CN103709617A - PBT/elastomer/micrometer calcium carbonate ternary composite material and preparation method thereof - Google Patents

PBT/elastomer/micrometer calcium carbonate ternary composite material and preparation method thereof Download PDF

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Publication number
CN103709617A
CN103709617A CN201210368749.2A CN201210368749A CN103709617A CN 103709617 A CN103709617 A CN 103709617A CN 201210368749 A CN201210368749 A CN 201210368749A CN 103709617 A CN103709617 A CN 103709617A
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calcium carbonate
pbt
micro
elastomerics
composite material
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不公告发明人
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Qingdao Xinzhan Plastic Co Ltd
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Qingdao Xinzhan Plastic Co Ltd
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Priority to CN201210368749.2A priority Critical patent/CN103709617A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing

Abstract

The invention discloses a PBT/elastomer/micrometer calcium carbonate ternary composite material and a preparation method thereof. The PBT/elastomer/micrometer calcium carbonate ternary composite material provided by the invention comprises the following components by mass: 60-75% of PBT, 10%-20% of the elastomer, 5%-20% of micrometer calcium carbonate, 0.1%-0.4% of a surface treating agent, 0.1%-1% of an antioxidant, 0.2-1.5% of a lubricant, 0.1-0.5% of a stabilizer and 0-1% of a color material. The PBT/elastomer/micrometer calcium carbonate ternary composite material has the beneficial effects that by blending the elastomer and micrometer calcium carbonate in PBT, impact strength can be greatly increased; rigidity and heat resistance can be increased; the PBT/elastomer/micrometer calcium carbonate ternary composite material has very good toughening, reinforcing and rigidity-enhancing effects; relatively good tensile strength can be protected; and comprehensive performance and processing performance of the PBT/elastomer/micrometer calcium carbonate ternary composite material are excellent. The preparation method provided by the invention is simple and convenient for operation, and can realize industrialization easily.

Description

PBT/ elastomerics/micro-calcium carbonate trielement composite material and preparation method thereof
Technical field
The present invention relates to a kind of macromolecular material, specifically a kind of PBT/ elastomerics/micro-calcium carbonate trielement composite material and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) is a kind of thermoplastic engineering plastic, the industries such as electronic apparatus, household electrical appliances, automotive industry have been widely used in, but due to its low-temperature impact toughness is poor and room temperature under the shortcomings such as notch sensitivity is large, limit its application in some field as a kind of macromolecular structure material.Adopt elastic body toughening can increase substantially the shock resistance of material, but also cause intensity, rigidity, thermotolerance and the processing characteristics of material significantly to decline, cost is also high simultaneously simultaneously.Adopt Rigid Particles Toughened to show toughness reinforcing enhancing simultaneously under certain condition, but the increase rate of toughness is limited.
Summary of the invention
The object of the invention is to, provide a kind of elastomerics and rigid particles and with toughness reinforcing with increase substantially toughness, rigidity, thermotolerance and keep PBT/ elastomerics/micro-calcium carbonate trielement composite material of better intensity and preparation method thereof simultaneously.
The technical solution adopted for the present invention to solve the technical problems is: PBT/ elastomerics/micro-calcium carbonate trielement composite material, its component by mass percent proportioning is: PBT 60%～75%, elastomerics 10%～20%, micro-calcium carbonate 5%～20%, surface treatment agent 0.1%～0.4%, oxidation inhibitor 0.1%～1%, lubricant 0.2%～1.5%, stablizer 0.1%～0.5%, colorant 0～1%.
Described PBT is polybutylene terephthalate, and limiting viscosity is 0.85～1.25dl/g.
Described elastomerics is polyolefin elastomer (POE), maleic anhydride stem grafting polyolefin elastomerics, terpolymer EP rubber, maleic anhydride graft terpolymer EP rubber, ethylene propylene rubber, maleic anhydride graft ethylene propylene rubber and ethylene-vinyl acetate copolymer (EVA).
The median size of described micro-calcium carbonate is between 1 μ m～10 μ m.
Described surface treatment agent is a kind of in stearic acid, calcium stearate, sodium stearate, Magnesium Stearate and silane coupling agent.
Described oxidation inhibitor is a kind of in compound, antioxidant 1010 or the antioxidant 1076 of antioxidant 1010, antioxidant 1076, antioxidant 1010 or antioxidant 1076 and irgasfos 168 and the compound of oxidation inhibitor JC-242.
Described lubricant is one or more the mixture in polysiloxane, EVA wax, TAS-2A, ethylene bis stearic amide.
Described stablizer is one or more the compound in benzotriazole stablizer, benzophenone stablizer, hindered amine stabilizer.
The preparation method of above-mentioned PBT/ elastomerics/micro-calcium carbonate trielement composite material, comprises the following steps:
(1) PBT is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(2) after micro-calcium carbonate and surface treatment agent are taken by weight ratio, add sonic oscillation producer or be not less than in the high-speed mixer of 3000 revs/min, at 80 ℃～120 ℃ temperature, stir 10～60 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated micro-calcium carbonate;
(3) take by weight ratio elastomerics, and mix with above-mentioned surface-treated micro-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make elastomerics/micro-calcium carbonate master batch;
(4) take by weight ratio PBT, oxidation inhibitor, lubricant, stablizer and the colorant after drying treatment, add high-speed mixer, add elastomerics/micro-calcium carbonate master batch simultaneously, make fully to mix 3～5 minutes;
(5) again the mixture of step (4) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, each of twin screw extruder section temperature is 120 ℃～125 ℃, 140 ℃～150 ℃, 155 ℃～170 ℃, 180 ℃～185 ℃, 190 ℃～205 ℃, by twin screw extruder blend, extruding pelletization, obtain PBT/ elastomerics/micro-calcium carbonate trielement composite material.
The invention has the beneficial effects as follows; in PBT, add elastomerics and micro-calcium carbonate blend; when can increase substantially shock strength; improve its rigidity and thermotolerance; make to have well toughness reinforcing, strengthen and increase firm effect; protect good tensile strength, its high comprehensive performance, good processability simultaneously.Preparation method provided by the invention is simple and easy to operate, is easy to realize industrialization.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention.
Embodiment 1:
A kind of PBT/ elastomerics/micro-calcium carbonate trielement composite material, its component by mass percent proportioning is: PBT 70%, polyolefin elastomer (POE) 15%, micro-calcium carbonate 12%, stearic acid 0.3%, antioxidant 1010 0.7%, polysiloxane 1.2%, benzotriazole stablizer 0.4%, colorant 0.4%, wherein, the limiting viscosity of PBT is 0.85～1.25dl/g, and the median size of micro-calcium carbonate is between 1 μ m～10 μ m.
Preparation method: (1) is dried 3～5 hours by PBT at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) after micro-calcium carbonate and stearic acid are taken by weight ratio, add sonic oscillation producer or be not less than in the high-speed mixer of 3000 revs/min, at 80 ℃～120 ℃ temperature, stir 10～60 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated micro-calcium carbonate; (3) take by weight ratio polyolefin elastomer (POE), and mix with above-mentioned surface-treated micro-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make polyolefin elastomer (POE)/micro-calcium carbonate master batch; (4) take by weight ratio PBT, antioxidant 1010, polysiloxane, benzotriazole stablizer and the colorant after drying treatment, add high-speed mixer, add polyolefin elastomer (POE)/micro-calcium carbonate master batch simultaneously, make fully to mix 3～5 minutes; (5) again the mixture of step (4) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, each of twin screw extruder section temperature is 120 ℃～125 ℃, 140 ℃～150 ℃, 155 ℃～170 ℃, 180 ℃～185 ℃, 190 ℃～205 ℃, by twin screw extruder blend, extruding pelletization, obtain PBT/ elastomerics/micro-calcium carbonate trielement composite material.
Embodiment 2:
A kind of PBT/ elastomerics/micro-calcium carbonate trielement composite material, its component by mass percent proportioning is: the compound 0.5% of PBT 60%, terpolymer EP rubber 20%, micro-calcium carbonate 18%, calcium stearate 0.4%, antioxidant 1076 and irgasfos 168, polysiloxane 0.6%, hindered amine stabilizer 0.2%, colorant 0.3%, wherein, the limiting viscosity of PBT is 0.85～1.25dl/g, and the median size of micro-calcium carbonate is between 1 μ m～10 μ m.
Preparation method: (1) is dried 3～5 hours by PBT at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) after micro-calcium carbonate and calcium stearate are taken by weight ratio, add sonic oscillation producer or be not less than in the high-speed mixer of 3000 revs/min, at 80 ℃～120 ℃ temperature, stir 10～60 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated micro-calcium carbonate; (3) take by weight ratio terpolymer EP rubber, and mix with above-mentioned surface-treated micro-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make terpolymer EP rubber/micro-calcium carbonate master batch; (4) take by weight ratio compound, polysiloxane, hindered amine stabilizer and the colorant of PBT, antioxidant 1076 and irgasfos 168 after drying treatment, add high-speed mixer, add terpolymer EP rubber/micro-calcium carbonate master batch simultaneously, make fully to mix 3～5 minutes; (5) again the mixture of step (4) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, each of twin screw extruder section temperature is 120 ℃～125 ℃, 140 ℃～150 ℃, 155 ℃～170 ℃, 180 ℃～185 ℃, 190 ℃～205 ℃, by twin screw extruder blend, extruding pelletization, obtain PBT/ elastomerics/micro-calcium carbonate trielement composite material.
Embodiment 3:
A kind of PBT/ elastomerics/micro-calcium carbonate trielement composite material, its component by mass percent proportioning is: the compound 0.5% of PBT 75%, maleic anhydride stem grafting polyolefin elastomerics 15%, micro-calcium carbonate 8%, silane coupling agent 0.2%, antioxidant 1076 and oxidation inhibitor JC-242, ethylene bis stearic amide 1%, benzophenone stablizer 0.3%, wherein, the limiting viscosity of PBT is 0.85～1.25dl/g, and the median size of micro-calcium carbonate is between 1 μ m～10 μ m.
Preparation method: (1) is dried 3～5 hours by PBT at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) after micro-calcium carbonate and silane coupling agent are taken by weight ratio, add sonic oscillation producer or be not less than in the high-speed mixer of 3000 revs/min, at 80 ℃～120 ℃ temperature, stir 10～60 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated micro-calcium carbonate; (3) take by weight ratio maleic anhydride stem grafting polyolefin elastomerics, and mix with above-mentioned surface-treated micro-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make maleic anhydride stem grafting polyolefin elastomerics/micro-calcium carbonate master batch; (4) take by weight ratio compound, ethylene bis stearic amide and the benzophenone stablizer of PBT, antioxidant 1076 and oxidation inhibitor JC-242 after drying treatment, add high-speed mixer, add maleic anhydride stem grafting polyolefin elastomerics/micro-calcium carbonate master batch simultaneously, make fully to mix 3～5 minutes; (5) again the mixture of step (4) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, each of twin screw extruder section temperature is 120 ℃～125 ℃, 140 ℃～150 ℃, 155 ℃～170 ℃, 180 ℃～185 ℃, 190 ℃～205 ℃, by twin screw extruder blend, extruding pelletization, obtain PBT/ elastomerics/micro-calcium carbonate trielement composite material.

Claims (9)

1. PBT/ elastomerics/micro-calcium carbonate trielement composite material, it is characterized in that, its component by mass percent proportioning is: PBT 60%～75%, elastomerics 10%～20%, micro-calcium carbonate 5%～20%, surface treatment agent 0.1%～0.4%, oxidation inhibitor 0.1%～1%, lubricant 0.2%～1.5%, stablizer 0.1～0.5%, colorant 0～1%.
2. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, described PBT is polybutylene terephthalate, and limiting viscosity is 0.85～1.25dl/g.
3. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, it is characterized in that, described elastomerics is polyolefin elastomer (POE), maleic anhydride stem grafting polyolefin elastomerics, terpolymer EP rubber, maleic anhydride graft terpolymer EP rubber, ethylene propylene rubber, maleic anhydride graft ethylene propylene rubber and ethylene-vinyl acetate copolymer (EVA).
4. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, the median size of described micro-calcium carbonate is between 1 μ m～10 μ m.
5. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, described surface treatment agent is a kind of in stearic acid, calcium stearate, sodium stearate, Magnesium Stearate and silane coupling agent.
6. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, it is characterized in that, described oxidation inhibitor is a kind of in compound, antioxidant 1010 or the antioxidant 1076 of antioxidant 1010, antioxidant 1076, antioxidant 1010 or antioxidant 1076 and irgasfos 168 and the compound of oxidation inhibitor JC-242.
7. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, described lubricant is one or more the mixture in polysiloxane, EVA wax, TAS-2A, ethylene bis stearic amide.
8. PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, described stablizer is one or more the compound in benzotriazole stablizer, benzophenone stablizer, hindered amine stabilizer.
9. the preparation method of PBT/ elastomerics/micro-calcium carbonate trielement composite material according to claim 1, is characterized in that, comprises the following steps:
(1) PBT is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(2) after micro-calcium carbonate and surface treatment agent are taken by weight ratio, add sonic oscillation producer or be not less than in the high-speed mixer of 3000 revs/min, at 80 ℃～120 ℃ temperature, stir 10～60 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated micro-calcium carbonate;
(3) take by weight ratio elastomerics, and mix with above-mentioned surface-treated micro-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make elastomerics/micro-calcium carbonate master batch;
(4) take by weight ratio PBT, oxidation inhibitor, lubricant, stablizer and the colorant after drying treatment, add high-speed mixer, add elastomerics/micro-calcium carbonate master batch simultaneously, make fully to mix 3～5 minutes;
(5) again the mixture of step (4) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, each of twin screw extruder section temperature is 120 ℃～125 ℃, 140 ℃～150 ℃, 155 ℃～170 ℃, 180 ℃～185 ℃, 190 ℃～205 ℃, by twin screw extruder blend, extruding pelletization, obtain PBT/ elastomerics/micro-calcium carbonate trielement composite material.
CN201210368749.2A 2012-09-28 2012-09-28 PBT/elastomer/micrometer calcium carbonate ternary composite material and preparation method thereof Pending CN103709617A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210368749.2A CN103709617A (en) 2012-09-28 2012-09-28 PBT/elastomer/micrometer calcium carbonate ternary composite material and preparation method thereof

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Application Number Priority Date Filing Date Title
CN201210368749.2A CN103709617A (en) 2012-09-28 2012-09-28 PBT/elastomer/micrometer calcium carbonate ternary composite material and preparation method thereof

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CN103709617A true CN103709617A (en) 2014-04-09

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Application publication date: 20140409