CN103709631A - Nanocomposite toughened and flame-retardant modified polybutylene terephthalate - Google Patents
Nanocomposite toughened and flame-retardant modified polybutylene terephthalate Download PDFInfo
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- CN103709631A CN103709631A CN201210370189.4A CN201210370189A CN103709631A CN 103709631 A CN103709631 A CN 103709631A CN 201210370189 A CN201210370189 A CN 201210370189A CN 103709631 A CN103709631 A CN 103709631A
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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
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
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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
- 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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a nanocomposite toughened and flame-retardant modified polybutylene terephthalate. The nanocomposite toughened and flame-retardant modified polybutylene terephthalate comprises components by mass: 30%-70% of polybutylene terephthalate, 5%-25% of an elastomer, 5%-25% of nanoparticles, 0.1%-0.5% of a surface treating agent, 6%-20% of a compound flame retardant, 0.2-1.5% of a lubricant, 0.1%-1% of an antioxidant and 0-0.5% of an antioxidant. Compared with conventional polybutylene terephthalate, the polybutylene terephthalate prepared by the invention can greatly overcome defects of insufficient notch impact strength of a product, has excellent notch impact strength, rigidity and heat resistance and keeps relatively good tensile strength, and has high flame-retardant property, good processing property and low cost.
Description
Technical field
The present invention relates to a kind of macromolecular material, specifically the flame-retardant modified polybutylene terephthalate of a kind of nano composite material toughening.
Background technology
Polybutylene terephthalate (PBT) is the linear saturated polyester resin of a kind of crystal type, because thering is good over-all properties by the widespread use of many fields, if but polybutylene terephthalate use separately have that heat-drawn wire is low, that easy firing, product shrink warpage, mechanical property is outstanding, the not high weak point of goods notched Izod impact strength particularly.So polybutylene terephthalate is used seldom separately, great majority all need just can be employed through modification.The modification of polybutylene terephthalate is mainly set about from two aspects, the one, adopt chemical modification method, by copolymerization, grafting, block, be cross-linked or the chemical process such as degraded, make it have better properties and new function; The 2nd, adopt physical modification method, by adopt inorganic materials fill and strengthen, with other resin alloys and add the methods such as various auxiliary agents to improve and improve the over-all properties of polybutylene terephthalate, but all there are many undesirable parts at the aspect of performance that improves polybutylene terephthalate in the aforesaid method of prior art.
Summary of the invention
The object of the present invention is to provide a kind of flame-retardant modified polybutylene terephthalate of nano composite material toughening with premium properties and high flame retardant efficiency.
The technical solution adopted for the present invention to solve the technical problems is: the flame-retardant modified polybutylene terephthalate of nano composite material toughening, its component by mass percent proportioning is: polybutylene terephthalate 30%～70%, elastomerics 5%～25%, nanoparticle 5%～25%, surface treatment agent 0.1%～0.5%, compound flame redundant 6%～20%, lubricant 0.2～1.5%, oxidation inhibitor 0.1%～1%, other additives 0～0.5%.
Described elastomerics is ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA).
Described nanoparticle is a kind of in nano silicon, nano-calcium carbonate, nanomete talc powder, nano diatomite, nano imvite, nano kaoline and the nano-silicon nitride of median size between 1nm～100nm and silicon carbide compound.
Described surface treatment agent is a kind of in stearic acid, calcium stearate, sodium stearate, Magnesium Stearate, titanic acid ester, Aluminate, silane and phosphoric acid ester.
Described compound flame redundant is poly-2,6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) compound that (RDP) 25wt% and aluminium hydroxide 25wt% three mix.
Described lubricant is one or more the mixture in polysiloxane, EVA wax, TAS-2A, ethylene bis stearic amide.
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.
Other described additives are photostabilizer and colorant.
The preparation method of the above-mentioned flame-retardant modified polybutylene terephthalate of nano composite material toughening, comprises the following steps:
(1) take by weight ratio poly-2,6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) be 25wt% and aluminium hydroxide 25wt% (RDP), makes to mix, and makes compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by;
(2) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(3) after nanoparticle 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 20～100 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated nanoparticle;
(4) take by weight ratio elastomerics, and mix with above-mentioned surface-treated nanoparticle, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make elastomerics/nanoparticle master batch;
(5) take by weight ratio polybutylene terephthalate, compound flame redundant, lubricant, oxidation inhibitor and other additives after drying treatment, add high-speed mixer, add elastomerics/nanoparticle master batch simultaneously, make fully to mix 2～10 minutes;
(6) again the mixture of step (5) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, barrel zone temperature is at 150 ℃～220 ℃, by twin screw extruder blend, extruding pelletization, obtain the flame-retardant modified polybutylene terephthalate of nano composite material toughening.
The invention has the beneficial effects as follows, compared with prior art, the prepared polybutylene terephthalate of the present invention can improve the deficiency that its goods notched Izod impact strength is not high greatly, there is the good tensile strength of good notch impact toughness, rigidity, thermotolerance and maintenance, and flame-retarded efficiency is high, good processability, cost is low etc.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention.
Embodiment 1:
The flame-retardant modified polybutylene terephthalate of a kind of nano composite material toughening, its component by mass percent proportioning is: polybutylene terephthalate 50%, ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA) 15%, nano silicon 15%, stearic acid 0.3%, compound flame redundant 18%, polysiloxane 0.8%, antioxidant 1010 0.6%, other additives 0.3%, wherein, the median size of nano silicon is between 1nm～100nm, compound flame redundant is poly-2, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) compound that (RDP) 25wt% and aluminium hydroxide 25wt% three mix, other additives are photostabilizer and colorant.
Preparation method: (1) takes poly-2 by weight ratio, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) be 25wt% and aluminium hydroxide 25wt% (RDP), make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (2) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by; (3) after nano silicon 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 20～100 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated nano silicon; (4) take by weight ratio ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), and mix with above-mentioned surface-treated nano silicon, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make E-MA-GMA/nano silicon master batch; (5) take by weight ratio polybutylene terephthalate, compound flame redundant, polysiloxane, antioxidant 1010 and other additives after drying treatment, add high-speed mixer, add E-MA-GMA/nano silicon master batch simultaneously, make fully to mix 2～10 minutes; (6) again the mixture of step (5) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, barrel zone temperature is at 150 ℃～220 ℃, by twin screw extruder blend, extruding pelletization, obtain the flame-retardant modified polybutylene terephthalate of nano composite material toughening.
Embodiment 2:
The flame-retardant modified polybutylene terephthalate of a kind of nano composite material toughening, its component by mass percent proportioning is: polybutylene terephthalate 30%, ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA) 25%, nano-calcium carbonate 25%, calcium stearate 0.5%, compound flame redundant 18%, polysiloxane 1%, the compound 0.3% of antioxidant 1076 and irgasfos 168, other additives 0.2%, wherein, the median size of nano-calcium carbonate is between 1nm～100nm, compound flame redundant is poly-2, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) compound that (RDP) 25wt% and aluminium hydroxide 25wt% three mix, other additives are photostabilizer and colorant.
Preparation method: (1) takes poly-2 by weight ratio, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) be 25wt% and aluminium hydroxide 25wt% (RDP), make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (2) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by; (3) after nano-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 20～100 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated nano-calcium carbonate; (4) take by weight ratio ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), and mix with above-mentioned surface-treated nano-calcium carbonate, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make E-MA-GMA/nano-calcium carbonate master batch; (5) take by weight ratio compound and other additives of polybutylene terephthalate, compound flame redundant, polysiloxane, antioxidant 1076 and irgasfos 168 after drying treatment, add high-speed mixer, add E-MA-GMA/nano-calcium carbonate master batch simultaneously, make fully to mix 2～10 minutes; (6) again the mixture of step (5) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, barrel zone temperature is at 150 ℃～220 ℃, by twin screw extruder blend, extruding pelletization, obtain the flame-retardant modified polybutylene terephthalate of nano composite material toughening.
Embodiment 3:
The flame-retardant modified polybutylene terephthalate of a kind of nano composite material toughening, its component by mass percent proportioning is: polybutylene terephthalate 70%, ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA) 10%, nano kaoline 5%, silane 0.1%, compound flame redundant 14%, ethylene bis stearic amide 0.5%, the compound 0.4% of antioxidant 1076 and oxidation inhibitor JC-242, wherein, the median size of nano kaoline is between 1nm～100nm, compound flame redundant is poly-2, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) compound that (RDP) 25wt% and aluminium hydroxide 25wt% three mix.
Preparation method: (1) takes poly-2 by weight ratio, 6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) be 25wt% and aluminium hydroxide 25wt% (RDP), make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (2) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by; (3) after nano kaoline and silane 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 20～100 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated nano kaoline; (4) take by weight ratio ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), and mix with above-mentioned surface-treated nano kaoline, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make E-MA-GMA/nano kaoline master batch; (5) take by weight ratio polybutylene terephthalate, compound flame redundant, ethylene bis stearic amide and antioxidant 1076 after drying treatment and the compound of oxidation inhibitor JC-242, add high-speed mixer, add E-MA-GMA/nano kaoline master batch simultaneously, make fully to mix 2～10 minutes; (6) again the mixture of step (5) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, barrel zone temperature is at 150 ℃～220 ℃, by twin screw extruder blend, extruding pelletization, obtain the flame-retardant modified polybutylene terephthalate of nano composite material toughening.
Claims (8)
1. the flame-retardant modified polybutylene terephthalate of nano composite material toughening, it is characterized in that, its component by mass percent proportioning is: polybutylene terephthalate 30%～70%, elastomerics 5%～25%, nanoparticle 5%～25%, surface treatment agent 0.1%～0.5%, compound flame redundant 6%～20%, lubricant 0.2～1.5%, oxidation inhibitor 0.1%～1%, other additives 0～0.5%.
2. the flame-retardant modified polybutylene terephthalate of nano composite material toughening according to claim 1, is characterized in that, described elastomerics is ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA).
3. the flame-retardant modified polybutylene terephthalate of nano composite material toughening according to claim 1, it is characterized in that, described nanoparticle is a kind of in nano silicon, nano-calcium carbonate, nanomete talc powder, nano diatomite, nano imvite, nano kaoline and the nano-silicon nitride of median size between 1nm～100nm and silicon carbide compound.
4. the flame-retardant modified polybutylene terephthalate of nano composite material toughening according to claim 1, it is characterized in that, described surface treatment agent is a kind of in stearic acid, calcium stearate, sodium stearate, Magnesium Stearate, titanic acid ester, Aluminate, silane and phosphoric acid ester.
5. the flame-retardant modified polybutylene terephthalate of nano composite material toughening according to claim 1, it is characterized in that, described compound flame redundant is poly-2,6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) compound that (RDP) 25wt% and aluminium hydroxide 25wt% three mix.
6. the flame-retardant modified polybutylene terephthalate of nano composite material toughening 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.
7. the flame-retardant modified polybutylene terephthalate of nano composite material toughening 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.
8. the preparation method of the flame-retardant modified polybutylene terephthalate of nano composite material toughening according to claim 1, is characterized in that, comprises the following steps:
(1) take by weight ratio poly-2,6-dibromo phenylene ether (PBO) 50wt%, Resorcinol (diphenyl phosphoester) be 25wt% and aluminium hydroxide 25wt% (RDP), makes to mix, and makes compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by;
(2) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(3) after nanoparticle 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 20～100 minutes, make dispersedly, be then cooled to lower than 40 ℃ and make surface-treated nanoparticle;
(4) take by weight ratio elastomerics, and mix with above-mentioned surface-treated nanoparticle, add in two roller mills or Banbury mixer, in 120 ℃～140 ℃ mixing 5～10 minutes, then after pulling-on piece, blank, make elastomerics/nanoparticle master batch;
(5) take by weight ratio polybutylene terephthalate, compound flame redundant, lubricant, oxidation inhibitor and other additives after drying treatment, add high-speed mixer, add elastomerics/nanoparticle master batch simultaneously, make fully to mix 2～10 minutes;
(6) again the mixture of step (5) is added in parallel dual-screw extruding machine, controlling screw speed is 120～200 revs/min, barrel zone temperature is at 150 ℃～220 ℃, by twin screw extruder blend, extruding pelletization, obtain the flame-retardant modified polybutylene terephthalate of nano composite material toughening.
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| CN201210370189.4A CN103709631A (en) | 2012-09-29 | 2012-09-29 | Nanocomposite toughened and flame-retardant modified polybutylene terephthalate |
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| CN201210370189.4A CN103709631A (en) | 2012-09-29 | 2012-09-29 | Nanocomposite toughened and flame-retardant modified polybutylene terephthalate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385118A (en) * | 2015-11-18 | 2016-03-09 | 南通开普乐工程塑料有限公司 | High-CTI-value flame-retardant and reinforced PBT (polybutylene terephthalate) composite material |
| WO2019011152A1 (en) * | 2017-07-13 | 2019-01-17 | 山东农业大学 | Master batch with enhanced strength, toughness and transmittance, preparation method therefor and use thereof |
| CN110628189A (en) * | 2019-10-14 | 2019-12-31 | 武汉融科包装材料有限公司 | Plastic steel inner guard plate for low-cost steel coil protective packaging and preparation method thereof |
| WO2020224183A1 (en) * | 2019-05-09 | 2020-11-12 | 王金琪 | Nano-toughening and wear-resistant plastics masterbatch and preparation method |
-
2012
- 2012-09-29 CN CN201210370189.4A patent/CN103709631A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385118A (en) * | 2015-11-18 | 2016-03-09 | 南通开普乐工程塑料有限公司 | High-CTI-value flame-retardant and reinforced PBT (polybutylene terephthalate) composite material |
| WO2019011152A1 (en) * | 2017-07-13 | 2019-01-17 | 山东农业大学 | Master batch with enhanced strength, toughness and transmittance, preparation method therefor and use thereof |
| WO2020224183A1 (en) * | 2019-05-09 | 2020-11-12 | 王金琪 | Nano-toughening and wear-resistant plastics masterbatch and preparation method |
| CN110628189A (en) * | 2019-10-14 | 2019-12-31 | 武汉融科包装材料有限公司 | Plastic steel inner guard plate for low-cost steel coil protective packaging and preparation method thereof |
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Application publication date: 20140409 |