CN112646331A - Polybutylene terephthalate mixture and preparation method thereof - Google Patents
Polybutylene terephthalate mixture and preparation method thereof Download PDFInfo
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention relates to a polybutylene terephthalate mixture and a preparation method thereof. The mixture comprises the following components in percentage by weight: 91.9-99.19 wt% of polybutylene terephthalate resin, 0.8-6 wt% of hydrolysis resistance agent and 0.01-1 wt% of strontium compound. The mixture has excellent barrier property, toughness and solvent resistance, and simultaneously has excellent comprehensive properties such as impact strength, tensile strength, bending modulus and the like.
Description
Technical Field
The invention belongs to the technical field of modified plastics, and particularly relates to a polybutylene terephthalate mixture and a preparation method thereof.
Background
The polybutylene terephthalate has excellent mechanical property, electrical property, heat resistance, fatigue resistance and creep resistance, and has low water absorption rate and good dimensional stability. The polybutylene terephthalate has fast crystallization and excellent chemical solvent resistance. The polybutylene terephthalate modified material is widely applied to a plurality of fields of automobiles, industry, electronics and electrics, IT, household appliances, OA and the like.
The polybutylene terephthalate has better barrier property, so the polybutylene terephthalate material also has certain application in the fields of film packaging and sealed containers. As the polybutylene terephthalate material has very outstanding organic solvent resistance, very few reports are made on the polybutylene terephthalateThe solvent resistance of the butanediol formate modified material can be improved. In some special fields, such as single-component rubber tubes and double-component rubber tubes, especially when used for containing chemically corrosive glue solution, the solvent resistance of the polybutylene terephthalate modified material can hardly meet the requirement. The rubber tube is usually filled with acrylic acid glue, epoxy resin, PU glue, electronic potting glue, bi-component organic silica gel and the like, and is required to have good glue corrosion resistance and good toughness to resist damage caused by accidental falling in the use process, and the impact strength of a cantilever beam notch under the ISO standard is usually required to be not lower than 6kJ/m2. Taking an acrylic adhesive as an example, the acrylic adhesive generally contains a methacrylic acid monomer, an acrylate copolymer, benzoin propyl ether, an alpha-methyl styrene oligomer, an activator and the like, has high requirements on barrier property and corrosion resistance of the rubber hose, and any decrease in corrosion resistance of the acrylic adhesive can cause yellowing of the rubber hose and surface sticking of plastic rubber, which affects normal use. The way in which toughness is improved by adding an elastomer has conventionally greatly influenced barrier properties and solvent resistance.
Chinese patent CN100548610C discloses that polybutylene terephthalate modified material has improved toughness by adding thermoplastic elastomer and improved solvent resistance by adding epoxy compound and aromatic carbodiimide. The problem with this patent is that the addition of thermoplastic elastomer and epoxy compound improves the compatibility with the glue, reduces the barrier properties of the material, and reduces the resistance to corrosion by the glue.
Disclosure of Invention
The invention aims to solve the technical problem of providing a polybutylene terephthalate mixture and a preparation method thereof, so as to overcome the defects of poor barrier property and corrosion resistance of a polybutylene terephthalate material in the prior art and the like.
The invention provides a polybutylene terephthalate mixture, which comprises the following components in percentage by weight: 91.9-99.19 wt% of polybutylene terephthalate resin, 0.8-6 wt% of hydrolysis resistance agent and 0.01-1 wt% of strontium compound.
Preferably, in the above mixture, the relative density of the polybutylene terephthalate resin is 1.30 to 1.35.
The intrinsic viscosity of the polybutylene terephthalate resin is not particularly limited, but is preferably 0.6 to 1.5dl/g, more preferably 0.9 to 1.3 dl/g. When the polybutylene terephthalate resin is used in the above range, the obtained polybutylene terephthalate mixture is more excellent in properties and the processability is more easily realized. The polybutylene terephthalate resin may be a single resin having a predetermined intrinsic viscosity, or may be a mixed resin in which two or more resins are blended to obtain a predetermined intrinsic viscosity. For example, a polybutylene terephthalate resin having an intrinsic viscosity of 1.1dl/g is obtained by mixing two kinds of polybutylene terephthalate resins having an intrinsic viscosity of 1.3dl/g and an intrinsic viscosity of 1.0 dl/g.
Preferably, in the above mixture, the hydrolysis resistance agent includes one or more of thermoplastic epoxy resin, thermosetting epoxy resin, epoxidized soybean oil, monomeric carbodiimide and polymeric carbodiimide.
Preferably, in the above mixture, the strontium compound includes one or more of strontium titanate, strontium carbonate, strontium nitrate, strontium chloride, strontium bromide, strontium oxide, strontium sulfate, and strontium stearate. The strontium compound is not affected by the morphological structure (such as spherical, needle-shaped, lamellar structure and porous structure), the strontium compound with the grain size less than 3 μm is preferably selected according to the obtained effects of barrier property, solvent resistance and mechanical property, and the grain size can also reach the required size range by a grinding process before use.
Preferably, in the mixture, the mixture further comprises 0.1-1.0 wt% of a nucleating agent, 0.1-1.0 wt% of an antioxidant and 0.1-1.0 wt% of a weather resisting agent.
Preferably, in the above mixture, the nucleating agent is inorganic mineral powder or organic salt, the inorganic mineral powder is micron-sized inorganic nucleating agent, and includes one or more of ultrafine talcum powder, barium sulfate, calcium carbonate, titanium dioxide and white carbon black, and the organic salt includes one or more of aliphatic carboxylic acid metal compound, sorbierite benzylidene derivative and aromatic carboxylic acid metal compound.
Preferably, in the mixture, the antioxidant comprises one or more of hindered phenol antioxidant, phosphite antioxidant, diphenylamine antioxidant, copper salt antioxidant and thioether antioxidant.
Preferably, in the mixture, the weather-resistant agent comprises one or more of benzotriazole light stabilizer, hindered amine light stabilizer and benzophenone light stabilizer.
The invention also provides a preparation method of the polybutylene terephthalate mixture, which comprises the following steps:
all the components are mixed and then added into a double-screw extruder, and after extrusion, the mixture is cooled and granulated to obtain the polybutylene terephthalate mixture.
Preferably, in the method, the temperature of the feeding section of the twin-screw extruder is 30-200 ℃, the temperature of the plasticizing section is 220-.
The invention also provides application of the polybutylene terephthalate mixture in packaging equipment or electronic and electric parts. For example, for hoses.
Advantageous effects
The hydrolysis resistance agent and the strontium compound have a synergistic effect, so that the barrier property, the toughness and the solvent resistance of the polybutylene terephthalate mixture can be obviously improved, and the comprehensive properties of the polybutylene terephthalate mixture, such as impact strength, tensile strength, bending modulus and the like, are excellent.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The examples and comparative examples relate to the following starting materials, but are not limited to the following:
(A) the polybutylene terephthalate resin has the model of PBT GX121, the relative density of 1.31, the melting point of 223 plus or minus 2 ℃, the intrinsic viscosity of 1.0dl/g, and is purchased from China petrochemical group asset management company, Inc., symbol division;
(B1) hydrolysis resistance agent, model Stabilizer9000, is an aromatic carbodiimide, purchased from Raschig GmbH;
(B2) hydrolysis resistant agent, epoxy resin, model CYD-011, purchased from Yueyang Barring Huaxing petrochemical Co., Ltd;
(C1) strontium compound, anhydrous strontium chloride with particle size of 5000 mesh, purchased from Chongqing Xianfeng strontium salt chemical Co., Ltd;
(C2) strontium compound, strontium bromide, with particle size of 5000 mesh, purchased from Chongqing Xianfeng strontium salt chemical Co., Ltd;
(C3) strontium compound, strontium phosphate, 5000 mesh, purchased from Hubeixin Rundchemical Co., Ltd;
(D1) elastomers, acrylate impact modifiers, model EXL-2314, available from dow chemical (shanghai) ltd;
(D2) elastomer, EBA-GMA, model Elvaloy resins PTW, available from Shanghai Branch of DuPont, China group, Inc.;
(E) nucleating agent, superfine talcum powder, model number HTPUltra5L, purchased from Liaoning Aihaiyi Rice mining Co., Ltd;
(F) antioxidant, namely tetra [ beta (3.5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, the type of which is antioxidant 1010, and the antioxidant is purchased from wind-light chemical industry Co., Ltd, Yingkou city;
(G) the weather resisting agent, 2- (2 ' -hydroxy-3 ', 5 ' -dicumylphenyl) benzotriazole, model number THASORB UV-234, was purchased from Tianjin Lianlong New materials, Inc.
The formulation components of the polybutylene terephthalate mixtures in the examples and comparative examples are shown in tables 1 and 2 in terms of weight percent.
The preparation method of the polybutylene terephthalate mixture in the examples and the comparative examples is as follows:
uniformly mixing the dried polybutylene terephthalate resin with the components according to the proportion shown in the tables 1 and 2, and adding the mixture into a double-screw extruder with the length-diameter ratio of 40:1, wherein the processing conditions are as follows: the temperature of the first zone is 60 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 250 ℃, the temperature of the fourth zone is 230 ℃, the temperature of the fifth zone is 230 ℃, the temperature of the sixth zone is 230 ℃, the temperature of the seventh zone is 230 ℃, the temperature of the eighth zone is 230 ℃, the temperature of the ninth zone is 230 ℃, the temperature of a machine head is 240 ℃, the retention time is 2 minutes, the rotating speed of a main machine is 400 revolutions per minute, and the extruded materials are cooled and granulated. And (3) putting the prepared granules into a blast oven, drying for 4 hours at the temperature of 120 ℃, and then preparing the dried granules into sample strips by using an injection molding machine. The injection molding mold temperature was 60 ℃.
The performance tests of the polybutylene terephthalate mixtures in the examples and comparative examples are as follows (test results are shown in tables 1 and 2):
(1) and (3) testing tensile property: the procedure was carried out according to ISO 527-2, the specimen size being 150 x 10 x 4mm and the drawing speed being 50 mm/min.
(2) And (3) testing the bending property: the test specimens were 80X 10X 4mm in size, 2mm/min in bending speed and 64mm in span, carried out according to ISO 178.
(3) Notched izod impact strength: the test specimens were 80 × 10 × 4mm in size and 2mm in notch depth, according to ISO 180.
(4) And (3) testing the glossiness: the test was carried out according to GB/T8807 at an angle of 20 ℃ and the sample size was 80X 55X 2mm plaques.
(5) Gas barrier property test: preparing a plastic plate with a proper size, polishing the plastic plate into a sheet with a uniform thickness of 0.3mm, and testing the oxygen transmission capacity of the material for 24 hours by using a differential pressure method gas permeameter according to GB/T1038 'test method for gas permeability of plastic films and sheets-differential pressure method', wherein the test temperature is 23 ℃ and the relative humidity is 50%.
(6) And (3) solvent resistance test: the ISO standard izod notched impact bars and 80 × 55 × 2mm plastic color plates were cleaned, dried at 120 ℃ for 6h, completely immersed in a mixed solution of methyl methacrylate/butyl methacrylate/methacrylic acid 5/5/1 in mass ratio, and heated in a water bath at 60 ℃ for 168 h. In order to avoid solvent volatilization and solidification, the test environment is kept closed as much as possible.
And cleaning the surfaces of the impact sample strips and the color plates after the solvent resistance test by using alcohol and clean water, and performing notch impact test and glossiness test according to corresponding standards.
The b value of the sample is recorded under a colorimeter. The difference between the b values after the solvent resistance test and before the solvent resistance test is represented by Δ b. The comprehensive mechanical properties of the material are judged through numerical values such as notched impact strength, tensile strength, bending modulus and the like of a cantilever beam obtained by testing, the glossiness test and the delta b value are used for representing the influence of a solvent resistance test on the surface viscosity or yellowing of a plastic part, and the smaller the glossiness change and the delta b value before and after the solvent resistance test are, the stronger the solvent resistance is.
TABLE 1
TABLE 2
As can be seen from tables 1 and 2, the comparative example 1 does not add a hydrolysis resistance agent, the comparative example 2 does not add a strontium compound, the attenuation degree of the cantilever beam notched impact strength after the solvent resistance test, the change of the gloss after the solvent resistance test, Δ b are both greater than those of the example 1, the comparative example 1 and the comparative example 2 have poor acrylic resistance, the color plate is yellowed, and the oxygen transmission amount is significantly greater than that of the example 1, i.e., the gas barrier properties of the two are not as good as those of the example 1. The surface solvent corrosion effect caused a significant change in gloss of comparative example 2. Comparative example 3 was no hydrolysis resistance agent, comparative example 4 was no strontium compound, both comparative example 3 and comparative example 4 had greater attenuation of notched impact strength of the cantilever beam after the solvent resistance test, change in gloss after the solvent resistance test, Δ b than example 8, and the gas barrier properties were all different from example 8. Comparative example 5 used strontium phosphate strontium salt, comparative example 6 used an elastomer, both of which were greater in the degree of attenuation of the notched impact strength of the cantilever beam after the solvent resistance test, in the change in the gloss after the solvent resistance test, Δ b than in example 1, and were inferior in the gas barrier property to example 1. Comparative example 7 using the prior art formulation, the degree of attenuation of the notched impact strength of the cantilever beam after the solvent resistance test, the change in gloss after the solvent resistance test, Δ b were all greater than example 4, and the gas barrier properties were inferior to example 4. In addition, the polybutylene terephthalate mixtures of examples 1-8 have better comprehensive properties such as notched Izod impact strength, tensile strength, flexural modulus, and the like. Therefore, the hydrolysis resistance agent and the strontium compound have a synergistic effect, so that the polybutylene terephthalate mixture has excellent toughness, solvent resistance and gas barrier property, and simultaneously has excellent comprehensive properties such as strength, rigidity and the like.
Claims (10)
1. A polybutylene terephthalate mixture, characterized in that the mixture components comprise, in weight percent: 91.9-99.19 wt% of polybutylene terephthalate resin, 0.8-6 wt% of hydrolysis resistance agent and 0.01-1 wt% of strontium compound.
2. The mixture of claim 1, wherein the polybutylene terephthalate resin has a relative density of 1.30 to 1.35.
3. The mixture of claim 1, wherein the hydrolysis resistance agent comprises one or more of thermoplastic epoxy resin, thermosetting epoxy resin, epoxidized soybean oil, monomeric carbodiimide, and polymeric carbodiimide.
4. The mixture of claim 1, wherein the strontium compound comprises one or more of strontium titanate, strontium carbonate, strontium nitrate, strontium chloride, strontium bromide, strontium oxide, strontium sulfate, and strontium stearate.
5. The compound of claim 1, further comprising 0.1-1.0 wt% of a nucleating agent, 0.1-1.0 wt% of an antioxidant, and 0.1-1.0 wt% of a weathering agent.
6. The mixture of claim 5, wherein the nucleating agent is inorganic mineral powder or organic salt, the inorganic mineral powder comprises one or more of ultrafine talcum powder, barium sulfate, calcium carbonate, titanium pigment and white carbon black, and the organic salt comprises one or more of aliphatic carboxylic acid metal compound, sorbierite benzylidene derivative and aromatic carboxylic acid metal compound.
7. The mixture of claim 5, wherein the antioxidant comprises one or more of hindered phenol antioxidants, phosphite antioxidants, diphenylamine antioxidants, copper salt antioxidants, and thioether antioxidants.
8. The mixture according to claim 5, wherein the weather-resistant agent comprises one or more of benzotriazole light stabilizer, hindered amine light stabilizer and benzophenone light stabilizer.
9. A method of preparing the mixture of claim 1, comprising:
all the components are mixed and then added into a double-screw extruder, and after extrusion, the mixture is cooled and granulated to obtain the polybutylene terephthalate mixture.
10. Use of the mixture according to claim 1 in packaging equipment or in electronic and electrical components.
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CN113119562A (en) * | 2021-05-12 | 2021-07-16 | 苏州清之绿新材料有限公司 | High-barrier plastic sheet and production process thereof |
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