CN106479085A - A kind of high-impact Graphene modifying character for PVC material - Google Patents
A kind of high-impact Graphene modifying character for PVC material Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
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Abstract
The invention discloses a kind of high-impact Graphene modifying character for PVC material, including following raw material：PVC material, Graphene, PPG, vinyl three (β methoxy ethoxy) silane, ethanedioic acid polyester, zinc acrylate resin, converted starch, montmorillonite, silica, zinc oxide, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene ethyl acrylate copolymer, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, toughener, dispersant, tackifier, curing agent, antibacterial, antioxidant, light stabilizer, ultra-violet absorber, fire retardant.High-impact Graphene modifying character for PVC material obtained in the present invention, is greatly improved mechanical property, such as improves mechanical strength, toughness, rub, resistance to impact, heat endurance, 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 high-impact Graphene modifying character for PVC material.
Background technology
PVC is the English abbreviation of polyvinyl chloride, is the thermoplastic resin being polymerized under initiator effect by vinyl chloride,
It is the homopolymers 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 autocatalysis is decomposed further, draw
Discoloration is played, physical and mechanical properties also declines rapidly.
The Geim and Novoselov of Man Chesidun university 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 as 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, thermal conductivity factor is up to 5300W/m k, higher than CNT and diamond.Graphene is one kind by carbon atom structure
The new material of the individual layer laminated structure for becoming, high with intensity, specific surface area is big, high chemical reactivity, the feature of high fillibility.
Chinese patent notification number CN103044811A, April 17 2013 day for announcing, a kind of entitled PVC material, should
Application case discloses a kind of PVC material, including the composition of following weight content：Calcium stearate 3-10 part, acrylate 2-6
Part, amide waxe 1-3 part, PVC 80-120 part.Which is disadvantageous in that, the PVC material of the formula although nontoxic odorless, but
Be its PVC material that produces mechanical strength 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 high-impact Graphene modifying character for PVC material, to solve existing PVC
The mechanical strength of material is low, fracture toughness, rub resistance, resistance to impact and the problems such as poor flame retardant properties.High obtained in the present invention
Anti-impact Graphene modifying character for PVC material, improves mechanical strength, toughness, rub, resistance to impact, heat endurance, anti-flammability.
In order to solve above technical problem, the present invention is employed the following technical solutions：
A kind of high-impact Graphene modifying character for PVC material, in units of weight portion, including following raw material：PVC material 163-208
Part, Graphene 54-70 part, PPG 12-19 part, vinyl three ('beta '-methoxy ethyoxyl) silane 6-12 part, second
Two acid polyester 10-15 parts, zinc acrylate resin 7-11 part, converted starch 9-14 part, montmorillonite 4-8 part, silica 2-5 part, oxygen
Change zinc 3-6 part, titanium dioxide 2-4 part, dicalcium powder 2-3 part, vinal 4-6 part, Fypro 5-8 part, glass fibers
Dimension 3-5 part, amide waxe 6-12 part, ethylene-ethyl acrylate copolymer 2-3 part, polyvinyl acetate emulsion 3-6 part, dimethyl-silicon
Oily 4-7 part, triethanolamine 1-2 part, surfactant 0.4-0.8 part, initiator 0.3-0.6 part, crosslinking agent 0.3-0.5 part, urge
Agent 0.2-0.3 part, accelerator 0.1-0.2 part, plasticizer 0.3-0.5 part, toughener 0.4-0.6 part, dispersant 0.2-0.5
Part, tackifier 0.3-0.4 part, curing agent 0.8-1.2 part, antiseptic 0.7-1.2 part, antioxidant 0.3-0.6 part, light stabilizer
0.2-0.3 part, ultra-violet absorber 0.3-0.5 part, fire retardant 1.3-1.6 part；
The converted starch, in units of weight portion, including following raw material：Tapioca 86-118 part, isoamyl acetate 10-14
Part, dimethylacetylamide 8-12 part, epoxychloropropane 2-4 part, urea 1.8-3.2 part, potassium hydroxide 1-2 part, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 part, organic tin stabilizer 0.2-0.3 part, poly-
Oxygen ethene polyoxypropylene pentaerythrite ether 0.4-0.6 part, propyl trimethoxy silicane 0.3-0.5 part, boric acid 0.2-0.4 part；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The crosslinking 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 part, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 part, APP 15-22 part, pentaerythrite 10-18 part, urea 9-14 part, aluminium hydroxide
6-10 part, antimony oxide 8-12 part, manganese oxide 4-8 part, atlapulgite 6-12 part, bleeding agent 1.2-1.5 part, synergist 0.6-
0.9 part；
The preparation method of the high-impact Graphene 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 is added in Graphene energy powder obtained in step S1, be 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 189-262W in microwave power, temperature be 125-133 DEG C, rotating speed be 300-500r/min under
Stirring 2.3-3.4h, is obtained mixture I；
S4：Converted starch, curing agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 72-76 DEG C in temperature, and rotating speed is to stir 1-1.5 h under 100-200r/min, and mixture II is obtained；
The preparation method of the converted starch, comprises the following steps：
（A）Compound concentration is para arrowroot slurry I of 18-26Be ', the pH value for 3.4-3.8；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, are then 61-65 DEG C in temperature, and speed of agitator is to be crosslinked under 100-160r/min
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, gelatinization
42-50min, gelatinization are down to 35-38 DEG C after terminating, and add polyoxyethylene polyoxypropylene pentaerythrite ether, are 80- in rotating speed
12-14min is stirred under 100r/min, converted starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 part are added in microwave reactor, is stirred under speed of agitator is for 400-600r/min
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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, under rotating speed is for 3000-5000r/min
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 high-impact Graphene modifying character for PVC material.
Further, the tackifier are butyl trimethoxy silane.
Further, the curing agent is epoxylite curing agent.
Further, the antiseptic is lithium carbonate.
Further, the antioxidant is antioxidant 626.
Further, the light stabilizer is light stabilizer 3853.
Further, the ultra-violet absorber is septichen phenyl ester.
The invention has the advantages that：
The present invention adds Graphene to be modified in PVC material is 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 high-impact Graphene modifying character for PVC material, in units of weight portion, including following raw material：
PVC material 163-208 part, Graphene 54-70 part, PPG 12-19 part, vinyl three ('beta '-methoxy ethyoxyl)
Silane 6-12 part, ethanedioic acid polyester 10-15 part, zinc acrylate resin 7-11 part, converted starch 9-14 part, montmorillonite 4-8 part,
Silica 2-5 part, zinc oxide 3-6 part, titanium dioxide 2-4 part, dicalcium powder 2-3 part, vinal 4-6 part, polyamide are fine
Dimension 5-8 part, glass fibre 3-5 part, amide waxe 6-12 part, ethylene-ethyl acrylate copolymer 2-3 part, polyvinyl acetate emulsion
3-6 part, dimethicone 4-7 part, triethanolamine 1-2 part, surfactant 0.4-0.8 part, initiator 0.3-0.6 part, crosslinking
Agent 0.3-0.5 part, catalyst 0.2-0.3 part, accelerator 0.1-0.2 part, plasticizer 0.3-0.5 part, toughener 0.4-0.6 part,
Dispersant 0.2-0.5 part, tackifier 0.3-0.4 part, curing agent 0.8-1.2 part, antiseptic 0.7-1.2 part, antioxidant 0.3-0.6
Part, light stabilizer 0.2-0.3 part, ultra-violet absorber 0.3-0.5 part, fire retardant 1.3-1.6 part；
The converted starch, in units of weight portion, including following raw material：Tapioca 86-118 part, isoamyl acetate 10-14
Part, dimethylacetylamide 8-12 part, epoxychloropropane 2-4 part, urea 1.8-3.2 part, potassium hydroxide 1-2 part, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 part, organic tin stabilizer 0.2-0.3 part, poly-
Oxygen ethene polyoxypropylene pentaerythrite ether 0.4-0.6 part, propyl trimethoxy silicane 0.3-0.5 part, boric acid 0.2-0.4 part；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The crosslinking 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 tackifier are butyl trimethoxy silane；
The curing agent is epoxylite curing agent；
The antiseptic is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The ultra-violet absorber is septichen phenyl ester；
The fire retardant in units of weight portion, including following raw material：Tributoxyethyl phosphate 45-62 part, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 part, APP 15-22 part, pentaerythrite 10-18 part, urea 9-14 part, aluminium hydroxide
6-10 part, antimony oxide 8-12 part, manganese oxide 4-8 part, atlapulgite 6-12 part, bleeding agent 1.2-1.5 part, synergist 0.6-
0.9 part；
The preparation method of the high-impact Graphene 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 is added in Graphene energy powder obtained in step S1, be 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 189-262W in microwave power, temperature be 125-133 DEG C, rotating speed be 300-500r/min under
Stirring 2.3-3.4h, is obtained mixture I；
S4：Converted starch, curing agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 72-76 DEG C in temperature, and rotating speed is to stir 1-1.5 h under 100-200r/min, and mixture II is obtained；
The preparation method of the converted starch, comprises the following steps：
（A）Compound concentration is para arrowroot slurry I of 18-26Be ', the pH value for 3.4-3.8；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, are then 61-65 DEG C in temperature, and speed of agitator is to be crosslinked under 100-160r/min
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, gelatinization
42-50min, gelatinization are down to 35-38 DEG C after terminating, and add polyoxyethylene polyoxypropylene pentaerythrite ether, are 80- in rotating speed
12-14min is stirred under 100r/min, converted starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 part are added in microwave reactor, is stirred under speed of agitator is for 400-600r/min
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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, under rotating speed is for 3000-5000r/min
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 high-impact Graphene modifying character for PVC material.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of high-impact Graphene modifying character for PVC material, in units of weight portion, including following raw material：187 parts of PVC material, stone
62 parts of black alkene, 16 parts of PPG, 10 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 12 parts of ethanedioic acid polyester, third
9 parts of olefin(e) acid zinc resin, 12 parts of converted starch, 6 parts of montmorillonite, 4 parts of silica, 5 parts of zinc oxide, 3 parts of titanium dioxide, dicalcium powder 2
Part, 5 parts of vinal, 7 parts of Fypro, 4 parts of glass fibre, 9 parts of amide waxe, ethylene-ethyl acrylate copolymer 2
Part, 5 parts of polyvinyl acetate emulsion, 6 parts of dimethicone, 1 part of triethanolamine, 0.6 part of surfactant, 0.5 part of initiator, friendship
0.4 part of agent of connection, 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, tackifier
0.3 part, 1 part of curing agent, 0.9 part of antiseptic, 0.5 part of antioxidant, 0.2 part of light stabilizer, 0.4 part of ultra-violet absorber, fire-retardant
1.5 parts of agent；
The converted 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 urea, 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 pentaerythrite 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 crosslinking 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 tackifier are butyl trimethoxy silane；
The curing agent is epoxylite curing agent；
The antiseptic is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The ultra-violet absorber is septichen 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 pentaerythrite, 12 parts of urea, 8 parts of aluminium hydroxide, antimony oxide
10 parts, 6 parts of manganese oxide, 9 parts of atlapulgite, 1.4 parts of bleeding agent, 0.8 part of synergist；
The preparation method of the high-impact Graphene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 400 mesh sieve are crossed, powder is obtained, gained powder is 6000GS in magnetic field intensity, ultrasonic 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 220W in microwave power, temperature is 132 DEG C, and rotating speed is to stir 3h under 400r/min, is obtained mixed
Compound I；
S4：Converted starch, curing 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 converted starch, comprises the following steps：
（A）Compound concentration is the para arrowroot slurry I that 22Be ', pH value is 3.6；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- diformazan that concentration is 7% is added in the para arrowroot slurry I of step A
Base -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, be subsequently added into epoxychloropropane, urea, 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, system
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, and 78 DEG C are warming up to, and 46min is gelatinized,
Gelatinization is down to 37 DEG C after terminating, and adds polyoxyethylene polyoxypropylene pentaerythrite ether, stirs 13min under rotating speed is for 90r/min,
Prepared converted starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 235 parts of water are added in microwave reactor, 8min are stirred under speed of agitator is for 500r/min, 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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, be centrifuged under rotating speed is for 4000r/min
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, is granulated at 146 DEG C,
Prepared high-impact Graphene modifying character for PVC material.
Embodiment 2
A kind of high-impact Graphene modifying character for PVC material, in units of weight portion, including following raw material：163 parts of PVC material, stone
54 parts of black alkene, 12 parts of PPG, 6 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 10 parts of ethanedioic acid polyester, third
7 parts of olefin(e) acid zinc resin, 9 parts of converted starch, 4 parts of montmorillonite, 2 parts of silica, 3 parts of zinc oxide, 2 parts of titanium dioxide, dicalcium powder 2
Part, 4 parts of vinal, 5 parts of Fypro, 3 parts of glass fibre, 6 parts of amide waxe, ethylene-ethyl acrylate copolymer 2
Part, 3 parts of polyvinyl acetate emulsion, 4 parts of dimethicone, 1 part of triethanolamine, 0.4 part of surfactant, 0.3 part of initiator, friendship
0.3 part of agent of connection, 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, tackifier
0.3 part, 0.8 part of curing agent, 0.7 part of antiseptic, 0.3 part of antioxidant, 0.2 part of light stabilizer, 0.3 part of ultra-violet absorber, resistance
1.3 parts of agent of combustion；
The converted 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 urea, 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 pentaerythrite 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 crosslinking 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 tackifier are butyl trimethoxy silane；
The curing agent is epoxylite curing agent；
The antiseptic is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The ultra-violet absorber is septichen 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 pentaerythrite, 9 parts of urea, 6 parts of aluminium hydroxide, antimony oxide 8
Part, 4 parts of manganese oxide, 6 parts of atlapulgite, 1.2 parts of bleeding agent, 0.6 part of synergist；
The preparation method of the high-impact Graphene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 300 mesh sieve are crossed, powder is obtained, gained powder is 5800GS in magnetic field intensity, ultrasonic 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 189W in microwave power, temperature be 125 DEG C, rotating speed be 300r/min under stir 3.4h, be obtained
Mixture I；
S4：Converted starch, curing agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 72 DEG C in temperature, and rotating speed is to stir 1.5 h under 100r/min, and mixture II is obtained；
The preparation method of the converted starch, comprises the following steps：
（A）Compound concentration is the para arrowroot slurry I that 18Be ', pH value is 3.4；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- diformazan that concentration is 5% is added in the para arrowroot slurry I of step A
Base -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, be subsequently added into epoxychloropropane, urea, 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, system
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, and 76 DEG C are warming up to, and 50min is gelatinized,
Gelatinization is down to 35 DEG C after terminating, and adds polyoxyethylene polyoxypropylene pentaerythrite ether, stirs 14min under rotating speed is for 80r/min,
Prepared converted starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 200 parts of water are added in microwave reactor, 9min are stirred under speed of agitator is for 400r/min, 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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, be centrifuged under rotating speed is for 3000r/min
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, is granulated at 142 DEG C,
Prepared high-impact Graphene modifying character for PVC material.
Embodiment 3
A kind of high-impact Graphene modifying character for PVC material, in units of weight portion, including following raw material：208 parts of PVC material, stone
70 parts of black alkene, 19 parts of PPG, 12 parts of vinyl three ('beta '-methoxy ethyoxyl) silane, 15 parts of ethanedioic acid polyester, third
11 parts of olefin(e) acid zinc resin, 14 parts of converted starch, 8 parts of montmorillonite, 5 parts of silica, 6 parts of zinc oxide, 4 parts of titanium dioxide, dicalcium powder 3
Part, 6 parts of vinal, 8 parts of Fypro, 5 parts of glass fibre, 12 parts of amide waxe, ethylene-ethyl acrylate copolymer
3 parts, 6 parts of polyvinyl acetate emulsion, 7 parts of dimethicone, 2 parts of triethanolamine, 0.8 part of surfactant, 0.6 part of initiator,
0.5 part of crosslinking agent, 0.3 part of catalyst, 0.2 part of accelerator, 0.5 part of plasticizer, 0.6 part of toughener, 0.5 part of dispersant, thickening
0.4 part of agent, 1.2 parts of curing agent, 1.2 parts of antiseptic, 0.6 part of antioxidant, 0.3 part of light stabilizer, 0.5 part of ultra-violet absorber,
1.6 parts of fire retardant；
The converted 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 urea, 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 pentaerythrite 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 crosslinking 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 tackifier are butyl trimethoxy silane；
The curing agent is epoxylite curing agent；
The antiseptic is lithium carbonate；
The antioxidant is antioxidant 626；
The light stabilizer is light stabilizer 3853；
The ultra-violet absorber is septichen 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 pentaerythrite, 14 parts of urea, 10 parts of aluminium hydroxide, three oxidations two
12 parts of antimony, 8 parts of manganese oxide, 12 parts of atlapulgite, 1.5 parts of bleeding agent, 0.9 part of synergist；
The preparation method of the high-impact Graphene modifying character for PVC material, comprises the following steps：
S1：Graphene is crushed, 500 mesh sieve are crossed, powder is obtained, gained powder is 6200GS in magnetic field intensity, ultrasonic 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 262W in microwave power, temperature be 133 DEG C, rotating speed be 500r/min under stir 2.3h, be obtained
Mixture I；
S4：Converted starch, curing agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 76 DEG C in temperature, and rotating speed is to stir 1h under 200r/min, and mixture II is obtained；
The preparation method of the converted starch, comprises the following steps：
（A）Compound concentration is the para arrowroot slurry I that 26Be ', pH value is 3.8；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- diformazan that concentration is 8% is added in the para arrowroot slurry I of step A
Base -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, be subsequently added into epoxychloropropane, urea, 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, system
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, and 79 DEG C are warming up to, and 42min is gelatinized,
Gelatinization is down to 38 DEG C after terminating, and adds polyoxyethylene polyoxypropylene pentaerythrite ether, stirs under rotating speed is for 100r/min
12min, is obtained converted starch；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, 265 parts of water are added in microwave reactor, 5min are stirred under speed of agitator is for 600r/min, 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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, be centrifuged under rotating speed is for 5000r/min
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, is granulated at 148 DEG C,
Prepared high-impact Graphene 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
Sample prepared by above-described embodiment 1-3 is tailored into the platelet of standard, then using oxygen index measurer HC-2（Nanjing
Jiangning District analytical instrument factory）With horizontal vertical burning analyzer CZF-3（Analytical instrument factory of Jiangning county）Respectively to high anti-
Rushing Graphene modifying character for PVC material carries out oxygen index (OI) and combustibility measure, oxygen index (OI) 33%-36%, horizontal vertical combustibility nothing
Catch fire, cigarette is light, and flame retardant effect is good.
（2）Mechanics Performance Testing is tested
Sample prepared by above-described embodiment 1-3 tailors the standard platelet of 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 system company）Respectively to height
Anti-impact Graphene modifying character for PVC material is stretched and impact test, tensile figure（Maximum pull, unit：N）542.7-
556.8, Impact Index（Toughness, non-notch）, unit：ki/m2, 7.462-8.372, note：Draw speed is 2mm/min.
In sum, the high-impact Graphene modifying character for PVC material good flame retardation effect of the present invention, strong shock resistance, toughness
By force, excellent fire resistance had not only been obtained but also the preferable mechanical property of high-impact Graphene modifying character for PVC material had been maintained, be a kind of
The excellent high-impact Graphene modifying character for PVC material of performance, 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 explanations, for the present invention affiliated 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 high-impact Graphene modifying character for PVC material, it is characterised in that in units of weight portion, including following raw material：PVC
Material 163-208 part, Graphene 54-70 part, PPG 12-19 part, vinyl three ('beta '-methoxy ethyoxyl) silane
6-12 part, ethanedioic acid polyester 10-15 part, zinc acrylate resin 7-11 part, converted starch 9-14 part, montmorillonite 4-8 part, silica
2-5 part, zinc oxide 3-6 part, titanium dioxide 2-4 part, dicalcium powder 2-3 part, vinal 4-6 part, Fypro 5-8
Part, glass fibre 3-5 part, amide waxe 6-12 part, ethylene-ethyl acrylate copolymer 2-3 part, polyvinyl acetate emulsion 3-6 part,
Dimethicone 4-7 part, triethanolamine 1-2 part, surfactant 0.4-0.8 part, initiator 0.3-0.6 part, crosslinking agent 0.3-
0.5 part, catalyst 0.2-0.3 part, accelerator 0.1-0.2 part, plasticizer 0.3-0.5 part, toughener 0.4-0.6 part, dispersant
0.2-0.5 part, tackifier 0.3-0.4 part, curing agent 0.8-1.2 part, antiseptic 0.7-1.2 part, antioxidant 0.3-0.6 part, light
Stabilizer 0.2-0.3 part, ultra-violet absorber 0.3-0.5 part, fire retardant 1.3-1.6 part；
The converted starch, in units of weight portion, including following raw material：Tapioca 86-118 part, isoamyl acetate 10-14
Part, dimethylacetylamide 8-12 part, epoxychloropropane 2-4 part, urea 1.8-3.2 part, potassium hydroxide 1-2 part, 2,5- dimethyl-
2,5- double (benzoyl peroxide)-hexane 0.4-0.7 parts, platinum catalyst 0.1-0.2 part, organic tin stabilizer 0.2-0.3 part, poly-
Oxygen ethene polyoxypropylene pentaerythrite ether 0.4-0.6 part, propyl trimethoxy silicane 0.3-0.5 part, boric acid 0.2-0.4 part；
The surfactant is surfactant TRITONCF-10；
The initiator is dibenzoyl peroxide；
The crosslinking 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 part, three（2,4- bis- uncles
Butyl phenyl）Phosphite ester 18-32 part, APP 15-22 part, pentaerythrite 10-18 part, urea 9-14 part, aluminium hydroxide
6-10 part, antimony oxide 8-12 part, manganese oxide 4-8 part, atlapulgite 6-12 part, bleeding agent 1.2-1.5 part, synergist 0.6-
0.9 part；
The preparation method of the high-impact Graphene 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 is added in Graphene energy powder obtained in step S1, be 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 material, polyether polyols are added in activation Graphene energy powder obtained in step S2
Alcohol, vinyl three ('beta '-methoxy ethyoxyl) silane, ethanedioic acid polyester, zinc acrylate resin, montmorillonite, silica, oxidation
Zinc, titanium dioxide, dicalcium powder, vinal, Fypro, glass fibre, amide waxe, ethylene-ethylacrylate are common
Polymers, polyvinyl acetate emulsion, dimethicone, triethanolamine, initiator, crosslinking agent, catalyst, accelerator, plasticizer, increasing
Tough dose, dispersant, tackifier, be 189-262W in microwave power, temperature be 125-133 DEG C, rotating speed be 300-500r/min under
Stirring 2.3-3.4h, is obtained mixture I；
S4：Converted starch, curing agent, antibacterial, antioxidant, light stabilizer, ultraviolet is added in mixture I obtained in step S3
Absorbent, fire retardant, are 72-76 DEG C in temperature, and rotating speed is to stir 1-1.5 h under 100-200r/min, and mixture II is obtained；
The preparation method of the converted starch, comprises the following steps：
（A）Compound concentration is para arrowroot slurry I of 18-26Be ', the pH value for 3.4-3.8；
（B）Isoamyl acetate, dimethylacetylamide, 2,5- bis- that concentration is 5%-8% is added in the para arrowroot slurry I of step A
Methyl -2,5- double (benzoyl peroxide)-hexane, platinum catalyst, are then 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 value, is subsequently added into epoxychloropropane, urine
Element, propyl trimethoxy silicane, boric acid, are then 61-65 DEG C in temperature, and speed of agitator is to be crosslinked under 100-160r/min
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, gelatinization
42-50min, gelatinization are down to 35-38 DEG C after terminating, and add polyoxyethylene polyoxypropylene pentaerythrite ether, are 80- in rotating speed
12-14min is stirred under 100r/min, converted starch is obtained；
The preparation method of the fire retardant, comprises the following steps：
（a）APP, water 200-265 part are added in microwave reactor, is stirred under speed of agitator is for 400-600r/min
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, pentaerythrite, urea, aluminium hydroxide, antimony oxide, manganese oxide, atlapulgite, bleeding 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, sediment is filtered, under rotating speed is for 3000-5000r/min
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 high-impact Graphene modifying character for PVC material.
2. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the tackifier are butyl
Trimethoxy silane.
3. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the curing agent is epoxy
Resinoid curing agent.
4. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the antiseptic is carbonic acid
Lithium.
5. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the antioxidant is antioxygen
Agent 626.
6. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the light stabilizer is light
Stabilizer 3853.
7. high-impact Graphene modifying character for PVC material according to claim 1, it is characterised in that the ultra-violet absorber
For septichen phenyl ester.
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| CN106893200A (en) * | 2017-03-12 | 2017-06-27 | 广西丰达三维科技有限公司 | A kind of preparation technology of Environmental-protection bamboo plastotype composite |
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