WO2025202965A1 - Procédé d'extraction de cire naturelle - Google Patents

Procédé d'extraction de cire naturelle

Info

Publication number
WO2025202965A1
WO2025202965A1 PCT/IB2025/053254 IB2025053254W WO2025202965A1 WO 2025202965 A1 WO2025202965 A1 WO 2025202965A1 IB 2025053254 W IB2025053254 W IB 2025053254W WO 2025202965 A1 WO2025202965 A1 WO 2025202965A1
Authority
WO
WIPO (PCT)
Prior art keywords
wax
leaflets
palm
fibres
solvent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/IB2025/053254
Other languages
English (en)
Inventor
Mohamad MIDANI
Ahmed HASSANIN
Tamer Hamouda
Said AWAD
Mahmoud MAROUF
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Scaleup Innovations Holdings Ltd
Original Assignee
Scaleup Innovations Holdings Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Scaleup Innovations Holdings Ltd filed Critical Scaleup Innovations Holdings Ltd
Publication of WO2025202965A1 publication Critical patent/WO2025202965A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B11/00—Recovery or refining of other fatty substances, e.g. lanolin or waxes

Definitions

  • 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 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.
  • 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.
  • 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 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 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.
  • United States patent application US 2021/403828A1 (Jena Trading APS) describes a method for separating wax and fibers from plants.
  • Patent application WO 9516013A1 discloses a process for production of Carnauba wax.
  • An object of the present invention is to efficientlyze 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.
  • a method for producing wax from raw palm material comprising the steps 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).
  • step b) is performed until the moisture level drops below 15%. In some embodiments step b) the leaflets are dried until the moisture level drops below 15%.
  • step b) the leaflets are air dried in the shade for 1 -4 days then sun dried for 2 - 4 days.
  • step c) comprises passing the dry leaflets against a rotating beating blade.
  • step c an additional step of chopping pulverizing, or grinding the dried leaves.
  • step d) is performed by at least one of: manual screening, centrifugal air or flotation separation.
  • step e) is applied after d) and includes purifying the wax from the residual vegetable matter.
  • 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. In some embodiments, optionally step e) comprises heating the crude wax powder in a solvent, optionally with stirring.
  • the solvent is from the group comprising: petroleum ether, xylene, toluene, alkanes, alkaline hydrogen peroxide, ethyl acetate, acetone, benzene, naphthas, alcohols or any other nonpolar organic solvent.
  • the solvent extraction is performed using, but not limited to, a Soxhlet extractor, distiller, or CO2 extractor.
  • a Soxhlet extractor distiller, or CO2 extractor.
  • any one or more of: active carbon, silica gel, activated clay and adsorbents are added to the melted wax or wax solvent mixture.
  • the bleach is hydrogen peroxide, sodium hypochlorite, acids such as but not only hydrochloric acid, chromo-sulphuric acid, phosphoric acid, or ozone bleaching or clays such as fullers earth bleaching.
  • Figure 1 is a process flow diagram illustrating steps of extraction of textile fibres and surface wax from palm leaflets
  • Figure 2 is a photograph of leaflet fibres morphology before degumming (left) and after degumming (right);
  • Figure 3 shows an image of palm leaflet fibres after scraping
  • Figure 4 shows an image of palm leaflet fibres after degumming
  • Figure 5 shows an image following wax extraction from a date palm leaflet
  • Figure 6 is an FTIR spectra of the resulting wax after the extraction method which indicates the quality of the extracted wax.
  • the FTIR provides information about functional groups present in a sample based on the absorption of infrared light at different wavelengths.
  • the leaflet wax a natural wax, is composed mainly of fatty acids, and esters.
  • the peaks around 2912 cm -1 , 2848 cm -1 , 1730 cm -1 , and 1 169 cm -1 are particularly indicative of the long-chain hydrocarbon structure of the wax and ester linkages. Some of the peaks at 2219 cm -1 and 2132 cm -1 may be due to impurities.
  • FIG. 1 there is shown a process flow diagram for extraction of textile fibres and surface wax from palm leaflets.
  • 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.
  • 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 for 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 enable the extraction of the surface wax.
  • 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.
  • the scraping method includes feeding the leaflets between two feed rollers into a rotating cylinder with a saw tooth wire, that has a tooth pitch between 6 - 16 teeth per inch, a tooth angle between 40° - 60°, a tooth height 1.5 - 5 mm, and a wire thickness 0.4 - 1 mm.
  • the fibres are heated in diluted sulfuric acid, or 0.2% phosphoric acid solution, or 0.1 M sodium phosphate buffer with pH ranging between 2 - 3 and the temperature ranging between 50 - 100°C and duration 0.5 - 3 hours.
  • 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.
  • an acid pectinase enzyme solution 4 g pectinase powder/ 100 g dry fibres
  • 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.
  • 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.
  • 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.
  • the treatment may include surfactant such as Triton X-100 and/or chelating agent such as Ethylenediaminetetraacetic acid (EDTA).
  • surfactant such as Triton X-100
  • chelating agent such as Ethylenediaminetetraacetic acid (EDTA).
  • the fibres are initially treated in a rich mix of alkaline pectinases enzyme solution, that may include but not limited to, polygalacturonases, pectin esterases, pectin lyases, pectate lyases, and rhamnogalacturonan lyases, at pH 8 - 9 and temperature 45°C - 80°C, for a duration of 2 - 48 hours depending on the treatment temperature.
  • alkaline pectinases enzyme solution that may include but not limited to, polygalacturonases, pectin esterases, pectin lyases, pectate lyases, and rhamnogalacturonan lyases, at pH 8 - 9 and temperature 45°C - 80°C, for a duration of 2 - 48 hours depending on the treatment temperature.
  • the fibres are boiled at 90 - 100 °C for 2 to 3 hours in a solution containing 0.5 - 1 % Sodium hydroxide, 0.1 - 0.5% hydrogen peroxide, 0.3% Ethylenediaminetetraacetic acid, in addition to, 0.3% sodium silicate or 1% sodium sulfite, while maintaining continuous agitation.
  • the fibres are neutralized in a 5% acetic acid solution and then rinsed in water.
  • 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 Figure 4.
  • Table 1 shows average properties of long textile fibres extracted from date palm leaflets after scraping and after degumming using the above methods.
  • 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.
  • 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) heating the crude wax powder in a solvent such as but is not limited to petroleum ether, xylene, toluene, alkanes, alkaline hydrogen peroxide, ethyl acetate, acetone, benzene, naphthas, alcohols or any other non-polar organic solvent.
  • the solvent extraction is performed using, but not limited to, a Soxhlet extractor, distiller, or CO2 extractor.
  • 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.
  • 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, Ozon bleaching or clays such as fullers earth bleaching.
  • 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.
  • 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 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.
  • 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 Figure 5.
  • the FTIR spectra of the resulting wax after the extraction method is shown in Figure 6.
  • 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, automobiles and furniture wax and as a coating for dental floss.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Paper (AREA)

Abstract

La présente invention concerne un procédé d'extraction de cire et plus particulièrement, mais pas exclusivement, l'invention concerne l'extraction de cire de surface à partir de palmes de dattes. Le procédé de production de cire à partir d'un matériau de palme brut comprend les étapes consistant à : traiter thermiquement les feuillets de palme séparés dans un liquide ; et sécher les feuillets. Les feuillets sont ensuite battus, et la cire est séparée du matériau résiduel restant. Facultativement, le matériau résiduel est chauffé dans un liquide entre 80 °C et 100 °C et facultativement cuit.
PCT/IB2025/053254 2024-03-28 2025-03-27 Procédé d'extraction de cire naturelle Pending WO2025202965A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB2404461.2 2024-03-28
GB2404461.2A GB2639925A (en) 2024-03-28 2024-03-28 Method of extraction of natural wax

Publications (1)

Publication Number Publication Date
WO2025202965A1 true WO2025202965A1 (fr) 2025-10-02

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ID=91023435

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2025/053254 Pending WO2025202965A1 (fr) 2024-03-28 2025-03-27 Procédé d'extraction de cire naturelle

Country Status (2)

Country Link
GB (1) GB2639925A (fr)
WO (1) WO2025202965A1 (fr)

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2275660A (en) * 1939-07-17 1942-03-10 Johnson & Son Inc S C Vegetable wax
WO1995016013A1 (fr) 1993-12-10 1995-06-15 Pvp Sociedade Anônima Procede de traitement et de production de cire de carnauba
WO2012108860A1 (fr) 2011-02-07 2012-08-16 Brown Laurence B Ustensile dentaire fabriqué à partir d'une feuille de palmier
US20130149512A1 (en) 2010-05-25 2013-06-13 Ananas Anam Limited Natural Nonwoven Materials
CN204079938U (zh) 2014-08-12 2015-01-07 张乃琼 植物蜡提取系统
WO2020139088A1 (fr) 2018-12-25 2020-07-02 Sultan Qaboos University Préparation de fibres à hautes performances à partir d'une fibre naturelle (palmier dattier)
JP2020532607A (ja) 2016-12-19 2020-11-12 サウジ アラビアン オイル カンパニー 弓形繊維トリオ−中程度から重度の逸泥制御のためのナツメヤシ廃棄物系３成分繊維混合物
US20210403828A1 (en) 2014-06-04 2021-12-30 Jena Trading Aps Separation of wax and fibers from plants
US11370953B2 (en) 2016-06-30 2022-06-28 Saudi Arabian Oil Company Date tree waste-based compound fibrous LCMs
WO2023007223A1 (fr) 2021-07-29 2023-02-02 Nama Women Advancement Establishment Procédé d'extraction de fibres à partir d'un palmier
US20230263182A1 (en) 2020-09-01 2023-08-24 The State Of Israel, Ministry Of Agriculture & Rural Development, Agricultural Research Organization Compositions isolated from date palm tree

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2275660A (en) * 1939-07-17 1942-03-10 Johnson & Son Inc S C Vegetable wax
WO1995016013A1 (fr) 1993-12-10 1995-06-15 Pvp Sociedade Anônima Procede de traitement et de production de cire de carnauba
US20130149512A1 (en) 2010-05-25 2013-06-13 Ananas Anam Limited Natural Nonwoven Materials
WO2012108860A1 (fr) 2011-02-07 2012-08-16 Brown Laurence B Ustensile dentaire fabriqué à partir d'une feuille de palmier
US20210403828A1 (en) 2014-06-04 2021-12-30 Jena Trading Aps Separation of wax and fibers from plants
CN204079938U (zh) 2014-08-12 2015-01-07 张乃琼 植物蜡提取系统
US11370953B2 (en) 2016-06-30 2022-06-28 Saudi Arabian Oil Company Date tree waste-based compound fibrous LCMs
JP2020532607A (ja) 2016-12-19 2020-11-12 サウジ アラビアン オイル カンパニー 弓形繊維トリオ−中程度から重度の逸泥制御のためのナツメヤシ廃棄物系３成分繊維混合物
WO2020139088A1 (fr) 2018-12-25 2020-07-02 Sultan Qaboos University Préparation de fibres à hautes performances à partir d'une fibre naturelle (palmier dattier)
US20230263182A1 (en) 2020-09-01 2023-08-24 The State Of Israel, Ministry Of Agriculture & Rural Development, Agricultural Research Organization Compositions isolated from date palm tree
WO2023007223A1 (fr) 2021-07-29 2023-02-02 Nama Women Advancement Establishment Procédé d'extraction de fibres à partir d'un palmier

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
AL BULUSHI KARIMA ET AL: "Optimisation and economic evaluation of the supercritical carbon dioxide extraction of waxes from waste date palm (Phoenix dactylifera) leaves", JOURNAL OF CLEANER PRODUCTION, ELSEVIER, AMSTERDAM, NL, vol. 186, 17 March 2018 (2018-03-17), pages 988 - 996, XP085376312, ISSN: 0959-6526, [retrieved on 20250611], DOI: 10.1016/J.JCLEPRO.2018.03.117 *
KARIMA AL BULUSHITHOMAS M. ATTARDMICHAEL NORTHANDREW J. HUNT: "Optimisation and economic evaluation of the supercritical carbon dioxide extraction of waxes from waste date palm (Phoenix dactylifera) leaves", vol. 186, 2018, JOURNAL OF CLEANER PRODUCTION, pages: 988 - 996

Also Published As

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GB202404461D0 (en) 2024-05-15
GB2639925A (en) 2025-10-08

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