Quartz-fiber-reinforced polysulfone composite material and preparation method therefor
By adding polyvinyl alcohol fibers with a specific degree of polymerization to quartz fiber reinforced polysulfone composites, the interfacial bonding between quartz fibers and the polysulfone resin matrix is improved, solving the problem of poor adhesion between quartz fibers and polysulfone resin, enhancing the mechanical properties of the composite material, and expanding its application in medical devices and food contact fields.
Patent Information
- Application Number
- PCT/CN2024/133887
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-08-13
- Filing Date
- 2024-11-22
- Publication Date
- 2026-02-19
AI Technical Summary
The poor adhesion between quartz fiber and polysulfone resin matrix results in poor mechanical properties of the composite material, limiting its application in fields such as medical devices and food contact.
By adding polyvinyl alcohol fibers with a specific degree of polymerization, the interfacial bonding between quartz fibers and polysulfone resin matrix is improved, and the bonding strength between the two is enhanced, thus preparing quartz fiber reinforced polysulfone composite materials.
It improves the mechanical strength and interfacial bonding strength of composite materials, making them suitable for applications such as medical devices and food contact, and meeting the needs of industrial production.
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Abstract
Description
Quartz fiber reinforced polysulfone composite material and preparation method thereof
[0001] Cross-reference to related applications
[0002] The present disclosure claims priority to and the benefit of Chinese Patent Application No. 202411105890.2, filed August 13, 2024, entitled “Quartz fiber reinforced polysulfone composite material and preparation method thereof,” which is incorporated by reference herein in its entirety. TECHNICAL FIELD
[0003] The present disclosure relates to a quartz fiber reinforced polysulfone composite material and a preparation method thereof, and belongs to the field of modified polysulfone composite materials. BACKGROUND
[0004] Polysulfone is an amorphous amber transparent special engineering plastic, which has extremely strong thermal stability. The glass transition temperature of polysulfone is 185°C, and it can be used at 160°C for a long time. It also has excellent hydrolysis resistance, chemical resistance and self-flame retardance, and is widely used in pipeline components, water treatment and other fields. Since pure polysulfone resin is difficult to meet the mechanical strength requirements of load-bearing components, in order to expand the application field of polysulfone resin, the existing technology often modifies pure polysulfone resin by filling with glass fiber.
[0005] The mechanical strength and modulus of polysulfone composite material filled with glass fiber are significantly improved compared with pure polysulfone resin. However, since glass fiber is usually composed of silicates, aluminates, phosphates, calcium salts, carbonates and other components, it will release alkali metal salts during application, limiting its application in medical devices or human implants and other fields. Quartz fiber is composed of more than 99.9% high-purity silicon dioxide. Compared with traditional glass fiber, it has single composition, high purity and does not release metal salts, so it has applications in medical plates in hospitals and dental clinics, food contact and other fields.
[0006] However, since quartz fiber itself has chemical inertness, the wettability of the polysulfone resin matrix is poor, which leads to low adhesion between quartz fiber and polysulfone resin matrix, and further leads to poor mechanical strength of the obtained composite material. Therefore, improving the interfacial adhesion between quartz fiber and polysulfone resin matrix is crucial to improve the mechanical properties of the composite material. SUMMARY
[0007] Problems to be solved by the invention
[0008] The present disclosure aims to solve the problems existing in the prior art, i.e., poor adhesion between quartz fibers and a polysulfone resin matrix, poor interfacial bonding, and poor mechanical properties of the composite material.
[0009] Solution for solving the problem
[0010] To achieve the above-mentioned purpose, the present inventors have conducted in-depth research and unexpectedly found that by blending a specific amount of polyvinyl alcohol fibers with a specific degree of polymerization, the interfacial bonding between quartz fibers and a polysulfone resin matrix can be improved, thereby enhancing the bonding strength of the two and further improving the mechanical strength of the composite material. Polyvinyl alcohol (PVA) fibers have excellent properties such as high strength, high modulus, acid and alkali resistance, and good biocompatibility. The multiple hydroxyl polar chemical bonds in PVA fibers have good chemical compatibility with the ether bonds in the polysulfone resin matrix and the silicon-oxygen bonds in the quartz fibers, which not only helps to enhance the interfacial bonding strength of the quartz fibers and the polysulfone resin matrix, but also allows PVA fibers to act as a reinforcing phase for the polysulfone resin matrix.
[0011] The present disclosure provides a quartz fiber reinforced polysulfone composite material, comprising:
[0012] 55-90 parts by weight of a polysulfone resin,
[0013] 10-30 parts by weight of quartz fibers,
[0014] 5-20 parts by weight of polyvinyl alcohol fibers, the degree of polymerization of the polyvinyl alcohol being 3000-3500.
[0015] The composite material according to the present disclosure, wherein the diameter of the quartz fibers is 6-15 μm and the length is 3-8 mm.
[0016] The composite material according to the present disclosure, wherein the length of the polyvinyl alcohol fibers is 3-6 mm and the diameter is 90-110 μm.
[0017] The composite material according to the present disclosure, wherein the polysulfone resin is a bisphenol A type polysulfone, preferably, the ash content of the polysulfone resin is less than 150 ppm based on the mass of the polysulfone resin, and the content of cyclic dimers in the polysulfone resin is less than 1.2%.
[0018] The composite material according to the present disclosure, wherein the weight average molecular weight Mw of the polysulfone resin is 50000-80000 g / mol, and the molecular weight distribution, i.e., Mw / Mn, is 1.5-2.0.
[0019] The present disclosure also provides a preparation method of a quartz fiber reinforced polysulfone composite material, comprising:
[0020] 55-90 parts by weight of a polysulfone resin, 10-30 parts by weight of quartz fibers, and 5-20 parts by weight of polyvinyl alcohol fibers having a degree of polymerization of 3000-3500 are uniformly mixed in a high-speed mixer;
[0021] The obtained mixture is melt-extruded, granulated, and dried in a twin-screw extruder.
[0022] The method of the present disclosure, wherein the quartz fibers have a diameter of 6-15 μm and a length of 3-8 mm.
[0023] The method of the present disclosure, wherein the polyvinyl alcohol fibers have a length of 3-6 mm and a diameter of 90-110 μm.
[0024] The method of the present disclosure, wherein the polysulfone resin is a bisphenol A type polysulfone, preferably, the ash content of the polysulfone resin is less than 150 ppm, and the content of cyclic dimers in the polysulfone resin is less than 1.2% based on the mass of the polysulfone resin.
[0025] The method of the present disclosure, wherein the polysulfone resin has a weight average molecular weight Mw of 50000-80000 g / mol and a molecular weight distribution, i.e., Mw / Mn, of 1.5-2.0.
[0026] Effects of the invention
[0027] The quartz fiber reinforced polysulfone composite provided by the present disclosure has a simple component composition, and does not contain phosphate, calcium salt, aluminate, and other small molecular components of organic additives, etc., compared with glass fiber reinforced polysulfone composite, which is beneficial to the application in the fields of medical devices, food contact, etc. In the present disclosure, polyvinyl alcohol fibers are used to improve the interfacial bonding between quartz fibers and the polysulfone resin matrix, which is beneficial to further improving the rigidity, bending strength, tensile strength, dimensional stability, and other properties of the composite. In addition, since polyvinyl alcohol also has the advantages of chemical stability and low biological toxicity, etc., it is also beneficial to the popularization and application of the obtained composite in the fields of medical devices, food contact, etc.
[0028] The method of the present disclosure has simple process, low cost, and does not need to modify the existing equipment, which is suitable for industrial production. DETAILED DESCRIPTION
[0029] Various exemplary embodiments, features, and aspects of the present disclosure will be described in detail below. The word "exemplary" is used herein to mean "serving as an example, instance, or illustration." Any implementation described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other implementations.
[0030] In addition, for a better understanding of the present disclosure, numerous specific details are given in the following detailed description. It will be understood by those skilled in the art that the present disclosure can be practiced without certain specific details. In other instances, well-known methods, apparatuses, equipment and procedures have not been described in detail so as not to obscure the subject matter of the present disclosure.
[0031] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. The meaning of "a", "an", and "the" includes plural references. The meaning of "in" includes "in" and "on." The use of "including", "comprising", or "having" means that there are no numerical limitations to the number of steps, components or elements. The use of "consisting essentially of" means that the number of steps, components or elements is limited to the number of steps, components or elements identified, and that other steps, components or elements can be included as long as they do not materially affect the basic and novel characteristics of the claimed disclosure. The use of "consisting of" means that the number of steps, components or elements is limited to the number of steps, components or elements identified.
[0032] In this specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
[0033] In this specification, the meaning of "some specific / preferred embodiments", "other specific / preferred embodiments", "embodiments", and the like means that the specific elements (for example, features, structures, properties, and / or characteristics) described in relation to the embodiments are included in at least one embodiment described herein, and can be present in other embodiments or can not be present in other embodiments. In addition, it should be understood that the elements can be combined in various embodiments in any suitable manner.
[0034] In this specification, the numerical range represented by "numerical value A to numerical value B" means a range including the end point values A and B.
[0035] The present disclosure provides a quartz fiber reinforced polysulfone composite material, which comprises:
[0036] 55-90 parts by weight of a polysulfone resin,
[0037] 10-30 parts by weight of quartz fiber,
[0038] 5-20 parts by weight of polyvinyl alcohol fiber, the degree of polymerization of the polyvinyl alcohol being 3000-3500.
[0039] When the degree of polymerization of the polyvinyl alcohol is 3000-3500, the resulting composite material has good processability and mechanical strength. If the degree of polymerization is less than 3000, the strength of the polyvinyl alcohol fiber is low and the filling and reinforcing effect is poor. If the degree of polymerization is higher than 3500, the viscosity of the polyvinyl alcohol is high and it is difficult to process.
[0040] When the content of the polyvinyl alcohol fiber is 5 to 20 parts by weight, the obtained composite material has suitable mechanical strength and fluidity. If the content of the polyvinyl alcohol fiber is less than 5 parts by weight, the polyvinyl alcohol fiber has a poor effect on improving the interfacial bonding strength between the quartz fiber and the polysulfone resin matrix, and the obtained composite material has a low strength. If the content of the polyvinyl alcohol fiber is more than 20 parts by weight, the obtained composite material has a poor fluidity due to the high crystallinity and viscosity of the polyvinyl alcohol fiber, and is difficult to process. Preferably, the content of the polyvinyl alcohol fiber is 5 to 15 parts by weight.
[0041] Preferably, the diameter of the quartz fiber is 6 μm to 15 μm, and the length is 3 mm to 8 mm.
[0042] If the diameter of the quartz fiber is less than 6 μm, the quartz fiber is easily broken during the extrusion process, and the obtained composite material has poor mechanical properties. If the diameter is more than 15 μm, the quartz fiber bundle is not easily dispersed in the composite material.
[0043] If the length of the quartz fiber is less than 3 mm, the obtained composite material has poor mechanical properties. If the length is more than 8 mm, the quartz fiber has a poor dispersion effect in the composite material, and is easily floated.
[0044] Preferably, the diameter of the quartz fiber is 6 μm to 10 μm, and the length is 3 mm to 6 mm.
[0045] Preferably, the quartz fiber has a silica content of more than 99% and an unmodified surface.
[0046] Preferably, the length of the polyvinyl alcohol fiber is 3 mm to 6 mm, and the diameter is 90 μm to 110 μm. When the length and the diameter are within the above ranges, it is beneficial to obtain excellent mechanical properties and good dispersion in the composite material.
[0047] Preferably, the polysulfone resin is a bisphenol A type polysulfone.
[0048] Preferably, the content of the polysulfone resin is 60 to 80 parts by weight.
[0049] Preferably, based on the mass of the polysulfone resin, the ash content of the polysulfone resin is less than 150 ppm, and the content of the cyclic dimer in the polysulfone resin is less than 1.2%, which is beneficial to meet the potential medical application requirements of the composite material.
[0050] Preferably, the weight average molecular weight Mw of the polysulfone resin is 50000 to 80000 g / mol, and more preferably 65000 to 70000 g / mol, and the molecular weight distribution, i.e. Mw / Mn, is 1.5 to 2.0.
[0051] When the weight average molecular weight Mw of the polysulfone resin is 50000-80000 g / mol, the composite material has suitable processing performance and mechanical properties, if the weight average molecular weight Mw is lower than 50000 g / mol, the mechanical strength of the composite material is poor, and if the weight average molecular weight Mw is higher than 80000 g / mol, it will result in low fluidity of the obtained composite material and difficult processing.
[0052] The present disclosure also provides a preparation method of a quartz fiber reinforced polysulfone composite material, which comprises:
[0053] 55-90 parts by weight of a polysulfone resin, 10-30 parts by weight of quartz fiber, and 5-20 parts by weight of polyvinyl alcohol fiber are uniformly mixed, wherein the polyvinyl alcohol has a degree of polymerization of 3000-3500;
[0054] The obtained mixture is subjected to melt extrusion, granulation and drying in a twin-screw extruder.
[0055] In the preparation method of the present disclosure, the descriptions of the polysulfone resin, quartz fiber and polyvinyl alcohol fiber are the same as those described above in the quartz fiber reinforced polysulfone composite material.
[0056] As the preparation method of the quartz fiber reinforced polysulfone composite material of the present disclosure, the following can be shown, for example:
[0057] 55-90 parts by weight of a polysulfone resin with a weight average molecular weight Mw of 50000-80000 g / mol and a molecular weight distribution Mw / Mn of 1.5-2.0, 10-30 parts by weight of quartz fiber with a diameter of 6-15 μm and a length of 3-8 mm, and 5-20 parts by weight of polyvinyl alcohol fiber with a degree of polymerization of 3000-3500 of polyvinyl alcohol are uniformly mixed in a high-speed mixer, preferably mixed at a frequency of 40-60 Hz for 5-8 min;
[0058] Then the obtained mixture is added to a twin-screw extruder for melt extrusion, granulation and drying to obtain the quartz fiber reinforced polysulfone composite material; wherein the extrusion temperature is 280-350℃, and the screw rotation speed is 250-500 rpm. Preferably, the extrusion temperature is: Zone 1: 280℃, Zones 2-8: 330℃, Zones 9-12: 350℃, and the die head is 350℃; and the screw rotation speed is 300-350 rpm.
[0059] Examples
[0060] The embodiments of the present disclosure will be described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustration of the present disclosure and should not be regarded as limiting the scope of the present disclosure. The specific conditions not noted in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not noted by the manufacturer, which are all conventional products that can be obtained by commercial means.
[0061] The raw materials of the following examples and comparative examples can be obtained by commercial means, and the details are as follows:
[0062] Polysulfone resin:
[0063] Bisphenol A type polysulfone, melt index 10-20 g / 10 min, weight average molecular weight 65000-70000, molecular weight distribution, i.e. Mw / Mn, 1.5-2.0, ash content 100-150 ppm, content of cyclic dimer 1.0-1.2%.
[0064] Quartz fiber:
[0065] Quartz fiber 1: specification: silica content ≥ 99.9%, length 4 mm, diameter 10 μm.
[0066] Quartz fiber 2: specification: silica content ≥ 99.9%, length 5 mm, diameter 10 μm.
[0067] Quartz fiber 3: specification: silica content ≥ 99.9%, length 4 mm, diameter 15 μm.
[0068] Polyvinyl alcohol fiber, polyvinyl alcohol polymerization degree 3000-3500, fiber length 6 mm, diameter 100 μm, linear density 2.0 dtex, breaking strength 10-12 cN / dtex, initial modulus, i.e. fiber elastic modulus, 200-220 cN / dtex, alcoholysis degree 95-100%.
[0069] The test methods or standards of each performance index are shown in Table 1 below:
[0070] Table 1
[0071] Preparation method of polysulfone composite of examples and comparative examples:
[0072] Examples 1-6 were prepared by dispersing the polysulfone resin, quartz fiber and polyvinyl alcohol fiber in a high-speed mixer according to the proportions shown in Table 2 (by weight parts), and then extruding and granulating in a twin-screw extruder to obtain a fiber-reinforced polysulfone composite material. The extrusion temperature was 280°C in Zone 1, 330°C in Zones 2-8, 350°C in Zones 9-12, and 350°C at the die. The screw rotation speed was 300-350 rpm.
[0073] The properties of the polysulfone composite materials obtained in each example and comparative example are also shown in Table 2 and Table 3 below.
[0074] Table 2 Note: "-" in the table means that the component is not added.
[0075] Table 3 Note: "-" in the table means that the component is not added.
[0076] As can be seen from the comparison of Comparative Examples 1-3 and Examples 1-8, in the composite material provided by the present disclosure, because the polysulfone resin, quartz fiber and polyvinyl alcohol fiber are simultaneously present and each has a content within a specific range, the obtained composite material simultaneously ensures excellent mechanical properties and processability.
[0077] It should be noted that although the technical solutions of the present disclosure are described with specific examples, those skilled in the art can understand that the present disclosure should not be limited thereto.
[0078] The above has described various embodiments of the present disclosure, and the above description is exemplary and is not exhaustive, and is also not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The choice of terms used herein is intended to best explain the principles of the embodiments, practical applications, or improvements to the technology in the market, or to enable other ordinary skilled persons in the art to understand the embodiments disclosed herein.
Claims
1. A quartz fiber-reinforced polysulfone composite material comprising: 55-90 parts by weight of a polysulfone resin, 10-30 parts by weight of quartz fiber, 5-20 parts by weight of polyvinyl alcohol fiber having a degree of polymerization of 3000-3500.
2. The composite material according to claim 1, wherein the quartz fiber has a diameter of 6-15 μm and a length of 3-8 mm.
3. The composite material according to claim 1 or 2, wherein the polyvinyl alcohol fiber has a length of 3-6 mm and a diameter of 90-110 μm.
4. The composite material according to claim 1 or 2, wherein the polysulfone resin is a bisphenol A-type polysulfone, preferably, the ash content of the polysulfone resin is less than 150 ppm based on the mass of the polysulfone resin, and the content of cyclic dimers in the polysulfone resin is less than 1.2%.
5. The composite material according to claim 1 or 2, wherein the polysulfone resin has a weight average molecular weight Mw of 50000-80000 g / mol and a molecular weight distribution, Mw / Mn, of 1.5-2.
0.
6. A method for producing a quartz fiber-reinforced polysulfone composite material, comprising: mixing 55-90 parts by weight of a polysulfone resin, 10-30 parts by weight of quartz fiber, and 5-20 parts by weight of polyvinyl alcohol fiber having a degree of polymerization of 3000-3500 in a high-speed mixer to homogeneity; melt-extruding, pelletizing, and drying the resulting mixture in a twin-screw extruder.
7. The method according to claim 6, wherein the quartz fiber has a diameter of 6-15 μm and a length of 3-8 mm.
8. The method according to claim 6 or 7, wherein the polyvinyl alcohol fiber has a length of 3-6 mm and a diameter of 90-110 μm.
9. The method according to claim 6 or 7, wherein the polysulfone resin is a bisphenol A-type polysulfone, preferably, the ash content of the polysulfone resin is less than 150 ppm based on the mass of the polysulfone resin, and the content of cyclic dimers in the polysulfone resin is less than 1.2%.
10. The method according to claim 6 or 7, wherein the polysulfone resin has a weight average molecular weight Mw of 50000-80000 g / mol and a molecular weight distribution, Mw / Mn, of 1.5-2.0.
Citation Information
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