KR100270090B1 - Process for preparing polyamideimide resin polymer composite - Google Patents
Process for preparing polyamideimide resin polymer composite Download PDFInfo
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- KR100270090B1 KR100270090B1 KR1019960070058A KR19960070058A KR100270090B1 KR 100270090 B1 KR100270090 B1 KR 100270090B1 KR 1019960070058 A KR1019960070058 A KR 1019960070058A KR 19960070058 A KR19960070058 A KR 19960070058A KR 100270090 B1 KR100270090 B1 KR 100270090B1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C53/00—Shaping by bending, folding, twisting, straightening or flattening; Apparatus therefor
- B29C53/56—Winding and joining, e.g. winding spirally
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Abstract
Description
본 발명은 용액상 폴리아미드아미드계 수지(이하, "PAI"수지라한다)를 이용하여 필라멘트 와인딩법으로 고분자 복합재료를 성형하는 방법에 관한 것이며, 보다 상세하게는 폴리아미드이미드계 수지를 용해시키고 섬유에 용해된 수지를 함침시켜 필라멘트 와인딩법으로 고분자복합재료를 성형하는 방법에 관한 것이다.The present invention relates to a method for forming a polymer composite material by filament winding method using a solution-like polyamide amide resin (hereinafter referred to as "PAI" resin), and more specifically, to dissolve the polyamide imide resin The present invention relates to a method of forming a polymer composite material by filament winding by impregnating a resin dissolved in fibers.
본 발명에서 사용되는 PAI수지를 성형하는 경우 종래에는 압축성형 및 사출성형등열에 의한 기계적 혼합방법만이 사용되었으나 열에 의한 기계적 혼합방법은 수지자체가 350℃이상의 고온에서만 용융이 되므로 가공하기 어려우며 또한 섬유강화제로서 장섬유를 사용할 수 없는 단점이 있는 것이다.In the case of molding the PAI resin used in the present invention, conventionally, only the mechanical mixing method by compression molding and injection molding isotherm was used, but the mechanical mixing method by heat is difficult to process because the resin itself is melted only at a high temperature of 350 ° C. or higher. There is a disadvantage that can not use long fibers as a reinforcing agent.
한편, 종래 필라멘트 와인딩 기법은 열경화성 수지의 성형에 사용되어 왔으나, 본 발명에서는 필라멘트 와인딩법으로 열가소성 수지를 성형하는 것이다.Meanwhile, the conventional filament winding technique has been used for molding thermosetting resins, but in the present invention, the thermoplastic resin is molded by the filament winding method.
이에 본 발명의 목적은 필라멘트와인딩법으로 열가소성 수지로 된 복합재료를 제조하는 방법을 제공하는 것이며, 나아가 본 발명의 또다른 목적은 필라멘트 와인딩법으로 폴리아미드이미드계 수지를 성형함으로써 가공이 용이하며, 제조된 성형물의 물성이 또한 우수하며 고온에서도 사용가능한 복합재료를 제조하는 방법을 제공하는 것이다.Accordingly, an object of the present invention is to provide a method for producing a composite material of thermoplastic resin by filament winding method, and further another object of the present invention is easy to process by molding a polyamideimide resin by filament winding method, It is to provide a method for producing a composite material which is also excellent in physical properties of the produced moldings and usable at high temperatures.
제1도는 필라멘트 와인딩법을 사용하여 종래의 에폭시 수지 및 본 발명에 의한 폴리아미드이미드수지로 제조된 시편의 마찰계수와 운동시간(sliding-time)과의 관계를 나타내는 그래프이다.1 is a graph showing the relationship between the friction coefficient and the sliding-time of a specimen made of a conventional epoxy resin and a polyamideimide resin according to the present invention using a filament winding method.
본 발명에 있어서, 폴리아미드이미드게 수지와 용매를 100:100∼300 중량비로 혼합함으로써 수지를 용매에 용해시켜 용액상 폴리아미드이미드계 수지를 제조하는 단계;및 탄소섬유에 상기 용액상 폴리아미드이미드계 수지를 함침한 후, 필라멘트 와인딩기법으로 성형하는 단계; 를 포함하는 복합재료 제조방법이 제공된다.In the present invention, the polyamideimide crab resin and the solvent in a 100: 100 to 300 weight ratio by dissolving the resin in a solvent to prepare a solution-like polyamideimide-based resin; and the solution-like polyamideimide to carbon fiber Impregnating the system resin and then molding the filament winding method; There is provided a composite material manufacturing method comprising a.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
종래 PAI 열가소성 수지 성형시에는 압출성형 및 사출성형등 열에 의한 기계적 혼합법만이 사용되어 왔으나, 본 발명은 필라멘트 와인딩법을 이용하여 PAI 수지로 복합재료를 제조하는 것이다.In the conventional PAI thermoplastic resin molding, only a mechanical mixing method by heat such as extrusion molding and injection molding has been used, but the present invention is to produce a composite material from PAI resin using a filament winding method.
즉, 종래의 기계적 혼합방법은 혼합기에서 350-370℃로 열에 의한 기계적 혼합방법으로 PAI수지와 탄소섬유를 혼합하고 여기에 첨가제를 첨가하여 혼합한 후 혼합되어진 수지를 다시 분쇄기에서 성형하기 편리한 크기로 분쇄하여 압축성형함으로써 성형하는 것이다.In other words, the conventional mechanical mixing method is a mechanical mixing method by heat at 350-370 ° C. in a mixer, and then mixes PAI resin and carbon fiber by adding an additive thereto, and then mixes the mixed resin into a convenient size for molding in a grinder. It is formed by grinding by compression molding.
이에 반하여, 본 발명에서는 PAI수지를 용매에 용해시켜 용액상 PAI 수지를 제조하고, 탄소섬유에 용액상 맴I 수지를 함침시킨 후 필라멘트 와인딩법으로 복합재료를 성형하게 된다.On the contrary, in the present invention, the PAI resin is dissolved in a solvent to prepare a solution PAI resin, and the carbon fiber is impregnated with the solution Mem resin, and then the composite material is molded by the filament winding method.
상기 본 발명에 사용되는 PAI 수지는 비결정성의 고온 엔지니어링 플라스틱으로 폴리이미드계 수지로서 폴리이미드에 비해 내열성이 약간 떨어지기는 하지만 성헝성은 월등히 뛰어나며 내크리프성은 열가소성 수지중 가장 뛰어난 기계적 특성을 갖는다.The PAI resin used in the present invention is an amorphous high-temperature engineering plastic, which is slightly inferior in heat resistance to polyimide as a polyimide-based resin, but has excellent mechanical properties and creep resistance.
또한 폴리이미드계 수지의 일반적인 특징인 내마모성이 매우 우수하고 유기용매에 대해 매우 안정하다.In addition, abrasion resistance, which is a general feature of polyimide resins, is very excellent and is very stable with respect to organic solvents.
상기 PAI 수지에 대한 용매로는 N-메틸피롤리돈(N-Methylpyrolidone: 이하, 단지 'NMP'라한다)을 이용하여 PAI 수지를 용해한다. 이때 PAI 수지와 NMP는 100:100∼300 중량비로 혼합한다. 용매의 비율이 100중량%이하인 경우에는 PAI수지가 용해되기 어려우며, 용해된다 하더라도 PAI 수지의 점도가 큼으로 수지가 섬유에 충분히 함침되기 어렵다. 용매의 비율이 300%이상인 경우 PAI 수지의 용해는 문제되지 않으며 과잉의 용매로 인하여 섬유에 대한 수지의 함침은 양호하나 많은 양의 수지가 함침되지 못하여 강도 증진을 기대하기 어렵다. NMP를 상기비율로 기계식 교반기(Mechanical stirrer)를 이용하여 2-3시간 혼합한다. 한편 상온에서 수지를 용해시키는데는 시간이 많이 걸리므로 100℃ 온도로 수지를 용해시키는 것이 바람직하다. 이렇게 준비되어진 PAI용액상 수지를 함침조에 넣고 수지 용액에 섬유를 통과시켜 섬유에 수지가 함침되도록 하고 필라멘팅 와인딩법으로 성형한다.As a solvent for the PAI resin, N-methylpyrrolidone (N-Methylpyrolidone: hereinafter referred to simply as 'NMP') is used to dissolve the PAI resin. At this time, PAI resin and NMP are mixed in a weight ratio of 100: 100 to 300. When the proportion of the solvent is 100% by weight or less, the PAI resin is difficult to dissolve, even if dissolved, the viscosity of the PAI resin is high, so that the resin is hardly sufficiently impregnated into the fiber. If the proportion of the solvent is more than 300%, dissolution of the PAI resin is not a problem, and the impregnation of the resin to the fiber is good due to the excess solvent, but it is difficult to expect the strength improvement because a large amount of the resin is not impregnated. NMP is mixed for 2-3 hours using a mechanical stirrer at the above ratio. On the other hand, since it takes a long time to dissolve the resin at room temperature, it is preferable to dissolve the resin at a temperature of 100 ℃. The PAI solution resin thus prepared is placed in an impregnation bath, and the fibers are passed through the resin solution so that the fibers are impregnated with resin and molded by filament winding.
성형후 PAI수지로 제조된 성형물을 경화장치에 넣어 200℃ 조건하에서 2-3시간 방치한다. 이때 제품속에 함유되어 있는 용매가 휘발되면서 제품으로 완성된다.After molding, the molded article made of PAI resin is placed in a curing apparatus and left for 2-3 hours under 200 ° C. At this time, the solvent contained in the product is volatilized to complete the product.
이하, 실시예를 통하여 본 발명에 대하여 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.
[실시예]EXAMPLE
본 실시예에서 고강도 자체윤활성 복합재료를 제조하기 위하여 사용된 원료중 강화섬유로는 고강도와 내마모성을 가진 탄소섬유를 사용하였으며 탄소섬유의 밀도는 1.80 g/㎤, 필라멘트 직경은 5.5 ㎛, 단위길이당 중량은 0.513 g/m, 그리고 탄성강도는 3920 MPa 이고 탄성율은 274 GPa 이다. 수지로는 에폭시 수지와 폴리아미드이미드수지를 사용하여 필라멘트 와인딩법으로 복합재료를 제조하았다. 폴리아미드이미드수지의 물성은 하기 표1 에 나타내었다.In this embodiment, carbon fiber having high strength and abrasion resistance was used as a reinforcing fiber among the raw materials used to prepare the high strength self-lubricating composite material. The density of the carbon fiber was 1.80 g / cm 3 and the filament diameter was 5.5 μm, per unit length. It has a weight of 0.513 g / m, an elastic strength of 3920 MPa and an elastic modulus of 274 GPa. As a resin, a composite material was prepared by filament winding using epoxy resin and polyamideimide resin. Physical properties of the polyamideimide resin are shown in Table 1 below.
에폭시 수지 및 폴리아미드이미드수지로 제조된 복합재 시편의 마모성을 측정하였다. 마모성은 내마모성을 필요로 하는 운동부위에서 중요시되는 특성인 마찰계수를 비교함으로써 평가하였다. 마모시험은 링-온-디스크(ring-on-disk)형태의 시험방법을 이용하여 상온에서 4시간 동안 수행하였다. 마모성을 측정하여 이로부터 마찰계수를 구하였으며, 종래의 에폭시 열경화성 수지 및 본 발명에 의한 PAI 열가소성 수지로 제조된 시편의 마찰계수와 운동시간(sliding-time)과의 관계를 제 1 도에 나타내었다.The wear properties of composite specimens made of epoxy resin and polyamideimide resin were measured. Abrasion was evaluated by comparing the friction coefficient, which is an important characteristic in the moving parts requiring wear resistance. The abrasion test was carried out at room temperature for 4 hours using a ring-on-disk type test method. The friction coefficient was calculated from the wearability, and the relationship between the friction coefficient and sliding-time of the specimen made of the conventional epoxy thermosetting resin and the PAI thermoplastic resin according to the present invention is shown in FIG. .
PAI 열가소성 수지를 이용하여 복합재를 제조한 경우에는 운동초기에 윤활피막이 형성되면서 마모시험이 끝날때까지 균일한 마찰계수를 나타내며, 또한 상당히 작은 마찰계수를 나타내어 운동중에도 안정함을 보인 반면 종래의 에폭시 필라멘트와인딩 제품의 경우에는 마찰계수가 상당히 불안정하며 마찰계수값 또한 크게 나타나 계속적인 운등부위에 사용이 어려움을 확인할 수 있다. 그리고 에폭시 필라멘트와인딩 제품의 경우 200℃이상에서 사용하기 어려운 반면 본 발명에 의한 PAI 필라멘트와인딩 제품은 수지의 고온특성이 우수하기 때문에 200℃이상에서도 사용가능한 것이다.In case of manufacturing composite material using PAI thermoplastic resin, lubricating film is formed at the beginning of the movement, it shows uniform coefficient of friction until the end of abrasion test, and also shows a very small coefficient of friction. In the case of winding products, the coefficient of friction is quite unstable, and the coefficient of friction is also large, which makes it difficult to use in continuous running areas. In the case of epoxy filament winding products, the PAI filament winding products according to the present invention are difficult to use at 200 ° C. or higher, and thus, the resin can be used even at 200 ° C. or higher.
이와같이 PAI 수지를 용매에 용해시킨 후 탄소섬유에 용액상 PAI 를 함침시켜 필라멘트와인딩법으로 복합재를 제조함으로써, 종래 에폭시 수지를 필라멘트 와인딩법으로 성형하는 경우에 비하여 성형물의 마찰계수등 마모특성이 개선되어 고온 운동부위에 열경화성 필라멘트 와인딩 제품으로 사용가능하며 200℃이상의 고온에서도 적용가능하며, 또한 PAI를 열성형법으로 성형하는 경우에 비하여 용이하게 가공할 수 있는 것이다.Thus, by dissolving PAI resin in a solvent and impregnating carbon fiber with solution phase PAI to produce a composite material by filament winding method, wear characteristics such as friction coefficient of the molded article is improved as compared to the case of molding an epoxy resin by filament winding method It can be used as a thermosetting filament winding product on high temperature moving parts, and can be applied even at high temperature of 200 ° C or higher, and can be easily processed as compared with the case of forming PAI by thermoforming method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102127894B1 (en) | 2020-01-14 | 2020-06-29 | 킴텍(주) | Facility for manufacturing the composite pressure vessel |
| KR102147369B1 (en) | 2019-08-01 | 2020-08-24 | 킴텍(주) | Facility for manufacturing the composite pole |
| KR20210113930A (en) | 2020-03-09 | 2021-09-17 | 킴텍 주식회사 | Facility for manufacturing the composite device without a brake or a clutch for tension |
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1996
- 1996-12-23 KR KR1019960070058A patent/KR100270090B1/en not_active IP Right Cessation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102147369B1 (en) | 2019-08-01 | 2020-08-24 | 킴텍(주) | Facility for manufacturing the composite pole |
| KR102127894B1 (en) | 2020-01-14 | 2020-06-29 | 킴텍(주) | Facility for manufacturing the composite pressure vessel |
| KR20210113930A (en) | 2020-03-09 | 2021-09-17 | 킴텍 주식회사 | Facility for manufacturing the composite device without a brake or a clutch for tension |
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| Publication number | Publication date |
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| KR19980051184A (en) | 1998-09-15 |
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