CN112175347A - High-performance composite modified material and preparation process thereof - Google Patents

High-performance composite modified material and preparation process thereof Download PDF

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CN112175347A
CN112175347A CN202010843840.XA CN202010843840A CN112175347A CN 112175347 A CN112175347 A CN 112175347A CN 202010843840 A CN202010843840 A CN 202010843840A CN 112175347 A CN112175347 A CN 112175347A
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parts
stirring
reaction
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reaction cavity
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许建勇
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Ningbo Jutaiyuan Polymer Material Co ltd
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Ningbo Jutaiyuan Polymer Material 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0812Aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/262Alkali metal carbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009Sulfides
    • 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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Abstract

The invention discloses a high-performance composite modified material and a preparation process thereof, wherein the preparation process comprises the following steps: preparing raw materials; adding water, polyether-ether-ketone and diphenyl sulfone into the reaction cavity, and heating the reaction cavity after the reaction cavity is in a vacuum environment; adding molybdenum disulfide and graphite into a reaction cavity and stirring; adding a toughening agent into the reaction cavity and stirring; adding aluminum powder into the reaction cavity and stirring; after stirring, adding sodium carbonate into the reaction cavity; cooling to room temperature to obtain a finished material; the equipment of the preparation process comprises a reaction box, a feeding pipe, a heating group, a ceramic plate, a vacuum pump, a motor, a stirring assembly, a discharging pipe, a discharging valve, a temperature sensor, a nitrogen pipe and a switch group. The invention improves the mechanical stability, self-lubricating property, toughness, bearing strength and high and low temperature resistance of the material by adding various raw materials; the preparation process realizes the preparation effect of heating, temperature rising and stirring the added raw materials and integration, achieves the reaction condition more quickly, improves the preparation effect, is simple to operate and meets the requirement of the preparation process.

Description

High-performance composite modified material and preparation process thereof
Technical Field
The invention relates to the technical field of composite modified materials, in particular to a high-performance composite modified material and a preparation process thereof.
Background
The composite material is a material with new performance formed by two or more than two materials with different properties through a physical or chemical method on a macroscopic (microscopic) scale. The materials mutually make up for the deficiencies in performance to generate a synergistic effect, so that the comprehensive performance of the composite material is superior to that of the original composition material to meet various different requirements. The polyether ether ketone (PEEK) resin is a high polymer formed by repeating units containing one ketone bond and two ether bonds in a main chain structure, and belongs to a special high polymer composite material. The high-temperature-resistant composite material has physical and chemical properties such as high temperature resistance and chemical corrosion resistance, is a special engineering plastic with excellent performance, has more remarkable advantages compared with other special engineering plastics, can be used for high-end science and technology such as machinery, nuclear engineering and aviation, can be used as a high-temperature-resistant structural material and an electrical insulating material, and can be compounded with glass fibers or carbon fibers to prepare a reinforcing material. The material has a great deal of application in the aerospace field, the medical appliance field (as an artificial bone for repairing bone defects) and the industrial field.
However, the existing polyetheretherketone material still has the problems of poor mechanical stability and pressure resistance, poor lubricity due to high viscosity of the material, low toughness and bearing strength of the material, poor sealing effect due to low density, short service life and poor performance due to insufficient high-temperature and low-temperature resistance; the existing preparation process of polyether-ether-ketone is not beneficial to the preparation of the whole process, has complex operation, does not have excellent heating and stirring and integrated preparation effects, does not have the accident that a protective structure is easy to generate high-temperature scald, causes the speed of reaching reaction conditions to slowly reduce the preparation efficiency, does not meet the preparation requirements of the process, and directly influences the performance of the prepared material.
Disclosure of Invention
Aiming at the existing polyether-ether-ketone material and the preparation process, the molybdenum disulfide and graphite are added into the material, so that the mechanical stability and pressure resistance of the material are improved, and the self-lubricating property of the material is improved; the toughening agent is added, so that the toughness and the bearing strength of the material are improved, and the density of the material is improved, so that the sealing effect of the material is better; aluminum powder is added, so that the high-temperature resistance and low-temperature resistance of the material are improved; the sodium carbonate is added, so that the reaction time of the raw materials is effectively shortened, and the preparation efficiency is improved; the heating, temperature rising and stirring of the added raw materials and the integrated preparation effect are realized by setting the preparation process equipment, so that the reaction conditions are reached more quickly, the preparation effect is improved greatly, the operation is simple, and the preparation process requirements are met.
In order to achieve the purpose, the invention provides the following technical scheme: a high-performance composite modified material is prepared from the following raw materials in parts by weight: 200 parts of 150-one water, 70-90 parts of polyether-ether-ketone, 60-80 parts of diphenyl sulfone, 30-50 parts of molybdenum disulfide, 30-50 parts of graphite, 10-20 parts of a toughening agent, 20-30 parts of aluminum powder and 15-30 parts of sodium carbonate.
A high-performance composite modified material is composed of the following raw materials in parts by weight: 170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium carbonate.
The molybdenum disulfide adopts PA66 glass fiber reinforced molybdenum disulfide; the graphite is prepared from lubricating graphite powder with a Lutang brand of 659823.
The toughening agent adopts HZ-403 universal ABS toughening agent, the appearance of the adopted toughening agent is granular, and the content of effective substances is 98%.
The aluminum powder is fine aluminum powder with the trade mark of FLX1, and the granularity of the aluminum powder is 0.35-0; the sodium carbonate adopts AR type anhydrous pure sodium carbonate powder.
The utility model provides a preparation equipment of high performance composite modified material preparation technology, includes the reaction box, the inlet pipe, heats the group, and the ceramic plate, the vacuum pump, the motor, the stirring subassembly, the discharging pipe, the bleeder valve, temperature sensor, nitrogen gas pipe and switch block, wherein: the bottom of the reaction box is in a conical shape, the interior of the reaction box forms a reaction cavity, the upper side part of the reaction box is provided with a feeding pipe, and a pipe cover is arranged on the feeding pipe in a threaded manner; the two sides of the bottom of the reaction box are respectively fixed with a base, the side part of the reaction box is provided with a heating group through screws, the inner side of the heating group is contacted with a ceramic plate, and the ceramic plate is integrally arranged on the side wall of the reaction box; the vacuum pump is arranged on one side of the upper part of the reaction box through a bolt, the upper middle part of the reaction box is provided with a motor through a bolt, the working part of the motor is provided with a stirring component, and the stirring component is positioned in the reaction cavity; the discharge pipe is arranged at the bottom of the reaction box, one end of the discharge pipe is communicated with the reaction cavity, and the other end of the discharge pipe is provided with a discharge valve and is positioned outside the reaction box; the temperature sensor and the switch group are sequentially arranged on the other side of the upper part of the reaction box through screws, wherein the sensing part of the temperature sensor is arranged on the inner upper wall of the reaction box and is positioned in the reaction cavity; the nitrogen pipe is arranged at the other upper side part of the reaction box, one end of the nitrogen pipe is communicated with the reaction cavity in the reaction box, and the other end of the nitrogen pipe is externally connected with a nitrogen bottle;
the switch group is including heating switch, vacuum switch, speed governing switch and ejection of compact switch, wherein: the heating switch, the vacuum switch, the speed regulation switch and the discharging switch are respectively connected with an external proper power supply through four groups of power lines and are sequentially arranged on the body of the switch group; the heating switch is a common start-stop switch and is respectively connected with a temperature sensor and an electric heating plate through two groups of power lines, wherein the temperature sensor adopts a 9120 type high-precision temperature sensor capable of displaying by a large-screen LED, and the electric heating plate adopts an HT-200 type ceramic electric heating plate; the vacuum switch is a common start-stop switch and is connected with a vacuum pump through a power line, and the vacuum pump adopts an RS-3 type electric small vacuum pump; the speed regulating switch adopts a HW-A-1040 speed regulator switch, and the speed regulating switch is connected with a motor through a power line, and the motor adopts a small motor with the model ZY 77-10-129; the discharging switch is a common start-stop switch and is connected with a discharging valve through a power line, and the discharging valve adopts a DF-50F type large-diameter flange electromagnetic valve.
The heating groups are provided with two heating groups which are same in structure arrangement, the two heating groups are respectively arranged at two side parts of the reaction box in a mirror image manner, and ceramic plates are respectively integrally arranged at the two side parts of the reaction box; the heating group includes protection casing and electric plate, wherein: the protective cover is made of asbestos materials and is fixed on the side part of the reaction box through screws and positioned on one side of the ceramic plate; the electric plate passes through the internally mounted of bolt and protection casing, and the working position of electric plate and ceramic plate contact setting, realizes the heating effect of rising the temperature to the heating that adds the raw materials to reach the condition of reaction, and rate of heating is fast, and reliable and stable, have protective structure simultaneously and improve the security, be difficult for receiving external damage, and prevent that the staff is scalded in the high temperature accident.
The stirring subassembly includes the pivot, stirs the leaf and promotes the leaf, wherein: the rotating shaft is installed with the working part of the motor through a bearing, three groups of stirring blades are sequentially welded on the rotating shaft from top to bottom, and each group of the stirring blades is provided with two stirring blades; promote the leaf and be two sets of, and promote the leaf and be the welding of fan blade form on the stirring leaf of bottommost, realize increasing substantially the speed of reaction in the effect of an organic whole to the stirring effect of interpolation raw materials, with the cooperation of heating group realization heating stirring, and the setting up of promotion leaf makes whole stirring more even, satisfies the needs of design.
A preparation process of a high-performance composite modified material comprises the following steps:
preparing raw materials: selecting the prepared raw materials, specifically: 170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium carbonate;
adding 170 parts of water, 85 parts of polyether-ether-ketone and 70 parts of diphenyl sulfone into a reaction cavity, vacuumizing, heating after the reaction cavity is in a vacuum environment, and stopping heating after the temperature reaches 60 ℃;
thirdly, adding 45 parts of molybdenum disulfide and 45 parts of graphite into the reaction chamber, and stirring for 10-15min at the rotating speed of 600 plus materials and 800 r/min;
adding 17 parts of toughening agent into the reaction cavity, and stirring for 30-35min at the rotating speed of 700-900 r/min;
adding 28 parts of aluminum powder into the reaction cavity, and stirring for 30-40min at the rotating speed of 1200-1300 r/min;
sixthly, after the stirring is finished, adding 27 parts of sodium carbonate into the reaction cavity, vacuumizing again, introducing nitrogen, starting to heat to 100 ℃, and then continuing stirring at the rotating speed of the fifth step so as to perform catalytic reaction for 1 hour under the action of the sodium carbonate;
after the reaction is finished, the raw materials in the reaction cavity are cooled for 1-2 hours to room temperature in a nitrogen environment to obtain the high-performance composite modified polyether-ether-ketone material, and then the high-performance composite modified polyether-ether-ketone material can be led out according to the requirement and is granulated by an injection molding or double-screw extruder.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the high-performance composite modified material, the molybdenum disulfide, the graphite, the toughening agent, the aluminum powder and the potassium carbonate are added into the material, so that the mechanical stability and the pressure resistance of the material are improved, the viscosity of the material is reduced, and the self-lubricating property of the material is obviously improved; the toughness and the bearing strength of the material are improved, and the density of the material is improved, so that the sealing effect of the material is better; the high-temperature resistance and low-temperature resistance of the material are improved, and the material is more resistant to weather and aging; shortens the reaction time of the raw materials and improves the preparation efficiency.
2. The preparation process of the high-performance composite modified material provided by the invention has the advantages that the preparation of the whole process is better completed by setting the equipment of the preparation process, the preparation effect of heating, heating and stirring the added raw materials and integrating the heating, the heating speed is high, the stirring is uniform, the reaction condition is more quickly achieved, the preparation effect is greatly improved, the switch group is operated by one key, the use is simple, and the preparation process requirements are met.
3. According to the preparation equipment of the preparation process of the high-performance composite modified material, the heating and temperature rising effects of the added raw materials are realized by setting the heating group, so that the reaction conditions are achieved, the heating speed is high, the stability and the reliability are realized, meanwhile, the protection structure is provided, the safety is improved, the damage to the outside is avoided, and the accidental scalding of workers due to high temperature is prevented.
4. According to the equipment for the preparation process of the high-performance composite modified material, the stirring effect of the added raw materials is realized by setting the stirring component, the effect of integrating heating and stirring is realized by combining the stirring component with the heating component, the reaction speed is greatly increased, the integral stirring is more uniform by improving the arrangement of the blades, and the design requirement is met.
Drawings
FIG. 1 is a schematic structural diagram of the equipment of the preparation process of the high-performance composite modified material of the invention;
FIG. 2 is a schematic diagram of the heating group of FIG. 1;
FIG. 3 is a schematic view of the construction of the stirring assembly of FIG. 1;
FIG. 4 is a schematic diagram of the switch block of FIG. 1;
FIG. 5 is a schematic view of the working principle of FIG. 1;
FIG. 6 is a schematic view of the process for preparing the high-performance composite modified material of the invention.
In the figure:
1-reaction box, 2-feeding pipe, 3-heating group, 31-protective cover, 32-electric hot plate, 4-ceramic plate, 5-vacuum pump, 6-motor, 7-stirring component, 71-rotating shaft, 72-stirring blade, 73-lifting blade, 8-discharging pipe, 9-discharging valve, 10-temperature sensor, 11-nitrogen pipe, 12-switching group, 121-heating switch, 122-vacuum switch, 123-speed regulation switch and 124-discharging switch.
Detailed Description
The technical scheme of the embodiment of the invention is clearly and completely described below, the steps in the technical scheme are not separated, and the final grouting material can be obtained only by implementing the steps. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: a preparation process of a high-performance composite modified material comprises the following steps:
preparing raw materials: selecting the prepared raw materials, specifically: 155 parts of water, 75 parts of polyether-ether-ketone, 65 parts of diphenyl sulfone, 32 parts of molybdenum disulfide, 32 parts of graphite, 11 parts of a toughening agent, 21 parts of aluminum powder and 17 parts of sodium carbonate; the molybdenum disulfide adopts PA66 glass fiber reinforced molybdenum disulfide, and is used for enhancing the water resistance and mechanical stability and pressure resistance of the material; the graphite adopts lubricated graphite powder with a Lutang brand of 659823 for improving the self-lubricating property of the material; the toughening agent adopts HZ-403 universal ABS toughening agent, the appearance of the adopted toughening agent is granular, the content of effective substances is 98%, and the toughening agent is used for improving the toughness and the bearing strength of the material and simultaneously improving the sealing property; the aluminum powder is fine aluminum powder with the trade mark of FLX1, the granularity of the aluminum powder is 0.35-0, and the aluminum powder is used for improving the high-temperature resistance and low-temperature resistance of a finished product, so that the material is not easy to age and the service life is prolonged; the sodium carbonate adopts AR type anhydrous pure sodium carbonate powder, is used for accelerating the reaction speed of raw materials, improves the preparation efficiency and does not interfere the reaction process.
Taking down a tube cover of the feeding tube 2, adding 155 parts of water, 75 parts of polyether ether ketone and 65 parts of diphenyl sulfone into the reaction cavity, then sealing the feeding tube 2, controlling a vacuum pump 5 to be opened through a vacuum switch 122 to vacuumize the reaction cavity, then closing the reaction cavity, controlling electric heating plates 32 on two sides of the reaction box 1 to work through a heating switch 121 to generate heat after the reaction cavity is in a vacuum environment, guiding the heat into the reaction cavity through a ceramic plate 4 to heat the added raw materials, detecting the temperature in the reaction cavity in real time and displaying the temperature on a display screen of the reaction cavity after the heating switch 121 is opened by a temperature sensor 10 connected with the heating switch, and stopping heating when the temperature reaches 60 ℃ to melt the raw materials;
opening the feeding pipe 2, adding 32 parts of molybdenum disulfide and 32 parts of graphite into the reaction chamber, then opening the speed regulating switch 123 to enable the motor 6 to work, so as to drive the rotating shaft 71 of the stirring component 7 to rotate, uniformly stirring the added raw materials under the action of the stirring blades 73 and the lifting blades 73, and adjusting the rotating speed of the motor 6 by the speed regulating switch 123 in the stirring process, so as to stir the added raw materials for 10-15min by the stirring component 7 at the rotating speed of 600 plus 800 r/min;
adding 11 parts of toughening agent into the reaction cavity through the feeding pipe 2, then adjusting the rotating speed of the motor 6 to 700-900r/min through the speed regulating switch 123, and stirring the added raw materials for 30-35min through the stirring component 7 at the rotating speed;
21 parts of aluminum powder is added into the reaction chamber through the feeding pipe 2, then the rotating speed of the motor 6 is adjusted to 1200 and 1300r/min through the speed regulating switch 123, and the added raw materials are stirred for 30-40min by the stirring component 7 at the rotating speed;
after stirring, adding 17 parts of sodium carbonate into the reaction chamber through the feeding pipe 2, closing the feeding pipe 2, opening the vacuum switch 122 again, vacuumizing the reaction chamber through the vacuum pump 5, introducing nitrogen into the reaction chamber through the nitrogen pipe 11 by using an external nitrogen bottle, opening the electric heating plate 32 to heat the raw materials added into the reaction chamber, heating to 100 ℃, and continuing stirring at the rotating speed of the fifth step so as to perform catalytic reaction for 1.5 hours under the action of the sodium carbonate;
after the reaction is finished, the raw materials in the reaction cavity are cooled for 1-2 hours to room temperature in a nitrogen environment to obtain the high-performance composite modified polyether-ether-ketone material, then the high-performance composite modified polyether-ether-ketone material can be externally connected with a double-screw extruder through a discharge pipe 8 according to needs, and then the discharge valve 9 is opened through discharge 124 to be led out, so that injection molding or granulation by the double-screw extruder can be carried out according to needs, and the preparation of the high-performance composite modified polyether-ether-ketone material is completed.
Example 2: a preparation process of a high-performance composite modified material comprises the following steps:
preparing raw materials: selecting the prepared raw materials, specifically: 165 parts of water, 80 parts of polyether-ether-ketone, 67 parts of diphenyl sulfone, 37 parts of molybdenum disulfide, 37 parts of graphite, 13 parts of a toughening agent, 23 parts of aluminum powder and 22 parts of sodium carbonate; the molybdenum disulfide adopts PA66 glass fiber reinforced molybdenum disulfide, and is used for enhancing the water resistance and mechanical stability and pressure resistance of the material; the graphite adopts lubricated graphite powder with a Lutang brand of 659823 for improving the self-lubricating property of the material; the toughening agent adopts HZ-403 universal ABS toughening agent, the appearance of the adopted toughening agent is granular, the content of effective substances is 98%, and the toughening agent is used for improving the toughness and the bearing strength of the material and simultaneously improving the sealing property; the aluminum powder is fine aluminum powder with the trade mark of FLX1, the granularity of the aluminum powder is 0.35-0, and the aluminum powder is used for improving the high-temperature resistance and low-temperature resistance of a finished product, so that the material is not easy to age and the service life is prolonged; the sodium carbonate adopts AR type anhydrous pure sodium carbonate powder, is used for accelerating the reaction speed of raw materials, improves the preparation efficiency and does not interfere the reaction process.
Taking down a tube cover of the feeding tube 2, adding 165 parts of water, 80 parts of polyether ether ketone and 67 parts of diphenyl sulfone into the reaction cavity, then sealing the feeding tube 2, controlling the vacuum pump 5 to be opened through the vacuum switch 122 to vacuumize the reaction cavity, then closing the reaction cavity, controlling the electric heating plates 32 on two sides of the reaction box 1 to work through the heating switch 121 to generate heat after the reaction cavity is in a vacuum environment, guiding the heat into the reaction cavity through the ceramic plate 4 to heat the added raw materials, detecting the temperature in the reaction cavity in real time and displaying the temperature on a display screen of the reaction cavity after the heating switch 121 is opened by the temperature sensor 10 connected with the heating switch, and stopping heating when the temperature reaches 60 ℃ to melt the raw materials;
opening the feeding pipe 2, adding 37 parts of molybdenum disulfide and 37 parts of graphite into the reaction chamber, then opening the speed regulating switch 123 to enable the motor 6 to work, so as to drive the rotating shaft 71 of the stirring component 7 to rotate, uniformly stirring the added raw materials under the action of the stirring blades 73 and the lifting blades 73, and adjusting the rotating speed of the motor 6 by the speed regulating switch 123 in the stirring process, so as to stir the added raw materials for 10-15min by the stirring component 7 at the rotating speed of 600 plus 800 r/min;
adding 13 parts of toughening agent into the reaction chamber through the feeding pipe 2, then adjusting the rotating speed of the motor 6 to 700-900r/min through the speed regulating switch 123, and stirring the added raw materials for 30-35min through the stirring component 7 at the rotating speed;
adding 23 parts of aluminum powder into the reaction chamber through the feeding pipe 2, adjusting the rotating speed of the motor 6 to 1200 and 1300r/min through the speed regulating switch 123, and stirring the added raw materials for 30-40min by the stirring assembly 7 at the rotating speed;
after stirring, adding 22 parts of sodium carbonate into the reaction chamber through the feeding pipe 2, then sealing the feeding pipe 2, opening the vacuum switch 122 again, vacuumizing the reaction chamber through the vacuum pump 5, introducing nitrogen into the reaction chamber through the nitrogen pipe 11 by using an external nitrogen bottle, then opening the electric heating plate 32 to heat the raw materials added into the reaction chamber, heating to 100 ℃, and then continuing stirring at the rotating speed of the fifth step, thereby carrying out catalytic reaction for 1.3 hours under the action of the sodium carbonate;
after the reaction is finished, the raw materials in the reaction cavity are cooled for 1-2 hours to room temperature in a nitrogen environment to obtain the high-performance composite modified polyether-ether-ketone material, then the high-performance composite modified polyether-ether-ketone material can be externally connected with a double-screw extruder through a discharge pipe 8 according to needs, and then the discharge valve 9 is opened through discharge 124 to be led out, so that injection molding or granulation by the double-screw extruder can be carried out according to needs, and the preparation of the high-performance composite modified polyether-ether-ketone material is completed.
Example 3: a preparation process of a high-performance composite modified material comprises the following steps:
preparing raw materials: selecting the prepared raw materials, specifically: 170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium carbonate; the molybdenum disulfide adopts PA66 glass fiber reinforced molybdenum disulfide, and is used for enhancing the water resistance and mechanical stability and pressure resistance of the material; the graphite adopts lubricated graphite powder with a Lutang brand of 659823 for improving the self-lubricating property of the material; the toughening agent adopts HZ-403 universal ABS toughening agent, the appearance of the adopted toughening agent is granular, the content of effective substances is 98%, and the toughening agent is used for improving the toughness and the bearing strength of the material and simultaneously improving the sealing property; the aluminum powder is fine aluminum powder with the trade mark of FLX1, the granularity of the aluminum powder is 0.35-0, and the aluminum powder is used for improving the high-temperature resistance and low-temperature resistance of a finished product, so that the material is not easy to age and the service life is prolonged; the sodium carbonate adopts AR type anhydrous pure sodium carbonate powder, is used for accelerating the reaction speed of raw materials, improves the preparation efficiency and does not interfere the reaction process.
Taking down a tube cover of the feeding tube 2, adding 170 parts of water, 85 parts of polyether ether ketone and 70 parts of diphenyl sulfone into the reaction cavity, then sealing the feeding tube 2, controlling the vacuum pump 5 to be opened through the vacuum switch 122 to vacuumize the reaction cavity, then closing the reaction cavity, controlling the electric heating plates 32 on two sides of the reaction box 1 to work through the heating switch 121 to generate heat after the reaction cavity is in a vacuum environment, guiding the heat into the reaction cavity through the ceramic plate 4 to heat the added raw materials, detecting the temperature in the reaction cavity in real time and displaying the temperature on a display screen of the reaction cavity after the heating switch 121 is opened by the temperature sensor 10 connected with the heating switch, and stopping heating when the temperature reaches 60 ℃ to melt the raw materials;
opening the feeding pipe 2, adding 45 parts of molybdenum disulfide and 45 parts of graphite into the reaction chamber, then opening the speed regulating switch 123 to enable the motor 6 to work, so as to drive the rotating shaft 71 of the stirring component 7 to rotate, uniformly stirring the added raw materials under the action of the stirring blades 73 and the lifting blades 73, and adjusting the rotating speed of the motor 6 by the speed regulating switch 123 in the stirring process, so as to stir the added raw materials for 10-15min by the stirring component 7 at the rotating speed of 600 plus 800 r/min;
17 parts of toughening agent is added into the reaction cavity through the feeding pipe 2, then the rotating speed of the motor 6 is adjusted to 700-900r/min through the speed regulating switch 123, and the added raw materials are stirred for 30-35min by the stirring component 7 at the rotating speed;
adding 28 parts of aluminum powder into the reaction cavity through the feeding pipe 2, adjusting the rotating speed of the motor 6 to 1200 and 1300r/min through the speed regulating switch 123, and stirring the added raw materials for 30-40min through the stirring assembly 7 at the rotating speed;
after stirring, adding 27 parts of sodium carbonate into the reaction chamber through the feeding pipe 2, closing the feeding pipe 2, opening the vacuum switch 122 again, vacuumizing the reaction chamber through the vacuum pump 5, introducing nitrogen into the reaction chamber through the nitrogen pipe 11 by using an external nitrogen bottle, opening the electric heating plate 32 to heat the raw materials added into the reaction chamber, heating to 100 ℃, and continuing stirring at the rotating speed of the fifth step so as to perform catalytic reaction for 1 hour under the action of the sodium carbonate;
after the reaction is finished, the raw materials in the reaction cavity are cooled for 1-2 hours to room temperature in a nitrogen environment to obtain the high-performance composite modified polyether-ether-ketone material, then the high-performance composite modified polyether-ether-ketone material can be externally connected with a double-screw extruder through a discharge pipe 8 according to needs, and then the discharge valve 9 is opened through discharge 124 to be led out, so that injection molding or granulation by the double-screw extruder can be carried out according to needs, and the preparation of the high-performance composite modified polyether-ether-ketone material is completed.
Comparative example 1: the high-performance composite modified material is prepared by the following method:
155 parts of water, 75 parts of polyether-ether-ketone, 65 parts of diphenyl sulfone, 32 parts of molybdenum disulfide, 32 parts of graphite, 11 parts of a toughening agent, 21 parts of aluminum powder and 17 parts of sodium carbonate, wherein the material taking method is manual material taking, and the raw materials are prepared according to the preparation process in the embodiment 1 to obtain the high-performance composite modified polyether-ether-ketone material A.
Comparative example 2: the high-performance composite modified material is prepared by the following method:
165 parts of water, 80 parts of polyether-ether-ketone, 67 parts of diphenyl sulfone, 37 parts of molybdenum disulfide, 37 parts of graphite, 13 parts of a toughening agent, 23 parts of aluminum powder and 22 parts of sodium carbonate, wherein the material taking method is manual material taking, and the raw materials are prepared according to the preparation process in the embodiment 2 to obtain the high-performance composite modified polyether-ether-ketone material B.
Comparative example 3: the high-performance composite modified material is prepared by the following method:
170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium carbonate, wherein the material taking method is manual material taking, and the raw materials are prepared according to the preparation process in the embodiment 3 to obtain the high-performance composite modified polyether-ether-ketone material C.
The high-performance composite modified polyether-ether-ketone materials prepared in comparative examples 1, 2 and 3 according to the preparation processes corresponding to the preparation processes in the examples described in the invention were subjected to experiments, and the experimental results are shown in table 1.
According to the data in table 1, the molybdenum disulfide and the graphite are added into the material, so that the mechanical stability and the pressure resistance of the material are improved, and the self-lubricating property of the material is improved; the toughening agent is added, so that the toughness and the bearing strength of the material are improved, and the density of the material is improved; aluminum powder is added, so that the high-temperature resistance and low-temperature resistance of the material are improved; and by adding sodium carbonate, the reaction time of the raw materials is effectively shortened, and the preparation efficiency is improved.
Figure BDA0002642364220000121
TABLE 1
In summary, the following steps: according to the high-performance composite modified material, the molybdenum disulfide, the graphite, the toughening agent, the aluminum powder and the potassium carbonate are added into the material, so that the mechanical stability and the pressure resistance of the material are improved, and the viscosity of the material is reduced, so that the self-lubricating property of the material is remarkably improved, and the material has excellent lubricating property with that of the existing material; the toughness and the bearing strength of the material are improved, and the density of the material is improved, so that the sealing effect of the material is better; the high-temperature resistance and low-temperature resistance of the material are improved, and the material is more weather-resistant, so that the material is not easy to age and the service life of the material is prolonged; the reaction time of raw materials is effectively shortened, and the preparation efficiency is improved;
the preparation process of the high-performance composite modified material has the advantages that the preparation of the whole process is better completed by setting the preparation equipment, the preparation effect is greatly improved, the switch group is operated by one key, the use is simple, and the efficiency is improved; and through setting for heating group and stirring subassembly, realize heating intensification stirring and integrative preparation effect to adding the raw materials, and rate of heating is fast, the stirring to the condition of reaction is reached faster, has protective structure simultaneously and prevents that the staff is scalded to the high temperature accident, satisfies the preparation technology needs.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. The high-performance composite modified material is characterized by being prepared from the following raw materials in parts by weight: 200 parts of 150-one water, 70-90 parts of polyether-ether-ketone, 60-80 parts of diphenyl sulfone, 30-50 parts of molybdenum disulfide, 30-50 parts of graphite, 10-20 parts of a toughening agent, 20-30 parts of aluminum powder and 15-30 parts of sodium carbonate.
2. The high-performance composite modified material according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium carbonate.
3. The high-performance composite modified material according to claim 1, wherein: the molybdenum disulfide adopts PA66 glass fiber reinforced molybdenum disulfide; the graphite is prepared from lubricating graphite powder with a Lutang brand of 659823.
4. The high-performance composite modified material according to claim 1, wherein: the toughening agent adopts HZ-403 universal ABS toughening agent, the appearance of the adopted toughening agent is granular, and the content of effective substances is 98%.
5. The high-performance composite modified material according to claim 1, wherein: the aluminum powder is fine aluminum powder with the trade mark of FLX1, and the granularity of the aluminum powder is 0.35-0; the sodium carbonate adopts AR type anhydrous pure sodium carbonate powder.
6. A preparation equipment for a preparation process of a high-performance composite modified material is characterized in that: including reaction box (1), inlet pipe (2), heating group (3), ceramic plate (4), vacuum pump (5), motor (6), stirring subassembly (7), discharging pipe (8), bleeder valve (9), temperature sensor (10), nitrogen gas pipe (11) and switch block (12), wherein: a reaction cavity is formed inside the reaction box (1), a feeding pipe (2) is installed at the upper side part of the reaction box (1), and a pipe cover is installed on the feeding pipe (2) in a threaded mode; the heating group (3) is arranged on the side part of the reaction box (1), the inner side of the heating group (3) is contacted with a ceramic plate (4), and the ceramic plate (4) is integrally arranged on the side wall of the reaction box (1); the vacuum pump (5) is arranged on one side of the upper part of the reaction box (1), the motor (6) is arranged in the middle of the upper part of the reaction box (1), the stirring component (7) is arranged on the working part of the motor (6), and the stirring component (7) is positioned in the reaction cavity; the discharge pipe (8) is arranged at the bottom of the reaction box (1), one end of the discharge pipe (8) is communicated with the reaction cavity, and the other end of the discharge pipe (8) is provided with a discharge valve (9) and is positioned outside the reaction box (1); the temperature sensor (10) and the switch group (12) are sequentially arranged on the other side of the upper part of the reaction box (1), wherein the sensing part of the temperature sensor (10) is arranged on the inner upper wall of the reaction box (1) and is positioned in the reaction cavity; the nitrogen pipe (11) is arranged at the other upper side part of the reaction box (1), one end of the nitrogen pipe (11) is communicated with the reaction cavity in the reaction box (1), and the other end of the nitrogen pipe (11) is externally connected with a nitrogen bottle;
the switch group (12) comprises a heating switch (121), a vacuum switch (122), a speed regulating switch (123) and a discharging switch (124), wherein: the heating switch (121), the vacuum switch (122), the speed regulating switch (123) and the discharging switch (124) are respectively connected with an external proper power supply through four groups of power lines and are sequentially arranged on the body of the switch group (12); the heating switch (121) is respectively connected with a temperature sensor (10) and an electric heating plate (32) through two groups of power lines, wherein the temperature sensor (10) adopts a 9120 type high-precision temperature sensor capable of displaying by a large-screen LED, and the electric heating plate (32) adopts an HT-200 type ceramic electric heating plate; the vacuum switch (122) is connected with a vacuum pump (5) through a power line; the speed regulating switch (123) adopts a HW-A-1040 speed regulator switch, and the speed regulating switch (123) is connected with a motor (6) through a power line; the discharging switch (124) is connected with a discharging valve (9) through a power line, and the discharging valve (9) adopts a DF-50F type large-caliber flange electromagnetic valve.
7. The preparation equipment of the preparation process of the high-performance composite modified material according to claim 6, wherein the preparation equipment comprises: the heating group (3) comprises a protective cover (31) and an electric heating plate (32), wherein: the protective cover (31) is in a [ -shape made of asbestos materials, and the protective cover (31) is fixed on the side part of the reaction box (1) and is positioned on one side of the ceramic plate (4); the electric heating plate (32) and the protective cover (31) are arranged inside, and the working part of the electric heating plate (32) is arranged in contact with the ceramic plate (4).
8. The preparation equipment of the preparation process of the high-performance composite modified material according to claim 6, wherein the preparation equipment comprises: the stirring assembly (7) comprises a rotating shaft (71), a stirring blade (72) and a lifting blade (73), wherein: the rotating shaft (71) and the working part of the motor (6) are arranged, and three groups of stirring blades (72) are sequentially welded on the rotating shaft (71) from top to bottom; the lifting blade (73) is welded on the stirring blade (72) at the bottommost part.
9. A preparation process of a high-performance composite modified material is characterized by comprising the following steps: the method comprises the following steps:
preparing raw materials: selecting the prepared raw materials, specifically: 170 parts of water, 85 parts of polyether-ether-ketone, 70 parts of diphenyl sulfone, 45 parts of molybdenum disulfide, 45 parts of graphite, 17 parts of a toughening agent, 28 parts of aluminum powder and 27 parts of sodium hydroxide;
adding water, polyether-ether-ketone and diphenyl sulfone into the reaction cavity, vacuumizing, heating after the reaction cavity is in a vacuum environment, and stopping heating after the temperature reaches 60 ℃;
adding molybdenum disulfide and graphite into the reaction chamber, and stirring for 10-15min at the rotating speed of 600 plus materials and 800 r/min;
adding a toughening agent into the reaction cavity, and stirring for 30-35min at the rotating speed of 700-900 r/min;
adding aluminum powder into the reaction cavity, and stirring for 30-40min at the rotating speed of 1200-1300 r/min;
after stirring, adding sodium carbonate into the reaction cavity, vacuumizing again, introducing nitrogen, heating to 100 ℃, continuing stirring at the rotating speed of the fifth step, and carrying out catalytic reaction for 1 hour under the action of sodium carbonate;
after the reaction is finished, the raw materials in the reaction cavity are cooled for 1-2 hours to room temperature in a nitrogen environment to obtain the high-performance composite modified polyether-ether-ketone material, and then the high-performance composite modified polyether-ether-ketone material can be led out according to the requirement and is granulated by an injection molding or double-screw extruder.
CN202010843840.XA 2020-08-20 2020-08-20 High-performance composite modified material and preparation process thereof Pending CN112175347A (en)

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