CN115960414A - Polypropylene composite material and preparation method and application thereof - Google Patents

Polypropylene composite material and preparation method and application thereof Download PDF

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CN115960414A
CN115960414A CN202211726273.5A CN202211726273A CN115960414A CN 115960414 A CN115960414 A CN 115960414A CN 202211726273 A CN202211726273 A CN 202211726273A CN 115960414 A CN115960414 A CN 115960414A
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polypropylene
polypropylene composite
fiber
composite material
polyamide
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CN115960414B (en
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胡佳旭
陈平绪
叶南飚
陈嘉杰
俞飞
吴亦建
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Kingfa Science and Technology Co Ltd
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Abstract

The invention provides a polypropylene composite material and a preparation method and application thereof. The polypropylene material comprises the following components in parts by weight: 88 to 95 portions of polypropylene, 2 to 5 portions of resin fiber, 1 to 3 portions of glass fiber, 2 to 5 portions of compatilizer, 0.1 to 0.4 portion of alpha nucleating agent and 0 to 1 portion of other additives; the resin fiber is a polyamide fiber, and the retention length of the polyamide fiber in the polypropylene composite material is more than or equal to 0.4mm. According to the invention, the low-flow polypropylene is adopted, and the alpha nucleating agent is added to improve the crystallinity of the material, so that a stable alpha crystal form is formed, the tensile strength of the material is increased, and the anti-damage capability is improved; the polypropylene has high strength, toughness and shrinkage rate under the combined action of the glass fiber and the resin fiber, has physical properties equivalent to that of polyformaldehyde, and is low in cost.

Description

Polypropylene composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of polymer composite materials, in particular to a polypropylene composite material and a preparation method and application thereof.
Background
Polyoxymethylene (POM), also known as acetal resin, polyoxymethylene, and polyacetal, are thermoplastic crystalline high molecular polymers and are known as "super steel" or "stainless steel". The engineering plastic has excellent comprehensive performance, high mechanical performance, such as strength, modulus, wear resistance, toughness, fatigue resistance and creep resistance, excellent electric insulating property, solvent resistance and machinability, and wide application in electronic and electric products, automobile parts, industrial mechanical devices and other fields. However, the conventional polyoxymethylene resin is short in supply and expensive, and therefore, a substitute product having low cost and equivalent performance to polyoxymethylene is required.
The polypropylene (PP) and the polyformaldehyde belong to five general engineering plastics, and the polypropylene has the advantages of low finished product production, good comprehensive mechanical property, no toxicity, corrosion resistance, easiness in recovery and the like, and is widely applied to the fields of chemical industry, buildings, packaging, automobiles and the like.
Therefore, the polypropylene is modified to have the performance (including strength, modulus, toughness, shrinkage performance and the like) equivalent to that of polyformaldehyde, and can be used as a substitute of polyformaldehyde, so that the cost is reduced.
Disclosure of Invention
The invention aims to provide a polypropylene composite material with the performance equivalent to that of polyformaldehyde in order to solve the problems that the conventional polyformaldehyde is short in supply and low in price. According to the invention, the reinforced glass fiber and the specific resin fiber are added into the polypropylene matrix, so that the strength, modulus, toughness and shrinkage of the obtained polypropylene composite material are equivalent to those of polyformaldehyde.
The invention also aims to provide a preparation method of the polypropylene composite material.
The invention also aims to provide application of the polypropylene composite material in preparing electronic and electric appliances, automobile parts or industrial mechanical devices.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polypropylene composite material comprises the following components in parts by weight:
Figure BDA0004030104510000021
wherein the melt mass flow rate of the polypropylene at 230 ℃ under a load of 2.16kg is not more than 11g/10min;
the retention length of the polyamide fiber in the polypropylene composite material is more than or equal to 0.4mm.
The invention adopts low-flow polypropylene and adds alpha nucleating agent to improve the crystallinity of the material, form stable alpha crystal form, increase the tensile strength of the material and improve the anti-damage capability. The glass fiber is added to further improve the tensile strength of the polypropylene material, but the increase of the content of the glass fiber can also cause the toughness of the material to be reduced, the shrinkage rate to be reduced, and the strength and the shrinkage rate of the polyformaldehyde cannot be achieved. Therefore, the special resin fiber and the glass fiber are added to the polypropylene composite material to act together, so that the strength and toughness of the polypropylene can be improved simultaneously under the condition of a small amount of fiber addition, and the polypropylene can keep higher crystallinity and shrinkage rate equivalent to polyformaldehyde by adding a small amount of fiber. On one hand, the resin fiber has good compatibility with polypropylene, and is beneficial to maintaining and even further improving the toughness of the polypropylene; on the other hand, the resin fiber with a certain length is uniformly dispersed in the polypropylene, is isotropic, improves the tensile strength of the polypropylene together with the glass fiber, has good toughness and deformability compared with the glass fiber, has little influence on the shrinkage rate of the polypropylene material, and can not obviously reduce the shrinkage rate while improving the strength of the material.
The compatibility of the resin fiber and PP can be improved by controlling the melt mass flow rate of the polypropylene, so that the surface of the resin fiber has stronger bonding force with a PP base material, and the reinforcing effect of the resin fiber is exerted. Preferably, the melt mass flow rate of the polypropylene at 230 ℃ under a 2.16kg load is 0.25 to 10g/10min. Further preferably, the melt mass flow rate of the polypropylene at 230 ℃ under a 2.16kg load is 0.3 to 0.4g/10min. However, when the melt mass flow rate of polypropylene is too small, the resulting polypropylene composite has poor mechanical strength.
Preferably, the polyamide fibers have a retention length in the polypropylene composite of 0.4 to 3.5mm. Further preferably, the polyamide fibers have a retention length in the polypropylene composite of 1.4 to 3mm. The polyamide fibers are too short to function as a co-reinforcement; the polyamide fibers are too long, are unevenly dispersed in the matrix, are easy to agglomerate, and are easy to extend to the surface of the composite material to influence the appearance of the material.
Conventional polyamide resins, can be prepared into polyamide fibers for use in the present invention. Optionally, the polyamide resin in the polyamide fiber includes, but is not limited to, at least one of PA6, PA66, or PA 610. The invention researches and discovers that the performance of the polypropylene material modified by adding the PA6 fiber is closer to that of polyformaldehyde, and the modification effect is better.
Preferably, the glass fibers have a diameter of ≦ 13 μm, such as 4-8um, 8-10um, 10-13 um. Glass fibers in this diameter range have good dispersion in the polypropylene matrix.
Conventional alpha nucleating agents may be used in the present invention, including, but not limited to, aryl phosphate-based nucleating agents. Compared with beta nucleating agent, the alpha nucleating agent is more stable, so that the crystallization performance of the obtained polypropylene is more stable. The aryl phosphate nucleating agent comprises at least one of MP-6, NA-11 (sodium 2,2' -methylene bis (4, 6-di-tert-butylphenyl) phosphate) and NA-21.
In the present invention, the other additives are functional additives, and may be optionally added or not added as required. The other additives include, but are not limited to, at least one of an antioxidant, a light stabilizer, or a lubricant.
Optionally, the antioxidant is a hindered phenolic antioxidant and/or a phosphite antioxidant.
Alternatively, the light stabilizer includes, but is not limited to, at least one of a hindered amine light stabilizer or a benzotriazole light stabilizer.
The lubricant is a stearate lubricant.
The preparation method of the polypropylene composite material comprises the following steps:
according to the formula, polypropylene, polyamide fiber, glass fiber, compatilizer, alpha nucleating agent and other additives are mixed and then melt-extruded at 180-230 ℃ to obtain the polypropylene composite material.
Preferably, the mixing is carried out in a high speed mixer.
Preferably, the melt extrusion is carried out in a twin-screw extruder, the screw length-diameter ratio of the twin-screw extruder is (48-56) 1, and the screw rotating speed is 350-450 rpm.
The application of the polypropylene composite material in preparing electronic and electric appliances, automobile parts or industrial mechanical devices is also within the protection scope of the invention. Specifically, the polypropylene composite material is used for preparing automobile door plates, bumper supports, automobile columns, air inlet pipes, air pipe valves, drawer slide rails and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts low-flow polypropylene and adds alpha nucleating agent to improve the crystallinity of the material, form stable alpha crystal form, increase the tensile strength of the material and improve the anti-damage capability; the polypropylene has the advantages that the polypropylene has high strength, toughness and shrinkage rate simultaneously under the combined action of the glass fiber and the resin fiber, the physical properties of the polypropylene are equivalent to those of polyformaldehyde, and the cost is low.
The polypropylene composite material has tensile strength of 50-57 MPa, impact strength of 4.2-5.9 MPa and molding shrinkage of 0.17-0.20%, and is equivalent to polyformaldehyde in performance.
Detailed Description
The present invention will be further described with reference to specific examples for better illustrating the objects, technical solutions and advantages of the present invention, but the examples are not intended to limit the present invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. Unless otherwise indicated, reagents and materials used in the present invention are commercially available.
The following raw materials are selected in the embodiment of the invention:
polypropylene:
PP-1: PP B8101, available from Yanshan petrochemical, having a melt mass flow rate of 0.3g/10min at 230 ℃ under a 2.16kg load;
PP-2: PPB-1801, melt mass flow rate of 0.4g/10min at 230 ℃ under 2.16kg load, purchased from Yanshan petrochemical;
and (3) PP-3: k9010, a melt mass flow rate of 10g/10min at 230 ℃ under a 2.16kg load, purchased from Taiwan;
PP-4: PPR-4220S, available from Yanshan petrochemical, having a melt mass flow rate of 0.25g/10min at 230 ℃ under a 2.16kg load;
PP-5: PPH-MM20-S, with a melt mass flow rate of 22g/10min at 230 ℃ under a load of 2.16kg, purchased from the mesopetrochemical industry;
the melt mass flow rate of the polypropylene was measured according to the method of the standard ISO 1133-2-2011.
Resin fiber:
PA6 fiber: 840D-96F, purchased from Shenzhen Shenlixin material;
PA66 fiber: 15D-3MM, purchased from Shenzhen speciality new material;
polyester fiber: FX105, available from GRANITE;
carbon fiber: ST 600, purchased from guangzhou forest new material;
glass fiber:
glass fiber-1: e7CS10-03-508A, the diameter of the fiber is 10 μm, and the fiber is purchased from China poly-mineral glass fiber;
glass fiber-2: 249AF-10C 4MM, the diameter of the fiber is 10 mu m, and the fiber is purchased from Ohwenikong Ning;
maleic anhydride grafted polypropylene (MAH-g-PP): PC-1, a new polymer material purchased from south sea cypress morning of the mountain of Buddha;
aryl phosphate salt nucleating agent, NA-11, available from Aidic;
other additives:
antioxidant 1010: is sold on the market;
antioxidant 168: is sold on the market;
lubricant: calcium stearate, commercially available;
it should be noted that, in the present invention, the other additives (such as an antioxidant and a lubricant) described above are the same substance in the parallel test.
Examples 1 to 12
The embodiment of the invention provides a series of polypropylene composite materials, which are prepared by a preparation method comprising the following steps:
according to the formula in the table 1-2, polypropylene, resin fiber, glass fiber, compatilizer, alpha nucleating agent and other additives are added into a high-speed mixer, are uniformly mixed, and are fed into a double-screw extruder (the length-diameter ratio of a screw is 48: 1), the rotating speed of the screw is 350-450 rpm, and the polypropylene composite material is obtained by melt extrusion at 180-230 ℃ (wherein the temperatures of all areas from a machine head to a discharge port in the double-screw extruder are respectively 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃ and 230 ℃ in sequence from a feeding section to ten areas of the machine head.
TABLE 1 raw material formulation (parts by weight) of the polypropylene composites of examples 1 to 4
Figure BDA0004030104510000051
TABLE 2 raw material formulation (parts by weight) of the polypropylene composites of examples 5 to 12
Figure BDA0004030104510000061
As for the retention length of the resin fiber in the composite material of the present invention, it should be noted that the purchased resin fiber, which is originally a long fiber, needs to be cut into a predetermined length at the time of use and then added to the composite material, but the fiber length is reduced by the screw shearing of the twin-screw extruder during the processing, and therefore, in the present invention, the retention length of the resin fiber in the composite material is an average retention length calculated by observing the product under a microscope.
Comparative example 1
This comparative example provides a polypropylene composite prepared according to the method of example 1, except that the polypropylene was replaced with PP-5 having a higher melt mass flow rate than example 1.
Comparative example 2
This comparative example provides a polypropylene composite material prepared according to the method of example 1, differing from example 1 in that 3 parts of glass fiber are replaced by 3 parts of polyamide fiber PA6, and the other raw materials are unchanged, i.e. only polyamide fiber is added, and no glass fiber is added.
Comparative example 3
This comparative example provides a polypropylene composite material prepared according to the method of example 1, differing from example 1 in that 4 parts of polyamide fiber PA6 are replaced by 4 parts of glass fiber-1, and the other raw materials are unchanged, i.e. only glass fiber is added, and no resin fiber is added.
Comparative example 4
This comparative example provides a polypropylene composite material prepared according to the preparation method of example 1, which differs from example 1 in that polyamide fiber PA6 is replaced with polyester fiber in equal amounts.
Comparative example 5
This comparative example provides a polypropylene composite material prepared according to the preparation method of example 1, differing from example 1 in that the polyamide fiber PA6 is replaced with carbon fiber in equal amounts.
Comparative example 6
This comparative example provides a polypropylene composite material prepared according to the preparation method of example 1, differing from example 1 in that the retention length of the resin fiber in the composite material is 0.3mm.
Comparative example 7
This comparative example provides a polypropylene composite prepared according to the preparation method of example 1, which differs from example 1 in that the α nucleating agent is replaced by a β nucleating agent (TMB-5, available from chemical research institute, shanxi province).
Comparative example 8
This comparative example provides a polypropylene composite, prepared according to the method of preparation of example 1, differing from example 1 in that the PA6 fibers are replaced by a PA6 resin (PA 6 VOLGAMID28, available from cupbyshev).
Performance testing
The properties of the polypropylene composite materials obtained in the above examples and comparative examples and polyoxymethylene (M90-44, available from precious plastics) were characterized, and specific test items, test methods and results were as follows:
1. tensile strength (MPa): the composite material was injection molded into tensile bars (type IB), tested according to the method in standard ISO527-1-2010, and drawn at 50mm/min at room temperature (25 ℃), the test results detailed in table 3;
2. bending property: the composite material is injection molded into an impact sample strip, the flexural modulus (MPa) is tested by referring to a method in the ISO178-2011 standard, and the test result is detailed in a table 3;
3. toughness: the composite material is injection molded into an impact sample strip, the test is carried out according to the method in the standard ISO179-2010, the notch type of the sample strip is A type, and the notch impact strength (kJ/m) of the composite material is tested by adopting a Zwick HIT5.5P electronic display impact tester 2 ) The test results are detailed in table 3;
4. molding shrinkage rate: the composite material is subjected to injection molding by using a square plate mold of 80X 220X 2mm, and then is subjected to standing molding at the temperature of 23 ℃ and the relative humidity of 50 percentAnd after 48h, measuring the difference between the size of the molded rear plate and the size of the mold, and calculating the molding shrinkage rate (%), wherein the molding shrinkage rate in the invention is the average value of the transverse shrinkage rate and the longitudinal shrinkage rate, and the transverse shrinkage rate is calculated according to the following formula: transverse shrinkage (%) = | a t -a 0 ∣/a 0 *100% of them, a t To a post-formation length, a 0 Is the length of the mold; the longitudinal shrinkage rate is a shrinkage rate in the width direction, and its calculation formula is similar to that of the transverse shrinkage rate.
The test results are detailed in table 3.
Table 3 results of performance testing
Performance of Tensile strength Flexural modulus Notched impact strength Shrinkage ratio/%
Example 1 53 2715 4.9 0.2
Example 2 56 2688 4.5 0.18
Example 3 51 2523 5.1 0.2
Example 4 50 2510 5.7 0.2
Example 5 54 2762 5 0.17
Example 6 50 2522 5.9 0.17
Example 7 51 2656 4.8 0.18
Example 8 57 2776 5.2 0.18
Example 9 53 2630 4.2 0.19
Example 10 50 2552 4.6 0.19
Example 11 51 2681 5 0.19
Example 12 50 2643 4.8 0.2
Comparative example 1 48 2480 4.3 0.13
Comparative example 2 42 2250 4.5 0.21
Comparative example 3 57 2920 4.6 0.1
Comparative example 4 41 2289 4.3 0.19
Comparative example 5 50 2589 4.3 0.14
Comparative example 6 44 2320 4.5 0.19
Comparative example 7 45 2358 4.4 0.22
Comparative example 8 42 2253 4.6 0.14
Polyoxymethylene 60 2600 6 0.21
From the above results, it can be seen that:
the physical properties of the polypropylene composite material prepared by the embodiments of the invention are equivalent to that of polyformaldehyde, and the polypropylene composite material can be used as a substitute of polyformaldehyde in related application fields, so that the production cost is reduced.
The results of examples 1 to 4 show that the mechanical properties and molding shrinkage of the resulting polypropylene composite are closer to those of polyoxymethylene within the above-mentioned amount range of the present invention.
The results of examples 1, 5 to 6, example 12 and comparative example 1 show that the impregnation effect of the polypropylene molecular chain around the resin fiber and the adhesion effect of the resin fiber and the PP molecule can be improved by controlling the melt mass flow rate of the polypropylene, so that the adhesion between the surface of the resin fiber and the PP base material is stronger, and the reinforcing effect of the resin fiber is exerted. If the flow rate of polypropylene is too large (as in comparative example 1), the filling saturation of polypropylene with the same volume in the filler is higher, so that the shrinkage rate of the obtained polypropylene composite material product is obviously reduced, and the shrinkage rate of the polypropylene composite material product is greatly different from that of polyformaldehyde, so that the polypropylene composite material cannot be applied to products instead of polyformaldehyde.
The results of example 1, examples 7 to 9, and comparative example 6 show that the mechanical strength (e.g., tensile strength) of the polypropylene composite material prepared shows a tendency to increase first and then decrease as the remaining length (in the resin matrix) of the resin fiber increases. The polyamide fibers are too short in length (as in comparative example 6) to act as co-reinforcement; the polyamide fiber is too long, the dispersion in the matrix is gradually poor, and the agglomeration is easy to occur, so that the strength of the prepared polypropylene composite material is in a descending trend; and also easily extend to the surface of the composite material, affecting the appearance of the material.
The results of example 1 and examples 10 to 11 show that, within the selection range of suitable polyamide fibers and glass fibers of the present invention, polypropylene composites having properties similar to polyoxymethylene can be obtained; in particular, the polypropylene material obtained by using the PA6 fiber has the performance closer to that of polyformaldehyde, and has better modification effect.
The results of comparative examples 2 to 7 and example 1 show that the polyamide resin fiber can enhance the mechanical strength and the molding shrinkage of polypropylene together with the glass fiber, and for example, the mechanical strength and the molding shrinkage of the obtained polypropylene composite material cannot reach the same level as that of the polyformaldehyde resin at the same time by replacing the polyamide fiber with other resin fibers and only adding or not adding the polyamide fiber.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The polypropylene composite material is characterized by comprising the following components in parts by weight:
Figure FDA0004030104500000011
wherein the melt mass flow rate of the polypropylene at 230 ℃ under a 2.16kg load is not more than 11g/10min;
the retention length of the polyamide fiber in the polypropylene composite material is more than or equal to 0.4mm.
2. The polypropylene composite of claim 1, wherein the polypropylene has a melt mass flow rate of 0.3 to 0.4g/10min at 230 ℃ under a load of 2.16 kg.
3. The polypropylene composite of claim 1, wherein the polyamide fiber has a retained length in the polypropylene composite of 1.4 to 3mm.
4. The polypropylene composite of claim 1, wherein the polyamide in the polyamide fibers is at least one of PA6, PA66 or PA 610.
5. The polypropylene composite of claim 1, wherein the glass fibers have a diameter of 13 μm or less.
6. The polypropylene composite of claim 1, wherein the alpha nucleating agent is an aryl phosphate salt based nucleating agent.
7. The polypropylene composite of claim 1, wherein the compatibilizer is maleic anhydride grafted polypropylene.
8. The polypropylene composite of claim 1, wherein the other additives comprise at least one of an antioxidant, a light stabilizer, or a lubricant.
9. A process for the preparation of a polypropylene composite according to any one of claims 1 to 8, comprising the steps of:
the polypropylene, the polyamide fiber, the glass fiber, the compatilizer, the alpha nucleating agent and other additives are mixed according to the formula and then are melted and extruded at 180-230 ℃, and the polypropylene composite material is obtained.
10. Use of the polypropylene composite according to any one of claims 1 to 8 for the preparation of electronic appliances, automotive parts or industrial mechanical devices.
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