CN110172235A - A kind of hydrolysis-resistant low-warpage PBT composite and its preparation method and application - Google Patents
A kind of hydrolysis-resistant low-warpage PBT composite and its preparation method and application Download PDFInfo
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- CN110172235A CN110172235A CN201910529558.1A CN201910529558A CN110172235A CN 110172235 A CN110172235 A CN 110172235A CN 201910529558 A CN201910529558 A CN 201910529558A CN 110172235 A CN110172235 A CN 110172235A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention belongs to modified plastics field, a kind of hydrolysis-resistant low-warpage PBT composite and its preparation method and application is specifically disclosed.The composite material is made of polybutylene terephthalate (PBT) (PBT), acrylonitrile-butadiene-styrene terpolymer (ABS), glass, compatilizer, toughener, antioxidant and lubricant.The present invention starts with from raw material, using low terminal carboxy content PBT resin, hydrolysis glass, improves the anti-hydrolytic performance of PBT composite, and by compound with ABS, reduces the warpage of PBT composite.Operation of the present invention is simple, and the hydrolysis-resistant low-warpage PBT composite of acquisition has excellent hydrolytic Resistance and dimensional stability, can be used for having good market promotion prospect to hydrolytic Resistance and the higher automotive connector field of dimensional stability requirements.
Description
Technical field
The invention belongs to modified plastics fields, and in particular to a kind of hydrolysis-resistant low-warpage PBT composite and its preparation side
Method and application.
Background technique
Polybutylene terephthalate (PBT) (PBT), which is that milky is translucent, arrives opaque, crystal type thermoplasticity saturated polyester,
PBT resin with its excellent mechanical property, electrical property, heat resistance, processing performance, especially good comprehensive performance and in electricity
Sub- electric appliance, auto industry and machinery, instrument and meter and household electrical appliance etc. are widely applied in fields.But gather with other
The problem of ester is the same, and PBT is equally existed intolerant to hydrolysis.PBT is usually formed by terephthalic acid (TPA) and 1,4-butanediol dehydrating condensation,
This is a reversible reaction, and under the action of water, PBT may be hydrolyzed, so that strand shortens, the strength of materials is reduced, and is become fragile, very
To cracking, the progress of hydrolysis can be aggravated by increasing temperature.The mechanical performance of PBT resin and resistance to can be significantly improved by fiberglass reinforced
Hot property, but can be inconsistent due to flow direction and the contraction of perpendicular flow direction, lead to the problem of buckling deformation.
Chinese patent application CN 109294177 discloses a kind of hydrolysis PBT composition with good fluidity,
Composition is in percentage by weight, comprising: and PBT resin 50~70%, glass 20~40%, toughener 1~3%, chain extender 1~
5%, macromolecular multifunctional assistant 3~12%, anti-hydrolysis agent 0.2~0.5%, antioxidant 0.2~0.5% and lubricant 0.2~
0.5%.PBT composition of the present invention both reduces the carboxylic end group concentration of PBT under the coordinative role of anti-hydrolysis agent and chain extender,
It simultaneously rebuilds PBT strand to extend, the anti-hydrolytic performance of PBT composition can be improved.Chinese patent application CN104140649
A kind of hydrolysis enhancing PBT material is disclosed, composition is in percentage by weight, comprising: PBT resin 80~90%, poly- carbon
Change the double stearic acid acyls of diimine crosslinking agent 0.8~1%, butylated hydroxy anisole 0.1~0.4%, calcium naphthenate 1~2, vinyl
Amine 1~2%, propenyl 2~3%, triacetin 2~3%, hydroxy propyl methacrylate 1~2%, copper chloride 1~2%,
Maleic anhydride 1~2%, dipotassium hydrogen phosphate 1~2%, linseed oil 1~2%, nano-carbon powder 3~4%, processing aid 1~
2%.；The polycarbodiimide crosslinkers of addition make finished product have good water resistance, have widened the use scope of material.In
State patent CN 106519594 disclose it is a kind of for nanometer injection molding oil rub resistance hydrolysis PBT engineering plastic composition and its
Preparation method, composition in percentage by weight, comprising: PBT45-60%, glass fibre 20-40%, toughener 4-6%,
Metal adhesive 8-15%, weather resisting agent 0.3-0.4%, antioxidant 0.2-0.4%, lubricant 0.3-0.5%, hydrolytic-resistant modified dose
0.5-1.0%.
It is anti-hydrolysis agent that the above patent, which is all made of polycarbodiimide, is reacted by it with the carboxyl of PBT resin, and production is steady
Fixed uride inhibits the progress of hydrolysis.But there are deficiencies below for the above patent: (1) polycarbodiimide price is very high, i.e.,
A small amount of addition is set also to bring significantly improving for cost；(2) the content of carboxyl end group for influencing PBT resin anti-hydrolytic performance is not carried out
Illustrate or limits；(3) the warpage issues of PBT composite are not studied.
Summary of the invention
To solve the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is that providing that a kind of resistant to hydrolysis is low to stick up
Bent PBT composite.The composite material has excellent hydrolytic Resistance and low warpage properties energy simultaneously, can be used for steady to size
The qualitative and more demanding automotive connector field of hydrolytic Resistance.
Another object of the present invention is to provide the preparation methods of above-mentioned hydrolysis-resistant low-warpage PBT composite.
A further object of the present invention is to provide the applications of above-mentioned hydrolysis-resistant low-warpage PBT composite.
The object of the invention is achieved through the following technical solutions:
A kind of hydrolysis-resistant low-warpage PBT composite, the composite material is by polybutylene terephthalate (PBT) (PBT), third
Alkene nitrile-butadiene-styrene terpolymer (ABS), compatilizer, toughener, glass, antioxidant and lubricant composition, with weight
It measures percentage to calculate, dosage of each component is as follows:
Preferably, the hydrolysis-resistant low-warpage PBT composite dosage of each component is as follows:
Preferably, the PBT, inherent viscosity are 0.8~1.1dl/g, content of carboxyl end group≤12mol/t.
Preferably, the ABS, melt index are 10~30g/10min (220 DEG C of+10Kg).
Preferably, the glass is alkali-free resistant to hydrolysis glass fibre, and 7~17 μm of filament diameter, chopped length 3~
24mm。
Preferably, the compatilizer is that (acrylonitrile-butadiene-styrene terpolymer is grafted Malaysia to ABS-g-MAH
Acid anhydrides).
Preferably, the toughener is ethylene-random ternary polymerization of methyl acrylate-glycidyl methacrylate
Object.
Preferably, the antioxidant is the compounding antioxidant system that hindered phenol and phosphite ester form in any proportion.
Preferably, the lubricant is silicone powder.
The present invention is added resistant to hydrolysis glass, improves PBT composite using the PBT resin of low terminal carboxy content as substrate
Anti-hydrolytic performance.Further, amorphous ABS resin is added, reduces PBT composite flow direction and perpendicular flow direction is received
Shrinkage difference, to reduce the warpage of PBT composite.
A kind of preparation method preparing above-mentioned hydrolysis-resistant low-warpage PBT composite, include the following steps: by PBT, ABS,
Mixing machine mixing is added in compatilizer, toughener, antioxidant and lubricant, and extruder main feeding hopper is added in mixed material,
Glass is added by side spout, by double screw extruder extruding pelletization, hydrolysis-resistant low-warpage PBT composite is made.
Preferably, above-mentioned incorporation time is 3~5min；The revolving speed of double screw extruder is 300~500r/min, and temperature is
200~250 DEG C.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) low terminal carboxy content PBT resin is used, reduces the generation that PBT composite hydrolyzes from source；
(2) resistant to hydrolysis glass is added, while enhancing PBT, further improves the hydrolytic resistance of PBT composite
Energy；
(3) ABS resin is added, reduces the warpage of PBT composite, improves its dimensional stability.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
The embodiment of the present invention and comparative example are molded into the standard batten of test according to standard requirements and are tested.It is outstanding
Arm beam notch impact strength is according to ISO180 standard, and shrinking percentage is according to ISO294-4 standard.Hydrolysis testing standard is as follows: (1)
90 DEG C of regulating thermostatic constant humidity cabinet temperature, humidity 98%；(2) impact batten is placed in high temperature and humidity case；After (3) 1000 hours
Batten is taken out, 23 DEG C is placed in, carries out Izod notched impact strength test after 24 hours in the incubator of humidity 50%, each
5 battens of condition test and using average value as test result, and it is strong relative to initial tensile to calculate Izod notched impact strength
The percentage of degree.
The raw material used in the embodiment of the present invention and comparative example is as follows:
PBT:PBT1084HQ (0.82~0.85dl/g of intrinsic viscosity, 10~11mol/t of content of carboxyl end group), Nantong stars
Synthetic material Co., Ltd, PBTKH2083 (0.82~0.85dl/g of intrinsic viscosity, 18~22mol/t of content of carboxyl end group), Yingkou
Kang Hui petrochemical industry Co., Ltd；
ABS:ABS 0215A (melt flow rate (MFR) 20g/10min), PetroChina Company Ltd.'s Jilin stone
Change company；
Compatilizer: KT-2, Shenyang Ke Tong plastic cement Science and Technology Ltd.；
Toughener: AX8900, French A Kema (Arkema) company；
Glass: ECS13-3.0-T436HK, 13 μm of filament diameter, chopped length 3.0mm, ECS13-3.0-T436, monofilament
13 μm of diameter, chopped length 3.0mm, tai shan glass fibre Co., Ltd；
Anti-hydrolysis agent: N, N'- bis- (2,6- diisopropyl phenyl) carbodiimide, trade mark SY-7000, German Rhine chemistry are public
Department；
Antioxidant: hindered phenol 1010, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, Germany
BASF (Basf) company；Phosphite ester S-9228 (bis- (2,4-two cruel bases) pentaerythritol diphosphites), the U.S.'s all good fortune
(Dover) company；
Lubricant: silicone powder TEGOMER E525, German Degussa (Degussa AG) company.
Embodiment 1
A kind of preparation method of hydrolysis-resistant low-warpage PBT composite, comprising the following steps:
(1) raw material is weighed by the amount of PBT, ABS in table 1, compatilizer, toughener, antioxidant and lubricant；
(2) various raw materials are mixed into mixing machine 5min, extruder main feeding hopper is then added, be added in side feed hopper
Glass passes through double screw extruder extruding pelletization.
The revolving speed of double screw extruder is 300r/min, and temperature is 200~250 DEG C.Resulting hydrolysis-resistant low-warpage PBT is multiple
Condensation material performance is shown in Table 2.
Embodiment 2
A kind of preparation method of hydrolysis-resistant low-warpage PBT composite, comprising the following steps:
((1) weighs raw material by the amount of PBT, ABS in table 1, compatilizer, toughener, antioxidant and lubricant；
(2) various raw materials are mixed into mixing machine 3min, extruder main feeding hopper is then added, be added in side feed hopper
Glass passes through double screw extruder extruding pelletization.
The revolving speed of double screw extruder is 500r/min, and temperature is 200~250 DEG C.Resulting hydrolysis-resistant low-warpage PBT is multiple
Condensation material performance is shown in Table 2.
Embodiment 3~4
After embodiment 3~4 weighs raw material by table 1 respectively, hydrolysis-resistant low-warpage is prepared according to the method for embodiment 1
PBT composite, resulting hydrolysis-resistant low-warpage PBT composite performance are shown in Table 2.
Comparative example 1~5
After comparative example 1~5 weighs raw material according to table 3 respectively, it is compound that modified PBT is prepared according to the method for embodiment 1
Material.Resulting modified PBT composite material detection is shown in Table 4.
The composition of 1 hydrolysis-resistant low-warpage PBT composite of table
2 embodiment performance detection of table
The composition of 3 comparative example PBT composite of table
4 comparative example performance detection of table
It can be seen that the PBT resin using low terminal carboxy content compared with embodiment 1 by comparative example 1, PBT is compound
The hydrolytic Resistance of material is obviously improved.
Compared by comparative example 2 and embodiment 2 as can be seen that the addition of ABS resin can reduce PBT composite flowing
The shrinking percentage in direction and perpendicular flow direction, and the difference of both direction shrinking percentage is reduced, to reduce PBT composite
Warpage.In addition, ABS, which is added, reduces PBT content, also have some improvement to the anti-hydrolytic performance of PBT composite.
By comparative example 3 as can be seen that the addition of compatilizer can be obviously improved PBT composite compared with embodiment 3
Mechanical performance, while also having some improvement to anti-hydrolytic performance, this is because the addition of ABS-g-MAH can be significant
Improve the compatibility of PBT and ABS.
It can be seen that by the comparison of comparative example 4 and embodiment 4 using hydrolysis glass, it is compound PBT can be obviously improved
The hydrolytic Resistance of material.
It can be seen that by the comparison of comparative example 5 and embodiment 4 multiple using low terminal carboxy content PBT and hydrolysis glass
Match, compared to typical anti-hydrolysis agent (N, N'- bis- (2,6- diisopropyl phenyl) carbodiimide) is added, PBT composite resists
Hydrolysis property is more preferable.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of hydrolysis-resistant low-warpage PBT composite, which is characterized in that the composite material is by PBT, ABS, glass, compatible
Agent, toughener, antioxidant and lubricant composition, calculated in weight percent, dosage of each component is as follows:
The PBT, inherent viscosity are 0.8~1.1dl/g；The glass is alkali-free resistant to hydrolysis glass fibre.
2. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1, which is characterized in that the resistant to hydrolysis is low
Warpage PBT composite dosage of each component is as follows:
3. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1 or 2, which is characterized in that the ABS,
Its melt index is 10~30g/10min (220 DEG C of+10Kg).
4. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1 or 2, which is characterized in that the glass list
7~17 μm of diameter of silk, 3~24mm of chopped length.
5. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1 or 2, which is characterized in that described is compatible
Agent is ABS-g-MAH.
6. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1 or 2, which is characterized in that the toughener
For ethylene-methyl acrylate-glyceryl methacrylate random terpolymer.
7. a kind of hydrolysis-resistant low-warpage PBT composite according to claim 1 or 2, the antioxidant is hindered phenol
The compounding antioxidant system formed in any proportion with phosphite ester, lubricant are silicone powder.
8. a kind of described in any item preparation methods of hydrolysis-resistant low-warpage PBT composite of claim 1 to 7, feature exist
In including the following steps: by weight percentage, by 30~75%PBT, 10~20%ABS, 2~6% compatilizers, 2~6%
Extruder is added in mixed material by toughener, 0.4~0.6% antioxidant and 0.4~0.6% 3~5min of mix lubricant
Main feeding hopper is added 10~40% glasses in side feed hopper, by double screw extruder extruding pelletization, hydrolysis-resistant low-warpage is made
PBT composite.
9. the preparation method of hydrolysis-resistant low-warpage PBT composite according to claim 8, which is characterized in that described double
The revolving speed of screw extruder is 300~500r/min, and temperature is 200~250 DEG C.
10. a kind of described in any item hydrolysis-resistant low-warpage PBT composites of claim 1 to 7 are in automotive connector field
Application.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029244A (en) * | 2020-09-02 | 2020-12-04 | 江苏金发科技新材料有限公司 | Heat-resistant hydrolysis-resistant glass fiber reinforced PBT/EVOH composition and preparation method thereof |
| CN112608584A (en) * | 2020-11-30 | 2021-04-06 | 金发科技股份有限公司 | PBT modified material with high elongation at break as well as preparation method and application thereof |
| CN114806104A (en) * | 2022-03-31 | 2022-07-29 | 上海金发科技发展有限公司 | Polyester composition and preparation method and application thereof |
| CN115322531A (en) * | 2022-08-12 | 2022-11-11 | 湖北合聚新材料有限公司 | Hydrolysis-resistant laser welding PBT material and preparation method thereof |
| CN116144148A (en) * | 2023-04-17 | 2023-05-23 | 广东永鑫华新型材料有限公司 | Preparation method of low-warpage fatigue-resistant PBT composite material |
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| CN109081929A (en) * | 2018-07-06 | 2018-12-25 | 江苏裕兴薄膜科技股份有限公司 | A method of preparing hydrolysis-resistant polyester film |
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| CN112029244A (en) * | 2020-09-02 | 2020-12-04 | 江苏金发科技新材料有限公司 | Heat-resistant hydrolysis-resistant glass fiber reinforced PBT/EVOH composition and preparation method thereof |
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| CN116144148A (en) * | 2023-04-17 | 2023-05-23 | 广东永鑫华新型材料有限公司 | Preparation method of low-warpage fatigue-resistant PBT composite material |
| CN116144148B (en) * | 2023-04-17 | 2023-06-23 | 广东永鑫华新型材料有限公司 | Preparation method of low-warpage fatigue-resistant PBT composite material |
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Application publication date: 20190827 |