CN113400683A - Method and device for preparing fiber fabric reinforced polydicyclopentadiene composite material from dicyclopentadiene composite material - Google Patents

Method and device for preparing fiber fabric reinforced polydicyclopentadiene composite material from dicyclopentadiene composite material Download PDF

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Publication number
CN113400683A
CN113400683A CN202110699636.XA CN202110699636A CN113400683A CN 113400683 A CN113400683 A CN 113400683A CN 202110699636 A CN202110699636 A CN 202110699636A CN 113400683 A CN113400683 A CN 113400683A
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composite material
dicyclopentadiene
fiber fabric
mold
preparing
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张玉清
余东升
余志强
张航
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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
    • B29C70/40Shaping or impregnating by compression not applied
    • B29C70/42Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
    • B29C70/46Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
    • B29C70/48Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs and impregnating the reinforcements in the closed mould, e.g. resin transfer moulding [RTM], e.g. by vacuum
    • 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

Abstract

The invention belongs to the field of polydicyclopentadiene composite materials, and particularly relates to a method and a device for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material. The method mainly comprises the following steps: firstly, fixing a fiber fabric reinforcement in a mold, wherein the mold comprises a flash port and a feed port; secondly, after the mould is vacuumized, the impregnating compound enters the mould to carry out in-situ infiltration on the fiber fabric reinforcement, and then the impregnating compound is discharged; then, the dicyclopentadiene composite material enters a mould, is solidified, demoulded and taken out. According to the invention, the high-efficiency large-scale production of the high-performance polydicyclopentadiene/fiber fabric composite material is realized by combining in-situ infiltration with injection of the dicyclopentadiene composite material on the basis of ensuring the interface bonding effect.

Description

Method and device for preparing fiber fabric reinforced polydicyclopentadiene composite material from dicyclopentadiene composite material
Technical Field
The invention belongs to the field of polydicyclopentadiene composite materials, and particularly relates to a method and a device for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material.
Background
Polydicyclopentadiene (PDCPD) is a novel thermosetting engineering plastic, not only has excellent comprehensive properties of high impact strength, high modulus, high hardness, high creep resistance and the like, but also is worthy of attention, the monomer viscosity is low, the polymerization speed is high, so that the polydicyclopentadiene can be molded by adopting a reaction injection molding process, high mold locking pressure and high mold temperature are not needed during molding, the product is simple in post-treatment, post-curing is not needed after demolding, and the polydicyclopentadiene is particularly suitable for being made into high-strength large-area ultrathin products. Therefore, the material is widely applied to the fields of traffic vehicles, engineering machinery, chemical engineering environmental protection, national defense and military industry, medical treatment, sports equipment and the like.
However, the bulk polydicyclopentadiene material cannot meet the requirements of special fields in certain properties, such as application scenes needing higher rigidity as a covering part of a carrying vehicle and the like. Therefore, it is necessary to use a technique of compounding with fibers to reinforce the modulus of the material.
The Chinese patent application with publication number CN108058405A discloses a fiber fabric reinforced polydicyclopentadiene composite material and a preparation method thereof, wherein a dicyclopentadiene monomer containing a single-component ruthenium carbene catalyst is sprayed on a fiber fabric which is subjected to stranding treatment in advance, and then the fiber fabric reinforced polydicyclopentadiene composite material with good mechanical property is obtained after pultrusion, heating, forming and cooling in sequence.
The Chinese patent application with publication number CN109774798A discloses an automobile part and a preparation method thereof, and the method adopts dicyclopentadiene containing a single-component ruthenium catalyst to prepare a discontinuous reinforced polydicyclopentadiene composite outer plate and a continuous reinforced polydicyclopentadiene composite inner plate, thereby realizing the benefits of high performance, low cost, light weight and short-period manufacture of the automobile part. In the prior art, the fiber fabric reinforcement composite PDCPD material is proved to have better mechanical property performance (relative to non-fiber fabric reinforcement) and can be used as a main load-bearing part. Specifically, an RTM (resin transfer molding) process is used when forming a fiber fabric reinforced composite material.
Polydicyclopentadiene can be polymerized and formed by two catalytic systems. One is a single-component ruthenium carbene catalyst, and the other is a double-component material (namely a dicyclopentadiene composite material) which is composed of organic tungsten or molybdenum as a main catalyst and alkyl aluminum as an activator. The polymerization speed of the dicyclopentadiene catalyzed by the single-component ruthenium carbene catalyst is adjustable within a certain range, so that the full infiltration of the fibers can be met, and the mechanical property of the composite material can be ensured. According to the preparation technology of the fiber composite polydicyclopentadiene material, the ruthenium carbene catalyst is mainly adopted, but the price is higher, the material operation time window is small, the material needs to be prepared at present, and the preparation technology cannot be suitable for large-scale production.
At present, polydicyclopentadiene products are produced industrially by adopting two-component combined materials, and the polydicyclopentadiene production technology is characterized by low cost and quick reaction, and the adopted molding equipment is a high-pressure reaction injection molding machine (the two components need to be quickly and efficiently mixed uniformly by the high-pressure reaction injection molding machine). However, these two features (fast reaction, high pressure injection) limit the production of scale-up polydicyclopentadiene/fiber composites. The reason is that (1) the plunger pump of the high-pressure reaction injection molding machine cannot convey and meter the polymer material containing a large amount of short fibers and fillers; (2) the polymerization reaction is too fast, the fiber cannot be well infiltrated, and the good interface cohesiveness is difficult to ensure; (3) fiber fabrics are preset in the die, and the fiber paved in the die is easy to disperse due to high material injection speed and pressure.
Disclosure of Invention
The invention aims to provide a method for preparing a fiber fabric reinforced polydicyclopentadiene composite material by using a dicyclopentadiene composite material, and solves the problem that high-performance polydicyclopentadiene/fiber fabric composite material products cannot be efficiently produced in a large scale in the prior art.
The second purpose of the invention is to provide a device for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material.
In order to achieve the purpose, the technical scheme of the method for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material is as follows:
a method for preparing a fiber fabric reinforced polydicyclopentadiene composite material by using a dicyclopentadiene composite material comprises the following steps: firstly, fixing a fiber fabric reinforcement in a mold, wherein the mold comprises a flash port and a feed port; secondly, after the mould is vacuumized, the impregnating compound enters the mould to carry out in-situ infiltration on the fiber fabric reinforcement, and then the impregnating compound is discharged; then, the dicyclopentadiene composite material enters a mould, is solidified, demoulded and taken out.
According to the method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material, disclosed by the invention, efficient large-scale production of the high-performance polydicyclopentadiene/fiber fabric composite material is realized on the basis of ensuring the interface bonding effect by combining in-situ infiltration with injection of the dicyclopentadiene composite material.
The production device can be further simplified through in-situ infiltration, and the production efficiency is improved. The infiltration effect of the fiber fabric reinforcement can be ensured by the infiltration mode, the interfacial cohesiveness of the composite material is ensured, and the improvement of the performance of the composite material is facilitated.
From the viewpoint of cost and convenience of industrial implementation, it is preferable that the fixing is an adhesive fixing. Three or more point bonds may be used depending on the size of the article. More preferably, the adhesive fastening is performed at the corresponding back side position of the article. In operation, the fabric reinforcement is bonded to the back mold of the article to ensure the quality of the front side of the article.
Preferably, the dicyclopentadiene composite material enters a mould in the following way: the dicyclopentadiene composite material is firstly injected into a buffer container by an injection machine and then enters a mould from the buffer container under the action of negative pressure. The negative pressure feeding of the buffer container is added, compared with the direct injection feeding of an injection machine, the negative pressure feeding of the buffer container reduces the speed and the pressure of the material injection, is favorable for keeping the laying state of the fiber fabric reinforcement, and avoids the influence of the scattering of the fiber fabric reinforcement on the consistency of different parts of the material.
Preferably, the impregnating compound enters the die from the feed inlet to perform the in-situ impregnation, and the step of discharging the impregnating compound is to introduce gas into the die from the overflow port to extrude the impregnating compound from the feed inlet.
Preferably, the impregnating compound contains one or more of cyclopentadiene, dicyclopentadiene, norbornene, ethylidene norbornene, terpene and styrene, with or without addition of an organic metal, wherein the organic metal is an activator component of the dicyclopentadiene composite material. Organometallic such as alkylaluminum, alkylzinc, alkyltin, etc.
The technical scheme of the device for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material is as follows:
the injection machine is used for injecting the dicyclopentadiene composite material;
the forming die comprises a die cavity, a feeding hole and an overflow hole, wherein the die cavity is used for laying a fiber fabric reinforcement and receiving a dicyclopentadiene composite material;
the vacuumizing device is connected with the overflow port of the forming die and is used for vacuumizing the die cavity;
and the impregnating agent container is connected with the feed inlet of the forming die and is used for introducing the impregnating agent into the die cavity.
The commercial two-component combined material is divided by 1:1 and respectively contains a main catalyst and an activator. The device is an industrial production device suitable for bi-component combined materials, and can realize the balance of the quality, the production efficiency and the production cost of the composite material by adopting the existing mould and a reaction injection molding machine and only needing to prepare an auxiliary device (an impregnating compound container and the like).
In order to better ensure the quality of the product and reduce the setting of the bonding points, preferably, the device further comprises: and the buffer container is provided with an inlet and an outlet, the inlet is connected with the injection machine, and the outlet is connected with a feed inlet of the forming die.
Preferably, the forming die is connected with a blowing device for blowing air to the die cavity and pressing the impregnating compound back to the impregnating compound container. More preferably, the flash port of the forming mold is connected with a flash collecting container, the blowing device comprises a blowing pipeline, the blowing pipeline is connected with the flash collecting container, and gas enters the mold cavity from the blowing pipeline through the flash collecting container.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an apparatus for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material according to the invention;
in the figure, 1-forming die, 2-feeding inlet, 20-hose section, 200-hose hold-down device, 3-overflow port, 4-fiber fabric reinforcement, 5-sizing agent container, 50-nitrogen inlet, 51-sizing pipe, 510-sizing valve, 6-buffer container, 60-inlet, 61-outlet, 62-filling pipe, 620-filling valve, 63-washing solvent pipe, 7-flash collecting container, 70-flash valve, 8-vacuum pumping pipe, 80-vacuum pumping valve, 9-nitrogen inlet pipe, and 90-nitrogen inlet valve.
Detailed Description
The invention mainly provides a method and a device for preparing a fiber fabric reinforced polydicyclopentadiene composite material by adopting a combined material of a two-component catalytic system, and solves the problem that high-performance polydicyclopentadiene/fiber fabric composite material products cannot be efficiently produced in a large scale in the prior art.
The dicyclopentadiene composite material can be sold or prepared by self aiming at a bi-component material.
The method mainly comprises the following steps: firstly, fixing a fiber fabric reinforcement in a mold, wherein the mold comprises a flash port and a feed port; secondly, after the mould is vacuumized, the impregnating compound enters the mould to carry out in-situ infiltration on the fiber fabric reinforcement, and then the impregnating compound is discharged; then, the dicyclopentadiene composite material enters a mould, is solidified, demoulded and taken out.
The fiber fabric is selected from one or more of carbon fiber, glass fiber, chemical fiber, fabric fiber and mineral fiber. The fiber fabric reinforcement is a fabric formed by weaving fibers. The fiber fabric can adopt any reinforcing fiber in the prior art, such as carbon fiber, glass fiber, chemical fiber, plant fiber, mineral fiber, mixed fabrics of various fibers and the like. The reinforcing fibers may be further surface treated to improve their wetting and complexing effect. Chemical fibers such as aramid fibers, ultra-high molecular weight polyethylene fibers, polypropylene fibers, polyvinyl chloride fibers and the like, plant fibers such as flax fibers and the like, and mineral fibers such as basalt fibers.
The infiltration of the fiber fabric reinforcement is to further improve the interface bonding effect of the fiber fabric reinforcement and the polydicyclopentadiene. The sizing may be a reactive material compatible with the polydicyclopentadiene. For example, the wetting agent may be pure cyclopentadiene, dicyclopentadiene, norbornene, ethylidene norbornene, terpene, styrene, or a solution thereof mixed with organoaluminum, organolithium, or organotin. The interface bonding effect of the composite material can be further optimized by adopting the infiltration solution containing the components.
The dicyclopentadiene composite material is a commercial product or is self-prepared. The catalyst generally comprises dicyclopentadiene, pour point depressant, tackifier and two-component catalyst system, and the polydicyclopentadiene product is formed after the combined material is polymerized according to the reaction injection molding process.
One component of the composition contains a tungsten or molybdenum procatalyst and the other component contains an organoaluminum activator (organometallic). The two components are mixed according to the ratio of 1:1 and then injected into a mold, and the curing is carried out for about 4 minutes. The polymerization time can be adjusted by adding retarders, increasing the window time. The retarder can be esters and ethers, specifically, the ethers can be propyl ether, isopropyl ether, butyl ether, isobutyl ether, ethoxybenzene, propoxybenzene, tetrahydrofuran, dioxane, ethylene glycol dimethyl ether, etc.; the ester compound may be ethyl acetate, propyl acetate, butyl acetate, ethyl benzoate, propyl benzoate, butyl benzoate, etc. After adding a proper amount of retarder, the curing time can be prolonged to 8-20 minutes.
In order to better remove gas in the fibers and further improve the infiltration effect, the overflow port and the feed inlet are arranged up and down, and by adopting the mode, the material enters the die cavity and then is filled into the die from bottom to top, so that the exhaust effect is better. For air evacuation, evacuation can be performed before pre-soaking (in-situ infiltration process described below) and injection to achieve better air evacuation.
More preferably, after in-situ infiltration, the dicyclopentadiene composite material is firstly injected into a buffer container by an injection machine, and finally enters a mold under the action of negative pressure, and the product is solidified, demoulded and taken out. The method combines a reaction injection molding process (RIM) and a resin transfer molding process (VARTM), and realizes the preparation of the large-scale composite product reinforced by the fiber fabric by the injection mold, which can be called RIM/VARTM process for short.
The following further describes embodiments of the present invention with reference to the drawings.
First, the concrete embodiment of the device for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material
Example 1
The device for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material comprises a forming mold 1, a soaking system and a material injection system, as shown in fig. 1;
the forming die 1 comprises a die cavity formed by closing a female die and a male die, a feeding hole 2 and a flash hole 3; the fibre fabric reinforcement 4 is laid and fixed in the mould cavity. The overflow port 3 and the feed port 2 are arranged up and down, materials enter the die cavity from the feed port 2 and are filled upwards, and after the filling is finished, redundant materials overflow from the overflow port 3.
The infiltration system is connected with the feed inlet 2 of the die and comprises an infiltration agent container 5, a nitrogen inlet 50 is arranged on the infiltration agent container 5, and nitrogen can be introduced into the infiltration agent container 5 through the nitrogen inlet to reduce the contact between air and moisture and the infiltration agent and keep stress balance (the infiltration agent can conveniently enter a die cavity). The outlet of the impregnating agent container 5 is connected with the feed inlet 2 of the die through an impregnating pipeline 51. The infiltration pipe 51 is provided with an infiltration valve 510.
The material injection system is connected with the feed port 2 of the die and comprises a buffer container 6, the buffer container 6 is provided with an inlet 60 and an outlet 61, the inlet 60 is connected with an injection material outlet of the injection machine, and the outlet 61 is connected with the feed port 2 of the die through an injection pipeline 62. The material injection pipe 62 is provided with a material injection valve 620.
The flash port 3 of the mold is connected with a flash collecting container 7, the flash collecting container 7 is connected with a vacuum pipeline 8, and a vacuum valve 80 is arranged on the vacuum pipeline. The flash collecting container 7 is also connected with a nitrogen inlet pipeline 9, and a nitrogen inlet valve 90 is arranged on the nitrogen inlet pipeline 9. A flash valve 70 is arranged on the connecting pipeline of the flash port 3 and the flash collecting container 7.
When the device works, the flash valve 70 is in an open state, the nitrogen gas inlet valve 90, the infiltration valve 510 and the material injection valve 620 are closed, and the vacuum pump is started to vacuumize the mould through the vacuum-pumping pipeline 8; after a certain time, closing the vacuumizing valve 80, opening the soaking valve 510 to inject the impregnating agent into the mold cavity, ensuring that the whole fiber fabric reinforcement is in the impregnating agent, closing the soaking valve 510, after soaking for a certain time, opening the nitrogen gas inlet valve 90, opening the soaking valve 510, and introducing the nitrogen gas to make the impregnating agent in the mold flow back to the impregnating agent container 5 to finish fiber soaking.
Then, the soaking valve 510 and the nitrogen gas inlet valve 90 are closed, and the vacuum valve 80 is opened to vacuumize the mold again; after a certain time, the evacuation valve 80 is closed.
And (3) starting the RIM machine to inject the dicyclopentadiene combined material into the buffer container, starting the material injection valve 620 when the volume of the container is half of that of the container, so that the dicyclopentadiene combined material enters the die cavity from the buffer container, and closing the flash valve 70 until the material overflows. In the process, the RIM machine is stopped in advance according to the preset injection amount, and the dicyclopentadiene composite material is just enabled to completely enter the die cavity.
After the material is injected, the combined material is remained in the container and the pipeline, and the combined material can be polymerized and block the pipeline, so that the container and the pipeline are immediately cleaned by using a solvent after the material is injected.
Specifically, the wetting line 51 and the filling line 62 are merged and then connected to the inlet 2 of the mold through a hose section 20. The hose segment 20 is provided with a hose pressing device 200, and the hose pressing device 200 is an automatic control pressing mechanism and is immediately pressed after the flash is injected so as not to cause the backflow of the material. The hose section 20 is disposable and is replaced after each injection molding.
The buffer container 6 is connected with a washing solvent pipeline 63 for introducing washing solvent through the pipeline after the material injection is finished. The infiltration valve 510 is a three-way valve, and is connected to a washing waste collection device in addition to controlling the opening and closing of the infiltration pipe 51. After the material injection is finished, the washing solvent is introduced through the washing solvent pipeline 63, the materials in the buffer container and the pipeline are washed to prevent solidification and blockage, and the washing waste is collected in the washing waste collection device.
In other embodiments of the device for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material, if the fiber fabric is easy to fix and is not easy to be damaged by the dicyclopentadiene composite material entering the mold cavity, the buffer container 6 can be omitted, the injection material outlet of the injection machine is directly connected with the feed inlet 2, and the dicyclopentadiene composite material injected by the injection machine directly enters the mold cavity without being buffered to be compounded with the soaked fiber fabric. In other implementation cases, the flash collecting container 7 can be omitted, and a three-way valve is connected to the flash port of the mold to realize the respective connection with the vacuum-pumping pipeline 8 and the nitrogen gas introducing pipeline 9.
Secondly, the specific embodiment of the method for preparing the fiber fabric reinforced polydicyclopentadiene composite material by using the dicyclopentadiene composite material
Example 2
In the method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material, the device in the embodiment 1 is adopted, and the produced fiber fabric reinforced polydicyclopentadiene composite material consists of a polydicyclopentadiene matrix and a fiber fabric compounded in the polydicyclopentadiene matrix, wherein the fiber fabric reinforcement is a multilayer glass fiber felt which is laminated at different angles and is sewn in the vertical direction by glass fibers. In the composite material, the mass fraction of the fiber fabric reinforcement is 40%.
The upper and lower end edges (one end is positioned at the side of the feeding port and the other end is positioned at the side of the flash port) of the multilayer glass fiber mat are respectively bonded with the quick-drying adhesive on the back of the product. The adhesive fixation can be realized by using a commercially available quick-drying adhesive, such as 502 adhesive, to bond the edges of the fiber fabric reinforcement, and the adhesive fixation can be realized by using a dispensing method, so that the adhesive is used as little as possible and the surface is prevented from being penetrated by the adhesive on the premise of fixation, and the mark is prevented from being formed on the surface of the product.
In other implementation cases, when the fiber fabric reinforcement is bonded and fixed after being laid, the top and the bottom can be bonded and fixed according to needs, and whether other positions are fixed or not can be determined, so that the fiber fabric reinforcement can be kept in a close laying state with a mold in the forming process. Because the speed that reaction material got into the die cavity is comparatively gentle, does not have too high requirement to the fixed intensity of bonding, and on the contrary, lower fixed intensity is more favorable to the drawing of patterns on the contrary.
Firstly, infiltrating a plurality of layers of glass fiber mats by using an impregnating compound, wherein the impregnating compound comprises the following components in percentage by mass: 90% dicyclopentadiene, 10% ethylidene norbornene. In other embodiments, an organometallic activator component, such as an aluminum alkyl, may be further added to further improve the fiber wet out.
And then, vacuumizing the die cavity, and forming negative pressure in the die cavity and the buffer container. Mixing the two-component polymer material with an injection machine, injecting the mixture into a buffer container, opening a material injection valve when the volume of the reaction material reaches half of the volume of the buffer container, injecting the reaction material into a mold under negative pressure, filling the reaction material from the bottom of a mold cavity upwards, and taking out a product after curing.
The two-component polymer may be a commercially available two-component material in which one component comprises a tungsten or molybdenum procatalyst and the other component comprises an organoaluminum activator. The two components were mixed efficiently in a ratio of 1:1 in a high pressure injection machine. The curing time of the reaction material without retarder is about 5 minutes, a proper operation time window is determined according to the size of the product, and the retarder is added in a proper amount to prolong the curing time to 8-20 minutes.
Example 3
The method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material is different from the method in example 2 in that the bonding point between the fiber fabric and the mold is increased, the bonding force of the whole fiber fabric is improved, the buffering of a buffer container is not needed during feeding, and the injection machine directly injects the material from the inlet of the mold.
Example 4
The method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material of the embodiment is different from the method of the embodiment 2 in that the impregnating compound comprises the following components in percentage by mass: 98% of styrene and 2% of diethyl aluminum monochloride.
The tensile strength and the flexural modulus of the composite material prepared by the process are improved by 30-50% (relative to a polydicyclopentadiene matrix), the aim of reinforcing the polydicyclopentadiene material by using the fiber fabric reinforcement is fulfilled, the distribution and infiltration effects of the fiber fabric reinforcement are ensured, and the performance consistency of the obtained material is good. More importantly, the method for preparing the fiber fabric reinforced composite material by combining the two-component combined material with an industrial reaction injection machine is implemented smoothly, and has high efficiency and low cost.
By applying the technical scheme of the invention, the in-situ infiltration, negative pressure liquid absorption forming and slow polymerization of the combined material of the fiber fabric reinforcement are combined, so that the large-scale production of the fiber fabric reinforced polydicyclopentadiene composite material product can be realized, the product has excellent mechanical properties, and the whole process has the advantages of low cost and short manufacturing period.

Claims (10)

1. A method for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material is characterized by comprising the following steps: firstly, fixing a fiber fabric reinforcement in a mold, wherein the mold comprises a flash port and a feed port; secondly, after the mould is vacuumized, the impregnating compound enters the mould to carry out in-situ infiltration on the fiber fabric reinforcement, and then the impregnating compound is discharged; then, the dicyclopentadiene composite material enters a mould, is solidified, demoulded and taken out.
2. The method of claim 1, wherein the fixing is adhesive fixing.
3. The method of claim 2, wherein the bonding is performed at a location on the opposite side of the article.
4. The method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material as claimed in any one of claims 1 to 3, wherein the dicyclopentadiene composite material is put into a mould by adopting the following method: the dicyclopentadiene composite material is firstly injected into a buffer container by an injection machine and then enters a mould from the buffer container under the action of negative pressure.
5. The method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composite material as claimed in claim 1, wherein the impregnating compound is fed into the mold from a feeding port for the in-situ impregnation, and the discharging the impregnating compound is performed by introducing gas into the mold from the overflow port and pressing the impregnating compound out from the feeding port.
6. The method for preparing the fiber fabric reinforced polydicyclopentadiene composite material from the dicyclopentadiene composition as claimed in claim 1 or 5, wherein the sizing agent comprises one or more of cyclopentadiene, dicyclopentadiene, norbornene, ethylidene norbornene, terpene, and styrene, with or without the addition of an organometallic, and the organometallic is an activator component of the dicyclopentadiene composition.
7. A device for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material is characterized by comprising the following components:
the injection machine is used for injecting the dicyclopentadiene composite material;
the forming die comprises a die cavity, a feeding hole and an overflow hole, wherein the die cavity is used for laying a fiber fabric reinforcement and receiving a dicyclopentadiene composite material;
the vacuumizing device is connected with the overflow port of the forming die and is used for vacuumizing the die cavity;
and the impregnating agent container is connected with the feed inlet of the forming die and is used for introducing the impregnating agent into the die cavity.
8. The apparatus for preparing a fiber fabric reinforced polydicyclopentadiene composite material from a dicyclopentadiene composite material as claimed in claim 7, further comprising: and the buffer container is provided with an inlet and an outlet, the inlet is connected with the injection machine, and the outlet is connected with a feed inlet of the forming die.
9. The apparatus for preparing polydicyclopentadiene composite material reinforced by fiber fabric according to claim 7, wherein the forming mold is connected with a blowing device for blowing air into the mold cavity to press the sizing agent back into the sizing agent container.
10. The apparatus for preparing fiber fabric reinforced polydicyclopentadiene composite material from dicyclopentadiene composite material as claimed in claim 9, wherein the flash port of the forming mold is connected to a flash collecting container, and the blowing means comprises a blowing pipeline connected to the flash collecting container, and the gas enters the mold cavity from the blowing pipeline through the flash collecting container.
CN202110699636.XA 2021-06-23 2021-06-23 Method and device for preparing fiber fabric reinforced polydicyclopentadiene composite material from dicyclopentadiene composite material Pending CN113400683A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115302820A (en) * 2022-07-19 2022-11-08 陈宗良 Resin mixing device and method
CN115489091B (en) * 2022-11-16 2023-01-31 淄博鲁华泓锦新材料集团股份有限公司 Polymerization reaction-based polydicyclopentadiene tube continuous extrusion device and process
CN115895160A (en) * 2022-12-28 2023-04-04 东实汽车科技集团股份有限公司 Polyester fiber reinforced polydicyclopentadiene composite material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115302820A (en) * 2022-07-19 2022-11-08 陈宗良 Resin mixing device and method
CN115489091B (en) * 2022-11-16 2023-01-31 淄博鲁华泓锦新材料集团股份有限公司 Polymerization reaction-based polydicyclopentadiene tube continuous extrusion device and process
CN115895160A (en) * 2022-12-28 2023-04-04 东实汽车科技集团股份有限公司 Polyester fiber reinforced polydicyclopentadiene composite material and preparation method thereof

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