CN110576626A - Preparation method of composite material premix - Google Patents

Preparation method of composite material premix Download PDF

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Publication number
CN110576626A
CN110576626A CN201910755400.6A CN201910755400A CN110576626A CN 110576626 A CN110576626 A CN 110576626A CN 201910755400 A CN201910755400 A CN 201910755400A CN 110576626 A CN110576626 A CN 110576626A
Authority
CN
China
Prior art keywords
premix
heat treatment
resin
preparing
fibers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910755400.6A
Other languages
Chinese (zh)
Inventor
谢钟清
陈志诚
田杰
李涛
郭金海
毕华阳
常舰
刘启抱
李世成
柯常宜
林维飞
李朋欣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Composite Material Science and Technology Co Ltd
Original Assignee
Shanghai Composite Material Science and Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Composite Material Science and Technology Co Ltd filed Critical Shanghai Composite Material Science and Technology Co Ltd
Priority to CN201910755400.6A priority Critical patent/CN110576626A/en
Publication of CN110576626A publication Critical patent/CN110576626A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • B29C70/44Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding
    • B29C70/443Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding and impregnating by vacuum or injection
    • 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
    • B29K2061/00Use of condensation polymers of aldehydes or ketones or derivatives thereof, as moulding material
    • B29K2061/04Phenoplasts
    • 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/12Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of short lengths, e.g. chopped filaments, staple fibres or bristles

Abstract

the invention provides a preparation method of a composite material premix; the method comprises the following steps: a: uniformly laying the fibers on a platform, and uniformly mixing the resin and the fibers in a vacuum flow guide manner; b: and carrying out heat treatment and cutting on the mixed mixture to prepare the chopped fiber premix. The invention has the following beneficial effects: the fiber and the resin are mixed by adopting a vacuum diversion mode, so that the uniform mixing of the fiber and the resin can be ensured, and the condition that the fiber is not completely soaked is reduced. The heat treatment method can remove unnecessary volatile components in the premix, thereby improving the internal quality of the composite material prepared from the premix. The method can improve the production efficiency and is friendly to human body and environment.

Description

preparation method of composite material premix
Technical Field
The invention relates to a preparation method of a composite material premix, in particular to a preparation method of a composite material intermediate state formed by mixing carbon fibers and phenolic resin.
background
composite materials have found widespread use in many applications because of the many properties that are not possessed by a single material. Generally, the preparation process of polymer-based composite materials includes a one-step process and a two-step process, wherein the two-step process comprises mixing and impregnating fiber resins in advance to form a semi-finished product, and then forming a composite material product from the semi-finished product. The chopped fibers and the resin are mixed to form a semi-finished product, namely the composite material premix. The prior composite material premix is prepared by the way of firstly chopping fibers, then uniformly stirring the chopped fibers and resin and then carrying out heat treatment, and the prepreg prepared by the method has the defects of unstable quality, low production efficiency, poor production environment, harm to human bodies and the like due to the large use of manual operation.
The invention discloses a method for improving the toughness of a heat-resistant phenolic resin, which is found by searching the existing patent documents, and the Chinese patent application with the application number of 201811358259.8 discloses a method for improving the toughness of the heat-resistant phenolic resin, wherein the phenolic resin, (methyl) acrylic acid hydroxyl ester, modified sepiolite fiber, 2-acrylamide-2-methylpropanesulfonic acid, chitosan magnesium chelate, premix, stabilizer, antioxidant and demolding accelerator are added into a high-speed mixing mill to be uniformly mixed, and then the mixture is preformed in a mold and is hot-pressed. The fiber resin is uniformly stirred and then is subjected to heat treatment to prepare the composite material premix, and the defects of uneven fiber distribution, unstable quality and the like exist.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a composite material premix.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a composite material premix, which comprises the following steps:
A: laying the fibers on a platform, and uniformly mixing the resin and the fibers in a vacuum diversion manner to obtain a mixture;
B: and (3) performing heat treatment and cutting on the mixture to prepare the chopped fiber premix.
Preferably, the fibers are carbon fibers.
Preferably, the resin is a phenolic resin, and the state of the resin is a resin glue solution.
preferably, the step a specifically includes the following steps:
Laying a lower layer plastic film, a lower layer flow guide net, fibers, an upper layer flow guide net, a lower layer plastic film and sealing materials on the platform in sequence to form a sealed working space; two ends of the lower flow guide net are respectively communicated with two pipelines, one pipeline is connected with glue solution, the other pipeline is sequentially connected with a liquid collector and a vacuum source, and resin is fully paved with fibers by utilizing negative pressure generated by vacuum to complete mixing.
preferably, the heat treatment method is heat treatment by an oven or an autoclave; the heat treatment may also be performed by other heating devices.
Preferably, when the heat treatment method is to carry out heat treatment through an oven, the heat treatment temperature is 70-110 ℃, and the heat treatment time is 0.1-2 hours.
preferably, the mixture obtained in the step A needs to be kept still for 0-40 min.
preferably, the length of the mixture after cutting is 1-100 mm.
preferably, in step B, the cutting is performed after the heat treatment, or the cutting is performed before the heat treatment, or the heat treatment and the cutting are performed simultaneously.
Preferably, the platform is an aluminum plate.
Compared with the prior art, the invention has the following beneficial effects:
the fiber and the resin are mixed by adopting a vacuum diversion mode, so that the uniform mixing of the fiber and the resin can be ensured, and the condition that the fiber is not completely soaked is greatly reduced. The heat treatment method can remove unnecessary volatile components in the premix, thereby improving the internal quality of the composite material prepared from the premix. The method can improve the production efficiency and is friendly to human body and environment.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram of the preparation process of the composite premix;
FIG. 2 is a schematic diagram of the preparation of a premix by uniformly mixing fibers and resin;
FIG. 3 is a schematic view of conventional methods of fiber non-wetting; wherein, A is to form the large fiber bundle, B is to form the fiber cluster, C is to form the fiber bundle stuck with pile, D is to form the fiber bundle of the glue lacking after tearing open;
the device comprises a platform 1, a fiber 2, a lower flow guide net 3, an upper flow guide net 4, an upper plastic film 5, a lower plastic film 6, a sealing material 7, a first conversion head 8, a second conversion head 9, a plastic pipeline 10, a resin glue solution 11, a liquid collector 12, a second vacuum meter 13, a first vacuum meter 14 and a vacuum source 15, wherein the platform is arranged on the platform 1, the fiber 2 is arranged on the platform, the lower flow guide net 3 is arranged on the lower layer, the upper flow guide net 5 is arranged on the upper layer, the lower plastic film 6 is arranged on the.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment of the invention provides a preparation method of a composite material premix, which comprises a resin glue solution 11, an aluminum plate (a platform 1), fibers 2, a lower layer flow guide net 3, an upper layer flow guide net 4, silica gel (a sealing material 7), films (upper and lower layer plastic films 5 and 6), a liquid collector 12, a first conversion head 8, a second conversion head 9, a plastic pipeline 10 and a vacuumizing device, as shown in figure 1. The vacuum-pumping device comprises a vacuum source 15 connected with the liquid collector 12, and a second vacuum gauge 13 and a first vacuum gauge 14 which are sequentially arranged on a pipeline between the liquid collector 12 and the vacuum source 15.
the method comprises the following specific steps:
1. after the resin glue solution 11 (phenolic resin glue solution) is prepared, placing the resin glue solution into a container;
2. Carbon fibers are flatly laid on an aluminum plate paved with a plastic film, and a flow guide net is respectively arranged at the upper part and the lower part; the method specifically comprises the following steps: a lower layer plastic film 6, a lower layer flow guide net 3, fibers 2 (carbon fibers), an upper layer flow guide net 4, an upper layer plastic film 5 and a sealing material 7 are sequentially laid on the platform 1 (aluminum plate) from bottom to top to form a sealed working space;
3. One end of the lower layer flow guide net 3 is connected with a plastic pipeline 10 through a first conversion head 8 and is connected into a container filled with resin glue solution 11, and the other end is connected with the plastic pipeline through a second conversion head 9 and is sequentially connected with a liquid collector 12 and a vacuumizing device; the vacuum-pumping device comprises a vacuum source 15, a first vacuum gauge 14 and a second vacuum gauge 13 which are arranged on a connecting pipeline of the liquid collector 12 and the vacuum source 15;
4. Starting a vacuumizing device, and uniformly paving the resin on the fibers 2 by using negative pressure generated by vacuum to complete mixing;
5. standing the mixed mixture for 40 min;
6. Carrying out heat treatment on the mixed mixture through an oven, wherein the heat treatment temperature is 110 ℃, and the treatment time is 2 hours;
7. Chopping the mixture after heat treatment into chopped fiber premix with the length of 50 mm;
8. and sealing and storing the prepared composite material premix.
Example 2
The embodiment provides a preparation method of a composite material premix, which comprises the following steps:
1. Placing the phenolic resin glue solution into a container after the phenolic resin glue solution is prepared;
2. carbon fibers are flatly laid on an aluminum plate paved with a plastic film, and a flow guide net is respectively arranged at the upper part and the lower part; the specific operation was the same as in example 1;
3. one end of the diversion net is connected with the plastic pipeline and is placed in a container filled with resin glue solution, and the other end of the diversion net is connected with the plastic pipeline and is connected with the liquid collector and the vacuumizing device;
4. starting a vacuumizing device, and uniformly paving the resin with the fibers by using negative pressure generated by vacuum to complete mixing;
5. Standing the mixed mixture for 20 min;
6. Carrying out heat treatment on the mixed mixture through an oven, wherein the heat treatment temperature is 70 ℃, and the treatment time is 0.1 h;
7. Chopping the mixture after heat treatment into chopped fiber premix with the length of 100 mm;
8. And sealing and storing the prepared composite material premix.
example 3
The embodiment provides a preparation method of a composite material premix, which comprises the following steps:
1. Placing the phenolic resin glue solution into a container after the phenolic resin glue solution is prepared;
2. carbon fibers are flatly laid on an aluminum plate paved with a plastic film, and a flow guide net is respectively arranged at the upper part and the lower part; the specific operation was the same as in example 1;
3. one end of the diversion net is connected with the plastic pipeline and is placed in a container filled with resin glue solution, and the other end of the diversion net is connected with the plastic pipeline and is connected with the liquid collector and the vacuumizing device;
4. starting a vacuumizing device, and uniformly paving the resin with the fibers by using negative pressure generated by vacuum to complete mixing;
5. Carrying out heat treatment on the mixed mixture through an oven, wherein the heat treatment temperature is 90 ℃, and the treatment time is 1 h;
6. cutting the mixture after heat treatment into chopped fiber premix with the length of 1 mm;
7. And sealing and storing the prepared composite material premix.
the fibers and the resin are mixed in a vacuum diversion mode, so that the uniform mixing of the fibers and the resin can be ensured (wherein the arrangement of a diversion net is the key for enhancing the fluidity and the uniformity and finally obtaining the composite material premix), and the concrete figure is shown in fig. 2; the condition that the fiber is not completely infiltrated by the conventional method is greatly reduced, particularly as shown in figure 3, a large fiber bundle is formed (figure 3A), or a fiber cluster is formed (figure 3B), or a fiber bundle with a pile is adhered (figure 3C), or a fiber bundle with glue lacking after being torn off (figure 3D). Therefore, the invention can remove unnecessary volatile components in the premix by a heat treatment method, thereby improving the internal quality of the composite material prepared by the premix. The method can improve the production efficiency and is friendly to human body and environment.
the foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (10)

1. The preparation method of the composite material premix is characterized by comprising the following steps:
A: laying the fibers on a platform, and uniformly mixing the resin and the fibers in a vacuum diversion manner to obtain a mixture;
B: and (3) performing heat treatment and cutting on the mixture to prepare the chopped fiber premix.
2. the method for preparing the premix for composite materials according to claim 1, wherein the fiber is a carbon fiber.
3. the method for preparing a premix for composite materials according to claim 1, wherein the resin is a phenol resin in the state of a resin sol.
4. the method for preparing the premix for composite materials according to claim 1, wherein the step A comprises the following steps:
laying a lower layer plastic film, a lower layer flow guide net, fibers, an upper layer flow guide net, an upper layer plastic film and a sealing material on the platform from bottom to top in sequence to form a sealed working space; two ends of the lower flow guide net are respectively communicated with two pipelines, one pipeline is connected with glue solution, the other pipeline is sequentially connected with a liquid collector and a vacuum source, and resin is fully paved with fibers by utilizing negative pressure generated by vacuum to complete mixing.
5. The method for preparing the composite premix according to claim 1, wherein the heat treatment is performed by an oven or an autoclave.
6. The preparation method of the composite premix according to claim 5, wherein the heat treatment is performed in an oven at a temperature of 70 to 110 ℃ for 0.1 to 2 hours.
7. The method for preparing the premix for composite materials according to claim 1, wherein the mixture obtained in the step A is allowed to stand for 5-40 min.
8. the method for preparing the premix for composite materials according to claim 1, wherein the length of the mixture after cutting is 1 to 100 mm.
9. the method for preparing a premix for composite materials according to claim 1, wherein in the step B, the cutting is performed after the heat treatment, or the cutting is performed before the heat treatment, or the heat treatment and the cutting are performed simultaneously.
10. The method of preparing a composite premix of claim 1 wherein the platform is an aluminum plate.
CN201910755400.6A 2019-08-15 2019-08-15 Preparation method of composite material premix Pending CN110576626A (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112720916A (en) * 2020-12-08 2021-04-30 上海复合材料科技有限公司 Impregnation device and method for preparing chopped fiber premix

Citations (5)

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Publication number Priority date Publication date Assignee Title
DE19711247A1 (en) * 1997-03-18 1997-12-04 Thueringisches Inst Textil Thermoplastic pellets reinforced with natural fibres
CN105199297A (en) * 2015-10-13 2015-12-30 湖北三江航天江北机械工程有限公司 Bismaleimide resin premix with good dielectric property as well as preparation method and device of bismaleimide resin premix
CN205651673U (en) * 2016-01-27 2016-10-19 江苏恒神股份有限公司 Novel super thick combined material panel of leading -in preparation in vacuum device
CN106313579A (en) * 2015-06-19 2017-01-11 广州赛奥碳纤维技术有限公司 Short-cut tow prepreg tape preparation and mold pressing molding process
US10369754B2 (en) * 2017-02-03 2019-08-06 Oleksandr Biland Composite fibers and method of producing fibers

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19711247A1 (en) * 1997-03-18 1997-12-04 Thueringisches Inst Textil Thermoplastic pellets reinforced with natural fibres
CN106313579A (en) * 2015-06-19 2017-01-11 广州赛奥碳纤维技术有限公司 Short-cut tow prepreg tape preparation and mold pressing molding process
CN105199297A (en) * 2015-10-13 2015-12-30 湖北三江航天江北机械工程有限公司 Bismaleimide resin premix with good dielectric property as well as preparation method and device of bismaleimide resin premix
CN205651673U (en) * 2016-01-27 2016-10-19 江苏恒神股份有限公司 Novel super thick combined material panel of leading -in preparation in vacuum device
US10369754B2 (en) * 2017-02-03 2019-08-06 Oleksandr Biland Composite fibers and method of producing fibers

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* Cited by examiner, † Cited by third party
Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112720916A (en) * 2020-12-08 2021-04-30 上海复合材料科技有限公司 Impregnation device and method for preparing chopped fiber premix

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Application publication date: 20191217

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