WO2013019095A1 - Fils d'ambre composites - Google Patents

Fils d'ambre composites Download PDF

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Publication number
WO2013019095A1
WO2013019095A1 PCT/LV2012/000010 LV2012000010W WO2013019095A1 WO 2013019095 A1 WO2013019095 A1 WO 2013019095A1 LV 2012000010 W LV2012000010 W LV 2012000010W WO 2013019095 A1 WO2013019095 A1 WO 2013019095A1
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WO
WIPO (PCT)
Prior art keywords
amber
succinite
composite
particles
matrix
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Application number
PCT/LV2012/000010
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English (en)
Russian (ru)
Inventor
Инга ЛАСЕНКО
Марис ЗАМОВСКИС
Татьяна ЕРЕМКИНА
Original Assignee
Lasenko Inga
Zamovskis Maris
Eremkina Tatiana
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
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Application filed by Lasenko Inga, Zamovskis Maris, Eremkina Tatiana filed Critical Lasenko Inga
Publication of WO2013019095A1 publication Critical patent/WO2013019095A1/fr

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides

Definitions

  • the development relates to the field of textile production, and relates to the creation of composite amber threads, where the main component is technologically processed amber, the particles of which are evenly distributed in the polymer matrix.
  • the developed composite amber threads are designed to expand the range of textile materials, and are also applicable as a prophylactic material for various skin changes, including those that improve the skin condition in the presence of diabetes mellitus and for the production of surgical textiles.
  • Powdered functional minerals according to [0004] possess: antimicrobial, absorbing, moisture-absorbing properties, are able to emit in the far infrared region, delay electromagnetic waves, ultraviolet rays, emit negative ions, and prevent the accumulation of static electricity [1-8].
  • the particles of powdered functional minerals used in [0004] have various crystalline shapes in the form of polygonal spatial shapes such as prismatic, pyramidal, rhombohedral, hexagonal, octagonal or twelve-sided, which does not allow to obtain fiber with smooth surface resulting fiber “cutting” is provoked both in the process of its production and in the process of its operation [2, 5, 9].
  • particles of powdered functional minerals are mainly located on the surface of the fiber, which during the production of fibers accelerates the wear of elements of production equipment, because fibers work with respect to production equipment on the principle of abrasive material.
  • the aim of the present invention is to create a new type of product, composite amber threads, with an optimized content of technologically processed amber, particles of which are uniformly integrated into the matrix of the thermoplastic polymer and / or the content of additional components, threads with a smooth surface, which do not provoke allergic reactions, formation blood clots that reflect ultraviolet rays and are biocompatible with living tissue.
  • the product is a composite amber yarn (Fig. 1 pos. 1) containing technologically processed amber, preferably succinite (Fig. 1 pos. 2), with particles of a spherical shape and a size of 300-1000 cn, crushed to a grain size of less than 1/3 of the specified fineness of the filament fiber, uniformly integrated into the matrix of the thermoplastic polymer, preferably polyamide 66 (PA66) ( Figure 1, item 3), with the following ratio of components (March.%):
  • PA66 polyamide matrix
  • the product is a composite amber yarn (Figure 2, item 4) containing technologically processed amber, preferably succinite (Figure 2 item 5), with particles of a spherical shape and a size of 300-1000 sp, crushed up to a grain size of less than 1/3 of the specified filament fiber fineness uniformly integrated into the matrix of the thermoplastic polymer, more preferably polyamide 66 (PA66) ( Figure 2, item 6), and particles of an organic or inorganic compound ( Figure 2, item 7) in the following ratio components (March.%):
  • the invention is illustrated by drawing N ° 2.
  • PA66 6 - polyamide matrix
  • the term “technologically processed amber” means amber processed under the influence of: physical factors (micronization process), chemical factors (dissolution in solvents, alcohols, acids, oil), either physical and chemical factors. It is preferable to process amber under the influence of physical factors, which allows preserving the structure of individual particles of amber, characteristic of a holistic stone.
  • the method for producing composite amber yarns containing technologically processed succinite is that succinite is preliminarily purified by flotation, the succinite granules are dried at t ° +45 - + 60 ° ⁇ for 10 minutes, and the succinite granules are purified from crystals and mineral grains by the method of two-stage micronization in an Ar gas medium at a temperature of + 20 ° C at a processing speed of 150 - 250 rpm.
  • succinite microparticles within 50 to 350 minutes, sifting succinite microparticles to inorganic impurities in the microparticles up to 3%, fine grinding of succinite particles is carried out in an atmosphere of superheated steam, at a flow speed of 900-1200 m / s; secondary extrusion of the synthesized composite material in the main extruder for 5 minutes at an extrusion temperature of t ° + 235 + 255 ° ⁇ ; spinning of a thread from a mixture of technologically processed succinite with spherical particles and a polymer.
  • the PA66 polymer chain consists of the same units of linear polyamides parallelized along a filament (low entropy) [10], in the matrix of which succinite nanoparticles are introduced according to the principle of dosed conclusion, however, the relationship between the components of the units of linear polyamides 66 and particles of succinite is physical.
  • Amber is a high molecular weight organic acid compound containing an average of 79% carbon, 10.5% hydrogen, 10.5% oxygen.
  • the main structural elements of amber are compounds of the aromatic and hydroaromatic series with condensed nuclei, which contain conjugated double bonds of carboxyl, hydroxyl and ester groups.
  • - soluble organic acids can be isolated: succinic acid, succinoabietic acid, abietic acid; levopimaric, palustrinic, neo-abietic, dextropimaric and isodextropimaric acids; dehydroabietic, isodextropimaric, dehydroisopimaric, sandaracopymaric, diagenic acid;
  • amber processing is a complex process.
  • the main part of amber has a three-dimensional structure with rare crosslinking, which is destroyed by heating and mechanical stress due to the breaking of chemical bonds with the formation of free radicals [12].
  • volatile compounds and gases are released from amber, such as ⁇ 0 2 , ⁇ , ⁇ 2 , H 2 S, 0 2 , ⁇ ⁇ ⁇ 2 ⁇ + 2 (saturated hydrocarbons), ⁇ p H 2p (unsaturated hydrocarbons), C 4 H 6 0 4 succinic acid, etc.
  • solubility of individual amber varieties in organic compounds is not the same (from 6% - 63%), in some cases, solubility is a function of different intensities of fossilization processes. Under normal conditions, amber is insoluble in water [13].
  • step a When performing [0018] step a), it is known that Baltic amber is a fossil resin of conifers (Pinus succinifera) mainly of the Paleogene period, formed upon specific fossilization of the resin as a result of polycondensation of resin acids and terpenes.
  • the main conditions for fossilization - prolonged oxidation in the soil of the "amber forest"; - subsequent redeposition with burial in coastal-marine, lagoon and delta sediments with a weakly oxidizing alkaline environment.
  • the fossilization conditions affected the diagenesis processes, accompanied by the appearance of oxygen-containing compounds in succinite, including free succinic acid and its esters.
  • Succinite compared with other types of amber and amber-like resins contains the highest percentage of succinic acid 3% - 8%, which is a determining factor when choosing the main component for creating a composite amber filament, according to [0010], [OOP] (14).
  • step b When performing [0019] step b), it is known that the elemental chemical composition of succinite is not stoichiometric and is in the following ranges: C - 76.74 - 81.22%; H - 10.09 - 10.51%; O - 7.90 - 12.36%, i.e. Compared to other types of amber and amber-like resins, fluctuations in the values of the main components occupy an intermediate position [14].
  • succinite in the form of impurities contains up to 12 chemical elements: Ni, Cu, Mg, Fe, Na, Ca, Mn, Al, Si, Au, N, S.
  • Baltic amber Sr, Ba, V, Cr, Ti, Co, Pb, Zn, Sn, Mo, Ge, Cd, Sb, K, Y, Si, Nb, P, Yb. This fact is very important, since unlike other types of amber, Baltic amber does not contain salts of heavy metals, which allows its use not only for medicinal but also cosmetic purposes [14].
  • a known feature of the energy properties of technologically recycled amber is to donate free electrons to maintain energy potential in cells with aerobic respiration [15]. This feature is due to the size and shape of amber microparticles in the range of 5-125 ⁇ , which meet the requirements of the certification company ECOCERT ® [16]. Moreover, with a decrease in the particle size of amber to a nanostructure of 300-1000 cps, the process is more efficient.
  • a flotation machine adapted for cleaning amber (consisting of a series of chambers arranged in series, equipped with an aeration device and a foam remover), which ensures the separation of succinite granules from impurities (crystals and grains of quartz, mica, feldspar, glauconite, particles of carbonized wood, etc.), the principle of which is based on differences in the density of water, granules of succinite and impurities [17].
  • the process of accelerated lifting of succinate granules contributes to the aeration of an aqueous solution. Crystals and grains of quartz, mica, feldspar (due to their higher density) remain at the bottom of the chamber. Succinite granules are removed by a removable device mounted on the top of the chamber of the flotation machine.
  • step b two-stage micronization of granules was carried out on a Planetary ball mill device "PULVERISETTE 5" (Germany), which made it possible to grind samples without loss, as well as preserve the structure of individual amber particles characteristic of a holistic stone.
  • PULVERISETTE 5" Germany
  • the first step in the micronization of the granules included the purification of succinite granules from crystals and grains of minerals adhered to the amber resin during fossilization.
  • a set of works was carried out to optimize the process of micronization of coarse amber using a planetary mill to reduce energy costs for grinding coarse amber, to determine the dependence of the grinding quality (particle dispersion) on the ratio of material and ground particles, to reduce the tendency of particles to aggregate and adhere to grinding bodies and walls mills.
  • the content of impurities in the micronized material was checked by a known method on an Inductively Coupled Plasma analysis (ICP) instrument. As a result of qualitative and quantitative analysis, the content of inorganic impurities was established up to 3%, which is a statistically acceptable content of inorganic impurities in succite in order to consider the result reliable.
  • ICP Inductively Coupled Plasma analysis
  • the second stage of micronization of the granules included grinding of succinite obtained according to [0038], [0039], to microparticle sizes of 5 - 125 ⁇ , preferably 5 - 50 ⁇ , with a rotation speed of grinding mills of 150 - 250 about. / min., for 50 - 350 min.
  • stepwise separation according to the size of the microparticles was carried out by successive sieving on an Analysette 3 SPARTAN FRITSCH (Germany) using standard sieves with mesh sizes of 50 ⁇ , 20 ⁇ (ISO 3310.1). Step-by-step screening is necessary in order to exclude the possibility of particles of a non-standard size falling into the ground mass of the crushed material.
  • microparticles were finely ground to a nanostructure in an atmosphere of superheated steam at a flow velocity of 900-1200 m / s, preferably 1000-1 100 m / s, where grinding to a nanostructure was achieved due to a 4-fold increase in kinetic energy from the impact of particles in a fluidized bed of steam.
  • This method allows to obtain succinite nanoparticles of a given size of 300-1000 nm and shape.
  • the percentage of succinite nanoparticles corresponds to 95 ⁇ 2% by the quantitative composition of the fraction of the established nanoparticle size, and was determined in a known manner using a granulometer ("90 Plus" Dajinu izmeru un Zeta potenciala noteiksanas iekarta MAS ZetaPALS Brookhaven Instr. (USA )).
  • suspensions with technologically processed succinite with a concentration of 5%; 10%; 20% do not cause irritation of the epidermis and dermis; after application of the suspension, no negative skin reactions to the test material were detected.
  • Suspensions with technologically processed succinite exert a biostimulating effect on the formation of new skin cells, subcutaneous tissue, skin derivatives, which stimulates the renewal of cell and hair tissue, and stimulates pigmentation in the upper and middle layers of the dermis, hair follicles, and hair [18].
  • the optimal concentration of technologically processed succinite which does not provoke the appearance of side effects (hair growth, pigmentation in the upper and middle layers of the dermis, hair follicles and hair), is 5%, while the process of active regeneration of skin cells and its vacuolization began.
  • the process for producing a composite amber yarn includes the following main steps:
  • the developed two-stage production process allows to obtain a composite amber thread with a uniformly distributed technologically processed succinite and provides the necessary strength characteristics of the thread.
  • a composite amber thread (FIG. 1, item 1) is obtained by introducing nanostructured succinite into the matrix base PA66.
  • nanostructured succinite with spherical particles and a size of 300-1000 psh (Fig. 1 pos. 2), crushed to a grain size of less than 1/3 of the specified fineness of the filament fiber (preferably 10-12 filament fibers, which make up one composite amber thread).
  • the obtained nanostructured succinite in an amount of 0.1-10 May. %, introduced into the polymer matrix PA66 in the amount of 90-99.9 may. % ( Figure 1, pos.
  • composite amber yarns are obtained from the synthesized composite mixture of nanostructured succinite and PA66 using standard technology for spinning composite amber yarn.
  • the sizing (preferably brand of sizing from S + S Schill + Seilacher) of the composite amber thread and its pulling (with a fully oriented structure (FDY)) are produced at a drawing speed of 2000-4000 m / min.
  • a composite amber yarn (FIG. 2, item 4) is obtained by introducing nanostructured succinite into the matrix base PA66.
  • nanostructured succinite with spherical particles and a size of 300-1000 nm (Fig. 2 item 5), crushed to a grain size of less than 1/3 of the specified filament fiber fineness (preferably 10-12 filament fibers, which make up one composite amber thread).
  • the obtained nanostructured succinite in an amount of 0.1-10 May. %, introduced into the polymer matrix PA66 in the amount of 87 - 96.9 may. % ( Figure 2, item 6) and synthesize a composite material.
  • the synthesized composite material is subjected to secondary extrusion in the main extruder for 5 min, at an optimized extrusion temperature t ° + 235 ° ⁇ -255 ° ⁇ , at this introduces particles of organic or inorganic compounds (Figure 2, item 7) in an amount until May 3. %
  • composite amber yarns are obtained from the synthesized composite mixture of nanostructured succinite and PA66 using standard technology for spinning composite amber yarn.
  • the sizing (preferably brand of sizing from S + S Schill + Seilacher) of the composite amber thread and its pulling (with a fully oriented structure (FDY)) are produced at a drawing speed of 2000-4000 m / min.
  • the main object of the invention is completed: composite amber yarns (Fig. 1 pos. 1) containing technologically processed amber, preferably succinite (Fig. 1 pos. 2), with spherical particles and a size of 300-1000 nm, crushed to graininess of less than 1/3 of the specified filament fiber fineness, uniformly integrated into the thermoplastic polymer matrix, more preferably polyamide 66 (PA66) (Fig. 1 item 3), with the following ratio of components (May.%): nanostructured succinite, in an amount of 0.1-10 May. %, PA66 in the amount of 90-99.9 May.
  • composite amber filaments which has a significant advantage over the known composite polymer filaments, namely filaments with a smooth surface, do not provoke allergic reactions, stimulate the activity of the epidermis, and promote the regeneration of normal skin areas. reflect ultraviolet rays, prevent the formation of blood clots in contact with platelets and are biocompatible with living tissue.
  • composite amber threads (FIG. 2, item 4) containing technologically processed amber, preferably succinite (FIG. 2, item 5), with spherical particles and a size of 300-1000 nm, crushed to grit less than 1/3 of the specified filament fiber fineness, uniformly integrated into the matrix of the thermoplastic polymer, more preferably polyamide 66 (PA66) ( Figure 2, item 6), and particles of an organic or inorganic compound ( Figure 2, item 7) in the following ratio of components (May.%): nano structured succinite, in the amount of 0.1-10 May. %, PA66 in the amount of 87 - 96.9 May. %, organic or inorganic compound in an amount up to May 3.
  • composite amber filaments which has a significant advantage over known composite polymer filaments, namely filaments with a smooth surface, do not provoke allergic reactions, stimulate the activity of the epidermis, promote the regeneration of normal skin areas, reflect ultraviolet rays, and prevent blood clots in contact with platelets and are biocompatible with living tissue.
  • a method for producing composite amber yarns has been developed, which ensures uniform distribution of nanostructured succinite in the matrix of a thermoplastic polymer, more preferably polyamide 66 (PA66), due to the secondary extrusion of the synthesized composite fiber material in the main extruder for 5 minutes, optimized extrusion temperature t ° + 235 ° ⁇ -255 ° ⁇ .
  • PA66 polyamide 66
  • Amber acid according to [0056] is an electron donor and an important component of processes associated with energy metabolism in cells.
  • Succinic acid is involved in the tricarboxylic acid cycle, which is the central part of the general pathway of catabolism, a cyclic biochemical aerobic process, during which di- and tricarboxylic acids are converted, which are formed as intermediate products in living organisms during the breakdown of carbohydrates, fats and proteins, to C0 2 .
  • the released hydrogen is sent to the tissue respiration chain, where it is subsequently oxidized to water, taking a direct part in the synthesis of the universal energy source of ATP.
  • the Krebs cycle is a key stage in the respiration of all cells using oxygen, the center of intersection of many metabolic pathways in the body.
  • the cycle In addition to a significant energy role, the cycle also has a significant plastic function, i.e. an important source of precursor molecules, from which, in the course of other biochemical transformations, such important compounds as amino acids, carbohydrates, fatty acids, etc. are synthesized.
  • ATP is an energy accumulator and the more active ATP is formed, the more active the cell is, therefore, its immunity to physical, chemical and biological stresses is higher [19].
  • amber material prevents platelet adhesion and aggregation, and, consequently, the formation of blood clots on its surface [21, 22].
  • Thrombosis is a complex process consisting of several successive stages. By preventing one of the stages, it is possible to reduce the likelihood of a blood clot.
  • One such step is the formation of a fibrin polymer from fibrinogen protein. Under the influence of the thrombin enzyme, it passes into the fibrin monomer, which subsequently polymerizes [23, 24].
  • the material is a semiconductor, the forbidden zone of which is wider than the forbidden zone of fibrinogen.
  • the main object of the invention has been developed: composite amber threads containing technologically processed amber, preferably succinite (CAS Nr. 9000-02-6), with spherical particles and a size of 300-1000 nm, crushed to a grain size of less than 1/3 of the specified fineness filament fibers uniformly integrated into the matrix of a thermoplastic polymer, preferably polyamide 66 (PA66; CAS Nr. 32131-17-2), with the following ratio of components (May.%): nanostructured succinite, in the amount of 0.1-10 May. %, PA66 in the amount of 90-99.9 May.
  • succinite CAS Nr. 9000-02-6
  • PA66 polyamide 66
  • composite amber filaments which has a significant advantage over known composite polymer filaments, namely filaments with a smooth surface, do not provoke allergic reactions, stimulate the activity of the epidermis, promote the regeneration of normal skin areas, reflect ultraviolet rays, and prevent blood clots in contact with platelets and are biocompatible with living tissue, while the biological activity of technologically processed succinate with stored for more than a year.
  • the developed composite amber yarns according to the invention are intended to expand the range of textile materials, and are also applicable as a prophylactic material for various skin changes, including those that improve the skin condition in the presence of diabetes mellitus and for the production of surgical textiles.

Abstract

L'invention concerne le domaine de l'industrie textile et porte sur la création d'un type de produit nouveau, à savoir de fils d'ambre composites possédant une teneur optimisée en ambre traité technologiquement dont les particules sont intégrées de façon homogène dans la matrice de polymère thermoplastique et/ou de composants supplémentaires, des fils à surface lisse ne provoquant pas de réactions allergiques ou de formation de caillots, reflétant les rayons ultraviolets et possédant une biocompatibilité avec les tissus vivants. Les fils d'ambre composites de l'invention sont destinés à élargir la gamme des matériaux textiles disponibles et peuvent s'utiliser en tant que matériau prophylactique lors de différents changements subis par la peau, y compris pour favoriser l'état de la peau en cas de diabète sucré et pour fabriquer des articles textiles à usage chirurgical.
PCT/LV2012/000010 2011-07-29 2012-06-21 Fils d'ambre composites WO2013019095A1 (fr)

Applications Claiming Priority (2)

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LVP-11-103 2011-07-29
LVP-11-103A LV14446B (lv) 2011-07-29 2011-07-29 Dzintara kompozītpavedieni

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WO2013019095A1 true WO2013019095A1 (fr) 2013-02-07

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201700025111A1 (it) * 2017-03-07 2018-09-07 Mele Mariano Filato composito argento + ambra

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2208069C2 (ru) * 2001-02-16 2003-07-10 Ми Су СЕОК Способ производства волокна, содержащего порошкообразные функциональные минералы (варианты)
FR2886949A1 (fr) * 2005-06-10 2006-12-15 Rhodia Chimie Sa Fils, filaments et fibres polyamide a proprietes ameliorees
RU2408745C2 (ru) * 2006-04-28 2011-01-10 Фибервеб Коровин Гмбх Полимерная нить и нетканый материал

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2208069C2 (ru) * 2001-02-16 2003-07-10 Ми Су СЕОК Способ производства волокна, содержащего порошкообразные функциональные минералы (варианты)
FR2886949A1 (fr) * 2005-06-10 2006-12-15 Rhodia Chimie Sa Fils, filaments et fibres polyamide a proprietes ameliorees
RU2408745C2 (ru) * 2006-04-28 2011-01-10 Фибервеб Коровин Гмбх Полимерная нить и нетканый материал

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"De nouvelles fibres textiles composites d'argent et d'ambre promettent diverses applications medicales", BE LETTONIE NUMERO 2, 30 October 2009 (2009-10-30), AMBASSADE DE FRANCE EN LETTONIE/ ADIT, Retrieved from the Internet <URL:http://www.bulletins-electroniques.com/actualites/61011.htm> *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201700025111A1 (it) * 2017-03-07 2018-09-07 Mele Mariano Filato composito argento + ambra

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LV14446B (lv) 2012-04-20
PL399430A1 (pl) 2013-01-21

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