled at 100 °C from 2 to 3 hours in a solution containing 1% Sodium hydroxide, 0.1% hydrogen peroxide, 0.3% sodium silicate and 0.3% Ethylenediaminetetraacetic acid, while maintaining continuous agitation. After completing the chemical treatment, the fibres are neutralized in a 5% acetic acid solution and then rinsed in water. The fibres morphology before and after degumming is illustrated in Figure 2 Drying After washing, the fibres are dried to a moisture content of less than 20%, preferably less than 15%. The first step in the drying is either roll squeezing to remove as much water as possible or centrifugal dewatering using a mechanized drying system. The second drying step involves air drying the fibres in open air for several days depending on the ambient conditions or oven drying at temperature 80°C until the moisture content drops below 15%. The resulting fibres at the end of the scraping method is shown in Figure 3, while the resulting fibres after the degumming method are shown in Figures 4. Below is a Table which shows properties of the materials obtained using the abovementioned method steps. Technical Data Table 1 shows average properties of long textile fibres extracted from date palm leaflets after scraping and after degumming using the above methods. Average fibre properties Scraped Degummed Standard Cellulose wt. (%) 52.3 ±0.2 53.1 ± 0.3 T 203 cm-09 Hemicellulose wt. (%) 17.4 ±0.5 18.1 ±0.5 T223 cm-10 Lignin wt. (%) 15.2 ±0.6 13 ±0.5 T222 om-11 Ash wt. (%) 1.3 2.8 - Extractives wt. (%) 13.8 13 - Fibre length (mm) 139 ±100 43.1 ±28.9 - Equivalent diameter (pm) 58.7 ±12 20.2 ±9 SEM Density (g / cm3) 1.431 ±0.009 1.49 ±0.05 ASTM D8171 - 18 Tensile strength (MPa) 654 ±262 649 ±108 ASTM D 3822 - 01 Tensile modulus (GPa) 22.7 ±3.8 33.2 ±4.6 ASTM D 3822 - 01 Failure strain (%) 2.8 ±0.7 1.97 ±0.4 ASTM D 3822 - 01 It will be appreciated that variation may be made to the aforementioned embodiments, without departing from the scope of protection as defined by the claims. For example, the method can also be used to extract long textile fibres from the leaflets of other palm species, including but not limited to washingtonia palm, oil palm, coconut palm, and sugar palm. According to an aspect of the invention there is provided a fibrous product derived using the aforementioned method. Fibrous products produced according to the method may be used to make or incorporated in, a myriad different items or products, including: an item of clothing or footwear: a sheet of flexible material; items for use in automotive or construction, (such as boards or insulation panels) or rope or twine. Methodology for Wax Extraction The method is shown diagrammatically as a series of steps in Figure 1 Initial Preparation The leaflets are separated from the date palm fronds either manually by hand, knife, or by using a mechanized system with blades to peel off the leaflets, which are then bundled for further processing. Treatment Fresh or dry leaflets may be boiled between 80°C to 100°C from 1 hour to 5 hours, either in water only or in a chemical solution which may include but is not limited to alkaline solutions, surfactants, or acidic buffers. Drying The leaflets are then air died in the sun for 1-4 days, or inside an oven at 80 °C until the moisture level drops below 15%, other drying techniques can be applied such as using microwave. Beating After the leaflets become fully dry, they are then beaten to release the crude wax. Beating may be done manually by hand or mechanically by passing the dry leaflets against a rotating wooden or metal beating blade. Leaflets chopping (optional) Leaflets may be chopped to loosen more wax. The chopping may be performed using a rotary cutter, pulverizer, or grinder. Separation A separation method is then applied to separate wax from any other residual vegetable matter or impurities. The separation method may include but is not limited to manual screening, centrifugal air flotation separations, or both. Crude wax refinement Refinement of the crude wax is done to purify the wax from the residual vegetable matter. This process may include but is not limited to 1) simply heating the crude wax over the melting point with continuous stirring to melt the wax 2) dissolving and heating the wax with continuous stirring in a solvent such as but is not limited to xylene, toluene, alkanes, alkaline hydrogen peroxide, ethyl acetate, acetone, benzene, naphthas, alcohols or any other non-polar organic solvent chemical or vegetable based. Bleaching (optional) Bleaching may be done if needed to give a better appearance to the extracted wax. Chemical or other bleaching methods can be used such as hydrogen peroxide, sodium hypochlorite, acids such as but not only hydrochloric acid, chromo-sulphuric acid, phosphoric acid, or Ozon bleaching. Purification After wax melting the melt or wax solvent mixture is purified by any purifying technique such as but not limited to 1) addition of adsorbents like active carbon, silica gel, activated clay, or any other adsorbent. 2) filtration by passing the wax solution through paper, cloth, or membrane. 3) centrifugation. Any of those techniques may be used separately or combined. Mixing (optional) Palm leaflets wax can be mixed with other additives or waxes to improve its properties like color, hardness, gloss, melting point, or any other needed properties to serve the final application. This process can be done after or before the cooling of the purified wax. Cooling Cooling of the wax may be done by any of the following methods but not limited to 1) air cooling by letting the wax air dry at room temperature or lower temperature, 2) cooling in a mold to produce well-shaped products, and 3) water cooling by exposing the wax melt to cold water. Formation Solidified wax can be formed into any required shape such as but not limited to powder, pellets, flakes, and blocks. The resulting wax at the end of the extraction method is shown in Figures 5 Below is a Table which shows properties of a material obtained using the abovementioned method steps. Technical Data Table 2 Properties of surface wax extracted from date palm leaflets using the above method. Properties Melting point 81-87 °C Density 0.990-0.999 Refractive index 1.4500 Solubility Practically insoluble to insoluble in water, soluble on heating in ethyl acetate and in xylene, practically insoluble in alcohol. Form Powder or Flakes Color ranges from light yellow to dark brown Specific Gravity 0.990-0.999 Odor odorless Water Solubility Soluble in diethyl ether, alkali, chloroform. Slightly soluble in boiling ethanol. Insoluble in water. Stability Stable. Incompatible with strong oxidizing agents. Chemical composition Consists of fatty acid esters (80-85%), fatty alcohols (10-16%), acids (3-6%) and hydrocarbons (1-3%). It is around 20% esterified fatty diols, 10% methoxylated or hydroxylated cinnamic acid, and 6% hydroxylated fatty acids. Health impact Nontoxic and hypoallergic It will be appreciated that variation may be made to the aforementioned embodiments, without departing from the scope of protection as defined by the claims. For example, the method can also be used to extract surface wax from the leaflets of other palm species, including but not limited to washingtonia palm, oil palm, coconut palm, and sugar palm. Wax products produced according to the method may be used to make or incorporated in, a myriad different items or products, including: use in food, cosmetics, automobile and furniture wax and as a coating for dental floss.

Claims

1. A method for producing wax from raw palm material comprising the step of:a) heat treating the separated palm leaflets in a liquid;b) drying the leaflets;c) beating the leaflets;d) separating wax from the remaining residual material from c).

2. A method as claimed in claim 1 wherein step a) comprises treating in the liquid between 80°C to 100°C.

3. A method as claimed in claim 2 step a) comprise boiling in the liquid.

4. A method as claimed in claim 1 to 3 wherein the duration of the heat treatment isfrom 30 minutes to 6 hours, preferably 1 to 5 hours.

5. A method as claimed in claim 2 to 4 wherein the liquid is water or a chemical solution.

6. A method as claimed in claim 5 wherein the solution is an alkaline solution and / or includes surfactants, and / or acidic buffers.

7. A method as claimed in claims 1 to 6 wherein step b) is performed until the moisture level drops below 15%,8. A method as claimed in claims 1 to 7 wherein step c) comprises passing the dry leaflets against a rotating beating blade.9 . A method as claimed in claim 1 to 8 including after step c) the step of chopping pulverizing, or grinding the dried leaves.

10. A method as claimed in claim 1 to 9 wherein step d) performed by at least one of: manual screening, centrifugal air or flotation separation.

11. A method as claimed in claim 1 including further step e) after d) of purifying the wax from the residual vegetable matter.

12. A method as claimed in claim 11 where step e) includes heating the crude wax over its melting point; optionally with stirring.

13. A method as claimed in claim 11 or 12 where step e) comprises dissolving and heating the wax in a solvent, optionally with stirring.

14. A method as claimed in claim 13 where the solvent is one of: xylene, toluene, alkanes, alkaline hydrogen peroxide, ethyl acetate, acetone, benzene, naphthas, alcohols or any other non-polar organic solvent chemical or vegetable-based solvent.

15. A method as claimed in claim 11 to 14 including the step in step e) adding to the melted wax or wax solvent mixture adsorbents; preferably any one or more of: active carbon, silica gel, activated clay,16. A method as claimed in claim 11 to 15 including the step in step e) of filtration by passing the wax solution through paper, cloth, or membrane or by centrifugation.

17. A method as claimed in claim 1 to 16 including a bleach step after step d) and / or e).

18. A method as claimed in claims 1 to 17 including an initial step of separating palm leaflets from palm fronds.14

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