TWI709609B - A production method of flame retardant thermoplastic nylon composite and application thereof - Google Patents
A production method of flame retardant thermoplastic nylon composite and application thereof Download PDFInfo
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本發明涉及一種防火、耐燃材料的領域，特別是一種可達高階防火、耐燃等級的熱塑性尼龍複合材料及其製造方法。 The invention relates to the field of fire-resistant and flame-resistant materials, in particular to a thermoplastic nylon composite material with high-level fire-resistant and flame-resistant grades and a manufacturing method thereof.
隨著各式複合材料的發展，複合材料擁有絕佳的加工性能與機械性能優勢，使之廣泛應用於汽車工業、航天工業、建築裝飾與生活用品等各領域中，特別是建築領域，複合材料更是一個相當常見的材料之一。 With the development of various composite materials, composite materials have excellent processing performance and mechanical performance advantages, making them widely used in various fields such as automobile industry, aerospace industry, architectural decoration and daily necessities, especially in the field of construction, composite materials It is one of the fairly common materials.
建築、裝潢材料除了訴求耐震、高剛性等機械強度外，能夠一定程度的耐高溫、阻燃或阻火，甚至是達到更高階的耐燃、防火性能更是必要考量。一般常見的能夠達到前述耐燃、防火等高階防火性能的建材主要是金屬或石材等無機物建材，而塑料建材中則僅以熱固性樹脂的複合材料才可能達到耐燃、防火等高階性能，而熱塑性樹脂則往往僅能達到較為低階或基礎的阻燃、阻火性能。 In addition to demanding mechanical strength such as shock resistance and high rigidity, construction and decoration materials can be resistant to high temperature, flame retardant or fire to a certain degree, and even higher levels of flame resistance and fire resistance are necessary considerations. Generally, the common building materials that can achieve the aforementioned high-level fire resistance such as flame resistance and fire protection are mainly inorganic building materials such as metal or stone. In plastic building materials, only thermosetting resin composite materials can achieve high-level performance such as flame resistance and fire protection, while thermoplastic resins Often only relatively low-level or basic flame retardant and fire retardant properties can be achieved.
然而，金屬或石材等無機物建材雖然具有高階的耐燃、防火效能，但是其比重高、重量重，在裝潢材料上較難以靈活運用；而熱固性樹脂的複合材料也有著無法回收等環保問題。目前缺少著一種以熱塑性複合材料所製成的高階耐燃、防火材料，並且同時兼具可射出、押出等高加工特性與良好回收性的材料存在。 However, although inorganic building materials such as metal or stone have high-level flame resistance and fire resistance, their high specific gravity and heavy weight make it difficult to be flexibly used in decoration materials; and thermosetting resin composite materials also have environmental protection problems such as unrecyclable. At present, there is a lack of a high-end flame-resistant and fire-resistant material made of thermoplastic composite materials, and at the same time, there is a material that has high processing characteristics such as injection and extrusion and good recyclability.
為了解決前述金屬或石材等無機物建材雖具有高階耐火、防火效能，但難以靈活運用，以及熱固性樹脂的複合材料無法回收等種種問題，本發明對此經過申請人長期與反覆研究後，提出一種耐燃熱塑性尼龍複合材料，其包含：一尼龍樹脂30wt%以下；以多重耦合劑改質之玻璃纖維60~70wt%；以及一阻燃劑10wt%以下。 In order to solve the aforementioned problems of inorganic building materials such as metal or stone material having high-level fire resistance and fire resistance, but it is difficult to use flexibly, and thermosetting resin composite materials cannot be recycled, the present invention proposes a flame retardant after long-term and repeated research by the applicant. The thermoplastic nylon composite material comprises: a nylon resin of less than 30wt%; a glass fiber modified with a multiple coupling agent of 60~70wt%; and a flame retardant of less than 10wt%.
其中，上述的該多重耦合劑包含至少二種耦合劑。該阻燃劑包含氫氧化鎂阻燃劑或磷氮阻燃劑。 Wherein, the above-mentioned multiple coupling agent includes at least two coupling agents. The flame retardant contains magnesium hydroxide flame retardant or phosphorus nitrogen flame retardant.
其中，該至少二種耦合劑是包含至少二種矽烷耦合劑。 Wherein, the at least two coupling agents comprise at least two silane coupling agents.
其中，前述該矽烷耦合劑包含n-氨基丙基三已氧基矽烷、甲基丙烯醯氧丙基三甲氧基矽烷或β-(3,4-環氧環己基)-乙基三甲氧基矽烷。 Wherein, the aforementioned silane coupling agent comprises n-aminopropyl trihexoxysilane, methacryloxypropyl trimethoxysilane or β-(3,4-epoxycyclohexyl)-ethyltrimethoxysilane .
進一步地，本發明提供前述耐燃熱塑性尼龍複合材料的製造方法，其步驟包含：將一尼龍樹脂80wt%與一阻燃劑20%混煉為一尼龍母粒；利用一耦合劑將一玻璃纖維加以浸泡改質至少二次並乾燥；以及將該尼龍母粒與該改質之玻璃纖維混煉後得到一種熱塑性尼龍樹脂複合材料。 Further, the present invention provides a method for manufacturing the aforementioned flame-resistant thermoplastic nylon composite material. The steps include: mixing 80% by weight of a nylon resin and 20% of a flame retardant into a nylon masterbatch; using a coupling agent to add a glass fiber Soaking and modifying for at least two times and drying; and kneading the nylon masterbatch with the modified glass fiber to obtain a thermoplastic nylon resin composite material.
其中，前述該耦合劑以至少兩種不同耦合劑以兩次浸泡程序對該玻璃纖維加以改質。 Wherein, the aforementioned coupling agent uses at least two different coupling agents to modify the glass fiber in two immersion procedures.
其中，進一步地將該熱塑性尼龍樹脂複合材料射押出成型。 Wherein, the thermoplastic nylon resin composite material is further injection molded.
其中，該尼龍母粒與該改質之玻璃纖維混煉時使用異向雙軸螺桿機混煉。 Wherein, the nylon masterbatch and the modified glass fiber are kneaded using a counter-rotating twin screw machine.
其中，該尼龍母粒與該改質之玻璃纖維混煉時，混煉前段溫度設定於90℃內、中段溫度拉高到180℃，後段以280℃的溫度混煉，以及全段螺桿轉速為450rpm。 Among them, when the nylon masterbatch is mixed with the modified glass fiber, the temperature in the first stage of mixing is set at 90°C, the temperature in the middle stage is raised to 180°C, the latter is mixed at a temperature of 280°C, and the screw speed of the whole stage is 450rpm.
更進一步地，本發明提供一種建築、裝潢或飛行器材料，其係使用前述的耐燃熱塑性尼龍複合材料所製成。 Furthermore, the present invention provides a construction, decoration or aircraft material, which is made of the aforementioned flame-resistant thermoplastic nylon composite material.
藉由上述說明可知，本發明具有以下優勢與優點： According to the above description, the present invention has the following advantages and advantages:
1.本發明利用材料配方與製程搭配，成功研發出一種能夠達到CNS 14705-1規定之耐燃三級與防火效能的高階熱塑性複合材料，不僅具備可射押出成型的加工條件外，更擁有高機械強度的特性，特別適合但不限用於建築、裝飾等用料以及民生用品、工業或航空業領域，例如航空器(飛機、無人機)內外部裝置材料、汽車或列車車廂內部裝飾材料、地板或地磚或天花板等，且因為具備可射押出的特性，可以加工成型為各式形狀的產品，應用範疇廣且品質耐用優良。 1. The present invention utilizes the combination of material formula and manufacturing process to successfully develop a high-end thermoplastic composite material that can reach the third-class flame resistance and fire protection performance specified by CNS 14705-1. It not only has the processing conditions for injection and extrusion molding, but also has high machinery. The characteristics of strength, especially suitable for but not limited to construction, decoration and other materials, as well as civilian products, industrial or aviation fields, such as aircraft (aircraft, drones) internal and external equipment materials, car or train interior decoration materials, floors or Floor tiles or ceilings, etc., and because of the characteristics of injection molding, can be processed into products of various shapes, with a wide range of applications and excellent quality and durability.
進一步地，本發明主要是塑膠成分，作為航空器的外部材料，例如機殼或機翼等，可避免使用金屬材料而造成的雷擊風險。本發明所具有的優異機械強度也適用於製作產品的結構件，例如蜂巢板。 Further, the present invention is mainly a plastic component, which is used as an outer material of an aircraft, such as a casing or a wing, etc., to avoid the risk of lightning strikes caused by the use of metal materials. The excellent mechanical strength possessed by the present invention is also suitable for making structural parts of products, such as honeycomb panels.
2.本發明可取代現有的天花板裝潢所使用之矽酸鈣板材料，由於現有的矽酸鈣板會吸收空氣中潮溼或漏水的水份，長時間下來會導致材料腐壞或破損的問題，需要時常更換，更可能會因為吸飽水份而滋長細菌等問題。本發明的熱塑性尼龍複合材料擁有不吸水的特性，製程板片之產品時，可用於取代現有的天花板之矽酸鈣板材料，特別適用於醫療院所的天花板裝潢，可以細菌滋長導致環境污染的問題。 2. The present invention can replace the existing calcium silicate board material used in ceiling decoration. Because the existing calcium silicate board absorbs moisture or leaking water in the air, it will cause the problem of material decay or damage for a long time. It needs to be replaced frequently, and it is more likely to cause problems such as bacteria growth due to full water absorption. The thermoplastic nylon composite material of the present invention has the characteristics of non-absorbent, and can be used to replace the existing calcium silicate board material of the ceiling when the product of the sheet is processed. It is especially suitable for the ceiling decoration of medical institutions, which can cause bacterial growth and cause environmental pollution. problem.
圖1為本發明製程步驟一較佳實施例流程示意圖。 FIG. 1 is a schematic flow chart of a preferred embodiment of the process steps of the present invention.
為能詳細瞭解本發明的技術特徵及實用功效，並可依照說明書的內容來實施，進一步以如圖式所示的較佳實施例，詳細說明如下。 In order to understand the technical features and practical effects of the present invention in detail, and implement it according to the content of the specification, the preferred embodiment shown in the figure is further described in detail as follows.
本發明是一種熱塑性尼龍樹脂複合材料，不僅具有熱塑性樹脂般的可射出、押出等高加工特性，並且能達到高階的防火、耐燃效能。一種耐燃熱塑性尼龍複合材料配方的數個較佳實施例如下： The invention is a thermoplastic nylon resin composite material, which not only has the high processing characteristics of thermoplastic resin, such as injection and extrusion, but also can achieve high-level fire and flame resistance. Several preferred examples of a flame-resistant thermoplastic nylon composite formulation are as follows:
《配方第一實施例》"Formulation First Example"
尼龍樹脂30wt%以下；以多重耦合劑改質之玻璃纖維60~70wt%；以及氫氧化鎂阻燃劑或磷氮阻燃劑10wt%以下。 Nylon resin 30wt% or less; glass fiber modified with multiple coupling agent 60~70wt%; and magnesium hydroxide flame retardant or phosphorus nitrogen flame retardant 10wt% or less.
本實施例或本發明所使用的該多重耦合劑，是指至少兩種以上不同的耦合劑，較佳是三種不同的耦合劑將該玻璃纖維加以表面改質，此些耦合劑基本是為了增加有機高分子尼龍樹脂與無機增強材玻璃纖維與阻燃劑的混合均勻性，達到整體材料高分散與均勻混合的狀態後，可使本發明達到高階的耐火與耐燃的功效。本實施例具有使該尼龍樹脂具有防火、耐燃的效果的除了該氫氧化鎂阻燃劑或磷氮阻燃劑外，該多重耦合劑改質之玻璃纖維也具有提高本發明防火、耐燃的效果。 The multiple coupling agent used in this embodiment or the present invention refers to at least two or more different coupling agents, preferably three different coupling agents to modify the glass fiber surface, these coupling agents are basically for increasing The mixing uniformity of the organic polymer nylon resin, the inorganic reinforcing material glass fiber and the flame retardant achieves the high dispersion and uniform mixing of the overall material, and the present invention can achieve high-level fire and flame resistance. In addition to the magnesium hydroxide flame retardant or phosphorus nitrogen flame retardant, this embodiment has the effect of making the nylon resin fire-resistant and flame-resistant. The glass fiber modified by the multi-coupling agent also has the effect of improving the fire-resistant and flame resistance of the present invention. .
《配方第二實施例》"Formulation Second Example"
尼龍樹脂30wt%以下；以多重矽烷耦合劑改質之玻璃纖維60~70wt%；以及 氫氧化鎂阻燃劑或磷氮阻燃劑10wt%以下。 Nylon resin less than 30wt%; glass fiber modified with multiple silane coupling agent 60~70wt%; and Magnesium hydroxide flame retardant or phosphorus nitrogen flame retardant is less than 10wt%.
本實施例的多重矽烷耦合劑主要包含至少兩種以上不同的矽烷耦合劑，較佳是三種不同的矽烷耦合劑將該玻璃纖維加以表面改質，該矽烷耦合劑包含n-β-(氨基乙基)-γ-氨基丙基三甲氧基矽烷(n-β-(amino ethyl)-γ-amino propyl trimethoxy silane，又稱為UCC-A-1120，下簡稱1120矽烷耦合劑)、甲基丙烯醯氧丙基三甲氧基矽烷(γ-methacryloxy propyl trimethoxy silane，又稱為UCC-A-174，下簡稱為174矽烷耦合劑)、β-(3,4-環氧環己基)-乙基三甲氧基矽烷(β-(3,4-epoxy cyclohexyl)ethyl tri methoxy silane，又稱為UCC-A-186，下簡稱為186矽烷耦合劑)的兩種或兩種以上任意的組合，皆可對本發明的複合材料提供良好的混合均勻性，以及對本發明的防火與耐燃效能有實質上的提昇。 The multiple silane coupling agent of this embodiment mainly contains at least two or more different silane coupling agents, preferably three different silane coupling agents to modify the glass fiber surface. The silane coupling agent contains n-β-(aminoethyl Group)-γ-amino propyl trimethoxysilane (n-β-(amino ethyl)-γ-amino propyl trimethoxy silane, also known as UCC-A-1120, hereinafter referred to as 1120 silane coupling agent), methacrylic acid Γ-methacryloxy propyl trimethoxy silane (γ-methacryloxy propyl trimethoxy silane, also known as UCC-A-174, hereinafter referred to as 174 silane coupling agent), β-(3,4-epoxycyclohexyl)-ethyl trimethoxy silane Two or more arbitrary combinations of β-(3,4-epoxy cyclohexyl)ethyl tri methoxy silane (also known as UCC-A-186, hereinafter referred to as 186 silane coupling agent) can be used in the present invention The composite material provides good mixing uniformity and substantially improves the fire and flame resistance of the present invention.
進一步地，本發明以下提供數個前述尼龍熱塑性型樹脂複合材料的製造方法，並請參考圖1。 Further, the present invention provides several methods for manufacturing the aforementioned nylon thermoplastic resin composite materials, and please refer to FIG. 1.
《製程第一實施例》"The first embodiment of the process"
步驟S1：將一尼龍樹脂80wt%與一阻燃劑20%混煉為一尼龍母粒；步驟S2：利用一耦合劑將一玻璃纖維加以浸泡改質至少二次並乾燥後；步驟S3：將該尼龍母粒與該改質之玻璃纖維混煉後得到一種熱塑性尼龍樹脂複合材料。 Step S1: Mix 80% by weight of a nylon resin and 20% of a flame retardant into a nylon masterbatch; Step S2: Use a coupling agent to soak and modify a glass fiber for at least two times and dry; Step S3: Combine The nylon masterbatch is mixed with the modified glass fiber to obtain a thermoplastic nylon resin composite material.
其中，前述該阻燃劑與該耦合劑的種類與前述配方第一實施例與第二實施例已經詳細說明，於此不多加贅述。而步驟1與步驟2基本是可同時進行的步驟，並非用以限定此二步驟間的順序。該耦合劑於本發明或此實施例對該玻璃纖維加以改質的方法較佳是利用浸泡的方式，將該玻璃纖維完全浸沒於該耦合劑液體中，選用多種與多次的浸泡，可以讓玻璃纖維表面具有能與尼龍與該阻燃劑親近的表面，當後續所有材料混合時能更為均勻與分散。 Among them, the types of the flame retardant and the coupling agent and the first embodiment and the second embodiment of the aforementioned formulation have been described in detail, and will not be repeated here. Steps 1 and 2 are basically steps that can be performed at the same time, and are not used to limit the order between the two steps. The method for modifying the glass fiber with the coupling agent in the present invention or this embodiment is preferably to use a soaking method. The glass fiber is completely immersed in the coupling agent liquid, and multiple and multiple soaking can be selected. The glass fiber surface has a surface close to nylon and the flame retardant, and it can be more uniform and dispersed when all subsequent materials are mixed.
本實施例所謂的多種耦合劑種類可參照前述配方第二較佳實施例，而多種耦合劑對該玻璃纖維的多次改質方式較佳是先使用油性矽烷耦合劑(即174耦合劑與1120耦合劑各10wt%的醋酸溶液混合後對該玻璃纖維進行第一次浸泡，透過浸泡的方式使該耦合劑可以滲入到該玻璃纖維中並得以接觸到每一根纖維的表面，使該玻璃纖維表面的活性官能基，例如含氧官能基團打開鍵結。接著再利用水性矽烷耦合劑(即186矽烷耦合劑)浸泡該玻璃纖維進行第二次的耦合與改質，使打開的活性官能基鍵結能接枝上與尼龍可反應或結合的聚醯氨官能基(Acrylate)，也作為前述第一次改質之輔助改質製程。最後再將改質後的玻璃纖維切斷與乾燥後備用。 The so-called multiple coupling agent types in this embodiment can refer to the second preferred embodiment of the aforementioned formula, and the multiple modification method of multiple coupling agents to the glass fiber is preferably to use oily silane coupling agent (ie 174 coupling agent and 1120 The glass fiber is soaked for the first time after the 10wt% acetic acid solution of each coupling agent is mixed. Through the soaking method, the coupling agent can penetrate into the glass fiber and contact the surface of each fiber, so that the glass fiber The active functional groups on the surface, such as oxygen-containing functional groups, open the bond. Then the glass fiber is soaked with an aqueous silane coupling agent (ie 186 silane coupling agent) for the second coupling and modification, so that the opened active functional groups The bonding can be grafted onto the polyamide functional group (Acrylate) that can react or bond with nylon, which is also used as the auxiliary modification process for the first modification. Finally, the modified glass fiber is cut and dried for backup. use.
《製程第二實施例》"Second Embodiment of Manufacturing Process"
步驟S1：將一尼龍樹脂80wt%與一阻燃劑20%混煉為一尼龍母粒；步驟S2：利用一耦合劑將一玻璃纖維加以浸泡改質至少二次並乾燥後；步驟S3：將該尼龍母粒與該改質之玻璃纖維混煉後得到一種熱塑性尼龍樹脂複合材料；步驟S4：將該熱塑性尼龍樹脂複合材料射押出成型為一尼龍熱塑性型樹脂複合材料的成品。 Step S1: Mix 80% by weight of a nylon resin and 20% of a flame retardant into a nylon masterbatch; Step S2: Use a coupling agent to soak and modify a glass fiber for at least two times and dry; Step S3: Combine The nylon masterbatch is mixed with the modified glass fiber to obtain a thermoplastic nylon resin composite material; step S4: the thermoplastic nylon resin composite material is injection-extruded into a finished nylon thermoplastic resin composite material.
由於本發明是利用熱塑性尼龍樹脂作為基底材料，熱塑性材料的好加工特性，特別使本發明的複合材料加工時的流動性能導入射押出成型製程，相對於既有的熱固性型樹脂複合材料，本發明更具有優異的可加工性，其防火、耐燃的效果更甚於熱固性型樹脂複合材料。 Since the present invention uses thermoplastic nylon resin as the base material, the excellent processing characteristics of the thermoplastic material, especially the fluidity of the composite material of the present invention during processing, can be introduced into the injection extrusion molding process. Compared with the existing thermosetting resin composite material, the present invention It has excellent processability, and its fire and flame resistance effect is better than thermosetting resin composite material.
其中，本發明該尼龍母粒與該改質之玻璃纖維混煉時，可以使用異向雙軸螺桿機，過程中較佳需要調控混煉環境的螺桿混合組態，不可使混煉時材料內部所產生的內應熱增高到把高分子材料燒結的程度，較佳是混煉前段 溫度設定於90℃內、中段溫度拉高到180℃，以及最後後段以280℃的溫度混煉，全段螺桿轉速則較佳450rpm。 Wherein, when the nylon masterbatch of the present invention is mixed with the modified glass fiber, a counter-rotating twin-shaft screw machine can be used. During the process, it is better to adjust the screw mixing configuration of the mixing environment. The generated internal heat is increased to the extent that the polymer material is sintered, preferably before mixing The temperature is set within 90°C, the temperature in the middle section is raised to 180°C, and the last stage is mixed at a temperature of 280°C. The screw speed of the whole section is preferably 450rpm.
《檢測結果》"Test results"
本發明各實施例經過測試皆通過CNS 14705-1規定之耐燃三級的測試標準，請參考以下表1：
以上所述僅為本發明的較佳實施例而已，並非用以限定本發明主張的權利範圍，凡其它未脫離本發明所揭示的精神所完成的等效改變或修飾，均應包括在本發明的申請專利範圍內。 The foregoing descriptions are only preferred embodiments of the present invention, and are not intended to limit the scope of rights claimed by the present invention. All other equivalent changes or modifications completed without departing from the spirit disclosed by the present invention shall be included in the present invention. Within the scope of patent application.
Claims (4)
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| CN104017204A (en) * | 2014-05-20 | 2014-09-03 | 珠海万通化工有限公司 | Polyamide resin and polyamide composition formed by same |
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| CN104017204A (en) * | 2014-05-20 | 2014-09-03 | 珠海万通化工有限公司 | Polyamide resin and polyamide composition formed by same |
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