CN113021941A - Resin spraying device and preparation method of polyimide resin-based composite wave-transmitting cover - Google Patents

Resin spraying device and preparation method of polyimide resin-based composite wave-transmitting cover Download PDF

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Publication number
CN113021941A
CN113021941A CN202110229102.0A CN202110229102A CN113021941A CN 113021941 A CN113021941 A CN 113021941A CN 202110229102 A CN202110229102 A CN 202110229102A CN 113021941 A CN113021941 A CN 113021941A
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CN
China
Prior art keywords
resin
polyimide resin
fiber cloth
wave
transmitting cover
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CN202110229102.0A
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Chinese (zh)
Inventor
杨佳
高庆福
熊熙
杨斌
贺盛利
贺海平
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Hunan Ronglan Intelligent Technology Co ltd
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Hunan Ronglan Intelligent Technology Co ltd
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Priority to CN202110229102.0A priority Critical patent/CN113021941A/en
Publication of CN113021941A publication Critical patent/CN113021941A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28Shaping operations therefor
    • B29C70/30Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B29C70/34Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
    • B29C70/345Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation using matched moulds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B13/00Machines or plants for applying liquids or other fluent materials to surfaces of objects or other work by spraying, not covered by groups B05B1/00 - B05B11/00
    • B05B13/02Means for supporting work; Arrangement or mounting of spray heads; Adaptation or arrangement of means for feeding work
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B9/00Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
    • B05B9/03Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material
    • B05B9/04Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump
    • B05B9/0403Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump with pumps for liquids or other fluent material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28Shaping operations therefor
    • B29C70/54Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2079/00Use of polymers having nitrogen, with or without oxygen or carbon only, in the main chain, not provided for in groups B29K2061/00 - B29K2077/00, as moulding material
    • B29K2079/08PI, i.e. polyimides or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00Coating on the layer surface
    • B32B2255/02Coating on the layer surface on fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00Coating on the layer surface
    • B32B2255/26Polymeric coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10Inorganic fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10Inorganic fibres
    • B32B2262/106Carbon fibres, e.g. graphite fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/306Resistant to heat

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Mechanical Engineering (AREA)
  • Moulding By Coating Moulds (AREA)

Abstract

The invention discloses a resin spraying device and a preparation method of a polyimide resin matrix composite wave-transparent cover, which comprise the following steps: 1) pretreating polyimide resin; 2) pretreating the surface of the fiber cloth; 3) uniformly spraying polyimide on each surface of the fiber cloth by using a resin spraying device; 4) molding the prefabricated part; 5) and (5) curing at high temperature. The small wave-transmitting cover prepared by the invention has excellent mechanical property and wave-transmitting property, and the wave-transmitting cover has wide application range.

Description

Resin spraying device and preparation method of polyimide resin-based composite wave-transmitting cover
Technical Field
The invention belongs to the technical field of polyimide resin base, relates to a resin spraying device and a preparation method of a polyimide resin base composite material wave-transmitting cover, and particularly relates to a resin spraying device and a preparation method of a polyimide resin base composite material small-sized wave-transmitting cover.
Background
Polyimide is a polymer with a semi-trapezoidal structure, wherein the repeating unit of the main chain of the polymer contains an imide ring structure, and the chemical structure of the polymer is very regular. The polyimide has a wide variety, and mainly comprises the following components according to the current classification: thermoplastic polyimides, thermosetting polyimides, polyamideimides, soluble polyimides, insoluble and infusible polyamideimides, and low temperature cured polyimides, wherein thermoplastic polyimides and thermosetting polyimides are widely used. The molecular chains of the thermoplastic polyimide resin are not combined through chemical bonds, but are connected through intermolecular force, such as intermolecular and hydrogen bonds, and the thermosetting polyimide resin is mainly prepared by thermosetting and crosslinking through active end groups.
The resin-based composite material has the advantages of strong designability, high specific strength, large specific modulus, good fatigue resistance, good chemical corrosion resistance and weather resistance, and the like, is widely applied in the fields of aerospace, national defense and military industry, machinery, electronics, chemical industry and the like, is prepared by mainly taking high-performance continuous fibers as a reinforcement and organic high polymer materials as a matrix through a composite process, and commonly used fiber reinforcements mainly comprise carbon fibers, glass fibers, quartz fibers, aramid fibers, ultrahigh molecular weight polyethylene fibers and the like. The fiber reinforced thermosetting polyimide resin-based composite material has the advantages of light weight, excellent mechanical property and the like, and is widely applied to the fields of aerospace and automation.
The existing research on polyimide resin matrix composite materials and fiber reinforced composite materials, for example, chinese patent CN201610035838 discloses a high-strength and high-toughness polyimide resin matrix composite material and a preparation method thereof, which comprises the following steps: (1) preparing a polyimide resin solution; (2) carrying out surface treatment on the polyimide fiber; (3) dispersing the product obtained in the step (2) in the polyimide resin solution obtained in the step (1) under stirring; (4) heating the mixed slurry obtained in the step (3); (5) carrying out hot-press molding treatment on the product obtained in the step (4); the polyimide fiber is at least one of polyimide fiber pulp, polyimide chopped fiber and polyimide fibrid. For another example, chinese patent application CN201810962777 discloses a three-dimensional fiber fabric reinforced polyimide resin-based composite material and a preparation method thereof, wherein the composite material includes a polyimide resin matrix and a three-dimensional fiber fabric reinforced phase located inside the polyimide resin matrix, the three-dimensional fiber fabric is any one of a three-dimensional fiber woven fabric, a 2.5D fiber fabric, a needle punched fiber fabric or a sewn fiber fabric, and the polyimide resin is any one of a phenylene vinylene terminated polyimide resin, a phenylene vinylene terminated polyimide resin or an isomeric polyimide resin containing a side phenyl structure.
The molding process of the fiber reinforced composite material generally includes a hand lay-up molding method, a die pressing method, a pultrusion method, a resin molding transfer method, a winding method and the like. Each forming process has own advantages and disadvantages and respective application range, the hand lay-up forming process is the simplest and most common forming method in all the forming processes of the composite materials, various new process methods are continuously emerged along with the development of the composite material industry in recent years, the proportion occupied by the hand lay-up forming process is reduced year by year, however, the hand lay-up forming process has the characteristic that other processes cannot be replaced, particularly in the aspect of producing large-scale products, but the molding process product is greatly influenced by human factors, the quality is not easy to control, the product performance has larger discreteness, meanwhile, the process has high labor intensity, the quality of each part depends on the skill level of an operator, volatile substances generated by an organic resin system are difficult to manage, the operation environment is poor, and the production efficiency is low, so that the defect of the hand lay-up forming process is overcome.
Disclosure of Invention
The invention aims to overcome the defects of the existing hand lay-up forming process, provides a resin spraying device and a preparation method of a polyimide resin matrix composite material wave-transmitting cover, and particularly relates to a resin spraying device and a preparation method of a small polyimide resin matrix composite material wave-transmitting cover.
The invention is realized by adopting the following technical means:
a resin spraying device comprises a resin tank, a diaphragm pump, a pressure regulating valve, a pressure gauge, a material conveying pipeline, a mechanical arm, a switch valve, a resin atomizer, a mold, a rotary tray and a variable frequency motor workbench; wherein the mould and the rotary tray are arranged on a working platform of a variable frequency motor; the resin tank is connected with the diaphragm pump through a material conveying pipeline, a pressure regulating valve is arranged on the material conveying pipeline, and a pressure gauge is arranged on the diaphragm pump; one end of the material conveying pipeline is connected with the diaphragm pump, the other end of the material conveying pipeline is connected with the switch valve, and the other end of the material conveying pipeline is connected with the mechanical arm; the switch valve is connected with the resin atomizer; and screw holes are formed in the bottoms of the die and the rotary tray so as to facilitate die assembly.
The resin tank is used for containing resin required by the preparation of the resin-based composite material, and the size of the resin tank is adjusted according to the required amount;
the diaphragm pump is used for conveying resin and providing power for the atomizer;
the pressure regulating valve is used for regulating the flow of the resin and controlling the flow rate of the resin according to the reading of the pressure gauge;
the pressure regulating valve is used for controlling the flow rate of the resin by regulating the pressure;
the material conveying pipeline is a hose so as to facilitate the adjustment of the position of the resin atomizer;
the mechanical arm is used for controlling and adjusting the direction and the position of the resin atomizer, so that the resin is sprayed more uniformly, and the mechanical arm is selected from one of a full-automatic mechanical arm, a semi-automatic mechanical arm and a manual mechanical arm;
the switch valve is used for controlling the time for the resin to enter the resin atomizer;
the resin atomizer is used for atomizing resin, so that resin particles are smaller, and the resin is sprayed on the surface of the fiber more uniformly;
the mould and the rotary tray can automatically rotate.
The frequency conversion motor workbench is used for being equipped with a frequency conversion motor, so that the die can rotate on the workbench, and resin on the surface of the fiber can be uniformly sprayed.
The invention also relates to a preparation method of the wave-transmitting cover made of the polyimide resin matrix composite material, which comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of the polyimide resin solution is 5-30 wt%; the solvent is selected from one of ethanol, acetone and butanediol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from one of high-temperature heat treatment, acid washing and solvent cleaning; the fiber cloth is selected from one of quartz fiber cloth, carbon fiber cloth and silicon carbide fiber cloth;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, spraying one layer of fiber cloth, paving the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of a mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing the die, fixing and pressing for molding;
5) high-temperature curing: and (4) placing the mold obtained in the step 4) into a box type resistance furnace for curing to obtain the wave-transmitting cover of the polyimide resin matrix composite material.
In the invention:
the polyimide resin in the step 1) is thermosetting resin.
The high-temperature heat treatment in the step 2) is carried out at the temperature of 200 ℃ and 500 ℃ for 30-180 min; the acid washing is carried out, and the solvent is one of hydrochloric acid, nitric acid and sulfuric acid; the solvent is used for cleaning, and the solvent is one of ethanol, acetone, butanediol, chloroform, DMF and tetrahydrofuran.
The thickness of the fiber cloth in the step 2) is 0.2-0.6 mm; the diameter of the fiber cloth is 100-450 mm.
And 3) resin spraying, namely placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline through a diaphragm pump at the speed of 50-90mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber.
The mold in the step 4) has a hemispherical shape, a diameter of 100-800mm and a thickness of 2-6 mm.
And 5) curing, wherein the curing process comprises the steps of raising the temperature to 150 ℃ at the heating rate of 1-5 ℃, preserving the heat for 2-8h, raising the temperature to 260 ℃ at the heating rate of 2-6 ℃, and preserving the heat for 1-5 h.
The invention also relates to a wave-transmitting cover of the polyimide resin matrix composite material prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
1. the prior polyimide resin and fiber cloth compounding technology generally adopts a hand pasting forming method, the traditional hand pasting forming process is time-consuming and labor-consuming, and the uniformity of brushing can not be ensured.
2. According to the preparation method of the wave-transmitting cover of the polyimide resin matrix composite material, the polyimide resin is sprayed on the surface of the fiber cloth through the plasma spraying technology, and is pressed through a die and cured to form the high-strength wave-transmitting cover based on the polyimide resin matrix composite material.
3. According to the invention, the polyimide resin and the fiber cloth are compounded, so that the prepared material has excellent mechanical properties, good wave-transmitting performance and certain temperature resistance; the prepared polyimide resin matrix composite wave-transmitting cover can be widely applied to the fields of spaceflight, buildings and the like, and is simple in preparation process and high in operability.
Drawings
Fig. 1 is a schematic view of the overall structure of a resin spraying apparatus according to an embodiment of the present invention and a mold clamping process.
Reference numerals:
1. a resin tank; 2. a diaphragm pump; 3. a pressure regulating valve; 4. a pressure gauge; 5. a material conveying pipeline; 6. a mechanical arm; 7. an on-off valve; 8. a resin atomizer; 9. a mold and a rotating tray; 10. fiber cloth; 11. a variable frequency motor stage; 12. and (5) carrying out die assembly.
Detailed Description
The present invention is described in further detail below by way of examples, which should not be construed as limiting the invention thereto.
Example 1:
the resin spraying device comprises a resin tank 1, a diaphragm pump 2, a pressure regulating valve 3, a pressure gauge 4, a material conveying pipeline (hose) 5, a mechanical arm 6, a switch valve 7, a resin atomizer 8, a mould and rotary tray 9 and a variable frequency motor workbench 11; wherein the mold and the rotary tray 9 are arranged on a frequency conversion motor worktable 11; the resin tank 1 is connected with the diaphragm pump 2 through a material conveying pipeline (hose) 5, a pressure regulating valve 3 is arranged on the material conveying pipeline (hose) 5, and a pressure gauge 4 is arranged on the diaphragm pump 2; one end of the material conveying pipeline (hose) 5 is connected with the diaphragm pump 2, the other end of the material conveying pipeline is connected with the switch valve 7, and the other end of the material conveying pipeline is connected with the mechanical arm 6; the switch valve 7 is connected with the resin atomizer 8; the bottom of the mould and the rotary tray 9 are provided with screw holes so as to be convenient for mould closing.
A preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of the polyimide resin solution is 5 wt%;
the solvent is selected from ethanol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from high-temperature heat treatment, the temperature is 200 ℃, and the treatment time is 180 min;
the fiber cloth is selected from quartz fiber cloth, and the thickness dimension is 0.2 mm; the diameter of the fiber cloth is 450 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 50mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, the diameter of the mold is 100mm, and the thickness of the mold is 6 mm;
5) high-temperature curing: and (3) putting the mold obtained in the step 4) into a box type resistance furnace for curing, wherein the curing process comprises the steps of heating to 100 ℃ at the heating rate of 1 ℃, preserving heat for 2 hours, heating to 200 ℃ at the heating rate of 6 ℃, and preserving heat for 5 hours to obtain the wave-transmitting cover made of the polyimide resin matrix composite material.
Example 2:
a preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of a polyimide resin solution is 30 wt%;
the solvent is selected from acetone;
2) treating the surface of the fiber cloth: the surface treatment method is selected from acid washing, and the solvent is hydrochloric acid;
the fiber cloth is selected from carbon fiber cloth, and the thickness dimension is 0.6 mm; the diameter of the fiber cloth is 100 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 90mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, 800mm in diameter and 2mm in thickness;
5) high-temperature curing: putting the mold obtained in the step 4) into a box-type resistance furnace for curing, wherein the curing process comprises the steps of heating to 150 ℃ at the heating rate of 5 ℃, preserving heat for 6 hours, heating to 260 ℃ at the heating rate of 5 ℃, and preserving heat for 1 hour to obtain the wave-transmitting cover of the polyimide resin matrix composite material;
the resin spray apparatus was the same as in example 1.
Example 3:
a preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of a polyimide resin solution is 10 wt%;
the solvent is selected from butanediol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from solvent cleaning, and the used solvent is ethanol;
the fiber cloth is selected from silicon carbide fiber cloth, and the thickness dimension of the fiber cloth is 0.3 mm; the diameter of the fiber cloth is 200 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 60mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, 200mm in diameter and 5mm in thickness;
5) high-temperature curing: putting the mold obtained in the step 4) into a box-type resistance furnace for curing, wherein the curing process comprises the steps of heating to 120 ℃ at the heating rate of 2 ℃, preserving heat for 8 hours, heating to 220 ℃ at the heating rate of 2 ℃, and preserving heat for 4 hours to obtain a wave-transmitting cover of the polyimide resin matrix composite material;
the resin spray apparatus was the same as in example 1.
Example 4:
a preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of a polyimide resin solution is 15 wt%;
the solvent is selected from ethanol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from high-temperature heat treatment, the temperature is 500 ℃, and the treatment time is 30 min;
the fiber cloth is selected from quartz fiber cloth, and the thickness dimension is 0.4 mm; the diameter of the fiber cloth is 300 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 70mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, 400mm in diameter and 4mm in thickness;
5) high-temperature curing: putting the mold obtained in the step 4) into a box-type resistance furnace for curing, wherein the curing process comprises the steps of heating to 140 ℃ at the heating rate of 4 ℃, preserving heat for 4 hours, heating to 240 ℃ at the heating rate of 4 ℃, and preserving heat for 3 hours to obtain a wave-transmitting cover of the polyimide resin matrix composite material;
the resin spray apparatus was the same as in example 1.
Example 5:
a preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of a polyimide resin solution is 20 wt%;
the solvent is selected from acetone;
2) treating the surface of the fiber cloth: the surface treatment method is selected from solvent cleaning, and the used solvent is butanediol;
the fiber cloth is selected from carbon fiber cloth, and the thickness dimension is 0.5 mm; the diameter of the fiber cloth is 400 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 80mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, the diameter of the mold is 600mm, and the thickness of the mold is 3 mm;
5) high-temperature curing: putting the mold obtained in the step 4) into a box-type resistance furnace for curing, wherein the curing process comprises the steps of heating to 130 ℃ at the heating rate of 3 ℃, preserving heat for 3 hours, heating to 250 ℃ at the heating rate of 5 ℃, and preserving heat for 3 hours to obtain a wave-transmitting cover made of the polyimide resin matrix composite material;
the resin spray apparatus was the same as in example 1.
Example 6:
a preparation method of a wave-transmitting cover made of polyimide resin matrix composite material comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of a polyimide resin solution is 25 wt%;
the solvent is selected from butanediol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from solvent cleaning, and the used solvent is tetrahydrofuran;
the fiber cloth is selected from carbon fiber cloth, and the thickness dimension is 0.5 mm; the diameter of the fiber cloth is 400 mm;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through the resin spraying device, placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline (hose) through a diaphragm pump at a speed of 75mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber;
spraying one layer of fiber cloth, laying the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirement of the mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing a mold, fixing and pressing to form, wherein the mold is hemispherical, the diameter of the mold is 600mm, and the thickness of the mold is 3 mm;
5) high-temperature curing: putting the mold obtained in the step 4) into a box-type resistance furnace for curing, wherein the curing process comprises the steps of heating to 130 ℃ at the heating rate of 3 ℃, preserving heat for 3 hours, heating to 250 ℃ at the heating rate of 5 ℃, and preserving heat for 3 hours to obtain a wave-transmitting cover made of the polyimide resin matrix composite material;
the resin spray apparatus was the same as in example 1.
Comparative example 1:
compared with the example 1, the step 3) adopts the hand lay-up forming method without adopting a resin spraying device, and the other steps are the same as the example 1.
Comparative example 2:
step 3) lacks a pressure regulating valve and a pressure gauge (polyimide resin solution is transported by a diaphragm pump at a rate of 30 mL/min) as compared with example 1, and is otherwise the same as example 1.
Experimental example:
the prepared high-strength wave-transmitting cover is subjected to tests on parameters such as mechanical properties (density, tensile strength), dielectric constant and thermal conductivity along with a furnace flat plate sample, and the results are shown in table 1:
Figure BDA0002958212350000081
Figure BDA0002958212350000091
and (4) analyzing results:
1. by comparing examples 1 to 6 with comparative example 1, it was found that the polyimide resin-based composite material prepared without using the resin spray apparatus had a low density and had inferior mechanical properties, dielectric properties and heat conductivity to those of the composite material prepared using the resin spray apparatus.
2. The reason why the resin spray apparatus sprays the resin uniformly and the density is uniform and thus each property is excellent was analyzed by comparing examples 1 to 6 with comparative example 2, which indicates that the comparison between the pressure regulating valve and the pressure gauge is obvious because the spray can be made more uniform by controlling the flow rate (50 to 90mL/min) and the amount can be controlled and thus each property is excellent.
The data in table 1 show that the wave-transparent cover has good mechanical properties and wave-transparent properties.
The comparison of the basic properties of the examples and comparative examples shows that the preparation process of the examples is significantly superior to the comparative examples.

Claims (10)

1. A resin spraying device is characterized in that: the device comprises a resin tank (1), a diaphragm pump (2), a pressure regulating valve (3), a pressure gauge (4), a material conveying pipeline (5), a mechanical arm (6), a switch valve (7), a resin atomizer (8), a mould and rotary tray (9) and a variable frequency motor workbench (11); wherein the mould and the rotary tray (9) are arranged on a working table (11) of a variable frequency motor; the resin tank (1) is connected with the diaphragm pump (2) through a material conveying pipeline (5), a pressure regulating valve (3) is arranged on the material conveying pipeline (5), and a pressure gauge (4) is arranged on the diaphragm pump (2); one end of the material conveying pipeline (5) is connected with the diaphragm pump (2), the other end of the material conveying pipeline is connected with the switch valve (7), and the other end of the material conveying pipeline is connected with the mechanical arm (6); the switch valve (7) is connected with the resin atomizer (8); and screw holes are formed at the bottoms of the die and the rotary tray (9).
2. The resin spraying apparatus according to claim 1, wherein: the material conveying pipeline (5) is a hose.
3. The resin spraying apparatus according to claim 1, wherein: the mechanical arm (6) is selected from one of a full-automatic mechanical arm, a semi-automatic mechanical arm and a manual mechanical arm.
4. A preparation method of a wave-transmitting cover made of polyimide resin matrix composite material is characterized by comprising the following steps: the method comprises the following steps:
1) pretreatment of polyimide resin: mixing a polyimide resin base and a solvent together, wherein the mass concentration of the polyimide resin solution is 5-30 wt%; the solvent is selected from one of ethanol, acetone and butanediol;
2) treating the surface of the fiber cloth: the surface treatment method is selected from one of high-temperature heat treatment, acid washing and solvent cleaning; the fiber cloth is selected from one of quartz fiber cloth, carbon fiber cloth and silicon carbide fiber cloth;
3) resin spraying: uniformly spraying the polyimide resin pretreated in the step 1) on the surface of the fiber cloth obtained in the step 2) through a resin spraying device according to any one of claims 1 to 3, spraying one layer of fiber cloth, paving the next layer of fiber cloth on the previous layer of fiber cloth, and repeating the spraying step until the thickness of the fiber cloth meets the requirements of a mold;
4) and (3) forming a prefabricated part: trimming the redundant fiber cloth, closing the die, fixing and pressing for molding;
5) high-temperature curing: and (4) placing the mold obtained in the step 4) into a box type resistance furnace for curing to obtain the wave-transmitting cover of the polyimide resin matrix composite material.
5. The method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to claim 4, wherein the method comprises the following steps: the high-temperature heat treatment in the step 2) is carried out at the temperature of 200 ℃ and 500 ℃ for 30-180 min; the acid washing is carried out, and the solvent is one of hydrochloric acid, nitric acid and sulfuric acid; the solvent is used for cleaning, and the solvent is one of ethanol, acetone, butanediol, chloroform, DMF and tetrahydrofuran.
6. The method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to claim 4, wherein the method comprises the following steps: the thickness of the fiber cloth in the step 2) is 0.2-0.6 mm; the diameter of the fiber cloth is 100-450 mm.
7. The method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to claim 4, wherein the method comprises the following steps: and 3) resin spraying, namely placing the polyimide resin solution obtained in the step 1) into a resin tank, opening a pressure regulating valve to convey the polyimide resin solution into a material conveying pipeline through a diaphragm pump at the speed of 50-90mL/min, opening a switch valve to enable the polyimide resin solution to enter a resin atomizer, and adjusting the position of the resin atomizer through a mechanical arm to enable the resin atomizer to be sprayed on each surface of the fiber.
8. The method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to claim 4, wherein the method comprises the following steps: the mold in the step 4) has a hemispherical shape, a diameter of 100-800mm and a thickness of 2-6 mm.
9. The method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to claim 4, wherein the method comprises the following steps: and 5) curing, wherein the curing process comprises the steps of raising the temperature to 150 ℃ at the heating rate of 1-5 ℃, preserving the heat for 2-8h, raising the temperature to 260 ℃ at the heating rate of 2-6 ℃, and preserving the heat for 1-5 h.
10. A wave-transmitting cover made of polyimide resin matrix composite is characterized in that: the method for preparing the wave-transmitting cover made of the polyimide resin matrix composite material according to any one of claims 4 to 9.
CN202110229102.0A 2021-03-02 2021-03-02 Resin spraying device and preparation method of polyimide resin-based composite wave-transmitting cover Pending CN113021941A (en)

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CN113927922A (en) * 2021-10-15 2022-01-14 中国人民解放军国防科技大学 Mold for rapidly preparing radome, method for preparing broadband radome by using mold and material obtained by method
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CN109795137A (en) * 2017-11-16 2019-05-24 中国商用飞机有限责任公司 For fixing the method and device of reinforcing fibre in the molding of resin material workpiece
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CN113927922A (en) * 2021-10-15 2022-01-14 中国人民解放军国防科技大学 Mold for rapidly preparing radome, method for preparing broadband radome by using mold and material obtained by method
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