CN114456600A - Polysulfone composite material and preparation method and application thereof - Google Patents
Polysulfone composite material and preparation method and application thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/06—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a polysulfone composite material, which comprises the following components in parts by weight: 40-90 parts of polysulfone resin; 0.1-10 parts of polyaramide liquid crystal polymer; 20-40 parts of fibers; 0.1-0.2 part of an acid acceptor; 0-0.3 part of antioxidant. According to the invention, the polyaramid liquid crystal polymer with a special structure is selected and combined with the polysulfone resin in an in-situ compounding manner, and the specific fiber is added, so that the material fluidity can be obviously improved, the defect that the polysulfone resin is easy to stress crack is improved, the problem that the mechanical property of the material is seriously deteriorated due to the poor compatibility of the common liquid crystal polymer and the polysulfone resin in the prior art is effectively solved, the polysulfone composite material which simultaneously has high fluidity, high heat resistance and high toughness is prepared, and the polysulfone composite material is particularly suitable for thin-wall heat-resistant products or ultrathin-wall electrical parts and the like, and the application of the polysulfone material is further widened.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a polysulfone composite material and a preparation method and application thereof.
Background
Polysulfone (PSU) is a thermoplastic special engineering plastic, has the characteristics of high strength, flame resistance, radiation resistance, acid resistance, oxidation resistance, solvent resistance, biocompatibility, excellent physical and mechanical properties, excellent insulating property and the like, and is widely applied in many fields. However, polysulfone resin has a high melting point and a high melt viscosity, which is not conducive to processing and molding, and the impact resistance of general polysulfone materials is also poor, and the above disadvantages limit the application of polysulfone materials in many aspects. The development of novel reinforced polysulfones is the research direction of polysulfone materials in recent years. The Thermotropic Liquid Crystal Polymer (TLCP) and the thermoplastic resin are blended to form the in-situ composite material, which is a technical means for carrying out flow modification and mechanical modification on the material, however, researches show that the compatibility between most thermotropic liquid crystal polymers and polysulfone resin is very poor, the incompatibility causes that the TLCP reinforced microfiber phase is not uniformly dispersed in a matrix, an obvious skin-core structure appears, stress cannot be effectively transmitted at a two-phase interface, the impact resistance of the material is more deteriorated, and a product of the material is easy to generate a stress cracking phenomenon.
Disclosure of Invention
The invention aims to provide a polysulfone composite material which can simultaneously achieve high fluidity, high heat resistance and high mechanical strength.
The invention also aims to provide a preparation method of the polysulfone composite material.
The invention is realized by the following technical scheme:
the polysulfone composite material comprises the following components in parts by weight:
40-90 parts of polysulfone resin;
0.1-10 parts of polyaramide liquid crystal polymer;
20-40 parts of fibers;
0.1-0.2 part of an acid acceptor;
0-0.3 part of antioxidant.
Preferably, the polyaramide liquid crystal polymer is 0.5-5 parts; more preferably, the polyaramid liquid crystal polymer is 1.2-3.5 parts.
The polysulfone resin is preferably polysulfone with the weight-average molecular weight of 30000-75000 Dalton; more preferably polysulfone having a weight average molecular weight of 40000-60000 daltons.
The polyaramide liquid crystal polymer is composed of the following repeating units of formula (I) to formula (IV):
the content of the repeating unit of the formula (I) is less than or equal to 100mol% and is not equal to 0, wherein the mol total amount of the repeating units of the formula (I) to the formula (IV) is 100 mol%; the content of the repeating unit of the formula (II) is less than 100 mol%; the content of the repeating unit of the formula (III) is less than 100 mol%; the content of the repeating unit of the formula (IV) is less than 100 mol%;
wherein R is1The structure of (A) is selected from any one or more of a formula (V), a formula (VI) or a formula (VII);
wherein R is2Is selected from
、
、
Any one of a heterocyclic aromatic group or a polycyclic aromatic group; n is1Is a positive integer greater than or equal to 1; the R is3Is selected from
、
、
、
、
、
、
、
Oxygen atom, sulfur atom or a linear or branched aliphatic divalent group of more than 6 carbon atoms, wherein n2Is a positive integer of 1-6; the heterocyclic aromatic group is an aromatic group in which atoms forming a ring contain at least one hetero atom in addition to carbon atoms; the polycyclic aromatic group means an aromatic group in which two or more benzene rings are connected in a fused ring form.
Preferably, the content of the repeating unit of the formula (I) is 50-100 mol%; the content of the repeating unit of the formula (II) is less than or equal to 50 mol%; the content of the repeating unit of the formula (III) is less than or equal to 50 mol%; the content of the repeating unit of the formula (IV) is less than or equal to 50 mol%; preferably, the content of the repeating units in the formulas (II), (III) and (IV) is not equal to 0.
Preferred in the present invention are polyaramid liquid crystalline polymers having a weight average molecular weight of 20000-50000 daltons.
The preparation method of the polyaramide liquid crystal polymer refers to Chinese patent application CN 202011583382.7.
The fiber is selected from any one or more of glass fiber, carbon fiber, aramid fiber, basalt fiber, propionitrile fiber, boron fiber or whisker; preferably, the fiber is selected from any one or more of glass fiber, carbon fiber or aramid fiber; more preferably, the fiber is a glass fiber and a carbon fiber in a weight ratio (2-3): 1, compounding.
The acid acceptor of the invention can be selected from any one or more of aluminum oxide, calcium oxide or magnesium oxide.
The antioxidant can be any one or more of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 1, 3, 5-trimethyl-2, 4, 6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene or 2, 8-di-tert-butyl-4-methylphenol.
The invention also provides a preparation method of the polysulfone composite material, which comprises the following steps: adding the components into a double-screw extruder according to the proportion, carrying out melt mixing, extruding and granulating to obtain the polysulfone composite material. Preferably, the rotating speed of the screw is 410-480 r/min, and the processing temperature is 290-360 ℃.
The invention also provides application of the polysulfone composite material in preparing thin-wall heat-resistant parts or ultrathin-wall electrical parts.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the polyaramid liquid crystal polymer with a special structure is selected and combined with the polysulfone resin in an in-situ compounding manner, and the specific fiber is added, so that the material fluidity can be obviously improved, the defect that the polysulfone resin is easy to stress crack is overcome, the problem that the mechanical property of the material is seriously deteriorated due to poor compatibility of a common liquid crystal polymer (such as semi-aromatic polyester liquid crystal) and the polysulfone resin in the prior art is effectively solved, the polysulfone composite material which simultaneously has high fluidity, high heat resistance and high toughness is prepared, and the polysulfone composite material is particularly suitable for thin-wall heat-resistant products or ultrathin-wall electrical parts and the like, and the application of the polysulfone material is further widened.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw materials used in the examples and comparative examples of the present invention are described below, but are not limited to these materials:
polysulfone resin 1: the weight average molecular weight is 50000 dalton, and the product is prepared by self;
polysulfone resin 2: the weight average molecular weight is 35000 daltons, and the preparation method is self-made;
polysulfone resin 3: the weight average molecular weight is 25000 daltons, and the self-made product is prepared;
fiber 1: glass fiber, commercially available;
fiber 2: carbon fiber, commercially available;
acid-absorbing agent: alumina, commercially available;
antioxidant: tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester, commercially available.
The invention provides a preparation method of polysulfone resin, which comprises the following steps: adding 4, 4-dichlorodiphenyl sulfone, bisphenol A and sodium carbonate into a reaction kettle, adding an organic solvent N-methyl pyrrolidone, pressing nitrogen into the reaction kettle, and increasing the pressure in the kettle to 1-2 MPa; heating to 180-210 ℃ in the kettle, keeping the temperature for 1-3 hours, and then heating to 250 ℃ in the temperature range of 210 ℃. Keeping the temperature for 1-3 hours, adding bisphenol A to continue the reaction, and finishing the polymerization reaction to obtain the polymer mucus. And cooling, filtering, washing and drying the polymer mucus to obtain a product. The molecular weight is obtained by adjusting the proportion of 4, 4-dichlorodiphenyl sulfone and the reaction time.
The preparation methods of the polyaramid liquid crystal polymer used in the examples and the comparative examples of the invention refer to Chinese patent application CN 202011583382.7: according to the mixture ratio of table 1, nitrogen is introduced into a reactor with a stirring device, air in the reactor is exhausted, diamine monomer is added to dissolve in polar aprotic solvent, acid binding agent and end capping agent are added, and then diformyl chloride monomer is added to react for 3-7h under the ice bath condition of-15 ℃, and after the reaction is stopped, the polyaramide liquid crystal polymer is obtained through elutriation, crushing, washing and drying.
Table 1: molar ratio and weight average molecular weight parameter of monomers and reagents of polyaramid liquid crystal polymer
| A1 | A2 | A3 | A4 | |
| Bisphenol A type diethanediamine | 0.6 | 0.5 | ||
| Bisphenol S type diethanediamine | 0.4 | 0.4 | ||
| Diphenyl diphenol type diether diamine | 0.5 | |||
| 6,6 '-dihydroxy-2, 2' -bipyridyl diethanediamine | 0.1 | |||
| 2, 6-naphthalenediol type diether diamine | 0.5 | 0.5 | ||
| P-phenylenediamine | 0.5 | |||
| Terephthaloyl chloride | 0.8 | 1 | 0.2 | 1 |
| Isophthaloyl dichloride | 0.2 | 0.8 | ||
| N-methyl pyrrolidone | 4 | 4 | 4 | 4 |
| Acid-binding agent 2-methylpyridine | 1.8 | 1.6 | 2 | 1.5 |
| End-capping reagent benzoyl chloride | 0.03 | 0.04 | 0.05 | 0.04 |
| Weight average molecular weight | 3.4 ten thousand | 4.6 ten thousand | 3.5 ten thousand | 2.4 ten thousand |
Preparation methods of polysulfone composites of examples and comparative examples:
adding the components into a double-screw extruder according to the mixture ratio of table 2/table 3, carrying out melt mixing at the screw rotating speed of 410-480 r/min and the processing temperature of 290-360 ℃, and carrying out extrusion granulation to obtain the polysulfone composite material.
Relevant performance test methods or standards:
(1) melt flow rate: the test method refers to the standard ISO 1133-2005, the test condition is 365 ℃, and 5 kg;
(2) heat distortion temperature: the test method is referred to ISO 75-1/-2;
(3) tensile strength: test method reference ISO 527;
(4) bending strength: test method ISO 178;
(5) impact strength of the simply supported beam notch: ISO 180/1 a.
Table 2: EXAMPLES 1-7 proportions (in parts by weight) of the ingredients and the results of the associated Performance tests
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| Polysulfone resin 1 | 75 | 75 | 75 | 75 | 75 | 75 | 75 |
| Polyaramid liquid crystal polymer A1 | 0.5 | 1.2 | 2.5 | 5 | 10 | 2.5 | 2.5 |
| Glass fiber | 16.5 | 16.5 | 16.5 | 16.5 | 16.5 | 22 | |
| Carbon fiber | 5.5 | 5.5 | 5.5 | 5.5 | 5.5 | 22 | |
| Acid-absorbing agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant agent | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Melt flow Rate/g/10 min | 16.2 | 18.5 | 19.8 | 19.4 | 20.1 | 20.4 | 19.6 |
| Heat distortion temperature/. degree.C | 191.2 | 192.4 | 194.3 | 194.7 | 195.8 | 192.6 | 191.7 |
| Tensile strength/MPa | 107 | 108 | 112 | 113 | 113 | 103 | 104 |
| Flexural Strength/MPa | 142.1 | 146.4 | 151.7 | 149.6 | 148.9 | 132.4 | 129.4 |
| Impact strength/kJ/m of simply supported beam gap2 | 7.8 | 8.3 | 8.2 | 7.7 | 7.2 | 6.2 | 6.7 |
Table 3: distribution ratio (by weight) of each component in examples 8-12 and comparative examples 1-2 and related performance test results
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Comparative example 1 | Comparative example 2 | |
| Polysulfone resin 1 | 70 | 62 | 84 | 75 | 75 | ||
| Polysulfone resin 2 | 75 | ||||||
| Polysulfone resin 3 | 75 | ||||||
| Polyaramid liquid crystal polymer A1 | 2.5 | 2.5 | / | 2.5 | |||
| Polyaramid liquid crystal polymer A2 | 1.5 | ||||||
| Polyaramid liquid crystal polymer A3 | 1.0 | ||||||
| Polyaramid liquid crystal polymer A4 | 2.2 | ||||||
| Glass fiber | 16.5 | 16.5 | 21 | 16 | 25 | 16.5 | / |
| Carbon fiber | 5.5 | 5.5 | 7 | 8 | 10 | 5.5 | / |
| Acid-absorbing agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant agent | 0.1 | 0.1 | 0.2 | 0.2 | 0.2 | 0.1 | 0.1 |
| Melt flow Rate/g/10 min | 20.2 | 21.3 | 17.9 | 17.1 | 15.2 | 5.4 | 18.9 |
| Heat distortion temperature/. degree.C | 186.8 | 180.9 | 193.8 | 192.3 | 186.9 | 185.3 | 182.6 |
| Tensile strength/MPa | 107 | 103 | 114 | 108 | 107 | 102 | 94 |
| Flexural Strength/MPa | 145.6 | 141.3 | 152.3 | 146.6 | 145.3 | 140.8 | 135.7 |
| Impact strength/kJ/m of simply supported beam gap2 | 7.5 | 7.1 | 8.4 | 7.8 | 7.7 | 6.8 | 5.7 |
It is seen from the above examples and comparative examples that the invention can significantly improve the flowability of the material and simultaneously improve the stress cracking tendency of polysulfone resin by selecting the polyaramid liquid crystal polymer having a specific structure and adding specific fibers, and prepare the polysulfone composite material which simultaneously has high flowability, high heat resistance and high toughness.
Claims (10)
1. The polysulfone composite material is characterized by comprising the following components in parts by weight:
40-90 parts of polysulfone resin;
0.1-10 parts of polyaramide liquid crystal polymer;
20-40 parts of fibers;
0.1-0.2 part of an acid acceptor;
0-0.3 part of antioxidant.
2. The polysulfone composite 1 material according to claim 1, wherein the polyaramid liquid crystal polymer is 0.5-5 parts; preferably, the polyaramide liquid crystal polymer is 1.2-3.5 parts.
3. The polysulfone composite of claim 1, wherein the polysulfone resin has a weight-average molecular weight of 30000-75000 daltons; preferably, the weight average molecular weight of the polysulfone resin is 40000-60000 daltons.
4. The polysulfone composite according to claim 1, wherein the polyaramid liquid crystal polymer is composed of repeating units of the following formulae (I) to (IV):
based on the total mole amount of the repeating units shown in the formulas (I) to (IV) being 100mol%, the content of the repeating unit shown in the formula (I) is less than or equal to 100mol% and is not equal to 0; the content of the repeating unit of the formula (II) is less than 100 mol%; the content of the repeating unit of the formula (III) is less than 100 mol%; the content of the repeating unit of the formula (IV) is less than 100 mol%;
wherein R is1The structure of (A) is selected from any one or more of a formula (V), a formula (VI) or a formula (VII);
wherein R is2Is selected from
、
、
Any one of a heterocyclic aromatic group or a polycyclic aromatic group; n is1Is a positive integer greater than or equal to 1; the R is3Is selected from
、
、
、
、
、
、
、
Oxygen atom, sulfur atom or a linear or branched aliphatic divalent group of more than 6 carbon atoms, wherein n2Is a positive integer of 1-6; the heterocyclic aromatic group is an aromatic group in which atoms constituting a ring contain at least one hetero atom in addition to carbon atoms; the polycyclic aromatic group means an aromatic group in which two or more benzene rings are connected in a fused ring form.
5. The polysulfone composite according to claim 4, wherein the amount of the recurring unit of formula (I) is 50mol% to 100 mol%; the content of the repeating unit of the formula (II) is less than or equal to 50 mol%; the content of the repeating unit of the formula (III) is less than or equal to 50 mol%; the content of the repeating unit of the formula (IV) is less than or equal to 50 mol%; preferably, the content of the repeating units in the formulas (II), (III) and (IV) is not equal to 0.
6. The polysulfone composite of claim 1, wherein the polyaramid liquid crystalline polymer has a weight-average molecular weight of 20000-50000 daltons.
7. The polysulfone composite according to claim 1, wherein the fibers are selected from any one or more of glass fibers, carbon fibers, aramid fibers, basalt fibers, propionitrile fibers, boron fibers or whiskers; preferably, the fiber is selected from any one or more of glass fiber, carbon fiber or aramid fiber; more preferably, the fiber is a glass fiber and a carbon fiber in a weight ratio (2-3): 1, compounding.
8. The polysulfone composite material according to claim 1, wherein the acid acceptor is selected from any one or more of alumina, calcium oxide and magnesium oxide, and the antioxidant is selected from any one or more of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], n-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 1, 3, 5-trimethyl-2, 4, 6- (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene or 2, 8-di-tert-butyl-4-methylphenol.
9. The method of preparing a polysulfone composite according to any of claims 1-8, comprising the steps of: adding the components into a double-screw extruder according to the proportion, carrying out melt mixing, extruding and granulating to obtain the polysulfone composite material.
10. Use of the polysulfone composite according to any of claims 1-8 for the preparation of thin-walled, heat-resistant articles or ultra-thin-walled electrical components.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785672A (en) * | 2022-12-07 | 2023-03-14 | 广东优巨先进新材料股份有限公司 | Polyphenylene sulfone composite material and preparation method and application thereof |
| CN116218220A (en) * | 2023-01-05 | 2023-06-06 | 广东优巨先进新材料股份有限公司 | Polyphenyl sulfone composition and application |
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| CN109777105A (en) * | 2019-01-31 | 2019-05-21 | 珠海派锐尔新材料有限公司 | A kind of high flowing polysulfone composites and preparation method thereof |
| CN111187410A (en) * | 2019-12-27 | 2020-05-22 | 江门市优巨新材料有限公司 | Poly (p-phenylene terephthalamide) liquid crystal polymer and preparation method thereof |
| CN112625439A (en) * | 2020-12-28 | 2021-04-09 | 广东优巨先进新材料股份有限公司 | Low-dielectric polyaramide liquid crystal composite material and preparation method and application thereof |
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| CN108440961A (en) * | 2018-04-25 | 2018-08-24 | 长沙五犇新材料科技有限公司 | A kind of modified polysulfone composite material and preparation method and application |
| CN109777105A (en) * | 2019-01-31 | 2019-05-21 | 珠海派锐尔新材料有限公司 | A kind of high flowing polysulfone composites and preparation method thereof |
| CN111187410A (en) * | 2019-12-27 | 2020-05-22 | 江门市优巨新材料有限公司 | Poly (p-phenylene terephthalamide) liquid crystal polymer and preparation method thereof |
| CN112625439A (en) * | 2020-12-28 | 2021-04-09 | 广东优巨先进新材料股份有限公司 | Low-dielectric polyaramide liquid crystal composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115785672A (en) * | 2022-12-07 | 2023-03-14 | 广东优巨先进新材料股份有限公司 | Polyphenylene sulfone composite material and preparation method and application thereof |
| CN116218220A (en) * | 2023-01-05 | 2023-06-06 | 广东优巨先进新材料股份有限公司 | Polyphenyl sulfone composition and application |
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