CN113583382A - High-temperature-resistant and wear-resistant PEEK profile composite material and preparation method thereof - Google Patents

High-temperature-resistant and wear-resistant PEEK profile composite material and preparation method thereof Download PDF

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Publication number
CN113583382A
CN113583382A CN202111082783.9A CN202111082783A CN113583382A CN 113583382 A CN113583382 A CN 113583382A CN 202111082783 A CN202111082783 A CN 202111082783A CN 113583382 A CN113583382 A CN 113583382A
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peek
resistant
parts
micro powder
temperature
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乔金龙
何建
张洪结
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Nanjing Shousu Special Engineering Plastics Products Co ltd
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Nanjing Shousu Special Engineering Plastics Products Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/16Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a high-temperature-resistant and wear-resistant PEEK profile composite material and a preparation method thereof, relating to the technical field of composite materials, and the composite material comprises the following components in parts by weight: 65-85 parts of PEEK base material, 3-10 parts of polydiphenyl ether derivative coating, 8-12 parts of carbon fiber micro powder and 7-10 parts of glass fiber micro powder, and the preparation method comprises the following steps: firstly, the PEEK material is pretreated, then carbon fiber and glass fiber are prepared into dispersion liquid, then the PEEK and the dispersion liquid are mixed, and finally the mixture is extruded and injected. The invention relates to a high-temperature-resistant and wear-resistant PEEK profile composite material and a preparation method thereof.

Description

High-temperature-resistant and wear-resistant PEEK profile composite material and preparation method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a high-temperature-resistant and wear-resistant PEEK profile composite material and a preparation method thereof.
Background
PEEK (polyether ether ketone), which is a linear aromatic polymer compound containing chain segments in the molecular main chain. The constituent unit is oxygen-p-phenylene-oxygen-carbonyl-p-phenylene, and the thermoplastic material is semi-crystalline. The section bar has the outstanding characteristic advantages of high temperature resistance, wear resistance, hydrolysis resistance, chemical corrosion resistance, high strength, self lubrication and the like. Therefore, the section bar also has good machining performance, can be milled, turned, ground and carved, can also be ultrasonically welded, and has rigidity and toughness. The processing requirements can be met by using common machining equipment, so the method is widely applied to the fields of aerospace, automobiles, electronics and electrical, medical treatment, food processing and the like, and has a wide development and utilization prospect.
At present, most of PEEK (polyetheretherketone) materials are prepared by adding 30% of glass fiber reinforced materials or 30% of carbon fiber reinforced materials, but because the compatibility between the glass fiber or the carbon fiber and the PEEK is poor, the mechanical strength for reinforcing the PEEK is limited, the high temperature resistance and the wear resistance are also limited, and the corrosion resistance of the PEEK cannot meet the requirements of certain special fields, and the PEEK (polyetheretherketone) materials are required to be processed.
Disclosure of Invention
The invention mainly aims to provide a high-temperature-resistant and wear-resistant PEEK profile composite material and a preparation method thereof, which can effectively solve the problem that the corrosion resistance of PEEK in the background art cannot meet the requirements of some special fields.
In order to achieve the purpose, the invention adopts the technical scheme that: a high-temperature-resistant and wear-resistant PEEK profile composite material and a preparation method thereof comprise the following components in parts by weight: 65-85 parts of PEEK base material, 3-10 parts of polydiphenyl ether derivative coating, 8-12 parts of carbon fiber micro powder and 7-10 parts of glass fiber micro powder.
Preferably, the preparation method of the carbon fiber micro powder comprises the following steps:
a1, dissolving 15-25% of sodium polystyrene sulfonate in cyclohexanone according to parts by weight to form a saturated mixed solution;
a2, adding 8-12% of carbon fibers into the mixed solution for soaking, taking out the carbon fibers after soaking, and drying to obtain the carbon fibers;
a3, grinding the prepared carbon fiber into carbon fiber micro powder.
Preferably, the soaking time in the step A2 of the preparation method of the carbon fiber micro powder is 1-2 hours; the drying temperature is 60-80 ℃; the drying time is 1-3 hours.
Preferably, the carbon fiber fine powder has a particle size of 0.02 to 0.10 μm.
Preferably, the preparation method of the glass fiber micropowder comprises the following steps:
b1, adding 10-15% of cyclodextrin, 60-80% of cyclohexane, 2-4% of MDI and 30-40% of glass fiber into a reaction kettle according to parts by weight, and reacting for 2-3 hours at 60-70 ℃;
b2, conveying the reacted liquid to a rotary evaporator to remove the solvent, and then drying to obtain glass fiber;
and B3, grinding the prepared glass fiber into glass fiber micropowder.
Preferably, the drying temperature of the step B2 in the preparation method of the glass fiber micropowder is 50-60 ℃; the drying time is 1-2 hours.
Preferably, the glass fiber fine powder has a particle size of 0.01 to 0.04 μm.
Preferably, the method comprises the following steps:
s1, PEEK material pretreatment: uniformly spraying a polydiphenyl ether derivative coating on the surface of the PEEK granules;
s2, preparation of dispersion: adding carbon fiber micro powder and glass fiber micro powder into ethanol in proportion, performing ball milling, and performing ultrasonic dispersion to prepare dispersion liquid;
s3, mixing materials: adding PEEK granules into the dispersion liquid, heating and stirring to volatilize ethanol, and obtaining mixed powder;
s4, extrusion injection molding: and (3) carrying out melt extrusion and injection molding on the dried mixed material by using a double-cone screw machine and a micro injection molding machine.
Preferably, the specific operation of step S1 is: putting the polydiphenyl ether derivative coating into a spray gun hopper, controlling the pressure of the spray gun to be 0.5MPa, controlling the distance between a spray nozzle and the surface of the granules to be 8-10 cm, and after the spraying is finished, placing the granules in the air to naturally volatilize for 20 min; then putting the mixture into a 160 ℃ oven, and preserving the heat for 40 min; then taking out the product from the oven, and naturally cooling the product at room temperature; then carrying out secondary spraying, and naturally volatilizing for 20 min; then putting the mixture into a 160 ℃ oven, and preserving heat for 3 min; then heating to 200 ℃, and preserving heat for 1.5 min; taking out from the oven, and naturally cooling at room temperature.
Preferably, the parameters of the double-cone screw machine in the step S4 are set as follows: the temperature of the upper cavity plate is 350-400 ℃, the temperature of the lower cavity plate is 350-400 ℃, the rotating speed is 40-300 r/min, the feeding amount is 5-10 g/time, and the self-circulation time is 1-5 min; the parameters of the micro-injection molding machine are set as follows: the temperature of the charging barrel is 345-395 ℃, the temperature of the die is 30-120 ℃, and the pressure maintaining time is 5-20 s.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the PEEK is compounded by adding materials such as carbon fiber micro powder, glass fiber micro powder, polydiphenyl ether derivative coating and the like, wherein the carbon fiber micro powder and the glass fiber micro powder can ensure that the heat resistance and the toughness of the composite material are not reduced compared with the existing composite material, the polydiphenyl ether derivative coating can enable the composite material to be stored in 60% sulfuric acid or 40% sodium hydroxide for 30 days, and no change is observed on the composite material, which indicates that the composite material has strong corrosion resistance.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
A high-temperature-resistant wear-resistant PEEK profile composite material comprises the following components in parts by weight: 65-85 parts of PEEK base material, 10 parts of polydiphenyl ether derivative coating, 8 parts of carbon fiber micro powder and 7 parts of glass fiber micro powder.
The preparation method of the carbon fiber micro powder comprises the following steps:
a1, dissolving 15% sodium polystyrene sulfonate in cyclohexanone according to weight ratio to form saturated mixed solution;
a2, adding 9% of carbon fiber into the mixed solution, soaking for 1 hour, taking out the carbon fiber after soaking, and drying for 2 hours at 60 ℃ to obtain the carbon fiber;
a3, grinding the prepared carbon fiber into carbon fiber micro powder.
The preparation method of the glass fiber micro powder comprises the following steps:
b1, adding 10% of cyclodextrin, 60% of cyclohexane, 2% of MDI and 30% of glass fiber into a reaction kettle according to the weight ratio, and reacting for 2 hours at 60 ℃;
b2, conveying the reacted liquid to a rotary evaporator to remove the solvent, and then drying the liquid at 50 ℃ for 1 hour to obtain glass fiber;
and B3, grinding the prepared glass fiber into glass fiber micropowder.
The preparation method of the high-temperature-resistant and wear-resistant PEEK profile composite material is characterized by comprising the following steps of: the method comprises the following steps:
s1, placing the polydiphenyl ether derivative coating into a spray gun hopper, controlling the pressure of the spray gun to be 0.5MPa, controlling the distance between a spray nozzle and the surface of the granules to be 8-10 cm, and after spraying, placing the granules in the air to naturally volatilize for 20 min; then putting the mixture into a 160 ℃ oven, and preserving the heat for 40 min; then taking out the product from the oven, and naturally cooling the product at room temperature; then carrying out secondary spraying, and naturally volatilizing for 20 min; then putting the mixture into a 160 ℃ oven, and preserving heat for 3 min; then heating to 200 ℃, and preserving heat for 1.5 min; taking out the product from the oven, and naturally cooling the product at room temperature;
s2, adding the carbon fiber micro powder and the glass fiber micro powder into ethanol in proportion, and performing ultrasonic dispersion after ball milling to prepare dispersion liquid;
s3, mixing materials: adding PEEK granules into the dispersion liquid, heating and stirring to volatilize ethanol, and obtaining mixed powder;
s4, extrusion injection molding: using a double-cone screw machine and a micro injection molding machine to perform melt extrusion and injection molding on the dried mixed material, wherein the parameters of the double-cone screw machine are set as follows: the temperature of the upper cavity plate is 350-400 ℃, the temperature of the lower cavity plate is 350-400 ℃, the rotating speed is 40-300 r/min, the feeding amount is 5-10 g/time, and the self-circulation time is 1-5 min; the parameters of the micro-injection molding machine are set as follows: the temperature of the charging barrel is 345-395 ℃, the temperature of the die is 30-120 ℃, and the pressure maintaining time is 5-20 s.
Example 2
Example 2 is different from example 1 in that 75 parts by weight of PEEK base material, 7 parts by weight of diphenyl ether derivative coating, 10 parts by weight of carbon fiber fine powder, and 8 parts by weight of glass fiber fine powder are different from each other.
Example 3
Example 3 is different from example 1 in that 75 parts by weight of PEEK base material, 3 parts by weight of diphenyl ether derivative coating, 12 parts by weight of carbon fiber fine powder, and 10 parts by weight of glass fiber fine powder are different from each other.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that the PEEK base material is 85 parts, the polydiphenyl ether derivative coating is 0 part, the carbon fiber micro powder is 8 parts, and the glass fiber micro powder is 7 parts.
Comparative example 2
The comparative example 2 is different from the example 1 in the parts by weight of the components, namely 65 parts of PEEK base material, 13 parts of polydiphenyl ether derivative coating, 8 parts of carbon fiber micro powder and 7 parts of glass fiber micro powder.
TABLE 1 PEEK COMPOSITE MATERIAL PERFORMANCE TEST RESULTS
Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
PEEK base material weight portion ratio 75 75 75 85 65
Coating of poly diphenyl ether derivative in weight portion 10 7 3 0 13
Modified carbon fiber micropowder 8 10 12 8 8
Modified glass fiber micropowder 7 8 10 7 7
Impact Strength/kN.m 19.32 19.61 19.27 18.42 17.37
Heat resistance (280 ℃, 100h) Without change Without change Without change Without change There is a change in
Acid resistance (60% sulfuric acid, 30d) Without change Without change Without change There is a change in Without change
Acid resistance (20% sulfuric acid/, 30d) Without change Without change Without change Without change Without change
Alkali resistance (40% NaOH, 30d) Without change Without change Without change There is a change in Without change
As can be seen from the results shown in table 1 above, method examples 1 to 3 according to the present invention have no change in the condition of 250 c for 100 hours, good heat resistance, and good acid and alkali resistance compared to before the test.
As can be seen from the results shown in table 1 above, comparative example 1, in which the coating of the diphenyl ether derivative was not added, had poor acid resistance although it had good heat resistance and alkali resistance, whereas comparative example 2, in which the coating of the diphenyl ether derivative was added in a large amount, resulted in a decrease in heat resistance.
In conclusion, the corrosion resistance of the composite material is remarkably improved, the composite material has no obvious change after being placed for 100 hours at 280 ℃, the heat resistance is very good,
the foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. The utility model provides a high temperature resistant, wear-resisting type PEEK section bar combined material which characterized in that: comprises the following components in parts by weight: 65-85 parts of PEEK base material, 3-10 parts of polydiphenyl ether derivative coating, 8-12 parts of carbon fiber micro powder and 7-10 parts of glass fiber micro powder.
2. The high temperature resistant, wear resistant PEEK profile composite of claim 1, wherein: the preparation method of the carbon fiber micro powder comprises the following steps:
a1, dissolving 15-25% of sodium polystyrene sulfonate in cyclohexanone according to parts by weight to form a saturated mixed solution;
a2, adding 8-12% of carbon fibers into the mixed solution for soaking, taking out the carbon fibers after soaking, and drying to obtain the carbon fibers;
a3, grinding the prepared carbon fiber into carbon fiber micro powder.
3. The high temperature resistant, wear resistant PEEK profile composite of claim 2, wherein: the soaking time in the step A2 of the preparation method of the carbon fiber micro powder is 1-2 hours; the drying temperature is 60-80 ℃; the drying time is 1-3 hours.
4. A high temperature resistant, wear resistant PEEK profile composite as claimed in claim 3, wherein: the particle size of the carbon fiber micro powder is 0.02-0.10 μm.
5. The high temperature resistant, wear resistant PEEK profile composite of claim 1, wherein: the preparation method of the glass fiber micro powder comprises the following steps:
b1, adding 10-15% of cyclodextrin, 60-80% of cyclohexane, 2-4% of MDI and 30-40% of glass fiber into a reaction kettle according to parts by weight, and reacting for 2-3 hours at the temperature of 60-70 ℃;
b2, conveying the reacted liquid to a rotary evaporator to remove the solvent, and then drying to obtain glass fiber;
and B3, grinding the prepared glass fiber into glass fiber micropowder.
6. The high temperature resistant, wear resistant PEEK profile composite of claim 5, wherein: the drying temperature of the step B2 in the preparation method of the glass fiber micro powder is 50-60 ℃; the drying time is 1-2 hours.
7. The high temperature resistant, wear resistant PEEK profile composite of claim 6, wherein: the grain diameter of the glass fiber micro powder is 0.01-0.04 mu m.
8. The method for preparing a high temperature resistant, wear resistant PEEK profile composite material according to any one of claims 1-7, wherein: the method comprises the following steps:
s1, PEEK material pretreatment: uniformly spraying a polydiphenyl ether derivative coating on the surface of the PEEK granules;
s2, preparation of dispersion: adding carbon fiber micro powder and glass fiber micro powder into ethanol in proportion, performing ball milling, and performing ultrasonic dispersion to prepare dispersion liquid;
s3, mixing materials: adding PEEK granules into the dispersion liquid, heating and stirring to volatilize ethanol, and obtaining mixed powder;
s4, extrusion injection molding: and (3) carrying out melt extrusion and injection molding on the dried mixed material by using a double-cone screw machine and a micro injection molding machine.
9. The method for preparing the high-temperature-resistant wear-resistant PEEK profile composite material as claimed in claim 8, wherein the method comprises the following steps: the specific operation of step S1 is: putting the polydiphenyl ether derivative coating into a spray gun hopper, controlling the pressure of the spray gun to be 0.5MPa, controlling the distance between a spray nozzle and the surface of the granules to be 8-10 cm, and after spraying, naturally volatilizing in the air for 20 min; then putting the mixture into a 160 ℃ oven, and preserving the heat for 40 min; then taking out the product from the oven, and naturally cooling the product at room temperature; then carrying out secondary spraying, and naturally volatilizing for 20 min; then putting the mixture into a 160 ℃ oven, and preserving heat for 3 min; then heating to 200 ℃, and preserving heat for 1.5 min; taking out from the oven, and naturally cooling at room temperature.
10. The method for preparing the high-temperature-resistant wear-resistant PEEK profile composite material as claimed in claim 8, wherein the method comprises the following steps: the parameters of the double-cone screw machine in the step S4 are set as follows: the temperature of the upper cavity plate is 350-400 ℃, the temperature of the lower cavity plate is 350-400 ℃, the rotating speed is 40-300 r/min, the feeding amount is 5-10 g/time, and the self-circulation time is 1-5 min; the parameters of the micro-injection molding machine are set as follows: the temperature of the charging barrel is 345-395 ℃, the temperature of the die is 30-120 ℃, and the pressure maintaining time is 5-20 s.
CN202111082783.9A 2021-09-15 2021-09-15 High-temperature-resistant and wear-resistant PEEK profile composite material and preparation method thereof Pending CN113583382A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114133697A (en) * 2021-11-30 2022-03-04 江苏亨博复合材料有限公司 PEEK material with high wear resistance and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105602190A (en) * 2016-02-03 2016-05-25 黑龙江鑫达企业集团有限公司 Friction-resistant PEEK (polyetheretherketone) composite material and preparation method thereof
CN112646314A (en) * 2020-12-21 2021-04-13 江苏君华特种工程塑料制品有限公司 High-temperature-resistant and wear-resistant PEEK matrix composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105602190A (en) * 2016-02-03 2016-05-25 黑龙江鑫达企业集团有限公司 Friction-resistant PEEK (polyetheretherketone) composite material and preparation method thereof
CN112646314A (en) * 2020-12-21 2021-04-13 江苏君华特种工程塑料制品有限公司 High-temperature-resistant and wear-resistant PEEK matrix composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114133697A (en) * 2021-11-30 2022-03-04 江苏亨博复合材料有限公司 PEEK material with high wear resistance and preparation method thereof

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