CN106496844A - A kind of novel graphite alkene modifying character for PVC material - Google Patents
A kind of novel graphite alkene modifying character for PVC material Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention discloses a kind of novel graphite alkene modifying character for PVC material, including following raw material：PVC material, Graphene, polyether polyol, vinyl three (β methoxy ethoxy) silane, butylated amino resin, without benzene epoxy resin, modified starch, bentonite, white carbon black, zinc oxide, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene ethyl acrylate copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator, plasticizer, toughener, dispersant, viscosifier, firming agent, antibacterial, antioxidant, light stabilizer, UV absorbent, fire retardant.Obtained in of the invention, novel graphite alkene modifying character for PVC material, is greatly improved mechanical property, such as improves mechanical strength, toughness, rub, resistance to impact, heat stability, anti-flammability, can be widely applied to hotel, restaurant, building decoration and fitment.
Description
Technical field
The invention belongs to PVC material preparing technical field, and in particular to a kind of novel graphite alkene modifying character for PVC material.
Background technology
PVC is the English abbreviation of polrvinyl chloride, is the thermoplastic resin being polymerized under initiator effect by vinyl chloride,
It is the homopolymer of vinyl chloride, ryuron and vinyl chloride copolymer system are referred to as vinyl chloride resin.PVC material thermally-stabilised
Property poor, more than 100 DEG C or can decompose through long-time exposure in sunshine and produce hydrogen chloride, and further autocatalysiss decompose, draw
Discoloration is played, physical and mechanical propertiess also decline rapidly.
The Geim and Novoselov of Man Chesidun universities of Britain in 2004 peels off high starch breeding by adhesive tape and obtains solely
The vertical two-dimensional graphene for existing（Gra-phene, GN）Since crystal, it is extremely concerned that Graphene has become material science
One of study hotspot.The graphite of Graphene, actually monoatomic layer, it have the two-dimensional structure of uniqueness and excellent power
, thermodynamics, optically and electrically performance.
Graphene be at present most thin in the world be but also most hard nano material, it is almost fully transparent, to inhaling
2.3% light is received, heat conductivity is up to 5300W/m k, higher than CNT and diamond.Graphene be one kind by carbon atom structure
Into monolayer laminated structure new material, high with intensity, specific surface area is big, high chemical reactivity, the characteristics of high fillibility.
Chinese patent notification number CN103044811A, on April 17 2013 day for announcing, a kind of entitled PVC materials should
Application case discloses a kind of PVC materials, including the composition of following weight content：Calcium stearate 3-10 parts, acrylate 2-6
Part, brominated paraffin 1-3 parts, PVC 80-120 parts.Which is disadvantageous in that, the PVC material of the formula although nontoxic odorless,
But the mechanical strength of its PVC material that produces is low, fracture toughness is poor, rub resistance, resistance to impact and poor flame retardant properties.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of novel graphite alkene modifying character for PVC material, to solve existing PVC materials
The mechanical strength of material is low, fracture toughness, rub resistance, resistance to impact and the problems such as poor flame retardant properties.New obtained in of the invention
Graphene modifying character for PVC material, improves mechanical strength, toughness, rub, resistance to impact, heat stability, anti-flammability.
In order to solve above technical problem, the present invention is employed the following technical solutions：
A kind of novel graphite alkene modifying character for PVC material, in units of weight portion, including following raw material：PVC material 163-207 parts,
Graphene 54-68 parts, polyether polyol 12-18 part, vinyl three ('beta '-methoxy ethyoxyl) silane 6-13 parts, butyl ether
Amino resins 10-14 parts, without benzene epoxy resin 7-11 parts, modified starch 9-14 parts, bentonite 4-8 parts, white carbon black 2-5 parts, oxidation
Zinc 3-6 parts, Titanium Dioxide 2-4 part, dolomite dusts 2-3 parts, vinal 4-6 parts, polyvinyl chloride fibre 5-8 parts, glass
Fiber 3-5 parts, brominated paraffin 6-12 parts, ethylene-ethyl acrylate copolymer 2-3 parts, polyvinyl acetate emulsion 3-6 parts, diformazan
Base silicone oil 4-7 parts, triethanolamine 1-2 parts, surfactant 0.4-0.8 parts, initiator 0.3-0.6 parts, cross-linking agent 0.3-0.5
Part, catalyst 0.2-0.3 parts, accelerator 0.1-0.2 parts, plasticizer 0.3-0.5 parts, toughener 0.4-0.6 parts, dispersant 0.2-
0.5 part, viscosifier 0.3-0.4 parts, firming agent 0.8-1.2 parts, antibacterial 0.7-1.2 parts, antioxidant 0.3-0.6 parts, light stable
Agent 0.2-0.3 parts, UV absorbent 0.3-0.5 part, fire retardant 1.3-1.6 parts；
The modified starch, in units of weight portion, including following raw material：Tapioca 86-118 parts, isoamyl acetate 10-14
Part, dimethyl acetylamide 8-12 parts, epoxychloropropane 2-4 parts, carbamide 1.8-3.2 parts, potassium hydroxide 1-2 parts, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 parts, organic tin stabilizer 0.2-0.3 parts, poly-
Oxygen ethylene polyoxypropylene tetramethylolmethane ether 0.4-0.6 parts, propyl trimethoxy silicane 0.3-0.5 parts, boric acid 0.2-0.4 parts；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The fire retardant in units of weight portion, including following raw material：Tributoxyethyl phosphate 45-62 parts, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 parts, APP 15-22 parts, tetramethylolmethane 10-18 parts, carbamide 9-14 parts, aluminium hydroxide
6-10 parts, antimony oxide 8-12 parts, manganese oxide 4-8 parts, active hargil 6-12 parts, penetrating agent 1.2-1.5 parts, synergist 0.6-
0.9 part；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 300-500 mesh sieve is crossed, powder is obtained, gained powder is 5800-6200GS in magnetic field intensity,
Ultrasonic power is 300-500W, and temperature is 40-50 DEG C, and rotating speed is under 200-300r/min, stirs 20-35min, and graphite is obtained
Alkene energy powder；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 56-72 DEG C in temperature, rotating speed is
1-1.5h is activated under 100-130r/min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 192-264W in microwave power, and temperature is 128-135 DEG C, and rotating speed is 300-
2.4-3.2h is stirred under 500r/min, mixture I is obtained；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 71-75 DEG C in temperature, and rotating speed is to stir 1-1.4 h under 100-200r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 18-26Be ', and pH values are the para arrowroot slurry I of 3.4-3.8；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 52-56 DEG C in temperature, and speed of agitator is 90-130r/
Cross-linked graft reaction 2.4-3h is carried out under min, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.5-9.8 to adjust pH values, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, then temperature be 61-65 DEG C, speed of agitator be 100-160r/min under be crosslinked
Reaction 1.2-1.6h, is obtained slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, regulation pH value is 8.8-9.1, is warming up to 76-79 DEG C, gelatinizing
42-50min, gelatinizing are down to 35-38 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, are 80- in rotating speed
12-14min is stirred under 100r/min, modified starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 parts are added in microwave reactor, is to stir under 400-600r/min in speed of agitator
5-9min, is obtained mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 300-500r/min, microwave power is 160-200W, and temperature is to stir 1.8-2.5h at 84-92 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be under 3000-5000r/min in rotating speed
Centrifugal drying is obtained fire retardant to water content≤3.2%；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, is made at 142-148 DEG C
Grain, is obtained novel graphite alkene modifying character for PVC material.
Further, the viscosifier are butyl trimethoxy silane.
Further, the firming agent is epoxylite firming agent.
Further, the antibacterial is lithium carbonate.
Further, the antioxidant is antioxidant 626.
Further, the light stabilizer is light stabilizer 3853.
Further, the UV absorbent is oxybenzoic acid phenyl ester.
The invention has the advantages that：
The present invention adds Graphene to be modified in PVC materials are prepared, and is suitable for industrialized production, modified by Graphene
PVC material improves mechanical strength, toughness, rub, resistance to impact, heat steady on the original performance basis of PVC material are ensured
Qualitative, anti-flammability, can be widely applied to hotel, restaurant, building decoration and fitment.
Specific embodiment
For ease of more fully understanding the present invention, it is illustrated by following examples, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In an embodiment, the novel graphite alkene modifying character for PVC material, in units of weight portion, including following raw material：PVC
Material 163-207 parts, Graphene 54-68 parts, polyether polyol 12-18 part, vinyl three ('beta '-methoxy ethyoxyl) silane
6-13 parts, butylated amino resin 10-14 parts, without benzene epoxy resin 7-11 parts, modified starch 9-14 parts, bentonite 4-8 parts, charcoal
Black 2-5 parts, zinc oxide 3-6 parts, Titanium Dioxide 2-4 part, dolomite dusts 2-3 parts, vinal 4-6 parts, polrvinyl chloride are fine
Dimension 5-8 parts, glass fibre 3-5 parts, brominated paraffin 6-12 parts, ethylene-ethyl acrylate copolymer 2-3 parts, poly vinyl acetate emulsion
Liquid 3-6 parts, dimethicone 4-7 parts, triethanolamine 1-2 parts, surfactant 0.4-0.8 parts, initiator 0.3-0.6 parts, friendship
Connection agent 0.3-0.5 parts, catalyst 0.2-0.3 parts, accelerator 0.1-0.2 parts, plasticizer 0.3-0.5 parts, toughener 0.4-0.6
Part, dispersant 0.2-0.5 parts, viscosifier 0.3-0.4 parts, firming agent 0.8-1.2 parts, antibacterial 0.7-1.2 parts, antioxidant 0.3-
0.6 part, light stabilizer 0.2-0.3 parts, UV absorbent 0.3-0.5 part, fire retardant 1.3-1.6 parts；
The modified starch, in units of weight portion, including following raw material：Tapioca 86-118 parts, isoamyl acetate 10-14
Part, dimethyl acetylamide 8-12 parts, epoxychloropropane 2-4 parts, carbamide 1.8-3.2 parts, potassium hydroxide 1-2 parts, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 parts, organic tin stabilizer 0.2-0.3 parts, poly-
Oxygen ethylene polyoxypropylene tetramethylolmethane ether 0.4-0.6 parts, propyl trimethoxy silicane 0.3-0.5 parts, boric acid 0.2-0.4 parts；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The viscosifier are butyl trimethoxy silane；
The firming agent is epoxylite firming agent；
The antibacterial is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The UV absorbent is oxybenzoic acid phenyl ester；
The fire retardant in units of weight portion, including following raw material：Tributoxyethyl phosphate 45-62 parts, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 parts, APP 15-22 parts, tetramethylolmethane 10-18 parts, carbamide 9-14 parts, aluminium hydroxide
6-10 parts, antimony oxide 8-12 parts, manganese oxide 4-8 parts, active hargil 6-12 parts, penetrating agent 1.2-1.5 parts, synergist 0.6-
0.9 part；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 300-500 mesh sieve is crossed, powder is obtained, gained powder is 5800-6200GS in magnetic field intensity,
Ultrasonic power is 300-500W, and temperature is 40-50 DEG C, and rotating speed is under 200-300r/min, stirs 20-35min, and graphite is obtained
Alkene energy powder；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 56-72 DEG C in temperature, rotating speed is
1-1.5h is activated under 100-130r/min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 192-264W in microwave power, and temperature is 128-135 DEG C, and rotating speed is 300-
2.4-3.2h is stirred under 500r/min, mixture I is obtained；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 71-75 DEG C in temperature, and rotating speed is to stir 1-1.4 h under 100-200r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 18-26Be ', and pH values are the para arrowroot slurry I of 3.4-3.8；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 52-56 DEG C in temperature, and speed of agitator is 90-130r/
Cross-linked graft reaction 2.4-3h is carried out under min, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.5-9.8 to adjust pH values, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, then temperature be 61-65 DEG C, speed of agitator be 100-160r/min under be crosslinked
Reaction 1.2-1.6h, is obtained slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, regulation pH value is 8.8-9.1, is warming up to 76-79 DEG C, gelatinizing
42-50min, gelatinizing are down to 35-38 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, are 80- in rotating speed
12-14min is stirred under 100r/min, modified starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 parts are added in microwave reactor, is to stir under 400-600r/min in speed of agitator
5-9min, is obtained mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 300-500r/min, microwave power is 160-200W, and temperature is to stir 1.8-2.5h at 84-92 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be under 3000-5000r/min in rotating speed
Centrifugal drying is obtained fire retardant to water content≤3.2%；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, is made at 142-148 DEG C
Grain, is obtained novel graphite alkene modifying character for PVC material.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of novel graphite alkene modifying character for PVC material, in units of weight portion, including following raw material：187 parts of PVC materials, graphite
62 parts of alkene, 16 parts of polyether polyol, 10 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 12 parts of butylated amino resin,
Without 9 parts of benzene epoxy resin, 12 parts of modified starch, 6 parts of bentonite, 4 parts of white carbon black, 5 parts of zinc oxide, 3 parts of Titanium Dioxide, dolomite dusts
2 parts, 5 parts of vinal, 7 parts of polyvinyl chloride fibre, 4 parts of glass fibre, 9 parts of brominated paraffin, ethylene-ethylacrylate common
2 parts of polymers, 5 parts of polyvinyl acetate emulsion, 6 parts of dimethicone, 1 part of triethanolamine, 0.6 part of surfactant, initiator 0.5
Part, 0.4 part of cross-linking agent, 0.2 part of catalyst, 0.1 part of accelerator, 0.4 part of plasticizer, 0.5 part of toughener, 0.4 part of dispersant, increasing
0.3 part of stick, 1 part of firming agent, 0.9 part of antibacterial, 0.5 part of antioxidant, 0.2 part of light stabilizer, 0.4 part of UV absorbent,
1.5 parts of fire retardant；
The modified starch, in units of weight portion, including following raw material：105 parts of tapioca, 12 parts of isoamyl acetate, two
10 parts of methylacetamide, 3 parts of epoxychloropropane, 2.5 parts of carbamide, 1.5 parts of potassium hydroxide, 2,5- dimethyl -2, double (the benzene first of 5-
Acyl peroxide) 0.6 part of-hexane, 0.1 part of platinum catalyst, 0.2 part of organic tin stabilizer, polyoxyethylene polyoxypropylene tetramethylolmethane ether
0.5 part, 0.4 part of propyl trimethoxy silicane, 0.3 part of boric acid；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The viscosifier are butyl trimethoxy silane；
The firming agent is epoxylite firming agent；
The antibacterial is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The UV absorbent is oxybenzoic acid phenyl ester；
The fire retardant in units of weight portion, including following raw material：54 parts of tributoxyethyl phosphate, three（2,4- bis- tertiary fourths
Base phenyl）25 parts of phosphite ester, 18 parts of APP, 15 parts of tetramethylolmethane, 12 parts of carbamide, 8 parts of aluminium hydroxide, antimony oxide
10 parts, 6 parts of manganese oxide, 9 parts of active hargil, 1.4 parts of penetrating agent, 0.8 part of synergist；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, cross 400 mesh sieve, be obtained powder, gained powder magnetic field intensity be 6000GS, ultrasound wave work(
Rate is 400W, and temperature is 46 DEG C, and rotating speed is under 250r/min, stirs 28min, and Graphene energy powder is obtained；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 65 DEG C in temperature, rotating speed is 120r/
1.3h is activated under min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 220W in microwave power, and temperature is 132 DEG C, and rotating speed is to stir under 400r/min
3h, is obtained mixture I；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 70 DEG C in temperature, and rotating speed is to stir 1.2 h under 150r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 22Be ', and pH values are 3.6 para arrowroot slurry I；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- diformazans that concentration is 7% is added in the para arrowroot slurry I of step A
Base -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 55 DEG C in temperature, and speed of agitator is to enter under 120r/min
Row cross-linked graft reacts 2.8h, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.6 to adjust pH values, be subsequently added into epoxychloropropane, carbamide, third
Base trimethoxy silane, boric acid, then temperature be 64 DEG C, speed of agitator be 150r/min under carry out cross-linking reaction 1.5h, make
Obtain slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, it is 8.9 to adjust pH value, is warming up to 78 DEG C, gelatinizing 46min,
Gelatinizing is down to 37 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, is to stir 13min under 90r/min in rotating speed,
Prepared modified starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 235 parts of water are added in microwave reactor, are 8min to be stirred under 500r/min in speed of agitator, are obtained
Mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 400r/min, microwave power is 180W, and temperature is to stir 2.2h at 88 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be to be centrifuged under 4000r/min in rotating speed
It is 3.2% to dry to water content, and fire retardant is obtained；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, pelletize at 146 DEG C,
Prepared novel graphite alkene modifying character for PVC material.
Embodiment 2
A kind of novel graphite alkene modifying character for PVC material, in units of weight portion, including following raw material：163 parts of PVC materials, graphite
54 parts of alkene, 12 parts of polyether polyol, 6 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 10 parts of butylated amino resin,
Without 7 parts of benzene epoxy resin, 9 parts of modified starch, 4 parts of bentonite, 2 parts of white carbon black, 3 parts of zinc oxide, 2 parts of Titanium Dioxide, dolomite dusts 2
Part, 4 parts of vinal, 5 parts of polyvinyl chloride fibre, 3 parts of glass fibre, 6 parts of brominated paraffin, ethylene-ethylacrylate are common
2 parts of polymers, 3 parts of polyvinyl acetate emulsion, 4 parts of dimethicone, 1 part of triethanolamine, 0.4 part of surfactant, initiator 0.3
Part, 0.3 part of cross-linking agent, 0.2 part of catalyst, 0.1 part of accelerator, 0.3 part of plasticizer, 0.4 part of toughener, 0.2 part of dispersant, increasing
0.3 part of stick, 0.8 part of firming agent, 0.7 part of antibacterial, 0.3 part of antioxidant, 0.2 part of light stabilizer, UV absorbent 0.3
Part, 1.3 parts of fire retardant；
The modified starch, in units of weight portion, including following raw material：86 parts of tapioca, 10 parts of isoamyl acetate, diformazan
8 parts of yl acetamide, 2 parts of epoxychloropropane, 1.8 parts of carbamide, 1 part of potassium hydroxide, 2,5- dimethyl -2, double (the benzoyl mistakes of 5-
Oxygen) 0.4 part of-hexane, 0.1 part of platinum catalyst, 0.2 part of organic tin stabilizer, polyoxyethylene polyoxypropylene tetramethylolmethane ether 0.4
Part, 0.3 part of propyl trimethoxy silicane, 0.2 part of boric acid；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The viscosifier are butyl trimethoxy silane；
The firming agent is epoxylite firming agent；
The antibacterial is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The UV absorbent is oxybenzoic acid phenyl ester；
The fire retardant in units of weight portion, including following raw material：45 parts of tributoxyethyl phosphate, three（2,4- bis- tertiary fourths
Base phenyl）18 parts of phosphite ester, 15 parts of APP, 10 parts of tetramethylolmethane, 9 parts of carbamide, 6 parts of aluminium hydroxide, antimony oxide 8
Part, 4 parts of manganese oxide, 6 parts of active hargil, 1.2 parts of penetrating agent, 0.6 part of synergist；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, cross 300 mesh sieve, be obtained powder, gained powder magnetic field intensity be 5800GS, ultrasound wave work(
Rate is 300W, and temperature is 40 DEG C, and rotating speed is under 200r/min, stirs 35min, and Graphene energy powder is obtained；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 56 DEG C in temperature, rotating speed is 100r/
1.5h is activated under min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 192W in microwave power, and temperature is 128 DEG C, and rotating speed is to stir under 300r/min
3.2h, is obtained mixture I；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 71 DEG C in temperature, and rotating speed is to stir 1.4 h under 100r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 18Be ', and pH values are 3.4 para arrowroot slurry I；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- diformazans that concentration is 5% is added in the para arrowroot slurry I of step A
Base -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 52 DEG C in temperature, and speed of agitator is to carry out under 90r/min
Cross-linked graft reacts 3h, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.5 to adjust pH values, be subsequently added into epoxychloropropane, carbamide, third
Base trimethoxy silane, boric acid, then temperature be 61 DEG C, speed of agitator be 100r/min under carry out cross-linking reaction 1.6h, make
Obtain slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, it is 8.8 to adjust pH value, is warming up to 76 DEG C, gelatinizing 50min,
Gelatinizing is down to 35 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, is to stir 14min under 80r/min in rotating speed,
Prepared modified starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 200 parts of water are added in microwave reactor, are 9min to be stirred under 400r/min in speed of agitator, are obtained
Mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 300r/min, microwave power is 160W, and temperature is to stir 2.5h at 84 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be to be centrifuged under 3000r/min in rotating speed
It is 3% to dry to water content, and fire retardant is obtained；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, pelletize at 142 DEG C,
Prepared novel graphite alkene modifying character for PVC material.
Embodiment 3
A kind of novel graphite alkene modifying character for PVC material, in units of weight portion, including following raw material：207 parts of PVC materials, graphite
68 parts of alkene, 18 parts of polyether polyol, 13 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 14 parts of butylated amino resin,
Without 11 parts of benzene epoxy resin, 14 parts of modified starch, 8 parts of bentonite, 5 parts of white carbon black, 6 parts of zinc oxide, 4 parts of Titanium Dioxide, dolomite
3 parts of powder, 6 parts of vinal, 8 parts of polyvinyl chloride fibre, 5 parts of glass fibre, 12 parts of brominated paraffin, ethylene-acrylic acid second
3 parts of ester copolymer, 6 parts of polyvinyl acetate emulsion, 7 parts of dimethicone, 2 parts of triethanolamine, 0.8 part of surfactant, initiation
0.6 part of agent, 0.5 part of cross-linking agent, 0.3 part of catalyst, 0.2 part of accelerator, 0.5 part of plasticizer, 0.6 part of toughener, dispersant 0.5
Part, 0.4 part of viscosifier, 1.2 parts of firming agent, 1.2 parts of antibacterial, 0.6 part of antioxidant, 0.3 part of light stabilizer, UV absorbent
0.5 part, 1.6 parts of fire retardant；
The modified starch, in units of weight portion, including following raw material：118 parts of tapioca, 14 parts of isoamyl acetate, two
12 parts of methylacetamide, 4 parts of epoxychloropropane, 3.2 parts of carbamide, 2 parts of potassium hydroxide, 2,5- dimethyl -2, the double (benzoyls of 5-
Peroxide) 0.7 part of-hexane, 0.2 part of platinum catalyst, 0.3 part of organic tin stabilizer, polyoxyethylene polyoxypropylene tetramethylolmethane ether 0.6
Part, 0.5 part of propyl trimethoxy silicane, 0.4 part of boric acid；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The viscosifier are butyl trimethoxy silane；
The firming agent is epoxylite firming agent；
The antibacterial is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The UV absorbent is oxybenzoic acid phenyl ester；
The fire retardant in units of weight portion, including following raw material：62 parts of tributoxyethyl phosphate, three（2,4- bis- tertiary fourths
Base phenyl）32 parts of phosphite ester, 22 parts of APP, 18 parts of tetramethylolmethane, 14 parts of carbamide, 10 parts of aluminium hydroxide, three oxidations two
12 parts of antimony, 8 parts of manganese oxide, 12 parts of active hargil, 1.5 parts of penetrating agent, 0.9 part of synergist；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, cross 500 mesh sieve, be obtained powder, gained powder magnetic field intensity be 6200GS, ultrasound wave work(
Rate is 500W, and temperature is 50 DEG C, and rotating speed is under 300r/min, stirs 20min, and Graphene energy powder is obtained；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 72 DEG C in temperature, rotating speed is 130r/
1h is activated under min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 264W in microwave power, and temperature is 135 DEG C, and rotating speed is to stir under 500r/min
2.4h, is obtained mixture I；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 75 DEG C in temperature, and rotating speed is to stir 1 h under 1200r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 26Be ', and pH values are 3.8 para arrowroot slurry I；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- diformazans that concentration is 8% is added in the para arrowroot slurry I of step A
Base -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 56 DEG C in temperature, and speed of agitator is to enter under 130r/min
Row cross-linked graft reacts 2.4h, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.8 to adjust pH values, be subsequently added into epoxychloropropane, carbamide, third
Base trimethoxy silane, boric acid, then temperature be 65 DEG C, speed of agitator be 160r/min under carry out cross-linking reaction 1.2h, make
Obtain slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, it is 9.1 to adjust pH value, is warming up to 79 DEG C, gelatinizing 42min,
Gelatinizing is down to 38 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, is to stir under 100r/min in rotating speed
12min, is obtained modified starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 265 parts of water are added in microwave reactor, are 5min to be stirred under 600r/min in speed of agitator, are obtained
Mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 500r/min, microwave power is 200W, and temperature is to stir 1.8h at 84-92 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be to be centrifuged under 5000r/min in rotating speed
It is 2.6% to dry to water content, and fire retardant is obtained；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, pelletize at 148 DEG C,
Prepared novel graphite alkene modifying character for PVC material.
The composite can be widely applied to hotel, restaurant, building decoration and fitment, good flame retardation effect, it is impossible to burning and formation fire
Flame, stable and reliable for performance, its performance indications is given by following fire resistance test experiments and Mechanics Performance Testing experiment：
（1）Fire resistance test experiments
The platelet that sample prepared by above-described embodiment 1-3 is tailored into standard, then using oxygen index measurer HC-2（Nanjing
Jiangning District analytical tool factory）With horizontal vertical burning analyzer CZF-3（Analytical tool factory of Jiangning county）Respectively to new
Graphene modifying character for PVC material carries out oxygen index (OI) and combustibility is determined, and oxygen index (OI) 33%-39%, horizontal vertical combustibility are undeliverable
Fire, cigarette are light, and flame retardant effect is good.
（2）Mechanics Performance Testing is tested
The standard platelet that sample prepared by above-described embodiment 1-3 is tailored growth 115mm, width 10mm, thickness 2.5mm, then uses
Tester for elongation 5585（U.S. INSTRON）With impact specimen machine ZBC1251-B（Mei Tesi industrial systems company）Respectively to new
Type Graphene modifying character for PVC material is stretched and impact test, tensile figure（Maximum pull, unit：N）544.3-558.1,
Impact Index（Toughness, non-notch）, unit：ki/m2, 7.483-8.369, note：Draw speed is 2mm/min.
In sum, novel graphite alkene modifying character for PVC material good flame retardation effect of the invention, strong shock resistance, toughness are strong,
Not only excellent fire resistance had been obtained but also had maintained the preferable mechanical property of novel graphite alkene modifying character for PVC material, be a kind of performance
Excellent novel graphite alkene modifying character for PVC material, can be applicable, have significant economic and social benefit.
Above content it cannot be assumed that the present invention be embodied as be confined to these explanation, for belonging to the present invention technology neck
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, some simple deduction or replace can also be made,
The scope of patent protection that the present invention is determined should be all considered as belonging to by the claims that is submitted to.
Claims (7)
1. a kind of novel graphite alkene modifying character for PVC material, it is characterised in that in units of weight portion, including following raw material：PVC materials
Material 163-207 parts, Graphene 54-68 parts, polyether polyol 12-18 part, vinyl three ('beta '-methoxy ethyoxyl) silane
6-13 parts, butylated amino resin 10-14 parts, without benzene epoxy resin 7-11 parts, modified starch 9-14 parts, bentonite 4-8 parts, charcoal
Black 2-5 parts, zinc oxide 3-6 parts, Titanium Dioxide 2-4 part, dolomite dusts 2-3 parts, vinal 4-6 parts, polrvinyl chloride are fine
Dimension 5-8 parts, glass fibre 3-5 parts, brominated paraffin 6-12 parts, ethylene-ethyl acrylate copolymer 2-3 parts, poly vinyl acetate emulsion
Liquid 3-6 parts, dimethicone 4-7 parts, triethanolamine 1-2 parts, surfactant 0.4-0.8 parts, initiator 0.3-0.6 parts, friendship
Connection agent 0.3-0.5 parts, catalyst 0.2-0.3 parts, accelerator 0.1-0.2 parts, plasticizer 0.3-0.5 parts, toughener 0.4-0.6
Part, dispersant 0.2-0.5 parts, viscosifier 0.3-0.4 parts, firming agent 0.8-1.2 parts, antibacterial 0.7-1.2 parts, antioxidant 0.3-
0.6 part, light stabilizer 0.2-0.3 parts, UV absorbent 0.3-0.5 part, fire retardant 1.3-1.6 parts；
The modified starch, in units of weight portion, including following raw material：Tapioca 86-118 parts, isoamyl acetate 10-14
Part, dimethyl acetylamide 8-12 parts, epoxychloropropane 2-4 parts, carbamide 1.8-3.2 parts, potassium hydroxide 1-2 parts, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 parts, organic tin stabilizer 0.2-0.3 parts, poly-
Oxygen ethylene polyoxypropylene tetramethylolmethane ether 0.4-0.6 parts, propyl trimethoxy silicane 0.3-0.5 parts, boric acid 0.2-0.4 parts；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The cross-linking agent is Methacrylamide；
The catalyst is three（Dimethylamino-propyl）Hexahydrotriazine；
The accelerator is colourless cobalt；
The plasticizer is citrate；
The toughener is poly- propylene diene rubber；
The dispersant is dispersant NC；
The fire retardant in units of weight portion, including following raw material：Tributoxyethyl phosphate 45-62 parts, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 parts, APP 15-22 parts, tetramethylolmethane 10-18 parts, carbamide 9-14 parts, aluminium hydroxide
6-10 parts, antimony oxide 8-12 parts, manganese oxide 4-8 parts, active hargil 6-12 parts, penetrating agent 1.2-1.5 parts, synergist 0.6-
0.9 part；
The preparation method of the novel graphite alkene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 300-500 mesh sieve is crossed, powder is obtained, gained powder is 5800-6200GS in magnetic field intensity,
Ultrasonic power is 300-500W, and temperature is 40-50 DEG C, and rotating speed is under 200-300r/min, stirs 20-35min, and graphite is obtained
Alkene energy powder；
S2：Surfactant being added in Graphene energy powder obtained in step S1, being 56-72 DEG C in temperature, rotating speed is
1-1.5h is activated under 100-130r/min, activation Graphene energy powder is obtained；
S3：Under nitrogen protection, PVC materials, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, butylated amino resin, without benzene epoxy resin, bentonite, white carbon black, oxygen
Change zinc, Titanium Dioxide, dolomite dusts, vinal, polyvinyl chloride fibre, glass fibre, brominated paraffin, ethylene-propylene
Acetoacetic ester copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, cross-linking agent, catalyst, accelerator,
Plasticizer, toughener, dispersant, viscosifier, are 192-264W in microwave power, and temperature is 128-135 DEG C, and rotating speed is 300-
2.4-3.2h is stirred under 500r/min, mixture I is obtained；
S4：Modified starch, firming agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 71-75 DEG C in temperature, and rotating speed is to stir 1-1.4 h under 100-200r/min, and mixture II is obtained；
The preparation method of the modified starch, comprises the following steps：
（A）Compound concentration is 18-26Be ', and pH values are the para arrowroot slurry I of 3.4-3.8；
（B）Isoamyl acetate, dimethyl acetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2, then 5- double (benzoyl peroxide)-hexane, platinum catalyst are 52-56 DEG C in temperature, and speed of agitator is 90-130r/
Cross-linked graft reaction 2.4-3h is carried out under min, and slurry II is obtained；
（C）Paste agent is added in the slurry II of step B, it is 9.5-9.8 to adjust pH values, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, then temperature be 61-65 DEG C, speed of agitator be 100-160r/min under be crosslinked
Reaction 1.2-1.6h, is obtained slurry III；
（D）Organic tin stabilizer will be added in the slurry III of step C, regulation pH value is 8.8-9.1, is warming up to 76-79 DEG C, gelatinizing
42-50min, gelatinizing are down to 35-38 DEG C after terminating, add polyoxyethylene polyoxypropylene tetramethylolmethane ether, are 80- in rotating speed
12-14min is stirred under 100r/min, modified starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 parts are added in microwave reactor, is to stir under 400-600r/min in speed of agitator
5-9min, is obtained mixture A；
（b）To in mixture A obtained in step a add tributoxyethyl phosphate, three（2,4- di-tert-butyl-phenyls）Phosphorous acid
Ester, tetramethylolmethane, carbamide, aluminium hydroxide, antimony oxide, manganese oxide, active hargil, penetrating agent, synergist, in speed of agitator
For 300-500r/min, microwave power is 160-200W, and temperature is to stir 1.8-2.5h at 84-92 DEG C, and mixture B is obtained；
（c）Mixture B obtained in step b is cooled to after room temperature, precipitate is filtered, be under 3000-5000r/min in rotating speed
Centrifugal drying is obtained fire retardant to water content≤3.2%；
S5：Mixture obtained in step S4 II is sent into twin screw earnestly in air-cooled extruding granulator, is made at 142-148 DEG C
Grain, is obtained novel graphite alkene modifying character for PVC material.
2. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the viscosifier are butyl three
Methoxy silane.
3. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the firming agent is epoxiess
Resin curing agent.
4. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the antibacterial is lithium carbonate.
5. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the antioxidant is antioxidant
626.
6. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the light stabilizer is that light is steady
Determine agent 3853.
7. novel graphite alkene modifying character for PVC material according to claim 1, it is characterised in that the UV absorbent is
Oxybenzoic acid phenyl ester.
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| CN115073960A (en) * | 2022-06-30 | 2022-09-20 | 蜂巢能源科技股份有限公司 | Flame-retardant slurry and preparation method and application thereof |
| EP4390559A1 (en) * | 2022-12-22 | 2024-06-26 | The Swatch Group Research and Development Ltd | Method for coating a covering part, in particular in the timepiece area, and coated covering part |
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Application publication date: 20170315 |