CN104411796A - Hot-melt adhesive agent composition, and water-absorbable article manufactured using same - Google Patents
Hot-melt adhesive agent composition, and water-absorbable article manufactured using same Download PDFInfo
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- CN104411796A CN104411796A CN201480001723.1A CN201480001723A CN104411796A CN 104411796 A CN104411796 A CN 104411796A CN 201480001723 A CN201480001723 A CN 201480001723A CN 104411796 A CN104411796 A CN 104411796A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J153/02—Vinyl aromatic monomers and conjugated dienes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L13/00—Compositions of rubbers containing carboxyl groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J113/00—Adhesives based on rubbers containing carboxyl groups
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- Epidemiology (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Heart & Thoracic Surgery (AREA)
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Abstract
A hot-melt adhesive agent composition according to the present invention is characterized by comprising: 100 parts by weight of a thermoplastic block copolymer (A) that comprises at least one component selected from the group consisting of a styrene-isoprene-styrene block copolymer having a styrene component content of 15 to 35 wt%, a styrene-butadiene-styrene block copolymer having a styrene component content of 15 to 35 wt% and a styrene-butadiene/butylene-styrene block copolymer having a styrene component content of 15 to 35 wt%; 0.05 to 10 parts by weight of a liquid rubber (B) having a carboxyl group and/or a carboxylic acid anhydride group in the molecule; and an adhesiveness-imparting resin (C).
Description
Technical field
The present invention relates to a kind of hot-melt adhesive composition, particularly relate to a kind of can suitably for the manufacture of the hot-melt adhesive composition of the absorbent articles such as paper nappy.
Background technology
The assembling of the absorbent article such as paper nappy or sanitary napkin is carried out as follows: utilize hot-melt adhesive by adhering components such as polyolefin resin film, non-woven fabrics, thin paper and natural rubbers together.
As the hot-melt adhesive used in absorbent article, use rubber based hot melt caking agent using styrenic block copolymer as main component and using ene-propylene-butene multipolymer or ethylene-vinyl acetate copolymer as the olefines hot-melt adhesive of main component.Wherein, compared to olefines hot-melt adhesive, the cementability of rubber based hot melt caking agent, cohesive force and creep resistant are excellent, therefore, are widely used.
In the assembling of absorbent article, when utilizing rubber based hot melt caking agent to carry out the porous substrate such as bonding non-woven fabrics or thin paper, make by the rubber based hot melt caking agent of heating and melting together with porous substrate pressure viscosity, utilize its cohesive force (bounding force) to make to be bonded together by the rubber based hot melt caking agent of heating and melting and porous substrate, and make to be flowed in the pore of porous substrate by the rubber based hot melt caking agent of heating and melting.Then, by making rubber based hot melt caking agent cooling curing carry out the bonding of porous substrate.
On the other hand, the porous substrate (thin paper etc.) be made up of natural materialss such as cellulose material or cotton class materials or the non-woven fabrics implementing hydrophilicity-imparting treatment etc. are hydrophilic porous base material.The surface of hydrophilic porous base material is like this high polarity, but the polarity of rubber based hot melt caking agent is low, and therefore, the affinity of hydrophilic porous base material and rubber based hot melt caking agent is low.Therefore, even if make the rubber based hot melt caking agent of heating and melting and hydrophilic porous base material pressure viscosity, rubber based hot melt caking agent also not easily flows in the pore of hydrophilic porous base material, the contact area of rubber based hot melt caking agent and hydrophilic porous base material reduces, therefore, the bonding effect produced by intermolecular forces or anchoring effect reduces.Under these circumstances, although can be obtained under the state of drying by the hydrophilic porous base material that rubber based hot melt caking agent is bonding can the bonding strength of resistance to practicality, but when becoming moisture state by the hydrophilic porous base material that rubber based hot melt caking agent is bonding when being soaked by body fluid such as urine, the significantly reduced problem of bonding strength can be produced.Therefore, for rubber based hot melt caking agent, in order to also can maintain excellent bonding strength to the hydrophilic porous base material becoming moisture state, need to improve moistening cementability.
Therefore, Patent Document 1 discloses a kind of hot-melt adhesive composition, it, except containing except styrenic block copolymer, also contains the wax with carboxylic acid and/or carboxylic acid anhydride modified.According to the wax of carboxylic acid and/or carboxylic acid anhydride modified, polarity can be given to hot-melt adhesive composition, thus, the affinity of hot-melt adhesive composition relative to hydrophilic porous base material can be improved, the moistening cementability of hot-melt adhesive composition can be improved.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2007-169531 publication
Summary of the invention
Invent technical problem to be solved
But although the hot-melt adhesive composition of citing document 1 is by adding above-mentioned wax, the elevated temperature melts viscosity more than 150 DEG C is low and can show excellent mobility, and be sharply cured at the temperature lower than it, melt viscosity uprises, mobility reduction.Therefore, if during coating the heating and melting temperature of hot-melt adhesive composition reduce or time (sphere time) to the hydrophilic porous base material of laminating after coating hot-melt adhesive composition elongated, then can cause significantly carrying out and hydrophilic porous base material that the hot-melt adhesive composition of mobility step-down is fitted in solidification, hot-melt adhesive composition not easily flows to the interior flowing of pore of hydrophilic porous base material, and the contact area of rubber based hot melt caking agent and hydrophilic porous base material reduces.Therefore, even if require that the hot-melt adhesive composition of citing document 1 also can play sufficient bonding strength to the hydrophilic porous base material of moisture state when carrying out low-temperature coating.
And then, low with the consistency of other composition contained in the wax of carboxylic acid and/or carboxylic acid anhydride modified and hot-melt adhesive composition.Therefore, the thermostability of hot-melt adhesive composition reduces because using such wax.If hot-melt adhesive composition low for thermostability is placed with heating and melting state for extended periods, then hot-melt adhesive composition variable color or cause coating bad because producing gelation or carbonization.
Therefore, the object of the invention is to, even if provide a kind of also can show excellent bonding strength to the hydrophilic porous base material of moisture state at a lower temperature, and the hot-melt adhesive composition of excellent heat stability.
For the technical scheme of technical solution problem
Hot-melt adhesive composition of the present invention, comprises thermoplastic block copolymers (A) 100 weight part, liquid rubber (B) 0.05 ~ 10 weight part and tackifying resin (C),
Described thermoplastic block copolymers (A) is containing being selected from styrene isoprene styrene block copolymer (SIS), the styrene content content at least one that to be the styrene-butadiene-styrene block copolymer of 15 ~ 35 % by weight and the content of styrene content be in the styrene butadiene/butylene-styrene segmented copolymer of 15 ~ 35 % by weight that styrene content content is 15 ~ 35 % by weight
Described liquid rubber (B) has carboxyl and/or acid anhydride in molecule.
[thermoplastic block copolymers (A)]
As thermoplastic block copolymers (A), can enumerate: styrene isoprene styrene block copolymer (SIS), styrene-butadiene-styrene block copolymer and styrene butadiene/butylene-styrene segmented copolymer.By using these multipolymers, a kind of hot-melt adhesive composition that can show excellent bonding strength to the hydrophilic porous base material of moisture state can be provided.In addition, thermoplastic block copolymers can be used alone one, also can combinationally use more than two kinds.
The content of the styrene content in styrene isoprene styrene block copolymer (SIS) is defined in 15 ~ 35 % by weight, and preferably 20 ~ 30 % by weight.The curing speed of the hot-melt adhesive composition after the styrene isoprene styrene block copolymer (SIS) of the too high levels of styrene content likely causes heating and melting accelerates, and the moistening cementability of hot-melt adhesive composition is reduced.In addition, the styrene isoprene styrene block copolymer (SIS) that the content of styrene content is too low likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.
The content of the styrene content in styrene-butadiene-styrene block copolymer is defined in 15 ~ 35 % by weight, and preferably 20 ~ 30 % by weight.The curing speed of the hot-melt adhesive composition after the styrene-butadiene-styrene block copolymer of the too high levels of styrene content likely causes heating and melting accelerates, and the moistening cementability of hot-melt adhesive composition is reduced.In addition, the styrene-butadiene-styrene block copolymer that the content of styrene content is too low likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.
The content of the styrene content in styrene butadiene/butylene-styrene segmented copolymer is defined in 15 ~ 35 % by weight, and preferably 20 ~ 30 % by weight.The curing speed of the hot-melt adhesive composition after the styrene butadiene/butylene-styrene segmented copolymer of the too high levels of styrene content likely causes heating and melting accelerates, and the moistening cementability of hot-melt adhesive composition is reduced.In addition, styrene butadiene/butylene-styrene segmented copolymer that the content of styrene content is too low likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.
Styrene content content in thermoplastic block copolymers (A) relative to the accuracy by immutable weight of thermoplastic block copolymers (A) in 15 ~ 35 % by weight, preferably 20 ~ 30 % by weight.The curing speed of the hot-melt adhesive composition after the thermoplastic block copolymers (A) of the too high levels of styrene content likely causes heating and melting accelerates, and the moistening cementability of hot-melt adhesive composition is reduced.In addition, the thermoplastic block copolymers (A) that the content of styrene content is too low likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.
The weight-average molecular weight (Mw) of styrene isoprene styrene block copolymer (SIS) preferably 50,000 ~ 300,000, more preferably 70,000 ~ 250,000, particularly preferably 100,000 ~ 200,000.The too small styrene isoprene styrene block copolymer (SIS) of weight-average molecular weight (Mw) likely causes the cohesive force making hot-melt adhesive composition itself to reduce, and bonding force is insufficient.In addition, the styrene isoprene styrene block copolymer (SIS) that weight-average molecular weight (Mw) is excessive likely causes the melt viscosity of hot-melt adhesive composition become too high and damage mobility.
The weight-average molecular weight (Mw) of styrene-butadiene-styrene block copolymer preferably 50,000 ~ 300,000, more preferably 70,000 ~ 250,000, particularly preferably 100,000 ~ 200,000.The too small styrene-butadiene-styrene block copolymer of weight-average molecular weight (Mw) likely causes the cohesive force of hot-melt adhesive composition self to reduce, and bonding force is insufficient.In addition, the styrene-butadiene-styrene block copolymer that weight-average molecular weight (Mw) is excessive likely causes the melt viscosity of hot-melt adhesive composition become too high and damage mobility.
The weight-average molecular weight (Mw) of styrene butadiene/butylene-styrene segmented copolymer preferably 50,000 ~ 300,000, more preferably 70,000 ~ 250,000, particularly preferably 100,000 ~ 200,000.Too small styrene butadiene/butylene-styrene the segmented copolymer of weight-average molecular weight (Mw) likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.In addition, styrene butadiene/butylene-styrene segmented copolymer that weight-average molecular weight (Mw) is excessive likely causes the melt viscosity of hot-melt adhesive composition become too high and damage mobility.
The weight-average molecular weight (Mw) of thermoplastic block copolymers (A) preferably 50,000 ~ 300,000, more preferably 70,000 ~ 250,000, particularly preferably 100,000 ~ 200,000.The too small thermoplastic block copolymers (A) of weight-average molecular weight (Mw) likely causes the cohesive force of hot-melt adhesive composition itself to reduce, and bonding force is insufficient.In addition, the thermoplastic block copolymers (A) that weight-average molecular weight (Mw) is excessive likely causes the melt viscosity of hot-melt adhesive composition become too high and damage mobility.
In addition, in the present invention, the weight-average molecular weight of so-called styrene isoprene styrene block copolymer (SIS), styrene-butadiene-styrene block copolymer, styrene butadiene/butylene-styrene segmented copolymer and thermoplastic block copolymers (A), refer to and use gel permeation chromatography device respectively, the measured value obtained by converting with polystyrene standard.
[liquid rubber (B)]
Hot-melt adhesive composition of the present invention contains the liquid rubber (B) in molecule with polar group.As polar group, can enumerate: carboxyl (-COOH) and acid anhydride (-CO-O-CO-).Liquid rubber (B) can have any one in carboxyl and acid anhydride, also can have both.
In addition, in the present invention, so-called " liquid rubber " refers at 23 DEG C, 1.01 × 10
5the rubber be in a liquid state under Pa (1atm).
Liquid rubber (B) makes to improve the affinity of the porous substrate be made up of natural materialss such as cellulose material or cotton class materials (thin paper etc.) or the hydrophilic porous base material such as non-woven fabrics that implements hydrophilicity-imparting treatment by its polar group, and the rubber based hot melt adhesive composite after heating and melting can be made easily to flow in the pore of hydrophilic porous base material.In addition, even if hot-melt adhesive composition is containing liquid rubber (B), after heating and melting, melt viscosity is also very low and show excellent mobility, and solidifies lentamente with temperature reduction due to it, therefore can significantly suppress melt viscosity sharply rise and mobility is reduced.Therefore, even if the heating and melting temperature of hot-melt adhesive composition during coating is low, sphere time is elongated, or the temperature of hot-melt adhesive composition becomes lower, hot-melt adhesive composition also can maintain excellent mobility, by the hydrophilic porous base material of pressure viscosity on such hot-melt adhesive composition, the pore of hot-melt adhesive composition flowing close relative water-based porous substrate is inner, can improve the contact area of hot-melt adhesive composition and hydrophilic porous base material.Therefore, hot-melt adhesive composition of the present invention can show excellent bonding strength to hydrophilic porous base material, and, even if when hydrophilic porous base material becomes moisture state, bonding strength excellent so also can be maintained.
In addition, utilize liquid rubber (B), the thermostability of hot-melt adhesive composition can also be improved.Therefore, after making hot-melt adhesive composition heating and melting of the present invention, even if store in tank for a long time under the state of heating and melting, also can suppress hot-melt adhesive composition that painted, gelation or carbonization occur higher.
As liquid rubber (B), can enumerate: main chain is made up of the hydride of the hydride of the homopolymer of alpha-olefin, ethene-alpha-olefin copolymer, ethylene-propylene copolymer, ethylene-propylene-diene copolymer, ethylene-propylene-diene copolymer, ethylene-butene copolymer, polyisoprene, polyhutadiene, polyprene, polycyclopentadiene, styrene-butadiene block copolymer, acrylonitrile butadiene copolymer or acrylonitrile butadiene copolymer, and at the end of above-mentioned main chain or side chain, there is the liquid rubber of polar group.In addition, liquid rubber (B) can be used alone one, also can combinationally use more than two kinds.
Wherein, the main chain of liquid rubber (B) is preferably made up of polyisoprene, polyhutadiene or styrene-butadiene block copolymer, is more preferably made up of polyisoprene.Such liquid rubber (B) is owing to having excellent consistency to above-mentioned thermoplastic block copolymers (A), therefore, not only can improve mobility and the thermostability of the hot-melt adhesive composition after heating and melting, also can improve moistening cementability.
The number-average molecular weight (Mn) of liquid rubber (B) preferably 1,000 ~ 150,000, more preferably 10,000 ~ 100,000.The too small liquid rubber (B) of number-average molecular weight (Mn) likely causes the cohesive force of hot-melt adhesive composition to reduce, and moistening cementability is insufficient.In addition, the liquid rubber (B) that number-average molecular weight (Mn) is excessive likely causes the melt viscosity of hot-melt adhesive composition become too high and mobility is reduced.
In addition, in the present invention, the number-average molecular weight (Mn) of so-called liquid rubber (B) refers to and uses gel permeation chromatography device, by the measured value obtained that converts with polystyrene standard.
In addition, as the liquid rubber (B) in molecule with polar group, commercially available product can be used.Such as the liquid polyisoprene with carboxyl, can enumerate: the product that Kuraray company produces " Kuraprene LIR-410 " by name etc.As the liquid polyisoprene with acid anhydride, can enumerate: the product that Kuraray company produces " Kuraprene LIR-403 " by name etc.As the propylene liquid nitrile butadienecopolymer with carboxyl, can enumerate: the product that BF Goodrich company produces " CTBN1300X8 " by name etc.
As the content of liquid rubber (B) in hot-melt adhesive composition, be defined in 0.05 ~ 10 weight part relative to thermoplastic block copolymers (A) 100 weight part, preferably 1 ~ 10 weight part, more preferably 3 ~ 10 weight parts.The hot-melt adhesive composition that the content of liquid rubber (B) is too low likely causes moistening cementability low.In addition, the hot-melt adhesive composition of the too high levels of liquid rubber (B) likely causes thermostability low.
[tackifying resin (C)]
Hot-melt adhesive composition of the present invention can also contain tackifying resin (C).As tackifying resin (C), can enumerate: natural rosin, modified rosin, staybelite, the glyceryl ester of natural rosin, the glyceryl ester of modified rosin, the pentaerythritol ester of natural rosin, the pentaerythritol ester of modified rosin, the pentaerythritol ester of staybelite, the multipolymer of natural terpenes, 3 dimensional polymers of natural terpenes, the hydrogenated derivatives of the multipolymer of hydriding terpene, polyterpene resin, the hydrogenated derivatives of phenolic modified terpene resin, aliphatic petroleum hydrocarbon resin, the hydrogenated derivatives of aliphatic petroleum hydrocarbon resin, aromatic base crude oil hydrocarbon resin, the hydrogenated derivatives of aromatic base crude oil hydrocarbon resin, annular aliphatic petroleum hydrocarbon resin, the hydrogenated derivatives of annular aliphatic petroleum hydrocarbon resin.Wherein, the hydrogenated derivatives of preferred aliphat petroleum hydrocarbon resin.
The softening temperature of tackifying resin (C) preferably 80 ~ 120 DEG C, more preferably 100 ~ 120 DEG C.Utilize the tackifying resin of softening temperature in above-mentioned scope (C), can further improve the moistening cementability of hot-melt adhesive.
In addition, in the present invention, the softening temperature of tackifying resin (C) adopts the value that the method for foundation JISK 6863 records.
The content of the tackifying resin (C) in hot-melt adhesive composition relative to thermoplastic block copolymers (A) 100 weight part preferably 10 ~ 500 weight parts, more preferably 40 ~ 400 weight parts, most preferably 150 ~ 300 weight parts.The hot-melt adhesive composition that the content of tackifying resin (C) is too low likely causes bonding force low.In addition, the hot-melt adhesive composition of the too high levels of tackifying resin (C) likely becomes hard and crisp cured article after hardening, causes the low adhesion of hot-melt adhesive composition to reduce.
Hot-melt adhesive composition of the present invention, except thermoplastic block copolymers (A), liquid rubber (B) and tackifying resin (C), can also contain other additive.As other additive, can enumerate: softening agent (D), antioxidant, UV light absorber and weighting agent etc.
[softening agent (D)]
As softening agent (D), such as, can enumerate: paraffin class process oil, naphthenic process oil and aromatic series generic operation wet goods.Wherein, more preferably paraffin class process oil and naphthenic process oil, particularly preferably paraffin class process oil.Utilize these softening agent, the hot-melt adhesive composition of moistening bonding strength excellence can be provided.In addition, these softening agent can be used alone, and also can combinationally use two or more.
Paraffin class process oil contains aliphatics chain hydrocarbon.The carbonatoms of aliphatics chain hydrocarbon contained in paraffin class process oil is not particularly limited, but preferably 16 ~ 40, and more preferably 20 ~ 30.
The number-average molecular weight (Mn) of paraffin class process oil preferably 100 ~ 1500, more preferably 250 ~ 1000.The too small paraffin class process oil of number-average molecular weight (Mn) likely causes the cohesive force of hot-melt adhesive composition to reduce, and moistening cementability is insufficient.In addition, the paraffin class process oil that number-average molecular weight (Mn) is excessive likely causes the melt viscosity of hot-melt adhesive composition too high and screening characteristics is reduced.
As paraffin class process oil, commercially available product can be used.As commercially available product, such as, can enumerate: the commodity that Japanese grease manufactures are called " NASolvent ", bright dipping is emerging produces commodity " PW-380 " by name, the commodity that commodity are called " PS-32 ", bright dipping petroleum chemistry (strain) manufactures " IP-Solvent 2835 " by name that commodity are called " Diana Fresia S32 ", bright dipping Xing Chan company manufactures of bright dipping Xing Chan company manufacture, the commodity " Neothiozole " by name etc. of the industrial manufacture of three photochemistry made.
As long as naphthenic process oil comprises aliphatic category cyclic hydrocarbon, be not particularly limited, the carbonatoms of aliphatic category cyclic hydrocarbon contained in naphthenic process oil is preferably more than 3, is more preferably 3 ~ 8.
The number-average molecular weight (Mn) of naphthenic process oil preferably 100 ~ 1500, more preferably 250 ~ 1000.The too small naphthenic process oil of number-average molecular weight (Mn) likely causes the cohesive force making hot-melt adhesive composition to reduce, and moistening cementability is insufficient.In addition, the naphthenic process oil that number-average molecular weight (Mn) is excessive likely causes the melt viscosity of hot-melt adhesive composition too high and screening characteristics is reduced.
As naphthenic process oil, commercially available product can be used.As commercially available product, such as, can enumerate: the commodity " Diana Fresia U46 " by name that the commodity that bright dipping Xing Chan company manufactures " Diana Fresia N28 " by name, bright dipping Xing Chan company manufacture and the commodity " Diana Process Oil NR " by name etc. that bright dipping Xing Chan company manufactures.
In addition, in the present invention, the number-average molecular weight (Mn) of so-called paraffin class process oil and naphthenic process oil refers to and uses gel permeation chromatography device respectively, by the measured value obtained that converts with polystyrene standard.
As the content of the softening agent (D) in hot-melt adhesive composition, relative to thermoplastic block copolymers (A) 100 weight part preferably 25 ~ 250 weight parts, more preferably 50 ~ 150 weight parts.The hot-melt adhesive composition of the too high levels of softening agent (D) likely causes creep resistant to reduce or cohesive force reduces and moistening cementability is reduced.In addition, the curing speed after the hot-melt adhesive composition that the content of softening agent (D) is too low likely causes heating and melting becomes too high and cementability, particularly moistening cementability is reduced.
[antioxidant]
As antioxidant, can enumerate: 2, 6-di-tert-butyl-4-methy phenol, Octadecane base-3-(4'-hydroxyl-3', 5'-di-tert-butyl-phenyl) propionic ester, 2, 2'-methylene-bis (4-methyl-6-tert-butylphenol), 2, 2'-methylene-bis(4-ethyl-6-t-butyl phenol), 2, two (pungent the butylthiomethyl)-ortho-cresol of 4-, the 2-tertiary butyl-6-(the 3-tertiary butyl-2-hydroxy-5-methyl base benzyl)-4-aminomethyl phenyl acrylate, 2, 4-bis-tert-pentyl-6-(1-(3, 5-bis-tert-pentyl-2-hydroxy phenyl) ethyl) phenyl acrylate, 2-[1-(2-hydroxyl-3, 5-di-tert-pentyl-phenyl)] acrylate, four (methylene radical-3-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester) hindered phenol anti-oxidants such as methane, the sulphur class antioxidants such as dilauryl thiodipropionate, lauryl stearyl-thio dipropionate, tetramethylolmethane four (3-lauryl thiopropionate), the phosphorus antioxidants etc. such as three (nonyl phenyl) phosphorous acid ester, three (2,4-di-tert-butyl-phenyl) phosphorous acid ester.Antioxidant can be used alone one, also can combinationally use more than two kinds.
[UV light absorber]
As UV light absorber, can enumerate: 2-(2'-hydroxyl-5'-aminomethyl phenyl) benzotriazole, 2-(2'-hydroxyl-3', 5'-tert-butyl-phenyl) Benzotriazole Ultraviolet Stabilizer such as benzotriazole, 2-(2'-hydroxyl-3', 5'-di-tert-butyl-phenyl)-5-chlorobenzotriazole; The benzophenone ultraviolet absorption agents such as ESCALOL 567; Salicylate ultraviolet absorption agent, cyanoacrylate ultraviolet absorption agent; Hindered amine light stabilizer.In addition, UV light absorber can be used alone one, also can be used together more than two kinds.
[weighting agent]
As weighting agent, such as, can enumerate: mica, calcium carbonate, kaolin, talcum, titanium oxide, diatomite, ureas resin, vinylbenzene pearl, burn till clay, starch etc.
[absorbent article]
The various parts such as hot-melt adhesive composition of the present invention is used for weaving cotton cloth, non-woven fabrics, thin paper, elastomeric element, polyolefin resin film carry out bonding.As mentioned above, hot-melt adhesive composition of the present invention also can play excellent moistening cementability to the porous substrate be made up of natural materialss such as cellulose material or cotton class materials (thin paper etc.) or the hydrophilic porous base material such as non-woven fabrics that implements hydrophilicity-imparting treatment, therefore, bonding component parts in the manufacture of absorbent article can be preferred for.
Absorbent article is not particularly limited, and has the first component parts, the second component parts and hot-melt adhesive composition of the present invention.Hot-melt adhesive composition can be utilized the first component parts and the second component parts to be bonded and integrated.And at least one party in the first component parts and the second component parts is preferably hydrophilic porous base material.
As the first component parts and the 2nd component parts, as long as the component parts for using in absorbent article, such as, can enumerate: the elastomeric elements such as rubber, weave cotton cloth, non-woven fabrics, paper, polyolefin resin film and hydrophilic porous base material.These component parts can be used alone one, also can combinationally use more than two kinds.In addition, as hydrophilic porous base material, the porous substrate be made up of Mierocrystalline cellulose or cotton and the porous substrate etc. implementing hydrophilicity-imparting treatment can be enumerated.As the porous substrate be made up of Mierocrystalline cellulose or cotton, such as, thin paper etc. can be enumerated.In addition, as the porous substrate implementing hydrophilicity-imparting treatment, can enumerate: implement the non-woven fabrics of hydrophilicity-imparting treatment or weave cotton cloth.
The object of absorbent article is, body fluid and other liquid such as absorbing blood or urine, sweat, purulence, gastric juice, saliva, nose secreting mucus.As other liquid, can enumerate, water, beverage and waste liquid etc.As absorbent article, such as, can enumerate: the Perserving materials etc. of processing blades, hospital's robe, operation gown of a doctor, wound coating material, first-aid dressing and meat or fish etc. urinated by paper nappy, sanitary napkin, sanitary towel, incontinence shield, Portable bathroom, portable type pollution treatment bag, animal dung.Wherein, preferably paper nappy can be enumerated.
The liquid permeable top sheet that opaque liquid tergite, non-woven fabrics etc. that paper nappy is made up of polyolefin resin film etc. are substantially made and configuration between which cartridge form.In order to decrease uptake body absorption urine etc. after be clamminess, cartridge uses under the state covering its surface with thieving papers such as thin papers.In addition, absorbent article adopts the structure being close to the belly of wearer and waist and preventing movement from spilling by being provided with the elastomeric elements such as rubber elastically.In the manufacture of such paper nappy, in order to integration that the hydrophilic porous base materials such as thin paper are bonded to each other, other porous substrates such as hydrophilic porous base material and non-woven fabrics such as thin paper be bonded and integrated or the hydrophilic porous base materials such as thin paper and other component parts such as polyolefin resin film or elastomeric element are bonded and integrated, preferably using hot-melt adhesive of the present invention.
As utilizing hot-melt adhesive composition of the present invention to be bonded to each other by component parts the method for integration, being not particularly limited, known method can be used.Such as can make with the following method etc.: after the hot-melt adhesive composition after heating and melting is coated on a component parts, after another component parts being superimposed on the hot-melt adhesive composition of coating, by they pressure viscosity.
The heating and melting temperature of hot-melt adhesive composition preferably 135 ~ 180 DEG C.In existing hot-melt adhesive composition, obtaining sufficient mobility to reduce melt viscosity, usually heating and melting temperature being set to more than 150 DEG C.But, likely there is following situation: if the temperature of hot-melt adhesive composition is reduced to lower than 150 DEG C, then the melt viscosity of hot-melt adhesive composition sharply rises and mobility is reduced, therefore, be difficult to coating hot-melt adhesive composition, if the heating and melting temperature step-down of hot-melt adhesive composition during coating or sphere time elongated, the pore that the hot-melt adhesive composition then applied is difficult to flow to the hydrophilic porous base material such as non-woven fabrics or thin paper is inner, cannot obtain the sufficient moistening cementability between hydrophilic porous base material.
But, even if hot-melt adhesive composition of the present invention in heating and melting temperature lower than under 150 DEG C, particularly 135 ~ 145 DEG C so comparatively low temperature, melt viscosity is also low and can easily apply.In addition, with regard to hot-melt adhesive composition of the present invention, the situation of sharply solidifying with the reduction of temperature is suppressed, even if compared with also maintaining excellent mobility under low temperature.Therefore, even if coating time hot-melt adhesive composition heating and melting temperature lower than 150 DEG C, be particularly low to moderate 135 ~ 145 DEG C or coating after sphere time elongated, the pore that hot-melt adhesive composition also can flow to hydrophilic porous base material is inner, the sufficient contact area of hot-melt adhesive composition and hydrophilic porous base material can be obtained, even if excellent bonding strength also can be maintained to the hydrophilic porous base material of moisture state.
As the coating method of the hot-melt adhesive composition after heating and melting, be not particularly limited, known method can be used.Such as can enumerate: the spiral coating that slit type coater coating, roller coating machine coating, helically carry out applying, wavy carry out applying Ω coating and control slit coating, carry out the slit spraying that applies and curtain spraying to planar and can carry out to point-like the point type coating etc. that applies.
Invention effect
Hot-melt adhesive composition of the present invention temperature after heat tracing melting can reduce and solidify lentamente.Therefore, even if the heating and melting temperature of hot-melt adhesive composition reduces or until elongated for the time on adherend laminating hot-melt adhesive composition after coating or temperature are reduced, hot-melt adhesive composition also can maintain excellent mobility, can easily flow in the pore of hydrophilic porous base material of pressure viscosity.
Use in the absorbent article of such hot-melt adhesive composition of the present invention, even if its component parts is moistening because of body fluid such as urine or blood, also maintain the bonding strength of the excellence between component parts by hot-melt adhesive composition.Therefore, when hot-melt adhesive composition of the present invention is used for the absorbent articles such as paper nappy, urine etc. can be suppressed higher externally to spill.
Embodiment
Below, use embodiment to be more specifically described the present invention, but the present invention is not limited thereto.
Embodiment
In embodiment described later and comparative example, thermoplastic block copolymers (A1) ~ (A11) used in manufacture about hot-melt adhesive composition, liquid rubber (B1) ~ (B4), wax, tackifying resin (C1) ~ (C3), softening agent (D1) ~ (D2) and antioxidant, record detailed description respectively below.
Thermoplastic block copolymers (A):
Styrene isoprene styrene block copolymer (SIS) (A1) [non-polar group, styrene content content 16 % by weight, weight-average molecular weight (Mw) 171,000, Nippon Zeon manufacture, ProductName " Quintac3433N "]
Styrene isoprene styrene block copolymer (SIS) (A2) [non-polar group, styrene content content 25 % by weight, weight-average molecular weight (Mw) 125,000, Nippon Zeon manufacture, ProductName " Quintac3280 "]
Styrene isoprene styrene block copolymer (SIS) (A3) [non-polar group, styrene content content 14 % by weight, weight-average molecular weight (Mw) 125,000, Nippon Zeon manufacture, ProductName " Quintac3421 "]
Styrene isoprene styrene block copolymer (SIS) (A4) [non-polar group, styrene content content 48 % by weight, weight-average molecular weight (Mw) 100,000, Nippon Zeon manufacture, ProductName " Quintac3390 "]
Styrene-butadiene-styrene block copolymer (A5) [non-polar group, styrene content content 30 % by weight, weight-average molecular weight (Mw) 122,300, chemical company of Asahi Chemical Industry manufacture, ProductName " AsapreneT-436 "]
Styrene-butadiene-styrene block copolymer (A6) [non-polar group, styrene content content 35 % by weight, weight-average molecular weight (Mw) 100,000, chemical company of Asahi Chemical Industry manufacture, ProductName " AsapreneT-438 "]
Styrene-butadiene-styrene block copolymer (A7) [non-polar group, styrene content content 45 % by weight, weight-average molecular weight (Mw) 70,000, chemical company of Asahi Chemical Industry manufacture, ProductName " AsapreneT-439 "]
Styrene butadiene/butylene-benzene second segmented copolymer (A8) [non-polar group, styrene content 30 % by weight, weight-average molecular weight (Mw) 100,000, chemical company of Asahi Chemical Industry manufacture, ProductName " TuftecP1500 "]
Styrene butadiene/butylene-benzene second segmented copolymer (A9) [non-polar group, styrene content 67 % by weight, weight-average molecular weight (Mw) 100,000, chemical company of Asahi Chemical Industry manufacture, ProductName " TuftecP2000 "]
Styrene-ethylene/propylene-styrene block multipolymer (A10) [non-polar group, styrene content content 30 % by weight, weight-average molecular weight (Mw) 55,000, Kuraray company manufacture, ProductName " Septon2002 "]
Styrene-ethylene/butylene-benzene second segmented copolymer (A11) [non-polar group, styrene content 30 % by weight, weight-average molecular weight (Mw) 200,000, chemical company of Asahi Chemical Industry manufacture, ProductName " TuftecH1041 "]
In addition, in table 1 and 2, by styrene isoprene styrene block copolymer (SIS) referred to as " SIS multipolymer ", by styrene-butadiene-styrene block copolymer referred to as " SBS multipolymer ", by styrene butadiene/butylene-styrene segmented copolymer referred to as " SBBS multipolymer ", by styrene-ethylene/propylene-styrene block multipolymer referred to as " SEPS multipolymer ", by styrene-ethylene/butylene-styrene block copolymer referred to as " SEBS multipolymer ".
Liquid rubber (B):
[main chain is made up of polyisoprene and has the liquid rubber of carboxyl at the end of main chain or side chain: number-average molecular weight (Mn) 30,000, at 23 DEG C, 1.01 × 10 to have the liquid polyisoprene (B1) of carboxyl
5be liquid state, fusing point less than 0 DEG C, the manufacture of Kuraray company under Pa (1atm), ProductName " Kuraprene LIR-410 "]
[main chain is made up of polyisoprene and has the liquid rubber of acid anhydride at the end of main chain or side chain: number-average molecular weight (Mn) 34,000, at 23 DEG C, 1.01 × 10 to have the liquid polyisoprene (B2) of acid anhydride
5be liquid state, fusing point less than 0 DEG C, the manufacture of Kuraray company under Pa (1atm), ProductName " Kuraprene LIR-403 "]
[main chain is made up of polyhutadiene and has the liquid rubber of acid anhydride at the end of main chain or side chain: in number-average molecular weight (Mn) 31,000,23 DEG C, 1.01 × 10 to have the liquid polybutadiene (B3) of acid anhydride
5be liquid state, fusing point less than 0 DEG C, the manufacture of Clay Valley company under Pa (1atm), ProductName " Ricon130MA20 "]
Liquid polyisoprene (B4) [non-polar group: number-average molecular weight (Mn) 54,000, at 23 DEG C, 1.01 × 10
5be liquid state, fusing point less than 0 DEG C, the manufacture of Kuraray company under Pa (1atm), ProductName " Kuraprene LIR-50 "]
Wax:
Have acid anhydride polyethylene (PE) wax [number-average molecular weight (Mn) Isosorbide-5-Nitrae 00, at 23 DEG C, 1.01 × 10
5be solid, fusing point 104 DEG C, the manufacture of Innospec company under Pa (1atm), ProductName " Viscowax261 "]
Tackifying resin (C):
The hydrogenated derivatives (C1) [softening temperature 100 DEG C, waste river chemistry manufacture, ProductName " Arkon M-100 "] of aliphatic petroleum hydrocarbon resin
The hydrogenated derivatives (C2) [softening temperature 80 DEG C, General company manufacture, ProductName " E5380 "] of aliphatic petroleum hydrocarbon resin
The hydrogenated derivatives (C3) [softening temperature 120 DEG C, emerging the producing of bright dipping are made, ProductName " I-MARV P120 "] of aliphatic petroleum hydrocarbon resin
Softening agent (D):
Paraffin class process oil (D1) (number-average molecular weight (Mn) 980, bright dipping oil company manufacture, ProductName " Diana Process Oil process oil PW-90 ")
Naphthenic process oil (D2) (number-average molecular weight (Mn) 100 ~ 1500, Shell chemical company manufacture, ProductName " Shell Flex 371N ")
[antioxidant]
Phenol antioxidant (BASF AG manufactures, ProductName " IRGANOX1010 ")
(embodiment 1 ~ 14 and comparative example 1 ~ 9)
After during above-mentioned thermoplastic block copolymers (A1) ~ (A11), liquid rubber (B1) ~ (B4), wax, tackifying resin (C1) ~ (C3), softening agent (D1) ~ (D2) and antioxidant are put into heating unit stirring mixing roll with the use level shown in table 1 and 2 respectively, while heating one hour one side is mixing at 150 DEG C, manufacture hot-melt adhesive composition.
(evaluation)
According to the main points shown in following, moistening bonding strength and thermostability are evaluated to the hot-melt adhesive composition made in embodiment and comparative example.
These results are shown in table 1 and 2.
(moistening bonding strength: thin paper-thin paper)
By hot-melt adhesive composition is heated to 140 DEG C make its melting after, sprayed by spiral with 3g/m
2glue spread be coated on thin paper (paper weigh 18 ~ 21g/m
2, thickness 70 ~ 90 μm) one side, after being coated with latter 1 second, to other thin paper of face lamination being coated with hot-melt adhesive composition of this thin paper.Then, by they at 23 DEG C with 50gf/cm
2exert pressure pressure viscosity 0.01 second, obtain duplexer thus.This duplexer is cut off, obtains the test film of the strip of wide 20mm × long 150mm thus.
Then, by test film 23 DEG C, keeping 24 hours under relative humidity 50% atmosphere, flood 1 minute in the water of 23 DEG C.Then, test film is taken out from water, wiping water, obtain the test film of moisture state thus.And, according to JIS K6854, divide to pull speed 100mm/ the stripping test of T mould is carried out to the test film of moisture state, measure bonding strength (× 10
-2n/20mm).The bonding strength obtained is shown in " moistening bonding strength " hurdle of table 1 ~ 2.
(thermostability 1)
For hot-melt adhesive composition is heated to 140 DEG C make its melting after and the coloring degree of hot-melt adhesive composition before heat test, measure Gardner color value according to the color test method of the chemical products of defined in JIS K0071.Then, hot-melt adhesive composition 20g is put into vial, vial do not added a cover but directly put into the hot air dryer of 190 DEG C, place after 72 hours, about the coloring degree of hot-melt adhesive composition, measure Gardner color value according to the color test method of the chemical products of defined in JIS K0071.By the differential of the Gardner color value before and after the heating of 190 DEG C in table 1 and 2.
(thermostability 2)
Hot-melt adhesive composition is heated to 140 DEG C and makes its melting, and this hot-melt adhesive composition 50g is put into vial, vial do not added a cover but directly put into the hot air dryer of 190 DEG C, after placing 1 week, hot-melt adhesive composition after visual confirmation heat test, is confirmed whether to produce gelation and carbonization.In table 1 and 2, " good " " bad " is as described below respectively.
" good ": do not produce gelation and carbonization.
" bad ": produce gelation or carbonization.
(association request cross-referenced)
No. 2013-158480th, the Japanese patent application that the application files an application based on No. 2013-142181st, the Japanese patent application of filing an application on July 5th, 2013 and on July 31st, 2013 and CLAIM OF PRIORITY, the disclosure of this application is introduced in this specification sheets by referring to their full content.
Industrial applicibility
Hot-melt adhesive composition of the present invention can be preferred for absorbent article, and described absorbent article can be preferred for the body fluid such as absorbing blood or urine, sweat, purulence, gastric juice, saliva, nose secreting mucus.
Claims (3)
1. a hot-melt adhesive composition, it comprises: thermoplastic block copolymers (A) 100 weight part, liquid rubber (B) 0.05 ~ 10 weight part and tackifying resin (C)
Described thermoplastic block copolymers (A) containing be selected from styrene content content be 15 ~ 35 % by weight styrene isoprene styrene block copolymer (SIS), styrene content content be 15 ~ 35 % by weight styrene-butadiene-styrene block copolymer and styrene content content be at least one in the styrene butadiene/butylene-styrene segmented copolymer of 15 ~ 35 % by weight
Described liquid rubber (B) has carboxyl and/or acid anhydride in molecule.
2. hot-melt adhesive composition according to claim 1, wherein, the softening temperature of tackifying resin (C) is 80 ~ 120 DEG C.
3. an absorbent article, it uses the adhesive composite described in claim 1 and obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611128003.9A CN106753092B (en) | 2013-07-05 | 2014-07-04 | Hot-melt adhesive composition and water-absorbing article obtained using same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013-142181 | 2013-07-05 | ||
| JP2013142181 | 2013-07-05 | ||
| JP2013-158480 | 2013-07-31 | ||
| JP2013158480A JP5404958B1 (en) | 2013-07-05 | 2013-07-31 | Hot melt adhesive composition and water absorbent article using the same |
| PCT/JP2014/067955 WO2015002308A1 (en) | 2013-07-05 | 2014-07-04 | Hot-melt adhesive agent composition, and water-absorbable article manufactured using same |
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| CN201611128003.9A Division CN106753092B (en) | 2013-07-05 | 2014-07-04 | Hot-melt adhesive composition and water-absorbing article obtained using same |
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| CN104411796A true CN104411796A (en) | 2015-03-11 |
| CN104411796B CN104411796B (en) | 2017-01-18 |
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| CN201611128003.9A Active CN106753092B (en) | 2013-07-05 | 2014-07-04 | Hot-melt adhesive composition and water-absorbing article obtained using same |
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| JP (1) | JP5404958B1 (en) |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109688992A (en) * | 2016-09-28 | 2019-04-26 | 日本瑞翁株式会社 | The manufacturing method of packaging structure |
| CN110741058A (en) * | 2017-06-12 | 2020-01-31 | 株式会社Moresco | Hot-melt adhesive |
| CN111148812A (en) * | 2017-10-03 | 2020-05-12 | 株式会社Moresco | Adhesive composition |
| CN114051504A (en) * | 2019-07-11 | 2022-02-15 | 株式会社可乐丽 | Modified conjugated diene polymer and polymer composition containing same |
| US20220282131A1 (en) * | 2021-03-03 | 2022-09-08 | Sumitomo Rubber Industries, Ltd. | Aqueous adhesive for tennis ball |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6544942B2 (en) | 2015-02-20 | 2019-07-17 | ヘンケルジャパン株式会社 | Hot melt adhesive and disposable products |
| JP6607182B2 (en) * | 2016-12-27 | 2019-11-20 | 横浜ゴム株式会社 | Hot melt composition |
| JP7356008B2 (en) * | 2019-10-03 | 2023-10-04 | 横浜ゴム株式会社 | Rubber composition for adhering steel cords and conveyor belts |
| EP3916053A1 (en) | 2020-05-27 | 2021-12-01 | Bostik SA | Hot melt adhesive composition having improved wet bonding strength |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51122135A (en) * | 1975-04-17 | 1976-10-26 | Nippon Zeon Co Ltd | Pressure-sensitive adhesive composition |
| JPS54152037A (en) * | 1978-05-23 | 1979-11-29 | Denki Kagaku Kogyo Kk | Vulcanizable hot-melt adhesive and its production |
| JP2007169531A (en) * | 2005-12-26 | 2007-07-05 | Nippon Nsc Ltd | Hot-melt adhesive and disposable product |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11106729A (en) * | 1997-09-30 | 1999-04-20 | Nichiban Co Ltd | Hot-melt pressure-sensitive adhesive composition |
| JP2001279212A (en) * | 1999-10-05 | 2001-10-10 | Sekisui Chem Co Ltd | Hot-melt adhesive composition |
-
2013
- 2013-07-31 JP JP2013158480A patent/JP5404958B1/en active Active
-
2014
- 2014-07-04 CN CN201480001723.1A patent/CN104411796B/en active Active
- 2014-07-04 CN CN201611128003.9A patent/CN106753092B/en active Active
- 2014-07-04 WO PCT/JP2014/067955 patent/WO2015002308A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51122135A (en) * | 1975-04-17 | 1976-10-26 | Nippon Zeon Co Ltd | Pressure-sensitive adhesive composition |
| JPS54152037A (en) * | 1978-05-23 | 1979-11-29 | Denki Kagaku Kogyo Kk | Vulcanizable hot-melt adhesive and its production |
| JP2007169531A (en) * | 2005-12-26 | 2007-07-05 | Nippon Nsc Ltd | Hot-melt adhesive and disposable product |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109688992A (en) * | 2016-09-28 | 2019-04-26 | 日本瑞翁株式会社 | The manufacturing method of packaging structure |
| US11465788B2 (en) | 2016-09-28 | 2022-10-11 | Zeon Corporation | Method of manufacturing package structure |
| CN110741058A (en) * | 2017-06-12 | 2020-01-31 | 株式会社Moresco | Hot-melt adhesive |
| CN111148812A (en) * | 2017-10-03 | 2020-05-12 | 株式会社Moresco | Adhesive composition |
| CN114051504A (en) * | 2019-07-11 | 2022-02-15 | 株式会社可乐丽 | Modified conjugated diene polymer and polymer composition containing same |
| US20220282131A1 (en) * | 2021-03-03 | 2022-09-08 | Sumitomo Rubber Industries, Ltd. | Aqueous adhesive for tennis ball |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106753092A (en) | 2017-05-31 |
| CN104411796B (en) | 2017-01-18 |
| JP5404958B1 (en) | 2014-02-05 |
| WO2015002308A1 (en) | 2015-01-08 |
| JP2015028118A (en) | 2015-02-12 |
| CN106753092B (en) | 2020-12-08 |
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