WO2021074398A1 - Procédé pour produire des microparticules destinées à être utilisées en tant que microbilles et microparticules produites selon le procédé - Google Patents

Procédé pour produire des microparticules destinées à être utilisées en tant que microbilles et microparticules produites selon le procédé Download PDF

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Publication number
WO2021074398A1
WO2021074398A1 PCT/EP2020/079242 EP2020079242W WO2021074398A1 WO 2021074398 A1 WO2021074398 A1 WO 2021074398A1 EP 2020079242 W EP2020079242 W EP 2020079242W WO 2021074398 A1 WO2021074398 A1 WO 2021074398A1
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WIPO (PCT)
Prior art keywords
microparticles
algae
microns
marine
marine macro
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PCT/EP2020/079242
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English (en)
Inventor
James Joseph LEAHY
Susan Claire KEATING
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Seagreen Bio Limited
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Publication of WO2021074398A1 publication Critical patent/WO2021074398A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9706—Algae
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9706—Algae
    • A61K8/9711—Phaeophycota or Phaeophyta [brown algae], e.g. Fucus
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9706—Algae
    • A61K8/9717—Rhodophycota or Rhodophyta [red algae], e.g. Porphyra
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9706—Algae
    • A61K8/9722—Chlorophycota or Chlorophyta [green algae], e.g. Chlorella
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/10—Washing or bathing preparations
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/38—Products in which the composition is not well defined
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns

Definitions

  • the present invention relates to a process for producing microparticles for use as microbeads, and the invention also relates to the microparticles produced according to the process.
  • the invention also relates to a process for producing a personal care product, and to personal care products.
  • Microbeads of plastics material are extensively used as an ingredient in personal care products and cosmetics products. Such microbeads fall within the scope of the more general term “microplastics”.
  • microplastics means particles of plastic material in the solid phase of size up to 1 mm, which are water insoluble and are non-degradable. Microplastics are used in the formulation of a variety of products including but not limited to personal care and cosmetics products, such as toothpaste, shower gel, shampoo, eye shadow, deodorant, blush powders, makeup foundation, skin creams, hairspray, nail polish, liquid makeup, mascara, shaving cream, baby products, facial cleansers, bath products, skincare lotions, sunscreen and hair colouring.
  • personal care and cosmetics products such as toothpaste, shower gel, shampoo, eye shadow, deodorant, blush powders, makeup foundation, skin creams, hairspray, nail polish, liquid makeup, mascara, shaving cream, baby products, facial cleansers, bath products, skincare lotions, sunscreen and hair colouring.
  • the microplastics may be large enough to be visible to the naked eye (for example, 50 microns to 1,000 microns), while others are relatively fine particles (low micron range of 2.5 microns to 50 microns), or very fine particles (typically of size less than 2.5 microns).
  • the microplastic may be of size smaller than 5 microns. Microplastics may be present in personal care products and cosmetics products at different percentages, ranging from a fraction of 1% to 10%, and in some cosmetic products may be higher, while in some domestic and industrial cleansing products may be considerably higher than 10%.
  • microplastic ingredients have been included in formulations with a number of functions including but not limited to: viscosity regulators; emulsifiers; exfoliants; film formers; opacifying agents; liquid absorbent binders; bulking agents, for example, fillers; and optical blurring agents, for example, to reduce appearance of facial lines.
  • the microplastics are commonly referred to as microbeads.
  • the term microbeads generally refers to solid particles of various shapes, for example, spherical, amorphic between 1 micron and 1 ,000 microns (UNEP, 2015 - Plastic in Cosmetics).
  • the filters in wastewater systems do not adequately remove microplastics smaller than 200 microns (EPA 2003), thus allowing many plastic microbeads from cosmetics and personal care products to pass through stormwater, sewage and septic systems and through rivers and streams into marine ecosystems (Browne MA, Crump P, Niven SJ, Teuten EL, Tonkin A, Galloway T, Thompson RC. 2011. Accumulations of microplastic on shorelines worldwide: sources and sinks. Environmental Science and Technology 45:9175-9179).
  • microbeads of non-degradable plastics materials enter the marine environment, they travel freely as aggregates, floating or in suspension in the water column. In the aquatic environment such microbeads of plastics material are consumed by aquatic organisms, potentially entering the human food chain (Wright SL, Thompson RC, Galloway TS. 2013. The physical impacts of microplastics on marine organisms: A review. Environmental Pollution 178:483-492). Estimates of half- lives of microplastics run in the hundreds of years, longer than any persistent organic pollutant (United Nations Environment Programme 2015 - Plastic in Cosmetics).
  • Treated wastewater effluents are also know to contain microplastics (Browne MA, Crump P, Niven SJ, Teuten EL, Tonkin A, Galloway T, Thompson RC. 2011. Accumulations of microplastic on shorelines worldwide: sources and sinks. Environmental Science and Technology 45:9175-9179), including microbeads similar to those contained in some personal care and cosmetics products (Leslie HA, Moester M, de Dreuk M, Vethaak AD. 2012. Exploratory study of the emission of microplastics from wastewater treatment plants. H2014/15: 45-47). Besides effluents, sewage sludge is another important receptacle of microplastics and microbeads from personal care and cosmetics products.
  • microbeads there are many channels through which microbeads can enter the food chain for subsequent ingestion by humans.
  • the ingestion of micro-particles of plastics material is increasingly recognised as having a range of adverse health effects on humans.
  • microbeads which are suitable for use as an ingredient in personal care and cosmetic products, as well as domestic and industrial cleanser products, and other products, which are biodegradable, and which preferably, are marine biodegradable.
  • the present invention is directed towards providing microparticles for use as microbeads, and to a process for producing the microparticles.
  • the invention is also directed towards a process for producing personal care products, and to personal care products comprising the microparticles.
  • a process for producing microparticles for use as microbeads comprising chopping marine macro-algae into pieces of an intermediate size, and mechanically processing the pieces of the intermediate size to produce the microparticles of size not exceeding 1,000 microns.
  • the pieces of intermediate size, into which the marine macro-algae is chopped are of maximum dimension not exceeding 20mm.
  • the pieces of intermediate size, into which the marine macro-algae is chopped are of maximum dimension lying in the range of 0.8mm to 20mm, and preferably, are of maximum dimension not exceeding 15mm, and advantageously, are of maximum dimension not exceeding 10mm, and ideally, are of maximum dimension not exceeding 5mm.
  • the pieces of intermediate size, into which the marine macro-algae is chopped are of maximum dimension lying in the range of 0.8mm to 5mm, and advantageously, lying in the range of 0.8mm to 3mm, and ideally, lying in the range of 0.9mm to 2.5mm.
  • the marine macro-algae is chopped in a mechanical chopper to produce the pieces of the intermediate size, and preferably, the marine macro-algae is chopped to produce the pieces of the intermediate size in a chopping drum.
  • the size of the microparticles lies in the range of 1 micron to 1,000 microns, and advantageously, lies in the range of 2.5 microns to 800 microns, and ideally, lies in the range of 10 microns to 600 microns.
  • the size of the microparticles is selected to suit the function to be fulfilled by the microparticles.
  • microparticles are configured for use in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns.
  • microparticles are configured for use in a personal care cleansing product for cleansing the face and other sensitive parts of a human subject, and the size of the microparticles lies in the range of 100 microns to 180 microns.
  • the microparticles are configured for use in a personal care product for cleansing the hands and other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns. In another embodiment of the invention the microparticles are configured for use in a body scrub product for scrubbing the human body, and the size of the microparticles lies in the range of 300 microns to 600 microns.
  • microparticles are configured for use in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350_microns.
  • microparticles are configured for use in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns. In another embodiment of the invention the microparticles are configured for use in a cosmetic product, and the size of the microparticles is less than 100 microns.
  • the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 100 microns.
  • the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 50 microns.
  • microparticles are of spherical or partly spherical shape.
  • each microparticle comprises a solid microparticle.
  • each microparticle comprises a homogeneous microparticle.
  • the pieces of the marine macro-algae of the intermediate size are mechanically processed in a milling process to produce the microparticles of size not exceeding 1,000 microns.
  • the milling process to which the pieces of the marine macro-algae of the intermediate size are subjected to produce the microparticles of size not exceeding 1 ,000 microns is carried out in either a ball mill or a hammer mill.
  • the marine macro-algae is desalted.
  • the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 7% by weight.
  • the marine macroalgae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 5% by weight.
  • the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 3% by weight. More preferably, the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2.5% by weight.
  • the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2% by weight.
  • the marine macro-algae is desalted by immersing and soaking the marine macro-algae in fresh water.
  • the marine macro-algae is desalted prior to chopping thereof to form the pieces of the intermediate size.
  • the desalted marine macro-algae is dried in a first drying process to a predefined moisture content of less than 10% by weight.
  • the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 5% by weight.
  • the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 3% by weight.
  • the marine macro-algae is dried during the first drying process in dehumidified warm air.
  • the desalted marine macro-algae is dried in the first drying process prior to chopping of the marine macro-algae into the pieces of the intermediate size.
  • the marine macro-algae is de-oiled.
  • the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.5% by weight.
  • the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.3% by weight.
  • the marine macro-algae is de-oiled to reduce the oil content thereof to not more than 0.1% by weight.
  • the marine macro-algae is de-oiled by one of a solvent extraction process, a supercritical extraction process and a mechanical pressing process.
  • the marine macro-algae is de-oiled in a solvent extraction process.
  • the oil extracted from the de-oiling of the marine macro-algae is recovered and saved.
  • the marine macro-algae is de-oiled after the marine macro-algae has been desalted.
  • the marine macro-algae is de-oiled after the marine macro-algae has been chopped into the pieces thereof of the intermediate size.
  • the marine macro-algae is de-oiled after the drying thereof in the first drying process.
  • the marine macro-algae is de-oiled prior to the mechanical processing of the marine macro-algae to form the microparticles.
  • the de-oiled marine macro-algae is dried in a second drying process.
  • the de-oiled marine macro-algae is dried in the second drying process until any residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 5% by weight.
  • the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 1% by weight.
  • the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro- algae has been reduced to not more than 0.1 % by weight, and ideally, until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 0.01% by weight.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out under vacuum.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 100 mbar absolute pressure.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 40 mbar absolute pressure.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 20 mbar absolute pressure.
  • the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 45°C.
  • the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 40°C.
  • the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 35°C.
  • the de-oiled marine macro-algae is dried during the second drying process at a temperature of approximately 35°C.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out in a convection oven.
  • the drying ofthe de-oiled marine macro-algae in the second drying process is carried out prior to the mechanical processing ofthe marine macro-algae to form the microparticles.
  • the marine macro-algae is bleached.
  • the marine macro-algae is bleached afterthe marine macro-algae has been formed into the microparticles.
  • the microparticles are bleached.
  • the bleaching of the marine macro-algae is carried out with an oxidising agent.
  • the oxidising agent comprises a mild oxidising agent.
  • the oxidising agent comprises one or more of the following oxidising agents: hydrogen peroxide (H 2 0 2 ); sodium percarbonate (Na 2 C0 .5H 2 0 2 ); sodium perborate (NaB0 3 -nH 2 0); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca(OCI) 2 ); Zinc Dust (Zn); Thiourea dioxide (CH 4 N 2 0 2 S); Sodium Dithionite(Na 2 S 2 0 4 ).
  • the marine macro-algae may be selected from any suitable marine macro-algae, or any suitable combination of marine macro-algae.
  • the marine macro-algae may be selected from any one or more of brown marine macro-algae, green marine macro-algae and red marine macro-algae.
  • Suitable brown marine macro-algae for example, are ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca.
  • Suitable green marine macro-algae for example, are porphyra dioica; cladophora rupestris; codium tomentosum; ulva intestinalis; ulva fenestrate.
  • Suitable red marine macro-algae for example are calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa.
  • brown, green and red marine macro-algae is not to be considered as being exhaustive or limiting, it is given solely as an example of suitable marine macro-algae.
  • the marine macro-algae comprises ascophyllum.
  • the invention also provides microparticles produced from the marine macro-algae according to the process according to the invention.
  • the microparticles are of size lying in the range of 1 micron to 1,000 microns.
  • the microparticles are of size lying in the range of 2.5 microns to 800 microns.
  • the microparticles are of size lying in the range of 10 microns to 600 microns.
  • the microparticles are configured for use in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns.
  • the microparticles are configured for use as microbeads in a personal care cleansing product for use on the face and on other sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 180 microns.
  • microparticles are configured for use as microbeads in a personal care cleansing product for use on the hands and on other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns.
  • microparticles are configured for use as microbeads in a personal care body scrub product, and the size of the microparticles lies in the range of 300 microns to 600 microns.
  • microparticles are configured for use as microbeads in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns. In another embodiment of the invention the microparticles are configured for use as microbeads in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350 microns.
  • the microparticles are configured for use as a microbead filler in a cosmetic product, and the size of the microparticles are less than 100 microns, and preferably, the size of the microparticles is less than 50 microns.
  • microparticles are configured for use as microbeads in a household domestic cleansing product, and the microparticles are of size lying in the range of 100 microns to 500 microns.
  • the microparticles are configured for use as microbeads in an industrial cleansing product, and the microparticles are of size lying in the range of 100 microns to 900 microns.
  • the invention provides a process for producing a personal care product comprising mixing the microparticles produced by the process according to the invention with a composition suitable for the personal care product.
  • the personal care product comprises a cosmetics product, the process comprising mixing the microparticles with a composition suitable for the cosmetic product.
  • the personal care product comprises an exfoliant product the product comprising mixing the microparticles with a composition suitable for the exfoliant product.
  • the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body, the process comprising mixing microparticles with a suitable cleansing composition.
  • the personal care product comprises a cleansing product for use on the hands and on other less sensitive parts of the human body, the process comprising mixing the microparticles with a suitable cleansing composition.
  • the personal care product comprises a body scrub product, the process comprising mixing the microparticles with a suitable body scrub composition.
  • the personal care product comprises a dentifrice
  • the process comprises mixing the microparticles with a suitable dentifrice composition.
  • the personal care product comprises a filler
  • the process comprises providing the microparticles as the filler, and mixing the microparticles with a suitable composition for producing the personal care product.
  • the oil recovered and saved from the de-oiling of the marine macro-algae is mixed with the microparticles and the composition.
  • the invention provides a personal care product comprising the microparticles produced by the process according to the invention.
  • the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body.
  • the personal care product comprises a cleansing product for use on the hands and other less sensitive parts of the human body.
  • the personal care product comprises a body scrub.
  • the personal care product comprises an exfoliant product.
  • the personal care product comprises a dentifrice.
  • the personal care product comprises a cosmetic product, and the microparticles form a filler in the cosmetic product.
  • the invention also provides a household domestic cleansing product comprising the microparticles produced by the process according to the invention.
  • the invention provides an industrial cleansing product comprising the microparticles produced by the process according to the invention.
  • microparticles according to the invention are many.
  • a particularly important advantage of the microparticles according to the invention is that the microparticles are biodegradable, and in particular, are marine biodegradable. Accordingly, when returned to the sea or ocean, the microparticles readily biodegrade, and cause no harm to the marine ecosystem. Indeed, it is believed that once the microparticles according to the invention enter the waste water system, the microparticles commence to biodegrade.
  • the microparticles according to the invention on entering the waste water system commence to biodegrade, and biodegrading of the microparticles is completed in the ocean, thereby avoiding the microparticles entering the food chain in particulate form. Even if the microparticles are ingested by marine life, the microparticles, being of marine micro-algae, are digestible, and therefore are unlikely to have any adverse effect on marine life, animal life or human life.
  • a further important advantage of the invention is also achieved when products, and in particular personal care products comprising the microparticles according to the invention also include the oil extracted from the ascophyllum, in that since the extracted oil is a marine product, it likewise readily biodegrades in a marine environment when returned thereto, and furthermore in many cases depending on the type of marine macro-algae from which the microparticles are produced, and from which the oil is extracted, the extracted oil may have beneficial health effects as well as anti-inflammatory effects.
  • the advantage of bleaching the marine macro-algae after de-oiling thereof is twofold. Firstly, the oil is extracted from the marine macro-algae without any danger of the oil being contaminated by the bleaching agent or agents, and secondly, the oil in many marine macro-algae tends to be of a relatively dark colour, and therefore, by bleaching the marine macro-algae after de-oiling thereof, the amount of the bleaching agent required is significantly reduced.
  • a particularly important advantage is achieved by deferring the bleaching of the marine macro-algae until the microparticles have been formed, since this reduces in many cases the volume of the marine macroalgae requiring bleaching, since for some applications, to which the microparticles are put, bleaching may not be required. Whether to bleach or not to bleach the marine macro-algae microparticles will to some extent be dependent on the use to which the microparticles will be put.
  • microparticles according to the invention are produced for use as microbeads in personal care products, such as, body scrubs, cosmetic products, fillers for cosmetic products, exfoliant products, dentifrice products, personal cleansing products and other cleansing products and the like, for the human or animal body, and in particular, for the human body.
  • personal care products such as, body scrubs, cosmetic products, fillers for cosmetic products, exfoliant products, dentifrice products, personal cleansing products and other cleansing products and the like, for the human or animal body, and in particular, for the human body.
  • microparticles produced according to the invention are also of size suitable for use in a dentifrice, shower gel, shampoo, eye shadow, deodorant, blush powders, makeup foundation, skin creams, hairspray, nail polish, liquid makeup, mascara, shaving cream, baby products, facial cleansers, bath products, skincare lotions, sunscreen, and hair colouring products, as well as other cosmetic and healthcare products, and personal cleansing products.
  • the microparticles produced according to the invention are also of size suitable for use in domestic household cleansing products, and in industrial cleansing products.
  • the microparticles according to the invention are solid microparticles and are substantially homogeneous throughout, and are produced from marine macro-algae, which in this case comprises ascophyllum.
  • the ascophyllum is harvested from the North Atlantic Ocean.
  • the marine macroalgae may comprise any suitable marine macro-algae or any suitable combination of marine macro-algae.
  • the marine macro-algae may be selected from any one or more of brown, green or red marine macro-algae.
  • suitable brown marine macro-algae may, for example, be any of ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca.
  • Suitable green marine macro-algae for example, are porphyradioica; cladophora rupestris; codiumtomentosum; ulva intestinalis; ulva fenestrate.
  • Suitable red marine macro-algae are calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa.
  • suitable marine macro-algae of the type commonly referred to as seaweed, may be used.
  • the marine macro-algae may be harvested from any other suitable ocean or sea instead of the North Atlantic Ocean.
  • the process according to the invention comprises a number of steps in order to produce the microparticles according to the invention from the marine macro-algae, comprises a number of steps, which will now be described with reference to the drawing.
  • Block 1 of the drawing represents the first step in the process for producing the microparticles from the marine macro-algae, and in the first step, the marine macro-algae is harvested from the North Atlantic Ocean, and in this embodiment of the invention has been harvested from the Irish coastline.
  • a desalting process represented by block 2 of the drawing.
  • the harvested marine macro-algae is subject to two desalting processes. In both desalting processes the marine macro-algae is subjected to two soaks in fresh water at ambient temperature in respective baths.
  • the marine macro-algae is sequentially immersed in the respective baths of fresh water for respective first and second predefined time periods each of approximately 120 minutes.
  • the marine macro-algae While immersed in the first bath during the first time period, the marine macro-algae is periodically agitated by pressing it down into the fresh water in the bath, to ensure that it is fully immersed in the fresh water in the bath.
  • the marine macro-algae is transferred from the first bath into the second bath and is immersed in fresh water in the second bath for a second predefined time period of 120 minutes, during which time it is also periodically agitated by pressing it down into the fresh water.
  • the marine macro-algae is removed from the second bath, and at that stage should have a salt content not exceeding 2% by weight.
  • the baths are recharged with fresh water prior to each soak of the marine macro-algae therein.
  • first and second predefined time periods have been described as being of equal duration, it is envisaged that the first and second predefined time periods may be the same or different.
  • the first predefined time period may be of duration lying in the range of 60 minutes to 180 minutes, while the duration of the second predefined time period may lie in the range of 90 minutes to 150 minutes.
  • the desalted marine macro-algae is then subjected to a first drying process as indicated by block 3 of the drawing.
  • the desalted marine macro-algae is suspended from racks, and a stream of warm dehumidified air at a temperature in the range of 25°C to 40°C is passed over the suspended desalted marine macroalgae.
  • the first drying process continues until the moisture content of the dry desalted marine macro- algae is reduced to less than 5% by weight, and preferably, is reduced to 3% by weight.
  • the dried desalted marine macro-algae is then subjected to a chopping process as indicated by block 4 of the drawing.
  • the chopping process is carried out in a multi-bladed drum chopper, and the drum chopper is configured to chop the dried marine macro-algae into pieces of an intermediate size of maximum dimension not exceeding 20mm, and preferably, of maximum dimension not exceeding 5mm, and advantageously, of maximum dimension lying in the range of 0.9mm to 2.5mm.
  • the chopped pieces of the marine macro-algae of the intermediate size are de-oiled as indicated by block 5 of the drawing whereby the oil content of the marine macro-algae pieces is reduced to approximately 0.1 % by weight or less.
  • the de-oiling process whereby the marine macro-algae is de-oiled may be carried out by any suitable process, for example, a solvent extraction process, a mechanical pressing process, a supercritical extraction process, or any other suitable process.
  • the de-oiling of the marine macro-algae is carried out by a solvent extraction process, and the extracted oil is recovered and saved.
  • the marine macro-algae pieces are subjected to a second drying process as indicated by block 6 of the drawing in order to reduce the residual solvent content in the marine macro-algae pieces remaining after the de-oiling process.
  • the second drying process in this embodiment of the invention is carried out in a convection oven under vacuum at a pressure not greater than 20 mbar absolute pressure, at a temperature of approximately 35°C.
  • the second drying process of block 6 is continued until the residual solvent content of the de-oiled marine macro-algae does not exceed 0.1% by weight, and preferably, does not exceed 0.01% by weight.
  • the second drying process of block 6 may be carried out at higher temperatures, it is preferable that the second drying process temperature should not exceed 45°C, and more preferably, the drying temperature should not exceed 40°C. A maximum drying temperature of 35°C is most preferable in order to avoid any chemical change in the marine macro-algae, which could reduce its biodegradability.
  • the dried, de-oiled marine macro-algae pieces are subjected to a mechanical process indicated by block 7 of the drawing, whereby the marine macro-algae pieces are reduced in size to form the microparticles.
  • the mechanical process of block 7 for reducing the marine macro-algae pieces to form the microparticles comprises a milling process, and is carried out in either a ball mill or a hammer mill.
  • the ball or hammer mill typically produces the microparticles to be of a spherical or a partly spherical shape, and since the microparticles are produced from marine macro-algae, the microparticles are essentially solid microparticles and are also homogeneous microparticles.
  • the ball or hammer mill is configured to produce the microparticles of selectable sizes up to 1,000 microns.
  • the size of the microparticles produced by the ball or hammer mill is dependent on the uses to which the microparticles are to be put.
  • the microparticles may be produced to be of a substantially constant size, or may be produced in ranges of sizes, depending on the use to which the microparticles are to be put. However, in general, the microparticles are produced to be of size in the range of 1 micron to 1 ,000 microns.
  • the microparticles are for use in a cleansing product or other personal care product for use on the sensitive parts of the human body, for example, the face and other such sensitive parts of the human body, the microparticles typically are formed to be of size lying in the range of 100 microns to 180 microns.
  • the microparticles are for use in a cleansing product, for example, soaps, both liquid and solid, or other personal care cleansing products for use on less sensitive parts of the human body, for example, the hands of the human body, typically, the microparticles are formed to be of size lying in the range of 100 microns to 350 microns.
  • the microparticles are formed to be of size lying in the range of 300 microns to 600 microns.
  • the microparticles are for use as a functional filler in a personal care product, or a cosmetics product, the microparticles are formed to be of size lying in the range of 2.5 microns to 50 microns, and in some filler applications up to 100 microns.
  • the microparticles are for use in a personal care exfoliant product, the microparticles are formed to be of size lying in the range of 100 microns to 600 microns.
  • the microparticles are for use in a dentifrice product, the microparticles are formed to be of size lying in the range of 100 microns to 350 microns.
  • the microparticles may be subjected to a process indicated by block 8 of the drawings, whereby the microparticles are subjected to a bleaching process, in order to whiten the microparticles so that they will visually blend in with other ingredients of the composition in which the microparticles are to be one of the ingredients. It is envisaged that the microparticles produced for use in certain personal care and cosmetic products will be subjected to the bleaching process.
  • the bleaching of the microparticles is carried out by the process of block 8 using a mild oxidising agent, which may be any one or more of the following oxidising agents: hydrogen peroxide (H 2 0 2 ); sodium percarbonate (Na 2 C0 .5H 2 0 2 ); sodium perborate ( NaB0 3 -nH 2 0); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca(OCI) 2 ); Zinc Dust (Zn); Thiourea dioxide (CH 4 N 2 0 2 S); Sodium Dithionite(Na 2 S 2 0 4 ).
  • a mild oxidising agent which may be any one or more of the following oxidising agents: hydrogen peroxide (H 2 0 2 ); sodium percarbonate (Na 2 C0 .5H 2 0 2 ); sodium perborate ( NaB0 3 -nH 2 0); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca
  • the bleaching process may be omitted.
  • the invention also provides a process for producing a personal care product according to the invention, for example, a cleansing product for use in cleansing of the skin of the human or animal body, which may be a cleansing product for sensitive skin, for example, the face and other such sensitive parts of the body, or a less sensitive part of the body, for example, the hands of a subject.
  • a cleansing product for use in cleansing of the skin of the human or animal body which may be a cleansing product for sensitive skin, for example, the face and other such sensitive parts of the body, or a less sensitive part of the body, for example, the hands of a subject.
  • the process for producing a personal care product may also include personal care products, such as, for example, cosmetic products, body scrubs, exfoliant products, dentifrices, shampoos, foundation creams, moisturising creams and the like.
  • the process according to the invention for producing such personal care products comprises mixing the microparticles produced by the process according to the invention described with reference to the drawing with a suitable cleansing composition or other suitable relevant composition depending on the product being produced.
  • a suitable cleansing composition or other suitable relevant composition depending on the product being produced.
  • the microparticles will be selected to be of a suitable size, and typically, will be selected to be in the range of 100 microns to 180 microns.
  • the microparticles In producing a personal care product for cleansing the hands and other less sensitive parts of the human body, the microparticles will be selected to be of a suitable size, and typically, will be selected to be in the range of 100 microns to 350 microns.
  • the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size in the range of 300 microns to 600 microns.
  • the microparticles will be selected to be of a suitable size, and typically, will be of size in the range of 100 microns to 350 microns.
  • the microparticles In producing an exfoliant product, the microparticles will be selected to be of a suitable size, and typically, will be of size in the range of 100 microns to 600 microns. In producing a cosmetic product, the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size less than 100 microns, and where the microparticles are to provide a filler for a cosmetic product, the microparticles will be selected to be of size less than 50 microns.
  • the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size lying in the range of 100 microns to 500 microns.
  • the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size in the range of 100_microns to 900 microns.
  • the microparticles will constitute in the range of 2% by weight to 25% by weight ofthe total weight of the above described personal care products, cosmetic products, dentifrices, body scrub products, household domestic cleansing products and industrial cleansing products, although in the majority of personal care products, in general, it is envisaged that the microparticles will constitute in the range of 2% to 10% by weight ofthe total weight ofthe personal care product.
  • the process according to the invention for producing a personal care product according to the invention may also comprise mixing the recovered and saved extracted oil from the marine macro-algae during the de-oiling process with the mixture ofthe microparticles and the cleansing composition and/or other relevant composition to produce personal care products, dentifrices, cosmetic products, personal cleansing products, household domestic cleansing products and industrial cleansing products also according to the invention. It is believed that the personal care and cleansing products comprising the recovered and saved oil may have anti-inflammatory properties for topical applications. It is expected that the proportion ofthe recovered and saved oil in the products, in general, will lie in the range of 0.1% by weight to 0.5% by weight ofthe total weight ofthe product.
  • personal care products according to the invention including the microparticles according to the invention will include many different types of personal care products, for example, shower gels, shampoos, eye shadows, deodorants, blush powders, makeup foundations, skin creams, moisturising creams, hair sprays, nail polish, nail polish removers, liquid makeup, mascara, shaving creams, baby products, facial cleansers, bath products, skincare lotions, sunscreens, anti-aging products and hair colouring products to name but a few, all of which will be according to the invention.
  • shower gels for example, shower gels, shampoos, eye shadows, deodorants, blush powders, makeup foundations, skin creams, moisturising creams, hair sprays, nail polish, nail polish removers, liquid makeup, mascara, shaving creams, baby products, facial cleansers, bath products, skincare lotions, sunscreens, anti-aging products and hair colouring products to name but a few, all of which will be according to the invention.
  • the microparticles may be used to fulfil many functions including but not limited to: viscosity regulators; emulsifiers; exfoliants; film formers; opacifying agents; liquid absorbent binders; bulking agents, for example, fillers; and optical blurring agents, for example, to reduce the appearance of facial lines.
  • viscosity regulators for example, viscosity regulators
  • emulsifiers for example, emulsifiers
  • exfoliants emulsifiers
  • film formers e.g., opacifying agents
  • liquid absorbent binders e.g., opacifying agents
  • bulking agents for example, fillers
  • optical blurring agents for example, to reduce the appearance of facial lines.
  • the size of the microparticles will be selected to be suitable for the type of products in which they are for use, and the functions for which they are to fulfil.
  • the microparticles according to the invention may be used in any other product or application, where microbeads are required
  • the marine macro-algae has been described as being chopped into pieces of specific intermediate size, it is envisaged that the marine macro-algae may be chopped into intermediate sizes of any suitable size. Needless to say, any other suitable means for chopping the marine macro-algae into pieces of intermediate size may be used besides a drum chopper.
  • the desalting of the marine macro-algae may be carried out at any suitable time in the process, and may be carried out before or after chopping the marine macro-algae into pieces of the intermediate size, and in some embodiments of the invention it is envisaged that the desalting of the marine macro-algae may be carried out after de-oiling thereof.
  • any other suitable mechanical processing may be used for producing the microparticles besides a ball mill or a hammer mill.
  • other suitable milling processes may be used for producing the microparticles besides a ball mill or a hammer mill.
  • the de-oiling process is carried out by a de-oiling process not based on a solvent extraction process, for example, a mechanical pressing process or a supercritical fluid extraction process, it is envisaged that the second drying process of block 6 may be omitted.
  • microparticles have been produced from ascophyllum, and the oil extract has also been produced from ascophyllum, it is envisaged that the microparticles may be produced from any other suitable marine macro-algae, and likewise, the oil extract may be extracted from any other marine macro-algae.
  • the microparticles and the extracted oil may be formed, and extracted, respectively, from any one or more of the following marine macro-algae: ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca; porphyra dioica; cladophora rupestris; codiumtomentosum; ulva intestinalis; ulva fenestrate; calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa, and any other suitable marine macro-algae.
  • marine macro-algae ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamaris
  • the marine macro-algae may be desalted by any other suitable desalting process.
  • the first drying process whereby the desalted marine macroalgae is dried may be carried out by any other suitable drying process, and may be carried out at any other suitable drying temperatures.
  • the drying of the de-oiled marine macro-algae which is carried out in the second drying process may be carried out by any other suitable drying process.
  • bleaching of the microparticles may not be required, for example, bleaching of the microparticles for use in domestic and industrial cleansing and detergent products may be unnecessary, and it will also be appreciated that the bleaching of the marine macro-algae may be carried out at any other suitable part of the process.

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Abstract

L'invention concerne un procédé de production de microparticules à partir de macroalgues marines destinées à être utilisées en tant que microbilles qui consiste à dessaler des macroalgues marines et à sécher les macroalgues marines dessalées. Les macroalgues marines dessalées et séchées sont ensuite soumises à un procédé de hachage qui hache les macroalgues marines en morceaux de dimension maximale, d'approximativement 5 mm. Les morceaux hachés des macroalgues marines sont ensuite soumis à un procédé de déshuilage mis en œuvre par un procédé d'extraction par solvants. Les morceaux déshuilés des macroalgues marines sont ensuite soumis à un second procédé de séchage pour réduire leur teneur en solvants. Les morceaux déshuilés séchés des macroalgues marines sont traités dans un broyeur à boulets pour produire les microparticules de taille située dans la plage allant de 1 micron à 1 000 microns, en fonction de l'utilisation à laquelle sont destinées les microparticules. Pour des produits de nettoyage de soins personnels, les microparticules sont produites de sorte à avoir une taille située dans la plage allant de 100 microns à 600 microns. Les microparticules peuvent être blanchies.
PCT/EP2020/079242 2019-10-18 2020-10-16 Procédé pour produire des microparticules destinées à être utilisées en tant que microbilles et microparticules produites selon le procédé WO2021074398A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023734A (en) * 1974-10-18 1977-05-17 Herve Rene A Method and apparatus for communiting marine algae and the resulting product
WO2017205586A1 (fr) * 2016-05-27 2017-11-30 Corning Incorporated Microbilles biodégradables

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023734A (en) * 1974-10-18 1977-05-17 Herve Rene A Method and apparatus for communiting marine algae and the resulting product
WO2017205586A1 (fr) * 2016-05-27 2017-11-30 Corning Incorporated Microbilles biodégradables

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ANNA LENA KLEIN: "Algae-Based Bioplastics", 1 January 2019 (2019-01-01), XP055765982, Retrieved from the Internet <URL:https://www.junge-wissenschaft.ptb.de/fileadmin/paper/2019/06/JUWI_06-2019_Klein.pdf> [retrieved on 20210118], DOI: 10.7795/320.201906 *
BROWNE MACRUMP PNIVEN SJTEUTEN ELTONKIN AGALLOWAY TTHOMPSON RC: "Accumulations of microplastic on shorelines worldwide: sources and sinks", ENVIRONMENTAL SCIENCE AND TECHNOLOGY, vol. 45, 2011, pages 9175 - 9179
FYTILI DZABANIOTOU A: "Utilization of sewage sludge in EU application of old and new methods - A review", RENEWABLE AND SUSTAINABLE ENERGY REVIEWS, vol. 12, 2008, pages 116 - 140, XP022289925, DOI: 10.1016/j.rser.2006.05.014
GEORGE DECKNER: "Finding Alternatives to Synthetic Exfoliating Beads", PROSPECTOR, 28 February 2014 (2014-02-28), XP002764466, Retrieved from the Internet <URL:http://knowledge.ulprospector.com/369/pcc-finding-alternatives-synthetic-exfoliating-beads/> [retrieved on 20210118] *
JUSTYNA KOZLOWSKA; WERONIKA PRUS; NATALIA STACHOWIAK: "Microparticles based on natural and synthetic polymers for cosmetic applications", INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES, vol. 129, 15 May 2019 (2019-05-15), pages 952 - 956, XP009525008 *
NAOHIRO KATO: "Production of crude bioplastic-beads with microalgae: Proof-of-concept", BIORESOURCE TECHNOLOGY REPORTS, vol. 6, 1 June 2019 (2019-06-01), pages 81 - 84, XP055765933, ISSN: 2589-014X, DOI: 10.1016/j.biteb.2019.01.022 *
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