KR100190317B1 - Fire retardant polyamide resin composition having good-flowing character - Google Patents
Fire retardant polyamide resin composition having good-flowing character Download PDFInfo
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Abstract
본 발명은 폴리아미드(Polyamide) 난연 수지의 흐름성을 개선한 조성물에 관한 것으로서, 폴리아미드 난연 수지를 제조할 때 옥시에틸렌 공중합체와 테플론(Teflon), 그리고 스테아린산 금속염을 첨가제로 사용하여 흐름성 및 난연성을 개선한 폴리아미드 수지조성물에 관한 것이다.The present invention relates to a composition which improves the flowability of polyamide flame retardant resins. The present invention relates to a composition of polyamide flame retardant resins in which an oxyethylene copolymer, Teflon, and a stearic acid metal salt are used as additives. The present invention relates to a polyamide resin composition having improved flame retardancy.
Description
본 발명은 폴리아미드(Polyamide) 난연 수지의 흐름성을 개선한 조성물에 관한 것으로서, 폴리아미드 난연 수지를 제조할 때 옥시에틸렌 공중합체와 테플론(Tef1on), 그리고 스테아린산 금속염을 첨가제로 사용하여 흐름성 및 난연성을 개선한 폴리아미드 수지조성물에 관한 것이다.The present invention relates to a composition that improves the flowability of polyamide flame retardant resins. The present invention relates to a composition of polyamide flame retardant resins in which an oxyethylene copolymer, Teflon, and a stearic acid metal salt are used as additives. The present invention relates to a polyamide resin composition having improved flame retardancy.
일반적으로 나일론은 높은 내열온도와 강도 등의 특성 때문에 자동차, 전기, 전자 등의 각종 용도에 가장 널리 사용되어지는 수지로서, 비강화 수지 뿐만 아니라 유리섬유, 무기물, 내총격제 등의 각종 첨가제가 보강된 제품으로서 여러 용도로 사용되는 엔지니어링 플라스틱 재료이다.In general, nylon is the resin most widely used in various applications such as automobiles, electrics, and electronics because of its high heat resistance temperature and strength. As an engineered product, it is an engineering plastic material used for many purposes.
과거부터 이러한 나일론은 적용용도에 따라 내열안정성, 난연성, 내충격성, 내마모성 등을 극대화시킨 제품들이 시장에 소개되었으며, 근래에 들어서는 특히 생산성과 작업성을 고려하여 다수 캐비티의 금형에서도 작업이 용이한 유동특성을 향상한 제품과, 결정화도 조절이나 공중합, 블랜드 등의 공법을 이용한 고내충격 제품 등이 꾸준히 개발되어 왔다.In the past, such nylon has been introduced to the market to maximize the heat stability, flame retardancy, impact resistance and abrasion resistance depending on the application, and in recent years, it is easy to work even in the mold of many cavities in consideration of productivity and workability. Products with improved properties and high impact products using methods such as crystallinity control, copolymerization and blending have been steadily developed.
그러나 폴리아미드 난연 수지는 흐름성이 불량하여 압출제조공정이나 그 이후 사출 공정에서의 가공시 작업성, 이형성 특히 생산성 저하의 단점을 가지고 있다.However, polyamide flame-retardant resins have poor flowability and have disadvantages in workability, mold release properties, and productivity in processing during extrusion and subsequent injection processes.
이러한 폴리아미드 수지의 흐름성 증진을 위하여 예전부터 여러가지의 첨가제가 사용되어져 왔다. 단순첨가제 사용기술로서 주로 사용한 첨가제는 술폰아미이드계로서 흐름성은 크게 개선되지만 수지의 색상이 나빠지는 단점이 있다.Various additives have been used in the past to improve the flowability of such polyamide resins. The additive mainly used as a simple additive use technique is sulfonamide-based, but the flowability is greatly improved, but the color of the resin is deteriorated.
또한 폴리아미드 난연 수지 자체의 특성을 손상시키는 단점이 있다.In addition, there is a disadvantage that impairs the properties of the polyamide flame retardant resin itself.
이에 본 발명자들은 폴리옥시 에틸렌글리콜과 테플론을 적용함으로써 나일론 난연수지의 본래의 우수한 특성을 그대로 유지하면서 흐름성올 대폭 개선하여 구조가 복잡하고 다수 캐비티가 있는 제품의 사출시 사출성형성이 우수하고, 또한 제품의 생산성 향상에 크게 기여할 수 있는 특성을가진 폴리아미드 난연 수지를 제조할 수 있음을 알게 되어 본 발명을 완성하게 되었다.Accordingly, the present inventors have greatly improved the flowability while maintaining the original excellent properties of nylon flame retardant resin by applying polyoxy ethylene glycol and Teflon, and excellent injection molding during injection of a product having a complex structure and a large number of cavities, The present invention has been accomplished by knowing that a polyamide flame retardant resin having properties that can greatly contribute to product productivity improvement can be produced.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 폴리아미드 수지 100중량%에 대하여 다음 구조식(I)로 표시되는 폴리옥시 에틸렌글리콜 0.05∼4.0중량%, 테플론 0.05∼10중량%, 스테아린산 금속염인 이형제 0.05∼2.0중량%로 이루어짐을 특징으로하는 흐름특성이 우수한 폴리아미드 난연 수지조성물에 관한 것이다.The present invention is characterized by consisting of 0.05 to 4.0% by weight of polyoxy ethylene glycol represented by the following structural formula (I), 0.05 to 10% by weight of Teflon, and 0.05 to 2.0% by weight of a release agent which is a metal salt of stearic acid based on 100% by weight of polyamide resin. The present invention relates to a polyamide flame retardant resin composition having excellent flow characteristics.
(n= 10∼50)(n = 10-50)
이하, 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.
본 발명은 폴리아미드 난연 수지의 흐름성을 개선하기 위한 것으로서 본 발명에서 사용한 나일론66는 다음과 같은 제조방법으로 제조하였다.The present invention is to improve the flowability of the polyamide flame retardant resin, nylon 66 used in the present invention was prepared by the following production method.
교반기와 열감지기, 온도조절기와 스팀 환류냉각기, 물이 순환될 수 있는 장치등이 장착된 나일론 중합용 오토클레이브에 나일론66의 중합원료인 헥사메틸렌디아민 아디페이트염(이하, AH염)과 이 AH염의 농도에따라 적당량의 물을 투입하고 온도를 올리면서 교반기를 사용해 균일하게녹인 후, 각종 첨가제를 투입원료 제조용 용기에서 메탄올과 물의 혼합 용매를 사용해 균일한 슬러리를 제조해 AH염이 녹아 있는 반응관에 투입하여 나일론66 수지를 제조할 수 있는데, 본 발명에서 사용한 통상의 나일론66 제조공정을 소개하면 하기 조건 표1과 같은데, 상기의 윈료외에도 점도 안정제로서 초산을, 과잉첨가물로 헥사메틸렌디아민 및 소포제 등을 소량 부가적으로 첨가할 수도 있으며, 모든 원료가 반응관에 투입되고 난후, 반응관을 고압에 견딜 수 있게 튼튼하게 실링하고 순도 높은 질소가스로 5회이상 퍼지하여 산소를 완전히 제거시킨 후 승온하여 아래 조건 표1에 의거하여 중합하였다.Hexamethylenediamine adipate salt (hereinafter referred to as AH salt), which is a polymerization material of nylon 66, in a nylon polymerization autoclave equipped with a stirrer, a heat sensor, a temperature controller, a steam reflux cooler, and a device capable of circulating water. Depending on the concentration of salt, the appropriate amount of water is added and the temperature is melted uniformly using a stirrer, and then various additives are prepared in a reactor for preparing raw materials to prepare a uniform slurry using a mixed solvent of methanol and water to dissolve the AH salt. It is possible to prepare a nylon 66 resin by introducing into a conventional nylon 66 manufacturing process used in the present invention as shown in Table 1 below, but in addition to the above-mentioned wincher as the viscosity stabilizer, hexamethylenediamine and antifoaming agent as an excess additive A small amount of additives can be added, and after all the raw materials are put into the reaction tube, the tube can withstand high pressure. The button and the sealing temperature increase was completely deoxygenated by purging 5 times or more as high purity nitrogen gas was polymerized under the conditions in Table 1 below.
[조건표 1][Conditional table 1]
위 조건표에서 승온, 승압단계에서는 온도가 증가함에 따라 스팀이 옥토클레이브내에 차게 되므로 압력이 계속 상승하게 된다. 이 때 온도가 120℃ 되는 지점에서부터 60분간 걸쳐 230℃까지 상승시킨다.In the above condition table, the pressure continues to rise because the steam is charged in the octoclave as the temperature increases in the temperature raising and increasing pressure stages. At this time, it raises to 230 degreeC over 60 minutes from the point where temperature becomes 120 degreeC.
그리고 압력이 17.5㎏/㎠이 되면 스팀을 외부로 유출시키면서 압력을 이 상태로 유지하며 온도를 250℃ 정도까지 상승시킨다. 그리고나서 스팀을 외부로 많이 유출시키면서 압력을 70분에 걸쳐 상압까지 떨어뜨린 후 30분간 유지하면서 안정화시킨 후 다시 질소가스를 2∼2.5㎏/㎤ 정도 투입하여 토출하여 스파게티 상태로 얻은 후, 칩상태로 컷팅하여 120℃에서 6시간 진공건조기를 이용하여 건조하여 나일론66 수지를 제조할 수 있다.And when the pressure is 17.5kg / ㎠ to keep the pressure in this state while flowing steam to the outside and raise the temperature to about 250 ℃. Then, the pressure was dropped to normal pressure over 70 minutes while flowing out of the steam, and then stabilized while maintaining for 30 minutes. Then, nitrogen gas was injected into the discharge at 2 to 2.5 kg / cm 3 to obtain a spaghetti state. The nylon 66 resin may be manufactured by cutting with a vacuum dryer at 120 ° C. for 6 hours using a vacuum dryer.
본 발명에 사용한 그 밖의 나일론 수지로는 나일론6, 나일론46, 나일론11, 나일론12 등을 들 수 있는데, 이 중에서 나일론6, 나일론66를 사용하는 것이 가장 적절하다.Other nylon resins used in the present invention include nylon 6, nylon 46, nylon 11, nylon 12 and the like, of which nylon 6 and nylon 66 are most suitable.
본 발명에서 사용한 가소제는 옥시에틸렌 공중합체로서 이에는 다음과 같은 구조의 물질이 사용될 수 있다.The plasticizer used in the present invention is an oxyethylene copolymer, in which a material having the following structure can be used.
(n= 10∼50)(n = 10-50)
n이 10 미만이면 휘발성이 강하여 가공시 가스가 많이 발생하고, 50을 초과하면 고른 분산을 얻기 어렵다. 또한 사용하는 함량은 나일론수지 자체에 대하여 0.05∼4.0중량%가 적합한 바, 사용량이 0.05중량%미만이면 윈하는 흐름성 개선을 얻기 어렵고, 4.0중량%를 초과하면 가소제의 열분해에 의한 수지의 색상 및 물성 저하가 발생하고, 제조윈가가 상승하기 때문에 이 이상 투입할 필요가 없다.If n is less than 10, the volatility is high, and a lot of gas is generated during processing, and if it is more than 50, it is difficult to obtain even dispersion. In addition, the content to be used is 0.05 to 4.0% by weight with respect to the nylon resin itself, if the amount is less than 0.05% by weight, it is difficult to obtain the flowability improvement, and when the content exceeds 4.0% by weight, the color of the resin by thermal decomposition of the plasticizer and Since physical property fall occurs and manufacturing cost rises, it is not necessary to add more than this.
또한 본 발명에서 흐름성 증진과 난연성 향상올 위하여 사용한 첨가제 테플론은 사불파에틸렌 CF2=CF2 의 중합체이며, 사용하는 함량은 나일론 수지 자체에 대하여 0.05∼10.0중량%가 적합한바, 사용량이 0.05 중량% 미만이면 원하는 개선을 얻기 어렵고, 10.0 중량%를 초과하면 제조원가가 상승하기 때문에 이 이상 투입할 필요가 없다.In addition, in the present invention, the additive teflon used for improving the flowability and improving the flame retardancy is a polymer of tetrafluoroethylene CF 2 = CF 2 , and the amount used is 0.05 to 10.0 wt% with respect to the nylon resin itself, and the amount used is 0.05 wt% If it is less than the desired improvement, it is difficult to obtain, and if it exceeds 10.0% by weight, the manufacturing cost rises, so it is not necessary to add more.
또한 나일론 수지의 이형효과와 첨가제의 분산효과, 그리고 용융가공시 체인간의 가소화효과를 부여하기 위해 통상의 이형제를 사용하는데, 본발명에서 사용된 이형제는 일반적으로 스테아린산 계통의 이형제가 사용가능하며 가장 널리 사용되는 이형제는 에틸렌비스(스테아릴)아미드, 스데아린산알미늄, 스테아린산칼슘, 스테아린산마그네슘, 스테아린산나트륨 등 금속 스테아린산과 스테아린산이 포함되는 아미드 폴리머계가 많이 사용되나 여기에 국한되는 것은 아니며, 첨가량은 나일론 수지 100중량%에 대해 0.05∼2.0중량%가 적당한 바, 0.05중량% 미만에서는 이형효과가 없으며, 2.0중량% 초과 투입시에는 이형효과의 개선 수준이 미미하여 투입할 필요가 없다.In addition, a general release agent is used to give a release effect of nylon resin, an additive dispersion effect, and a plasticization effect between chains during melt processing. The release agent used in the present invention is generally a stearic acid type release agent. The widely used release agents include amide polymers including metal stearic acid and stearic acid such as ethylene bis (stearyl) amide, aluminum stearate, calcium stearate, magnesium stearate, sodium stearate, but are not limited thereto. 0.05 to 2.0% by weight relative to 100% by weight of the resin is appropriate, there is no release effect at less than 0.05% by weight, when the addition of more than 2.0% by weight does not need to be added because the improvement level of the release effect is insignificant.
이와같이 본 발명에 따른 수지조성물은 이축압축기를 이용하여 제조할 수 있는데, 수지조성물의 기계적 물성을 최대화하기 위하여 투입구가 2개인 압출기를 시용하여 혼련하며,1차 투입구에서는 나일론과 내열제, 이형제를 혼합하여 투입하고, 2차 투입구에는 가소제를 투입하는 것이 바람직하다.As described above, the resin composition according to the present invention may be manufactured using a twin screw compressor. In order to maximize the mechanical properties of the resin composition, the resin composition is kneaded by using an extruder having two inlets. In the first inlet, nylon, a heat resistant agent, and a release agent are mixed. It is preferable to add a plasticizer to the secondary inlet.
이렇게 제조되어진 수지조성물은 건조를 통해 수분을 제거한 후, 원하는 모양의 금형이 장착된 사출성형기에서 용이하게 제품을 성형할 수 있다.The resin composition thus prepared can be easily molded in an injection molding machine equipped with a mold of a desired shape after removing moisture through drying.
따라서 본 수지조성물은 제품이 복잡하고 캐비티가 많은 케이블 타이등에 적용하여 사출성이 양호하면서 경제성이 있게 제품을 생산할 수 있다.Therefore, this resin composition can be applied to cable ties with a complicated product and a lot of cavities, so that the product can be produced with good injection properties and economical efficiency.
이하, 본 발명을 실시예 및 비교예에 의거하여 더욱 상세하게 설명하면 다음과 같은 바, 실시예에 의하여 본 발명이 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on Examples and Comparative Examples. However, the present invention is not limited to the Examples.
제조된 수지조성물은 다음과 같은 평가방법에 의거, 평가하였다.The prepared resin composition was evaluated based on the following evaluation method.
측정항목Metric
1) 인장강도 : ASTM D-638에 의거해 덤벨-1의 시편을 이용해 측정하였다.1) Tensile strength: measured using a specimen of dumbbell-1 in accordance with ASTM D-638.
2) 흐 름 성 : 나일론66, 270℃에서 ASTM D-1238에 의거 용융흐름지수를 평가하였다.2) Flowability: The melt flow index was evaluated according to ASTM D-1238 at nylon 66 and 270 ° C.
3) 색 상 : 정규 나일론 난연수지와 비교하여 CIE 칼라기준에 의거 칼라미터로 L, a, b치를 평가하였다.3) Color: L, a and b values were evaluated by colorimeter based on CIE color standard compared to regular nylon flame retardant resin.
4) 충격강도 : ASTM D-256에 의거해 평가하였다.4) Impact strength: evaluated according to ASTM D-256.
[실시예 1∼6, 비교예 1∼4][Examples 1-6, Comparative Examples 1-4]
나일론은 나일론66를 사용하였으며, 아래의 표1의 조성으로 2개의 투입구가 달려 있는 이축압축기롤 사용하여 제1 투입구에는 나일론, 이형재, 내열제롤 블랜딩하여 투입하고, 제2 투입구에는 가소제를 정량 투입한다. 이러한 방법으로 나일론66는 280℃로 이축압출기 내에서 용융혼랸히여 칩 상태로 제조한 다음, 이 칩을 90℃ 온도의 열풍건조기에서 5시간 동안 건조한 후, 255℃로 가열된 스크류식 사출기를 사용하여 각각의 시편을 제작, 위와같은 측정방법으로 평가했으며, 결과는 표2와 같다.Nylon 66 was used, and the composition of Table 1 below used a twin-screw compressor roll with two inlets, and blended nylon, mold release material, and heat-resistance roll into the first inlet, and plasticizer was injected into the second inlet. . In this way, nylon 66 was melted and mixed in a twin screw extruder at 280 ° C., and then dried in a hot air dryer at 90 ° C. for 5 hours, and then using a screw injection machine heated to 255 ° C. Each specimen was fabricated and evaluated by the same measurement method, and the results are shown in Table 2.
[표1 실험조성]Table 1 Experimental Composition
※ 가소제, 이형제는 나일론 수지 대비 중량%※ Plasticizer and release agent by weight compared to nylon resin
※ 내열제는 각각의 조성에 0.2중량% 투입※ 0.2% by weight of heat-resistant agent in each composition
(내열제 : 포스파이트/힌더드 페놀계 = 1/1 혼합물)(Heat Resistant: Phosphite / Hindered Phenolic Type = 1/1 Mixture)
※ 첨가제 : POEG-구조식(I)의 폴리옥시에틸클리콜(n=30)※ Additive: Polyoxyethyl glycol of POEG-Structure (I) (n = 30)
테플론 - 사불화에틸렌중합체Teflon-tetrafluoroethylene polymer
※ 나연제는 각각의 조성에 주난연제, 보조난연제를 합하여 30중량% 투입(주난연제 : 브롬화에폭시형, 보조난연제 : 삼산화안티몬)※ Flame retardant is added 30 wt% of main flame retardant and auxiliary flame retardant in each composition (main flame retardant: epoxy bromide, auxiliary flame retardant: antimony trioxide)
※ Al-St : 스테아린산알미늄, Ca-St : 스테아린산칼슘,※ Al-St: aluminum stearate, Ca-St: calcium stearate,
Na-St : 스테아린산나트륨Na-St: Sodium Stearate
[표2] 평가결과[Table 2] Evaluation Results
Claims (2)
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| KR1019940033995A KR100190317B1 (en) | 1994-12-13 | 1994-12-13 | Fire retardant polyamide resin composition having good-flowing character |
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