Preparation method and preparation device of tape paving material master batch with adjustable resin in thickness direction

Abstract

The invention belongs to the technical field of preparation of carbon fiber composite materials, and particularly relates to a preparation method and a preparation device of a tape laying master batch with adjustable resin in the thickness direction. According to the method, a reinforcing material is impregnated for the first time by utilizing a first pair of adhesive films, then the impregnated prepreg is impregnated for the second time by utilizing a second pair of adhesive films, and the resin content ratio in each group of adhesive films is controlled by controlling the impregnation conditions in the two impregnation processes and controlling the resin content ratio in each group of adhesive films, so that the resin content ratio in the prepreg is controlled under the condition that the adhesive film formula is qualitative. The tape laying master batch with impregnation degree and surface viscosity can be obtained, and the obtained prepreg has stable physical and chemical properties.

Description

Technical Field

[0001] The invention belongs to the technical field of carbon fiber composite material preparation, and in particular relates to a method and a device for preparing a tape masterbatch with adjustable resin in thickness direction. Background Art

[0002] Carbon fiber reinforced resin-based composite materials are currently widely used in various fields of the national economy, such as military industry, aerospace, etc. The current molding methods mostly use autoclave process, vacuum introduction process, hot molding process, etc. The implementation of these molding processes requires a lot of manpower, and for complex parts, the molding efficiency is slow, and the deviation of the fiber angle during laying is large. At present, domestic automatic laying technology has begun to take off, and various military aircraft and civil aircraft manufacturers have begun to use automatic laying technology (automatic tape laying technology, automatic wire laying technology) to produce related parts.

[0003] The quality of parts produced by automatic placement technology is related to the molding equipment on the one hand, and the raw materials used (tape laying materials, wire laying materials) are also important factors affecting the product quality and molding rate of the parts on the other hand.

[0004] Automatic tape laying prepreg is suitable for small curvature and large flat parts. During use, the tape laying material requires a certain high impregnation degree and a high surface viscosity. For thermosetting resin fiber prepreg, the impregnation degree and surface viscosity are contradictory. For the same thermosetting resin prepreg, the increase in the material impregnation degree will inevitably cause the material surface viscosity to decrease, and vice versa. When the resin formula is finalized, achieving both material impregnation degree and surface viscosity by adjusting the prepreg molding process is the key and difficulty in preparing prepreg suitable for tape laying. Summary of the invention

[0005] In view of the above problems existing in the prior art, the present invention provides a method and a device for preparing a tape masterbatch with adjustable resin in thickness direction, which can provide a prepreg with both impregnation degree and surface viscosity without changing the resin film formula.

[0006] To achieve the above object, the technical solution provided by the present invention is as follows:

[0007] In the first aspect, the present application provides a method for preparing a masterbatch of tape material with adjustable resin in the thickness direction, comprising the following steps: first, using a first pair of adhesive films to perform a first impregnation of a reinforcing material to obtain an impregnated prepreg; then, using a second pair of adhesive films to perform a second impregnation of the impregnated prepreg to obtain the tape material masterbatch; the temperature of the first impregnation process is 90-110°C, and the roller pressure is 0.4-0.7MPa; the temperature of the second impregnation process is 50-60°C, and the roller pressure is 0.2-0.3MPa.

[0008] Optionally, the weight of the resin in the second pair of adhesive films accounts for 10%-50% of the resin in the tape masterbatch.

[0009] Optionally, the first pair of adhesive films include a first upper adhesive film and a first lower adhesive film, and the first upper adhesive film and the first lower adhesive film are respectively bonded to the upper and lower surfaces of the reinforcing material; the second pair of adhesive films include a second upper adhesive film and a second lower adhesive film, and the second upper adhesive film and the second lower adhesive film are respectively bonded to the upper and lower surfaces of the impregnated prepreg.

[0010] Optionally, the first pair of adhesive films and the second pair of adhesive films are made of the same resin.

[0011] Optionally, the reinforcing material is carbon fiber, glass fiber or aramid fiber.

[0012] Optionally, the weight of the resin in the second pair of adhesive films accounts for 10%-30% of the resin in the tape masterbatch.

[0013] Optionally, the adhesive film is a thermosetting resin.

[0014] Optionally, the adhesive film is epoxy resin, bismaleimide resin, cyanate resin or phenolic resin.

[0015] Optionally, the first impregnation of the reinforcing material by the first pair of adhesive films specifically includes the following steps: first, the first upper adhesive film, the reinforcing material and the first lower adhesive film, which are sequentially attached to each other from top to bottom, enter the first impregnation roller A, and then pass through the first heating plate, at least one group of first impregnation rollers B and the first cooling plate in sequence to complete the first impregnation process and obtain the impregnated prepreg.

[0016] Optionally, the second pair of adhesive films impregnates the prepreg for the second time, specifically comprising the following steps: first, peeling off the upper release paper of the impregnated prepreg, and then laminating the second upper adhesive film to the upper surface of the impregnated prepreg, and at the same time peeling off the lower release paper of the impregnated prepreg, and laminating the second lower adhesive film to the lower surface of the impregnated prepreg, and completing the second impregnation process after being processed by the second impregnation roller A, the second heating plate, at least one group of second impregnation rollers B and the second cooling plate in sequence.

[0017] Optionally, after the second impregnation, the masterbatch of the tape material is rolled up after being coated with a glue film, and then the upper surface is attached to the PE film and squeezed by a PE film roller and rolled up.

[0018] In the second aspect, the present application provides a preparation device for a tape masterbatch with adjustable resin in the thickness direction based on the preparation method described in the first aspect, comprising a first impregnation roller A, a first heating plate, three groups of first impregnation rollers B, a first cooling plate, a first traction roller, a second traction roller, a second impregnation roller A, a second heating plate, three groups of second impregnation rollers B and a second cooling plate, a third traction roller, a PE film pressing roller and a prepreg winding shaft connected in sequence;

[0019] The feed end of the first impregnation roller A is connected to the first upper film unwinding device, the reinforcing material feeding device and the first lower film unwinding device; the discharge end of the first traction roller is also connected to the first upper film release paper roller; the feed end of the second traction roller is also connected to the second upper film unwinding device; the discharge end of the second traction roller is also connected to the first lower film release paper roller; the feed end of the second impregnation roller A is also connected to the second lower film unwinding device; the discharge end of the third traction roller is also connected to the second upper film release paper roller; the feed end of the PE film pressing roller is also connected to the PE film unwinding roller.

[0020] Compared with the prior art, this application has at least the following beneficial effects:

[0021] The present invention first uses a first pair of adhesive films to perform a first impregnation of the reinforcing material, and then uses a second pair of adhesive films to perform a second impregnation of the impregnated prepreg. When the first pair of adhesive films are used to impregnate the reinforcing material for the first time, the impregnation temperature and the impregnation pressure are kept in a relatively high range. The impregnation treatment under this temperature and pressure can make the resin and the reinforcing material have a relatively high degree of impregnation, and at the same time, the resin partially reacts to improve the overall stiffness of the prepreg; and when the second pair of adhesive films are used for the second impregnation, a relatively low impregnation temperature is maintained to reduce the degree of resin reaction, thereby providing a guarantee for the overall viscosity of the prepreg. By controlling the impregnation conditions of the two impregnation processes and controlling the proportion of the resin content in each group of adhesive films, a masterbatch of tape material with both impregnation degree and surface viscosity can be obtained under the condition of qualitative formulation of the adhesive films, and the physical and chemical properties of the obtained prepreg are stable. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic diagram of the structure of a device for preparing a tape masterbatch with adjustable resin in thickness direction in an embodiment of the present application;

[0023] Description of reference numerals:

[0024] 1. Reinforcement material feeding device; 2. First upper film unwinding device; 3. First lower film unwinding device; 4. First impregnation roller A; 5. First heating plate; 6. First impregnation roller B; 7. First cooling plate; 8. First traction roller; 9. First upper film release paper roller; 10. Second upper film unwinding device; 11. Second traction roller; 12. First lower film release paper roller; 13. Second lower film unwinding device; 14. Second impregnation roller A; 15. Second heating plate; 16. Second impregnation roller B; 17. Second cooling plate; 18. Third traction roller; 19. Second upper film release paper roller; 20. PE film unwinding roller; 21. PE film pressing roller; 22. Prepreg winding shaft. DETAILED DESCRIPTION

[0025] The present invention is further described in detail below in conjunction with the accompanying drawings:

[0026] The experimental methods used in the embodiments of the present invention are conventional methods unless otherwise specified.

[0027] The reagents and materials used in this example can all be purchased conventionally. The quantitative experiments involved in the examples were repeated at least three times, and the results were averaged.

[0028] Example 1

[0029] A preparation device for a tape masterbatch with adjustable resin in thickness direction, the structure of which is as follows Figure 1 As shown, it includes a first impregnation roller A4, a first heating plate 5, three groups of first impregnation rollers B6, a first cooling plate 7, a first traction roller 8, a second traction roller 11, a second impregnation roller A14, a second heating plate 15, three groups of second impregnation rollers B16 and a second cooling plate 17, a third traction roller 18, a PE film pressing roller 21 and a prepreg winding shaft 22 connected in sequence;

[0030] The feed end of the first impregnation roller A4 is connected to the first upper film unwinding device 2, the reinforcing material feeding device 1 and the first lower film unwinding device 3; the discharge end of the first traction roller 8 is also connected to the first upper film release paper roller 9; the feed end of the second traction roller 11 is also connected to the second upper film unwinding device 19; the discharge end of the second traction roller 11 is also connected to the first lower film release paper roller 12; the feed end of the second impregnation roller A14 is also connected to the second lower film unwinding device 13; the discharge end of the third traction roller 18 is also connected to the second upper film release paper roller 19; the feed end of the PE film pressing roller 21 is also connected to the PE film unwinding roller 20.

[0031] The above device is used to prepare a tape masterbatch with adjustable resin in thickness direction, and the steps are as follows:

[0032] First, the first upper glue film and the first lower glue film are drawn out from the glue film unwinding device, and are respectively compounded with the upper and lower surfaces of the reinforcing material, and then pass through the first impregnation roller A4, and the temperature and pressure of the first impregnation roller A4 make the first upper glue film and the first lower glue film melt and impregnate into the reinforcing material, and then pass through the first heating plate 5, three groups of first impregnation rollers B6, and then cool through the first cooling plate 7 to obtain the impregnated prepreg;

[0033] Then the impregnated prepreg is pulled by the first traction roller 8, and after the upper release paper is peeled off, the second upper adhesive film is drawn out through the adhesive film unwinding device 10, and combined with the upper surface of the impregnated prepreg, it enters the second traction roller 11, and after the lower release paper is peeled off, the second lower adhesive film is drawn out through the second lower adhesive film unwinding device 13, and combined with the lower surface of the impregnated prepreg, it enters the second impregnation roller A14 for impregnation, and then passes through the second heating plate 15, three groups of second impregnation rollers B16 and the second cooling plate 17 in sequence to complete the second impregnation process;

[0034] Finally, the tape masterbatch after the second impregnation is drawn out by the third traction roller 18 and rolled up through the adhesive film release paper, and then the upper surface is attached to the PE film released from the PE film unwinding roller 20 and is squeezed by the PE film pressing roller 21 and then rolled up.

[0035] The weight of the first upper film and the first lower film is 44g / m 2 The weight of the second upper film and the second lower film are 10g / m 2 .

[0036] During the first impregnation process, the temperature of the first impregnation roller A and the first impregnation roller B was 100°C, and the roller pressure was controlled at 0.6MPa;

[0037] During the second impregnation process, the temperature of the second impregnation roller A and the second impregnation roller B was controlled between 55° C., and the roller pressure was controlled at 0.25 MPa.

[0038] The temperature of the first heating plate is 115°C, and the temperature of the first cooling plate is 18±3°C; the temperature of the second heating plate is 80°C, and the temperature of the second cooling plate is 18±3°C.

[0039] Among them, the production speed is 3m / min, winding.

[0040] In this embodiment, Hengshen HF40F-12K fiber is used as the reinforcing material, and the adhesive film is made of Hengshen's high-temperature curing epoxy resin; the resin content of the prepared tape masterbatch is 35%, and the fiber surface density is 200g / m 2 The width of the tape masterbatch is 1000 mm. The upper and lower adhesive films of the tape masterbatch prepared by the present invention have the same gram weight, the resin content and resin state of the upper and lower surfaces of the prepreg are symmetrical, and the stability is better.

[0041] Example 2

[0042] The difference between this embodiment and embodiment 1 is that: during the first impregnation process, the temperature of the first impregnation roller A and the first impregnation roller B is 90° C., and the roller pressure is controlled at 0.7 MPa;

[0043] During the second impregnation process, the temperature of the second impregnation roller A and the second impregnation roller B was controlled between 50° C., and the roller pressure was controlled at 0.3 MPa.

[0044] Example 3

[0045] The difference between this embodiment and embodiment 1 is that the temperature of the first impregnation roller A and the first impregnation roller B is 110° C., and the roller pressure is controlled at 0.4 MPa;

[0046] During the second impregnation process, the temperature of the second impregnation roller A and the second impregnation roller B was controlled between 60° C., and the roller pressure was controlled at 0.2 MPa.

[0047] Comparative Example 1

[0048] The first upper glue film and the first lower glue film are drawn out from the glue film unwinding device, and are respectively compounded with the upper and lower surfaces of the reinforcing material, and then passed through the first impregnation roller A4, and the temperature and pressure of the first impregnation roller A4 make the first upper glue film and the first lower glue film melt and impregnate into the reinforcing material, and then sequentially pass through the first heating plate 5, three groups of first impregnation rollers B6, and then are cooled by the first cooling plate 7 to obtain the impregnated prepreg; and rolled up to obtain the masterbatch of the tape laying material;

[0049] The weight of the first upper film and the first lower film is 44g / m 2 ;

[0050] The temperature of the first impregnation roller A and the first impregnation roller B is 90-110°C, and the roller pressure is controlled at 0.4-0.7Mpa;

[0051] The temperature of the first heating plate is 115°C, and the temperature of the first cooling plate is 18±3°C;

[0052] Among them, the production speed is 3m / min, winding.

[0053] Comparative Example 2

[0054] The difference between this comparative example and comparative example 1 is that the temperature of the first impregnation roller A and the first impregnation roller B is controlled between 50-60° C., and the roller pressure is controlled between 0.2-0.3 MPa.

[0055] The double film impregnation production process prepared by the methods of Comparative Examples 1 and 2 cannot ensure that the impregnation degree and surface viscosity (referring to the adhesion between prepregs) meet the requirements. The impregnation degree of the tape masterbatch obtained in Comparative Example 1 is 4-6, but the bonding between the materials is not firm (when two layers of prepreg are pressed together, there is a partial separation between the layers without external force), and it is easy to separate. Although the tape masterbatch obtained in Comparative Example 2 has good viscosity and can achieve firm bonding between the materials, the impregnation degree is only 2-3.

[0056] By using the preparation method in the examples, the impregnation degree of the tape masterbatch can be above level 4, among which Example 1 is level 6, Example 2 is level 5, and Example 3 is level 5, and the surface viscosity of the prepregs prepared in Examples 1 to 3 can achieve bonding between the tape masterbatches at room temperature, and the bonding is firm (when two layers of prepreg are pressed together, there is no separation between the layers without external force).

[0057] The impregnation test method in this application is as follows:

[0058] 1. Cut the carbon fiber unidirectional prepreg with a size of 20cm*5cm (20cm is the width dimension of the prepreg, and 5cm is the length dimension of the prepreg);

[0059] 2. Tear off the protective film or release paper on the upper and lower surfaces of the prepreg, stick the upper and lower surfaces with pressure-sensitive tape, and compact them;

[0060] 3. Tear the pressure-sensitive tape with force, and determine the impregnation degree based on the remaining fibers of the upper and lower pressure-sensitive tapes. The higher the impregnation degree, the higher the degree of impregnation of the prepreg. See Table 1 for the impregnation degree evaluation standard.

[0061] Table 1 Evaluation criteria for impregnation degree

[0062] degree of impregnation Judgment criteria Level 2 The prepreg is severely delaminated (≥10cm), the fibers are clustered and very dry Level 3 The prepreg is severely delaminated (≥10cm), the hair is gathered and very dry Level 4 The prepreg sample has delamination between one quarter and half of the sample length (5cm-10cm), with a lot of hair and not dry. Level 5 Although the prepreg sample only has delamination within a quarter of the sample length (≤5cm), there are a lot of hairs and it is dry. Level 6 Although the prepreg sample only showed delamination within a quarter of the sample length (≤5cm), it had less hair and was dry.

Claims

1. A method for preparing a tape masterbatch with adjustable resin in thickness direction, characterized in that: The method comprises the following steps: firstly, using a first pair of adhesive films to carry out a first impregnation of the reinforcing material to obtain an impregnated prepreg; then using a second pair of adhesive films to carry out a second impregnation of the impregnated prepreg to obtain the tape masterbatch; the temperature of the first impregnation process is 90-110°C, and the roller pressure is 0.4-0.7MPa; the temperature of the second impregnation process is 50-60°C, and the roller pressure is 0.2-0.3MPa.

2. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The weight of the resin in the second pair of adhesive films accounts for 10%-50% of the resin in the tape masterbatch.

3. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The first pair of adhesive films includes a first upper adhesive film and a first lower adhesive film, which are respectively bonded to the upper and lower surfaces of the reinforcing material; the second pair of adhesive films includes a second upper adhesive film and a second lower adhesive film, which are respectively bonded to the upper and lower surfaces of the impregnated prepreg.

4. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The first pair of films and the second pair of films are made of the same resin.

5. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The reinforcing material is carbon fiber, glass fiber or aramid fiber.

6. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 2, characterized in that: The weight of the resin in the second pair of adhesive films accounts for 10%-30% of the resin in the tape masterbatch.

7. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The first impregnation of the reinforcing material by the first pair of adhesive films specifically includes the following steps: first, the first upper adhesive film, the reinforcing material and the first lower adhesive film, which are sequentially attached from top to bottom, enter the first impregnation roller A, and then pass through the first heating plate, at least one group of first impregnation rollers B and the first cooling plate in sequence to complete the first impregnation process and obtain the impregnated prepreg.

8. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 1, characterized in that: The second pair of adhesive films impregnates the prepreg after the impregnation for the second time, which specifically includes the following steps: first, peeling off the upper release paper of the prepreg after the impregnation, then laminating the second upper adhesive film to the upper surface of the prepreg after the impregnation, and at the same time peeling off the lower release paper of the prepreg after the impregnation, and laminating the second lower adhesive film to the lower surface of the prepreg after the impregnation, and completing the second impregnation process after being processed by the second impregnation roller A, the second heating plate, at least one group of second impregnation rollers B and the second cooling plate in sequence.

9. The method for preparing a tape masterbatch with adjustable resin in thickness direction according to claim 7, characterized in that: After the second impregnation, the masterbatch of the tape material is rolled up after being coated with a glue film, and the upper surface is attached to the PE film and squeezed by a PE film roller before being rolled up.

10. A device for preparing a tape masterbatch with adjustable resin in thickness direction based on the preparation method according to any one of claims 1 to 9, characterized in that: It includes a first impregnation roller A, a first heating plate, three groups of first impregnation rollers B, a first cooling plate, a first traction roller, a second traction roller, a second impregnation roller A, a second heating plate, three groups of second impregnation rollers B and a second cooling plate, a third traction roller, a PE film pressing roller and a prepreg winding shaft connected in sequence; The feed end of the first impregnation roller A is connected to the first upper film unwinding device, the reinforcing material feeding device and the first lower film unwinding device; the discharge end of the first traction roller is also connected to the first upper film release paper roller; the feed end of the second traction roller is also connected to the second upper film unwinding device; the discharge end of the second traction roller is also connected to the first lower film release paper roller; the feed end of the second impregnation roller A is also connected to the second lower film unwinding device; the discharge end of the third traction roller is also connected to the second upper film release paper roller; the feed end of the PE film pressing roller is also connected to the PE film unwinding roller.

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