CN102924884A - PBT (polybutylece terephthalate) composite and preparation method thereof - Google Patents
PBT (polybutylece terephthalate) composite and preparation method thereof Download PDFInfo
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- CN102924884A CN102924884A CN2012104610568A CN201210461056A CN102924884A CN 102924884 A CN102924884 A CN 102924884A CN 2012104610568 A CN2012104610568 A CN 2012104610568A CN 201210461056 A CN201210461056 A CN 201210461056A CN 102924884 A CN102924884 A CN 102924884A
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Abstract
The invention provides a high-performance halogen-free flame-resistant non-reinforced antistatic PBT (polybutylece terephthalate) composite and a preparation method thereof. The composite can still keep good flame-resistant, antistatic and mechanical properties under the condition that a reinforcing material is not added, and the phenomenon of fiber floating in the traditional reinforcing material system is avoided. The preparation method comprises the following steps that PBT resin, a fire retardant and a flexibilizer are dried, and a tackifier and an antistatic material are pretreated; the PBT resin and various padding are added into a low-speed mixer to be pre-mixed, the PBT resin and the padding are uniformly mixed and then are blend and extruded and pelleted through a double-screw extruder to be dried, and the halogen-free flame-resistant non-reinforced antistatic PBT material is obtained.
Description
Technical field
Patent of the present invention relates to a kind of high performance PBT matrix material and preparation method thereof, particularly PBT matrix material of a kind of halogen-free flame-proof antistatic and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) is the thermoplastic polyester plastic, has good thermotolerance, weathering resistance, resistance to chemical reagents, electrical insulating property, light absorptive is little, gloss is good, is widely used in electric, auto parts, machinery, house ornamentation articles for use etc.But its resistivity is high, easily produces static, and the general resistivity that reduces PBT by adding static inhibitor can effectively loss static charge, thus the harm of avoiding a large amount of accumulations of static to cause.Contain benzene ring structure on the PBT molecular chain simultaneously, be not easy to into charcoal, but be easy to burning, the melting drippage when burning, occurs continuously.In order to satisfy the growing high demand of people and further to expand Application Areas, this inevitable requirement is carried out modification to polymkeric substance, towards high performance, and functionalization, diversification future development.
In order to satisfy security requirement, the mode that fire retardant is added in general employing is carried out flame-retardant modified to PBT, and fire retardant can stop macromolecular material burning or the inhibition propagation of flame such as plastics.At present, the main fire retardant that uses mainly is divided three classes on the market: (1) Halogen flame-retardant system, such as the polybromodiphenyl ether compounds etc.; (2) halogen-free flame-retardant system is such as red phosphorus, magnesium oxide, magnesium hydroxide and nitride etc.; (3) synergistic flame-retarded technology.Wherein the Halogen flame-retardant system can produce a large amount of hydrogen halides after burning, has very strong corrodibility, and environment and human body are caused very large pollution and injury.Therefore, in recent years, people transferred to sight in the development research of halogen-free flame retardants and synergistic flame-retarded technology gradually, prepared the more superior PBT matrix material of flame retardant properties, processing characteristics and physical and mechanical property.Goods are in the process of using, keep away unavoidable contact and friction, this dual mode very easily produces and assembles a large amount of static charges, thereby the existence of static charge makes the PBT goods bring a lot of problems to limit its use range in storage with in using, as: the surface is absorption dust easily, affects appearance effect; The PBT goods are used for electronics, electric equipment products, and when buildup of static electricity arrived certain value, discharge caused security incident.Therefore, for safe handling and the scope that improves the PBT goods, must solve the antistatic problem of goods, at present, mainly be to use static inhibitor to improve its antistatic property.Static inhibitor mainly comprises: (1) carbon conductive filler, as: graphite, carbon black, carbon fiber and carbon nanotube etc.; (2) me tallic conductive filler such as metal-powder, fragment and fiber etc.; (3) other series are such as inorganic salt and metal oxide powder etc.Wherein graphite raw material is easy to get, and great variety of goods is cheap, and light weight also has preferably the characteristics such as thermal conductivity, is a kind of semi-conductor, therefore is widely used in improving the antistatic property of plastics.
At present, study about PBT halogen-free flame-proof antistatic composite manufacture in the prior art, mainly concentrate on the PBT halogen-free flame-proof antistatic system of enhancing system, such as patent: add 0 ~ 50% alkali-free glass fiber and halogen-free flame retardants and relevant auxiliary agent CN 101497738A(fire retardant PBT with no halogen and preparation method thereof), the fire-retardant rank of the matrix material for preparing can reach vertical combustion V-0 level; Antistatic PBT material of a patent CN 102532823A(excellent combination property and preparation method thereof) in, add the auxiliary agents such as glass fibre, carbon nanotube, the surface resistivity of the material for preparing is 106 Ω, in the process of using floating fine phenomenon can appear for thinner or little product, in the process of drawing a design, glass is easy to block the exhaust-duct, cause spontaneous combustion (glass is easy to burning in the high pressure oxygen environment), the product surface bad order affects the antistatic property of material.
Therefore, the PBT material of non-enhancement type, the PBT material that replaces having the enhancing system enters correlative technology field, but, in the prior art, the adding of various modified additives, over-all properties to material has produced very large negative impact, the effect of these modified additives, the synergetic property in material is unsatisfactory, causes product to lose use value.Thereby the PBT material of present non-enhancement type also has very large development space.
Summary of the invention:
Problem to be solved by this invention is: for halogen-free flame-proof antistatic PBT material, in traditional strongthener system, easily produce floating fine phenomenon, and in the prior art, in the PBT of non-enhancement type material, between halogen-free flameproof performance and the antistatic property, synergistic effect is undesirable again.
The object of the present invention is to provide antistatic PBT material of the non-enhancing of a kind of high-performance halogen-free flame retardant and preparation method thereof, this preparation method can improve the antistatic property of PBT matrix material effectively, adopt simultaneously the nitrogen phosphorus fire retardant composite, can effectively improve the flame retardant properties of material, has good workability, can effectively improve the impact property of PBT by the toughner that adds nucleocapsid structure, effectively improved the toughness of goods, simultaneously by adding a certain amount of tackifier, can effectively strengthen the mechanical property of PBT material, and these performances are collaborative the existence in product of the present invention, impels the diversification of non-reinforced PBT composite property.
Purpose of the present invention can be achieved by following technical scheme:
The antistatic non-enhancing PBT matrix material of a kind of high-performance halogen-free flame retardant, mark meter by weight, the PBT matrix material comprises following composition:
As preferably: PBT resin properties viscosity is 0.6 ~ 0.85dl/g; This resinoid has good moulding processability.
As preferably: fire retardant is in the halogen-free flame-retardant system, the compound of phosphorus flame retardant and nitrogenated flame retardant, wherein phosphorus flame retardant is methyl-phosphoric acid dimethyl ester, annular phosphate, N-methylol-3-(dioxy phosphoryl) a kind of in the propionic acid amide, triphenyl phosphite, isooctyl diphenyl phosphite or mixture more than two kinds; Nitrogenated flame retardant wherein is a kind of in ammonium polyphosphate, Dyhard RU 100, the melamine cyanurate or mixture more than two kinds, and wherein both composite mass ratioes are between 1:2 ~ 1:4.
As preferably: anti-dripping agent is the PTFE(tetrafluoroethylene) powder.
As preferably: toughner is a kind of toughner of nucleocapsid structure, its center is Afpol, shell is polymethylmethacrylate, this toughner has good dispersiveness in PBT, flowability affects to matrix resin is very little, be convenient to machine-shaping, effectively improved the toughness of goods.
As preferably: static inhibitor is surface treated carbon series conductive material, such as carbon black, graphite, carbon fiber and carbon nanotube etc.The surface treatment agent that wherein adds is the tensio-active agent of non-ionic type, such as glycerin fatty acid ester, polyol surfactant, polyoxyethylene-type surfactant, Pluronic F68 etc., result of use is polyalcohols preferably, such as ethylene glycol, has effectively isolated the carbon series conductive material, reduced the friction between the particle, reduced the viscosity of system, polymeric matrix is had certain strengthening action, cost is low.The mass ratio of surface treatment agent and carbon series conductive material is 1:100 ~ 5:100.
As preferably: tackifier are isocyanates, mainly can react with terminal hydroxy group, the end carboxyl of PBT, effectively improved the relative molecular mass of system, improved the mechanical property of PBT material, the compound of isocyanates is mainly tolylene diisocyanate, diphenylmethanediisocyanate etc.
As preferably: ethyl acetate is mainly as the solvent of isocyanic ester, in the process of adding, the viscosity of isocyanic ester is larger, in resin matrix, disperse uneven, affect the mechanical property of material, at first be mixed in proportion with ethyl acetate and isocyanic ester and stir in the process of experiment, add in the PBT resin system, extrude blending reaction.Mixing quality is than between 1:1 ~ 1:5.
The present invention also provides the non-enhancing of a kind of above-mentioned halogen-free flame-proof antistatic PBT composite manufacture method, may further comprise the steps:
(1) PBT resin, fire retardant and toughner is dry, tackifier and its solvent are even, and with carbon series conductive material and surface-active-treatment agent in proportion, leave standstill after the high-speed mixing;
As preferably: with PBT in 120 ~ 140 ℃ of lower forced air drying 3 ~ 5h;
As preferably: with fire retardant in 80 ~ 100 ℃ of lower forced air drying 3 ~ 5h;
As preferably: with toughner in 50 ~ 60 ℃ of lower forced air drying 3 ~ 5h;
As preferably: ethyl acetate is as the solvent of tackifier isocyanic ester, both in mass ratio 1:1 ~ 1:5 mix,
Because the viscosity of isocyanic ester is larger, in resin matrix, disperse inequality, affect the mechanical property of material, so at first will with the isocyanic ester solubilizing agent, mix in the process of experiment;
As preferably: carbon series conductive material and surface treatment agent are pressed the mass ratio of 1:100 ~ 5:100, and high-speed mixing leaves standstill 3 ~ 5h, and like this, surface treatment agent can infiltrate in the carbon series conductive material fully, mixes;
(2) PBT that drying is good, fire retardant, toughner and the static inhibitor of anticipating, tackifier are pre-mixed according to portion rate adding low speed mixer, mix rear with twin screw extruder blending extrusion, granulation, drying.
As preferably: disposable the joining in the low speed mixer of desired raw material mixed, and mixing time is 10 ~ 15 minutes;
As preferably: the barrel temperature of twin screw extruder is 230 ~ 250 ℃, and screw speed is 30 ~ 50r/min;
As preferably: with pellet again through 110 ~ 130 ℃ of forced air drying 3 ~ 5h.
Be injection molded into the stretching of standard and impact batten at injection moulding machine, injection temperature is 240 ~ 250 ℃.
The present invention has following beneficial effect:
Patent of the present invention is the halogen-free flame-proof antistatic high-performance PBT composite manufacture of non-enhancing system, avoided floating fine phenomenon in the traditional enhancing system, and impel the diversification of non-reinforced PBT composite property, enlarged the range of application of PBT matrix material:
(1) terminal hydroxy group of a certain amount of tackifier of interpolation and PBT, end carboxyl react, and have effectively improved the relative molecular mass of system, have improved the mechanical property of PBT material.
(2) fire retardant that adopts of patent of the present invention is nitrogen phosphorus compound system, has avoided the Halogen flame-retardant system can produce a large amount of hydrogen halides after burning, has very strong corrodibility, and environment and human body are caused very large pollution and injury.
(3) toughner that adopts of patent of the present invention is the toughner of nucleocapsid structure, its center is Afpol, shell is polymethylmethacrylate, this toughner has good dispersiveness in PBT, flowability affects to matrix resin is very little, be convenient to machine-shaping, improved the impact property of PBT matrix material, improved significantly toughness.
(4) static inhibitor that adopts of patent of the present invention is surface treated carbon series conductive material, such as carbon black, graphite, carbon fiber and carbon nanotube etc.The surface treatment agent that wherein adds is the tensio-active agent of non-ionic type, such as glycerin fatty acid ester, polyalcohols, polyoxyethylene-type, Pluronic F68 etc., result of use is polyalcohols preferably, such as ethylene glycol, effectively isolate the carbon series conductive material, reduced the friction between the particle, reduced the viscosity of system.
Description of drawings
Fig. 1 is the profile scanning figure of specific embodiment 1 sample, and as can be seen from the figure, fire retardant and antistatic particle are uniformly dispersed in matrix resin.
Embodiment
At first with PBT in 120 ~ 150 ℃ of lower forced air drying 3 ~ 5h, fire retardant is at 80 ~ 100 ℃ of lower forced air drying 3 ~ 5h.Toughner is in 50 ~ 60 ℃ of lower forced air drying 3 ~ 5h.Dry good PBT, fire retardant, toughner and static inhibitor, tackifier once add low speed mixer according to portion rate and are pre-mixed in advance according to the quality weighing that provides in the table 1, mixing time 10 ~ 15 minutes, after mixing, with twin screw extruder blending extrusion, granulation, 230 ~ 250 ℃ of barrel temperatures, the preferred 30 ~ 50r/min of screw speed.The gained pellet is injection molded into the stretching of standard and impacts batten at injection moulding machine again through 110 ~ 130 ℃ of forced air drying 3 ~ 5h, and injection temperature is 240 ~ 250 ℃.When having listed the carbon series conductive material surface and process, table 2 uses material formula, the test result of the sample that table 3 prepares for specific embodiment 1 ~ 5.
Table 1 specific embodiment 1 ~ 5 prescription
Table 2 carbon series conductive material surface treatment formulations
| Specific embodiment 1 | Specific embodiment 2 | Specific embodiment 3 | Specific embodiment 4 | Specific embodiment 5 | |
| Graphite | ?10 | ?5 | ?5 | ||
| Carbon fiber | ?15 | ?5 | ?5 | ||
| Graphitized carbon black | ?20 | ?5 | |||
| Ethylene glycol | ?0.1 | ?0.3 | ?0.4 | ?0.3 | ?0.15 |
Table 3 test result
Note: vertical combustion is mainly used in the not combustionproperty of the mensuration plastics under the regulation burning things which may cause a fire disaster directly burns to plastics or film, and in order to judge the fire resistance rating of refractory materials, flame retardant rating is by V-2, and V-1 increases progressively step by step to V-0.The typical thickness of sample has 0.8mm, 1.6mm, 3.2mm, and the thickness of sample is thinner, and is higher to the flame retardant properties requirement of sample.
Claims (10)
1. PBT matrix material is characterized in that: the halogen-free flame-proof antistatic PBT matrix material that described PBT matrix material is non-enhancement type, and mark meter by weight, matrix material comprises following composition:
2. PBT matrix material as claimed in claim 1, it is characterized in that: described PBT resin properties viscosity is 0.6 ~ 0.85dl/g.
3. PBT matrix material as claimed in claim 1, it is characterized in that: described fire retardant is in the halogen-free flame-retardant system, the compound of phosphorus flame retardant and nitrogenated flame retardant, both composite mass ratioes are 1:2 ~ 1:4.
4. PBT matrix material as claimed in claim 3, it is characterized in that: described phosphorus flame retardant is methyl-phosphoric acid dimethyl ester, annular phosphate, N-methylol-3-(dioxy phosphoryl) one or two or more kinds mixture in the propionic acid amide, triphenyl phosphite, isooctyl diphenyl phosphite; Described nitrogenated flame retardant is one or two or more kinds mixture in ammonium polyphosphate, Dyhard RU 100, the melamine cyanurate.
5. PBT matrix material as claimed in claim 1, it is characterized in that: described anti-dripping agent is the polytetrafluoroethylene PTFE powder.
6. PBT matrix material as claimed in claim 1, it is characterized in that: described toughner is a kind of toughner of nucleocapsid structure, and its center is Afpol, shell is polymethylmethacrylate.
7. PBT matrix material as claimed in claim 1 is characterized in that: the carbon series conductive material of described static inhibitor for processing through tensio-active agent, the mass ratio of tensio-active agent and carbon series conductive material is 1:100 ~ 5:100.
8. PBT matrix material as claimed in claim 7, it is characterized in that: described tensio-active agent is non-ionic type, is selected from one or more in glycerin fatty acid ester, polyol surfactant, polyoxyethylene-type surfactant or the Pluronic F68 tensio-active agent; Described carbon series conductive material is selected from one or more in carbon black, graphite, carbon fiber or the carbon nanotube.
9. PBT matrix material as claimed in claim 1, it is characterized in that: described tackifier are the isocyanates tackifier, be selected from tolylene diisocyanate or diphenylmethanediisocyanate, the mass ratio between tackifier and its solvent ethyl acetate is 1:1 ~ 5:1.
10. such as each described PBT composite manufacture method of claim 1 to 9, it is characterized in that concrete steps are:
(1) PBT resin, fire retardant and toughner is dry, tackifier and its solvent are even, and with carbon series conductive material and surface-active-treatment agent in proportion, leave standstill after the high-speed mixing;
(2) PBT that drying is good, fire retardant, toughner and the static inhibitor of anticipating, tackifier are pre-mixed according to portion rate adding low speed mixer, mix rear with twin screw extruder blending extrusion, granulation, drying.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194049A (en) * | 2013-04-10 | 2013-07-10 | 苏州旭光聚合物有限公司 | Enhanced PBT (polybutylece terephthalate) /PA alloy and preparation method of the same |
| CN103450642A (en) * | 2013-08-07 | 2013-12-18 | 上海日之升新技术发展有限公司 | High-strength carbon-fiber-reinforced halogen-free flame-retardant PBT (polybutylene terephthalate) composite material and preparation method thereof |
| CN103739917A (en) * | 2014-01-09 | 2014-04-23 | 北京工商大学 | Polyethylene plastic antistatic master batch, conductive material for master batch and application of master batch and conductive material |
| CN105062011A (en) * | 2015-07-31 | 2015-11-18 | 江阴职业技术学院 | Continuous long glass fiber reinforced PBT composite material and preparation method thereof |
| CN105331062A (en) * | 2014-07-15 | 2016-02-17 | 中国石油化工股份有限公司 | Carbon nanotube / polylactic acid conductive composite material and preparation method thereof |
| CN105504702A (en) * | 2015-12-24 | 2016-04-20 | 广东思汗新材料有限公司 | Flame-retardant electric conducting PBT composite material |
| CN106084685A (en) * | 2016-08-12 | 2016-11-09 | 太仓市华鼎塑料有限公司 | A kind of low floating fine high fire-retardance PBT material and preparation method thereof |
| CN108488541A (en) * | 2018-02-08 | 2018-09-04 | 深圳市骏鼎达新材料股份有限公司 | A kind of protection sleeve pipe and preparation method |
| CN112080112A (en) * | 2019-06-13 | 2020-12-15 | 上海朗亿功能材料有限公司 | Conductive plastic and raw material composition, preparation method and application thereof |
| CN113817298A (en) * | 2021-10-22 | 2021-12-21 | 金旸（厦门）新材料科技有限公司 | Reinforced PBT (polybutylene terephthalate) composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194049A (en) * | 2013-04-10 | 2013-07-10 | 苏州旭光聚合物有限公司 | Enhanced PBT (polybutylece terephthalate) /PA alloy and preparation method of the same |
| CN103450642A (en) * | 2013-08-07 | 2013-12-18 | 上海日之升新技术发展有限公司 | High-strength carbon-fiber-reinforced halogen-free flame-retardant PBT (polybutylene terephthalate) composite material and preparation method thereof |
| CN103739917A (en) * | 2014-01-09 | 2014-04-23 | 北京工商大学 | Polyethylene plastic antistatic master batch, conductive material for master batch and application of master batch and conductive material |
| CN105331062A (en) * | 2014-07-15 | 2016-02-17 | 中国石油化工股份有限公司 | Carbon nanotube / polylactic acid conductive composite material and preparation method thereof |
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| CN106084685A (en) * | 2016-08-12 | 2016-11-09 | 太仓市华鼎塑料有限公司 | A kind of low floating fine high fire-retardance PBT material and preparation method thereof |
| CN108488541A (en) * | 2018-02-08 | 2018-09-04 | 深圳市骏鼎达新材料股份有限公司 | A kind of protection sleeve pipe and preparation method |
| CN112080112A (en) * | 2019-06-13 | 2020-12-15 | 上海朗亿功能材料有限公司 | Conductive plastic and raw material composition, preparation method and application thereof |
| CN113817298A (en) * | 2021-10-22 | 2021-12-21 | 金旸（厦门）新材料科技有限公司 | Reinforced PBT (polybutylene terephthalate) composite material and preparation method thereof |
| CN113817298B (en) * | 2021-10-22 | 2023-04-14 | 金旸（厦门）新材料科技有限公司 | Reinforced PBT (polybutylene terephthalate) composite material and preparation method thereof |
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Application publication date: 20130213 |