CN106832960A - A kind of ceramic flame-retardant silicon rubber composite material and preparation method thereof - Google Patents

A kind of ceramic flame-retardant silicon rubber composite material and preparation method thereof Download PDF

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CN106832960A
CN106832960A CN201710102414.9A CN201710102414A CN106832960A CN 106832960 A CN106832960 A CN 106832960A CN 201710102414 A CN201710102414 A CN 201710102414A CN 106832960 A CN106832960 A CN 106832960A
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silicone rubber
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郭卫红
楼飞鹏
王权
成立鸿
姚威宇
赵雁军
熊娇阳
王瑜
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East China University of Science and Technology
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Abstract

本发明涉及一种陶瓷化阻燃耐火硅橡胶复合材料及其制备方法,其原料按质量份的组成为:硅橡胶40‑80份,聚磷酸铵1‑10份,碳酸钙1‑10份,硅酸盐填料10‑30份,助熔剂6‑25份,硫化剂0.3‑1.5份,制备步骤如下:按所述比例将硅橡胶、聚磷酸铵、碳酸钙、硅酸盐填料和助熔剂在开炼机上混合均匀;再加入硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下热压4‑20min成型,在200℃烘箱中进行二段硫化2h,得到所需的复合材料。本发明具有良好的阻燃性;燃烧后能在600‑1000℃下转化为坚硬的陶瓷体,且原料价格低廉,无毒环保,易加工成型,可广泛应用于电线电缆、电力通讯等领域。

The invention relates to a ceramic flame-retardant and refractory silicone rubber composite material and a preparation method thereof. The raw materials are composed of 40-80 parts of silicone rubber, 1-10 parts of ammonium polyphosphate, and 1-10 parts of calcium carbonate. 10-30 parts of silicate filler, 6-25 parts of flux, 0.3-1.5 parts of vulcanizing agent, the preparation steps are as follows: mix silicone rubber, ammonium polyphosphate, calcium carbonate, silicate filler and flux in the Mix evenly on the open mill; then add vulcanizing agent and continue to knead on the open mill to form a sheet evenly, the temperature is not higher than 30°C, and finally hot-press for 4-20min under the flat vulcanizer to form, and carry out two-stage vulcanization in an oven at 200°C 2h, the desired composite material was obtained. The invention has good flame retardancy; after being burned, it can be converted into a hard ceramic body at 600-1000°C, and the raw material is cheap, non-toxic and environmentally friendly, easy to process and shape, and can be widely used in the fields of wires and cables, electric power communications and the like.

Description

一种陶瓷化阻燃耐火硅橡胶复合材料及其制备方法A ceramic flame-retardant refractory silicone rubber composite material and its preparation method

技术领域technical field

本发明涉及一种陶瓷化的阻燃耐火硅橡胶及其制备方法,具体涉及一种兼具阻燃和耐火性能的陶瓷化硅橡胶复合材料及其制备方法,属于阻燃耐火材料领域。The invention relates to a ceramicized flame-retardant and refractory silicone rubber and a preparation method thereof, in particular to a ceramicized silicone rubber composite material having both flame-retardant and fire-resistant properties and a preparation method thereof, belonging to the field of flame-retardant and refractory materials.

背景领域background field

随着科学技术的发展和人们生活水平的提高,高分子材料已经渗入到在生活的方方面面了,扮演者越来越重要的角色。然而,合成的高分子材料通常具有易可燃的缺点,一旦发生火灾,给人们的生命和财产安全造成了很大的危险隐患,严重限制了它在电线电缆、电力通信、核电等领域的应用。随着人们对电线电缆材料的耐火性和产品质量的提高,制备新型的耐火电缆材料显得尤为的重要。With the development of science and technology and the improvement of people's living standards, polymer materials have penetrated into all aspects of life, playing an increasingly important role. However, synthetic polymer materials usually have the disadvantage of being flammable. Once a fire occurs, it will cause great danger to people's life and property safety, which seriously limits its application in the fields of wire and cable, power communication, nuclear power and so on. As people improve the fire resistance and product quality of wire and cable materials, it is particularly important to prepare new fire-resistant cable materials.

相比应用在电线电缆领域的有机高分子材料(如聚乙烯、聚氯乙烯、聚氯乙烯等),硅橡胶更适宜在高温和苛刻的环境条件下使用。硅橡胶具有无毒无害、高寿命以及低的使用热释放速率等优点使它在电缆工业中占有重要地位。另外,硅橡胶遇火或高温燃烧后会在表面覆盖着一层SiO2灰烬,这层白色的SiO2灰烬能够作为绝缘层,阻止热量和可燃气体的传递,从而阻止硅橡胶进一步发生分解。然而,这层SiO2灰烬几乎没有强度,容易破碎,不能保持连续的自支撑结构。Compared with organic polymer materials (such as polyethylene, polyvinyl chloride, polyvinyl chloride, etc.) used in the field of wire and cable, silicone rubber is more suitable for use under high temperature and harsh environmental conditions. Silicone rubber has the advantages of non-toxic, harmless, long life and low heat release rate, so it occupies an important position in the cable industry. In addition, the surface of silicone rubber will be covered with a layer of SiO 2 ash after being exposed to fire or high temperature combustion. This layer of white SiO 2 ash can be used as an insulating layer to prevent the transfer of heat and combustible gas, thereby preventing further decomposition of silicone rubber. However, this layer of SiO2 ash has little strength, is easily broken, and cannot maintain a continuous self-supporting structure.

虽然硅橡胶的燃点和氧指数较高,但仍可燃或者阴燃。为了提高硅橡胶的阻燃性,人们一般是通过添加含卤阻燃剂或无卤阻燃剂来提高硅橡胶的阻燃性能。但是添加的卤素阻燃剂在燃烧时会释放出有毒的烟和气体,造成环境污染。欧盟在欧盟电子电机中危害物资禁用指令中决定在2006年7月1日全面禁止PBB及PBDE等溴系阻燃剂的使用。如今,无卤、低烟、低毒的环保型阻燃剂已成为人们追求的目标,硅橡胶的无卤阻燃剂主要包括氢氧化铝,氢氧化镁,膨胀石墨,膨胀性阻燃剂以及铂化合物。Although silicone rubber has a high ignition point and oxygen index, it is still flammable or smoldering. In order to improve the flame retardancy of silicone rubber, people generally improve the flame retardancy of silicone rubber by adding halogen-containing flame retardants or halogen-free flame retardants. However, the added halogen flame retardant will release toxic smoke and gas when burned, causing environmental pollution. The European Union decided to completely ban the use of brominated flame retardants such as PBB and PBDE in the EU Directive on the Prohibition of Hazardous Substances in Electronic Motors on July 1, 2006. Nowadays, environmentally friendly flame retardants that are halogen-free, low-smoke, and low-toxicity have become the goal that people are pursuing. The halogen-free flame retardants for silicone rubber mainly include aluminum hydroxide, magnesium hydroxide, expanded graphite, intumescent flame retardants and Platinum compounds.

陶瓷化硅橡胶是一种新型的硅橡胶材料,它具有双重特性,室温条件下具有硅橡胶的基本特性,高温条件下具有陶瓷耐高温的特性。陶瓷化硅橡胶会在中高温(400-1000℃)由柔软的弹性体变成坚硬的陶瓷体,能够保持一定时间的电路完好,为被困人员的逃生和救援人员的工作赢取宝贵时间。因此兼具阻燃和耐火性能的陶瓷化硅橡胶显得尤为重要。Ceramic silicone rubber is a new type of silicone rubber material. It has dual characteristics. It has the basic characteristics of silicone rubber at room temperature and the high temperature resistance of ceramics at high temperature. Ceramic silicone rubber will change from soft elastic body to hard ceramic body at medium and high temperature (400-1000°C), which can keep the circuit intact for a certain period of time, and win valuable time for the escape of trapped people and the work of rescuers. Therefore, ceramic silicone rubber with flame retardancy and fire resistance is particularly important.

目前耐火电缆大多采用氧化镁矿物绝缘或云母带缠绕实现耐火的作用。氧化镁矿物绝缘耐火电缆生产所需的设备昂贵,运输和安装不方便,价格昂贵,因此没能被广泛普及和应用。另外一种云母带缠绕的耐火电缆,生产过程复杂,燃烧后绝缘体粉化严重,耐火效果差,难以保证电力通讯的正常运行。国内外已有多篇对陶瓷化硅橡胶复合材料的制备及其在电线电缆领域中的应用的报道。At present, most fire-resistant cables use magnesium oxide mineral insulation or mica tape winding to achieve fire resistance. The equipment required for the production of magnesium oxide mineral insulated fire-resistant cables is expensive, and the transportation and installation are inconvenient and expensive, so they have not been widely popularized and applied. Another kind of fire-resistant cable wrapped with mica tape has a complicated production process. After burning, the insulator is severely pulverized, and the fire-resistant effect is poor, so it is difficult to ensure the normal operation of power communication. There have been many reports at home and abroad on the preparation of ceramic silicone rubber composite materials and their application in the field of wire and cable.

中国专利文件CN103923465B公开了一种陶瓷化硅橡胶复合材料及其制备方法,该陶瓷化硅橡胶以生胶作为基体,添加补强剂、熔融助剂、瓷化粉和偶联剂制得,在1200℃燃烧得到发出清脆陶瓷声响的坚硬陶瓷体。但是,该陶瓷化硅橡胶的阻燃性能和加工性能比较差,难以满足实际的应用。Chinese patent document CN103923465B discloses a ceramic silicone rubber composite material and its preparation method. The ceramic silicone rubber is made of raw rubber as a matrix, adding reinforcing agent, melting aid, porcelain powder and coupling agent. Combustion at 1200°C results in a hard ceramic body that emits a crisp ceramic sound. However, the flame retardancy and processability of the ceramized silicone rubber are relatively poor, and it is difficult to meet practical applications.

中国专利文件CN104312159A公开了一种陶瓷化硅橡胶及其制备方法,主要由甲基乙烯基硅橡胶生胶、白炭黑、氢氧化铝和红磷混合物、纳米蒙脱土、羟基硅油、硬脂酸锌和1,3-二乙炔基四甲基二硅氧烷组成。该硅橡胶具有很高的阻燃性能,同时添加的填料不会影响硅橡胶的其它机械性能。但燃烧后得到的陶瓷体的力学性能低,不能承受外力的冲击,起不到有效耐火的作用。Chinese patent document CN104312159A discloses a kind of ceramic silicone rubber and its preparation method, which is mainly composed of methyl vinyl silicone rubber raw rubber, white carbon black, aluminum hydroxide and red phosphorus mixture, nano-montmorillonite, hydroxyl silicone oil, stearin Zinc acid and 1,3-diethynyltetramethyldisiloxane. The silicone rubber has high flame retardancy, and the added filler will not affect other mechanical properties of the silicone rubber. However, the ceramic body obtained after burning has low mechanical properties, cannot bear the impact of external force, and cannot effectively resist fire.

发明内容Contents of the invention

针对现有技术的缺陷,本发明着重研究了一种兼具阻燃和耐火性能的陶瓷化硅橡胶及其制备方法。Aiming at the defects of the prior art, the present invention focuses on researching a ceramic silicone rubber with flame-retardant and fire-resistant properties and a preparation method thereof.

为实现上述目的,本发明是通过以下技术方案实现的:To achieve the above object, the present invention is achieved through the following technical solutions:

一种陶瓷化阻燃耐火硅橡胶复合材料,其特征在于,所述的复合材料按质量份数计包括以下组分:A ceramic flame-retardant refractory silicone rubber composite material, characterized in that the composite material includes the following components in parts by mass:

所述的硅橡胶为二甲基硅橡胶、甲基苯基乙烯基硅橡胶和甲基乙烯基硅橡胶中的一种或几种,The silicone rubber is one or more of dimethyl silicone rubber, methyl phenyl vinyl silicone rubber and methyl vinyl silicone rubber,

所述的硅酸盐填料为云母、高岭土、蒙脱土、沸石、滑石粉、硅灰石中的一种或者多种,The silicate filler is one or more of mica, kaolin, montmorillonite, zeolite, talc, wollastonite,

所述的聚磷酸铵为聚合度大于1000的II型APP,且颗粒尺寸为500-3000目,所述的碳酸钙为微米级且颗粒尺寸为500-3000目,所述的硅酸盐填料颗粒尺寸为500-3000目,所述的助熔剂颗粒尺寸为500-3000目,The ammonium polyphosphate is type II APP with a degree of polymerization greater than 1000, and the particle size is 500-3000 mesh, the calcium carbonate is micron-sized and the particle size is 500-3000 mesh, and the silicate filler particles The size is 500-3000 mesh, and the flux particle size is 500-3000 mesh,

所述的助熔剂为软化点不低于300℃的玻璃粉、氧化锌、硼酸锌、硼砂、氧化硼中的一种或多种,The flux is one or more of glass powder, zinc oxide, zinc borate, borax, boron oxide with a softening point not lower than 300°C,

所述的硫化剂为过氧化二异丙苯,2,5-二甲基-2,5-双(过氧化叔丁基)己烷中的一种。The vulcanizing agent is one of dicumyl peroxide and 2,5-dimethyl-2,5-bis(t-butyl peroxide)hexane.

优选地,所述复合材料的组分中,聚磷酸铵:碳酸钙=1:1。Preferably, among the components of the composite material, ammonium polyphosphate: calcium carbonate = 1:1.

本发明还提供了一种陶瓷化阻燃耐火硅橡胶复合材料的制备方法:The present invention also provides a preparation method of ceramic flame-retardant and refractory silicone rubber composite material:

(1)将硅橡胶、聚磷酸铵、碳酸钙、硅酸盐填料和助熔剂在开炼机上混合均匀,再加入硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃;(1) Mix silicone rubber, ammonium polyphosphate, calcium carbonate, silicate filler and flux on the open mill evenly, then add vulcanizing agent and continue to knead evenly on the open mill to form flakes, the temperature is not higher than 30°C;

(2)将步骤(1)得到的胶料于160-180℃、15Mpa在平板硫化仪下热压4-20min成型;(2) Hot press the rubber compound obtained in step (1) at 160-180°C and 15Mpa for 4-20min under a flat vulcanizer;

(3)将步骤(2)压制成型的材料在200℃烘箱下进行二段硫化2h,即可得到陶瓷化阻燃耐火硅橡胶。(3) The material press-molded in step (2) is subjected to two-stage vulcanization in an oven at 200°C for 2 hours to obtain ceramicized flame-retardant and refractory silicone rubber.

有益效果Beneficial effect

本发明的优势:Advantages of the present invention:

本发明所使用的聚磷酸铵和碳酸钙作为无卤阻燃剂,无毒无味,不产生腐蚀气体,且在合适的配比下更能够大大改善硅橡胶的阻燃性及陶瓷表面的平整度。The ammonium polyphosphate and calcium carbonate used in the present invention are non-toxic, tasteless, and do not produce corrosive gas as halogen-free flame retardants, and can greatly improve the flame retardancy of silicone rubber and the smoothness of ceramic surfaces under a suitable ratio .

本发明所使用的助熔剂能在中高温下(600-1000℃)发生熔融,熔融后粘度很大,能够将SiO2与无机硅酸盐填料连接起来,形成一个整体;并且随着温度的延长,液相组分更多扩散并填充到固相颗粒之间,形成更加坚硬的陶瓷体。The flux used in the present invention can melt at medium and high temperature (600-1000° C.), has a high viscosity after melting, and can connect SiO2 with inorganic silicate filler to form a whole; and as the temperature prolongs , the liquid phase components diffuse more and fill between the solid phase particles, forming a harder ceramic body.

本发明所使用的硅酸盐填料具有很好的热阻隔作用,在高温下熔融与其它填料更好的粘结,且能够作为骨架结构,起着支撑的作用。The silicate filler used in the present invention has a good thermal barrier effect, can be melted at high temperature to better bond with other fillers, and can be used as a skeleton structure to play a supporting role.

本发明制备的陶瓷化硅橡胶制备方法简单,加工方便,可以被加工成各种挤出产品和模压成品,适合于产业化。本发明通过添加各种阻燃填料和助熔剂来制备兼具阻燃和耐火性能的陶瓷化硅橡胶复合材料,硅橡胶的拉伸强度达到5Mpa以上,断裂伸长率为250%以上,且氧指数能达到30以上,不易发生燃烧;另外本发明的陶瓷化硅橡胶能够在600-1000℃温度下形成坚硬的陶瓷体,能抵抗外力,保持一定时间的电路完好,保持一定的自支撑作用,并且随着烧结时间的延长和烧结温度的提高,陶瓷体越坚硬,起着优异的隔火隔热的作用。The ceramic silicone rubber prepared by the invention has simple preparation method and convenient processing, can be processed into various extruded products and molded finished products, and is suitable for industrialization. The present invention prepares ceramicized silicone rubber composite materials with both flame-retardant and fire-resistant properties by adding various flame-retardant fillers and fluxes. The index can reach more than 30, and it is not easy to burn; in addition, the ceramic silicone rubber of the present invention can form a hard ceramic body at a temperature of 600-1000 ° C, which can resist external forces, keep the circuit intact for a certain period of time, and maintain a certain self-supporting effect. And with the prolongation of sintering time and the increase of sintering temperature, the ceramic body becomes harder and plays an excellent role of fire and heat insulation.

附图说明Description of drawings

图1是本发明实施例1在400,600,800,1000℃煅烧60min后的扫描电子显微镜照片,图中,a为400℃煅烧处理后的电镜图;b为600℃煅烧处理后的电镜图;c为800℃煅烧处理后的电镜图;d为1000℃煅烧处理后的电镜图;Fig. 1 is a scanning electron micrograph of Example 1 of the present invention after calcination at 400, 600, 800, and 1000°C for 60 minutes. In the figure, a is the electron micrograph after calcination at 400°C; b is the electron micrograph after calcination at 600°C; c is 800°C The electron micrograph after calcination at ℃; d is the electron micrograph after calcination at 1000℃;

图2是本发明实施例1在不同温度(400,600,800,1000℃)煅烧得到的陶瓷体XRD晶型图;Fig. 2 is the XRD crystal pattern of the ceramic body calcined at different temperatures (400, 600, 800, 1000° C.) in Example 1 of the present invention;

图3是本发明实施例1在1000℃温度下表现出良好的自支撑性能图;Fig. 3 is a graph showing good self-supporting properties at a temperature of 1000°C in Example 1 of the present invention;

图4是本发明对比实施例1,对比实施例2,实施例1和纯硅橡胶通过微型量热仪测试的结果,其中SR0为纯硅橡胶,SR1为对比实施例1,SR2为对比实施例2,SR3为实施例1;HRC:热释放能力;Peak HRR:热释放速率峰值;Ignition temperature:最高裂解温度;THR:总热释放。Fig. 4 is the result of comparative example 1 of the present invention, comparative example 2, embodiment 1 and pure silicone rubber tested by microcalorimeter, wherein SR0 is pure silicone rubber, SR1 is comparative example 1, and SR2 is comparative example 2. SR3 is Example 1; HRC: heat release capacity; Peak HRR: peak heat release rate; Ignition temperature: maximum cracking temperature; THR: total heat release.

具体实施方法Specific implementation method

本发明的特征及优点将通过实施例进行详细说明,但所述实施例仅用于本发明而不是限制本发明。The features and advantages of the present invention will be described in detail through examples, but the examples are only for the present invention rather than limiting the present invention.

对比例1Comparative example 1

一种阻燃耐火陶瓷化硅橡胶,其原料按重量份的组成配制,具体如下:A flame-retardant refractory ceramic silicone rubber, its raw materials are prepared according to the composition of parts by weight, specifically as follows:

将甲基乙烯基硅橡胶50份、高岭土20份和玻璃粉12份在开炼机上混合均匀;再加入0.5份的双2,5硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:180℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到陶瓷化阻燃耐火硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为7.5Mpa,断裂伸长率为310%,氧指数为29.2%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,弯曲强度为7.8Mpa。Mix 50 parts of methyl vinyl silicone rubber, 20 parts of kaolin and 12 parts of glass powder on the open mill; then add 0.5 parts of double 2,5 vulcanizing agent and continue to knead on the open mill to form a uniform sheet, the temperature is not high At 30°C, and finally hot-pressed for 15 minutes under a flat vulcanizer (condition: 180°C, 15Mpa) for molding, and the molded material was subjected to two-stage vulcanization in an oven at 200°C for 2 hours to obtain a ceramic flame-retardant and refractory silicone rubber compound. Material. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant ceramic silicone rubber composite material into 40*4*3mm splines, and calcined in the muffle furnace , from room temperature to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of the composite material is 7.5Mpa, the elongation at break is 310%, and the oxygen index is 29.2%. It can be sintered into hard ceramics at 1000°C, and it can make a crisp ceramic sound when knocked. The bending strength is 7.8Mpa.

对比例2Comparative example 2

将甲基乙烯基硅橡胶50份、聚磷酸铵5份、云母粉18份和玻璃粉12份在开炼机上混合均匀;再加入0.5份的双2,5硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:180℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到陶瓷化阻燃耐火硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为6.65Mpa,断裂伸长率为289%,氧指数为29.8%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,但是烧结后的样品发生翘曲,无法测试陶瓷体的弯曲强度。Mix 50 parts of methyl vinyl silicone rubber, 5 parts of ammonium polyphosphate, 18 parts of mica powder and 12 parts of glass powder on the open mill; add 0.5 parts of double 2,5 vulcanizing agent and continue mixing on the open mill Uniformly formed into sheets, the temperature is not higher than 30°C, and finally hot-pressed for 15 minutes under a flat vulcanizer (condition: 180°C, 15Mpa) to form, and the formed material is subjected to two-stage vulcanization in an oven at 200°C for 2 hours to obtain ceramics Chemical flame retardant and refractory silicone rubber composite materials. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant ceramic silicone rubber composite material into 40*4*3mm splines, and calcined in the muffle furnace , from room temperature to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of this composite material is 6.65Mpa, the elongation at break is 289%, and the oxygen index is 29.8%. The sample warped, unable to test the bending strength of the ceramic body.

实施例1Example 1

本发明的一种阻燃耐火陶瓷化硅橡胶,其原料按重量份的组成配制,具体如下:A kind of flame-retardant refractory vitrified silicon rubber of the present invention, its raw material is prepared by the composition of weight part, specifically as follows:

将甲基乙烯基硅橡胶50份、聚磷酸铵5份、碳酸钙5份、蒙脱土20份和玻璃粉25份在开炼机上混合均匀;再加入0.7份的双2,5硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:180℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到阻燃耐火陶瓷化硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃耐火陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,试样两边夹在耐火砖上,中间悬空,中间跨距25mm,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为5.3Mpa,断裂伸长率为283%,氧指数为35%,在1000℃下能够烧结成坚硬的陶瓷,形成的陶瓷体表面平整光滑,敲击能发出清脆的陶瓷声音,并且有一定的自支撑能力,弯曲强度为16.5MPa。Mix 50 parts of methyl vinyl silicone rubber, 5 parts of ammonium polyphosphate, 5 parts of calcium carbonate, 20 parts of montmorillonite and 25 parts of glass powder on the open mill; add 0.7 parts of double 2,5 vulcanizing agent to continue Knead evenly on an open mill to form a sheet, the temperature is not higher than 30°C, and finally hot press for 15min under a flat vulcanizer (condition: 180°C, 15Mpa) to form, and the formed material is subjected to secondary processing in an oven at 200°C Stage vulcanization for 2 hours to obtain a flame-retardant and refractory ceramic silicone rubber composite material. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant and refractory ceramic silicone rubber composite material into 40*4*3mm splines, and clamp the sample on both sides On refractory bricks, the middle is suspended, the middle span is 25mm, calcined in a muffle furnace, the temperature is raised from room temperature to 1000°C at 10°C/min, and kept at 1000°C for 60min, and the calcined ceramic body is tested for mechanical properties. The measured tensile strength of the composite material is 5.3Mpa, the elongation at break is 283%, and the oxygen index is 35%. It can be sintered into hard ceramics at 1000°C. Crisp ceramic sound, and has a certain self-supporting ability, with a bending strength of 16.5MPa.

实施例2Example 2

本发明的一种阻燃耐火陶瓷化硅橡胶,其原料按质量份的组成配制,具体如下:A kind of flame-retardant refractory vitrified silicon rubber of the present invention, its raw material is prepared according to the composition of mass parts, specifically as follows:

将甲基乙烯基硅橡胶50份、聚磷酸铵1份、碳酸钙5份、云母20份和硼酸锌10份在开炼机上混合均匀;再加入0.5份的过氧化二异丙苯硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:160℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到阻燃耐火陶瓷化硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为6.3Mpa,断裂伸长率为315%,氧指数为32%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,弯曲强度为9.8Mpa。Mix 50 parts of methyl vinyl silicone rubber, 1 part of ammonium polyphosphate, 5 parts of calcium carbonate, 20 parts of mica and 10 parts of zinc borate on an open mill; add 0.5 parts of dicumyl peroxide vulcanizing agent to continue Knead evenly on an open mill to form a sheet, the temperature is not higher than 30°C, and finally hot press for 15min under a flat vulcanizer (condition: 160°C, 15Mpa) to form, and the formed material is subjected to secondary processing in an oven at 200°C Stage vulcanization for 2 hours to obtain a flame-retardant and refractory ceramic silicone rubber composite material. The mechanical properties and oxygen index tests were performed on the ceramicized silicone rubber composite material before ablation, and the prepared ceramicized silicone rubber composite material was cut into 40*4*3mm splines, calcined in a muffle furnace, and obtained from The room temperature was raised to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of the composite material is 6.3Mpa, the elongation at break is 315%, and the oxygen index is 32%. It can be sintered into hard ceramics at 1000°C, and it can make a crisp ceramic sound when knocked. The bending strength is 9.8Mpa.

实施例3Example 3

本发明的一种阻燃耐火陶瓷化硅橡胶,其原料按质量份的组成配制,具体如下:A kind of flame-retardant refractory vitrified silicon rubber of the present invention, its raw material is prepared according to the composition of mass parts, specifically as follows:

将甲基苯基乙烯基硅橡胶胶40份、甲基乙烯基硅橡胶30份、聚磷酸铵5份、碳酸钙5份、云母粉30份和氧化锌18份在开炼机上混合均匀;再加入1份的过氧化二异丙苯硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:160℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到陶瓷化阻燃耐火硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为3.1Mpa,断裂伸长率为150%,氧指数为37%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,弯曲强度为10.5MPa。Mix 40 parts of methyl phenyl vinyl silicone rubber, 30 parts of methyl vinyl silicone rubber, 5 parts of ammonium polyphosphate, 5 parts of calcium carbonate, 30 parts of mica powder and 18 parts of zinc oxide on an open mill; Add 1 part of dicumyl peroxide vulcanizing agent and continue to knead on the open mill to form a sheet evenly, the temperature is not higher than 30°C, and finally hot press for 15min under a flat vulcanizer (condition: 160°C, 15Mpa) to form. The molded material was subjected to two-stage vulcanization in an oven at 200°C for 2 hours to obtain a ceramicized flame-retardant and refractory silicone rubber composite material. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant ceramic silicone rubber composite material into 40*4*3mm splines, and calcined in the muffle furnace , from room temperature to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of the composite material is 3.1Mpa, the elongation at break is 150%, and the oxygen index is 37%. It can be sintered into hard ceramics at 1000°C, and it can make a crisp ceramic sound when knocked. The bending strength is 10.5MPa.

实施例4Example 4

本发明的一种阻燃耐火陶瓷化硅橡胶,其原料按重量份的组成配制,具体如下:A kind of flame-retardant refractory vitrified silicon rubber of the present invention, its raw material is prepared by the composition of weight part, specifically as follows:

将甲基苯基乙烯基硅橡胶50份、聚磷酸铵15份、碳酸钙10份、滑石粉20份和玻璃粉15份在开炼机上混合均匀;再加入0.4份的双2,5硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:170℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到陶瓷化阻燃耐火硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为3.6Mpa,断裂伸长率为168%,氧指数为36%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,弯曲强度为10.9Mpa。Mix 50 parts of methylphenyl vinyl silicone rubber, 15 parts of ammonium polyphosphate, 10 parts of calcium carbonate, 20 parts of talc powder and 15 parts of glass powder on the open mill; add 0.4 parts of double 2,5 vulcanizing agent Continue to knead on the open mill to form a uniform sheet, the temperature is not higher than 30°C, and finally hot press for 15min under the flat vulcanizer (condition: 170°C, 15Mpa) to form, and the formed material is processed in an oven at 200°C Two-stage vulcanization for 2 hours to obtain ceramic flame-retardant and refractory silicone rubber composite materials. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant ceramic silicone rubber composite material into 40*4*3mm splines, and calcined in the muffle furnace , from room temperature to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of the composite material is 3.6Mpa, the elongation at break is 168%, and the oxygen index is 36%. It can be sintered into hard ceramics at 1000°C, and it can make a crisp ceramic sound when knocked. The bending strength is 10.9 MPa.

实施例5Example 5

本发明的一种阻燃耐火陶瓷化硅橡胶,其原料按重量份的组成配制,具体如下:A kind of flame-retardant refractory vitrified silicon rubber of the present invention, its raw material is prepared by the composition of weight part, specifically as follows:

将二甲基硅橡胶80份、聚磷酸铵10份、碳酸钙5份、云母粉30份和硼酸锌18份在开炼机上混合均匀;再加入0.5份的双2,5硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃,最后在平板硫化仪下(条件:180℃,15Mpa)下热压15min成型,将成型后的材料在200℃的烘箱中进行二段硫化2h,得到陶瓷化阻燃耐火硅橡胶复合材料。将未烧蚀前的陶瓷化硅橡胶复合材料进行力学性能和氧指数测试,并将制备好的阻燃陶瓷化硅橡胶复合材料裁成40*4*3mm的样条,在马弗炉中煅烧,从室温以10℃/min升温到1000℃,并在1000℃下保温60min,将煅烧后的陶瓷体进行力学性能测试。该复合材料测得的拉伸强度为4.1Mpa,断裂伸长率为205%,氧指数为39%,在1000℃下能够烧结成坚硬的陶瓷,敲击能发出清脆的陶瓷声音,弯曲强度为10.3Mpa。Mix 80 parts of dimethyl silicone rubber, 10 parts of ammonium polyphosphate, 5 parts of calcium carbonate, 30 parts of mica powder and 18 parts of zinc borate on the open mill; Mix evenly on the mill to form a sheet, the temperature is not higher than 30°C, and finally hot press for 15min under a flat vulcanizer (condition: 180°C, 15Mpa) to form, and the formed material is subjected to two-stage vulcanization in an oven at 200°C After 2 hours, a ceramicized flame-retardant and refractory silicone rubber composite material was obtained. Test the mechanical properties and oxygen index of the ceramic silicone rubber composite material before ablation, and cut the prepared flame-retardant ceramic silicone rubber composite material into 40*4*3mm splines, and calcined in the muffle furnace , from room temperature to 1000°C at a rate of 10°C/min, and kept at 1000°C for 60 minutes, and the mechanical properties of the calcined ceramic body were tested. The measured tensile strength of the composite material is 4.1Mpa, the elongation at break is 205%, and the oxygen index is 39%. It can be sintered into hard ceramics at 1000°C, and it can make a crisp ceramic sound when knocked. The bending strength is 10.3Mpa.

微型量热仪测试结果如说明书附图4所示,其对应的数据见表1The test results of the microcalorimeter are shown in Figure 4 of the specification, and the corresponding data are shown in Table 1

表1Table 1

其中,HRC:热释放能力;Peak HRR:热释放速率峰值;Ignition temperature:Among them, HRC: heat release capacity; Peak HRR: peak heat release rate; Ignition temperature:

最高裂解温度;THR:总热释放Maximum cracking temperature; THR: total heat release

从表1可以看出,本发明的阻燃耐火硅橡胶的热释放速率和总释放热有明显的下降,效果明显。且从各实施例可以看出,本发明所制备的阻燃耐火硅橡胶复合材料完全能够满足一定的力学强度,与此同时还具备优异的阻燃耐火性能,故能够在电线电缆、电力通讯等领域发挥重要作用。It can be seen from Table 1 that the heat release rate and total release heat of the flame-retardant and refractory silicone rubber of the present invention are significantly reduced, and the effect is obvious. And it can be seen from each embodiment that the flame-retardant and refractory silicone rubber composite material prepared by the present invention can fully satisfy a certain mechanical strength, and at the same time also has excellent flame-retardant and fire-resistant properties, so it can be used in wires and cables, power communications, etc. areas play an important role.

Claims (4)

1.一种陶瓷化阻燃耐火硅橡胶复合材料,其特征在于,所述的复合材料按质量份数计包括以下组分:1. A ceramic flame-retardant refractory silicone rubber composite material, characterized in that, the composite material comprises the following components in parts by mass: 所述的硅橡胶为二甲基硅橡胶、甲基苯基乙烯基硅橡胶和甲基乙烯基硅橡胶中的一种或几种,The silicone rubber is one or more of dimethyl silicone rubber, methyl phenyl vinyl silicone rubber and methyl vinyl silicone rubber, 所述的聚磷酸铵为聚合度大于1000的II型APP,The ammonium polyphosphate is type II APP with a degree of polymerization greater than 1000, 所述的硅酸盐填料为云母、高岭土、蒙脱土、沸石、滑石粉、硅灰石中的一种或者多种,The silicate filler is one or more of mica, kaolin, montmorillonite, zeolite, talc, wollastonite, 所述的助熔剂为软化点不低于300℃的玻璃粉、氧化锌、硼酸锌、硼砂、氧化硼中的一种或多种,The flux is one or more of glass powder, zinc oxide, zinc borate, borax, boron oxide with a softening point not lower than 300°C, 所述的硫化剂为过氧化二异丙苯,2,5-二甲基-2,5-双(过氧化叔丁基)己烷中的一种。The vulcanizing agent is one of dicumyl peroxide and 2,5-dimethyl-2,5-bis(t-butyl peroxide)hexane. 2.如权利要求1所述的一种陶瓷化阻燃耐火硅橡胶复合材料,其特征在于,所述的聚磷酸铵的颗粒尺寸为500-3000目,所述的碳酸钙为微米级且颗粒尺寸为500-3000目,所述的硅酸盐填料颗粒尺寸为500-3000目,所述的助熔剂颗粒尺寸为500-3000目。2. A kind of ceramization flame-retardant refractory silicone rubber composite material as claimed in claim 1, is characterized in that, the particle size of described ammonium polyphosphate is 500-3000 order, and described calcium carbonate is micron order and particle The size is 500-3000 mesh, the silicate filler particle size is 500-3000 mesh, and the flux particle size is 500-3000 mesh. 3.如权利要求1所述的一种陶瓷化阻燃耐火硅橡胶复合材料,其特征在于,所述复合材料的组分中,聚磷酸铵:碳酸钙=1:1。3. A ceramic flame-retardant and refractory silicone rubber composite material as claimed in claim 1, characterized in that, among the components of the composite material, ammonium polyphosphate: calcium carbonate=1:1. 4.一种陶瓷化阻燃耐火硅橡胶复合材料的制备方法,其特征在于,所述方法包括如下步骤:4. a preparation method of ceramic flame-retardant refractory silicone rubber composite material, is characterized in that, described method comprises the steps: (1)将硅橡胶、聚磷酸铵、碳酸钙、硅酸盐填料和助熔剂在开炼机上混合均匀,再加入硫化剂继续在开炼机上混炼均匀成片,温度不高于30℃;(1) Mix silicone rubber, ammonium polyphosphate, calcium carbonate, silicate filler and flux on the open mill evenly, then add vulcanizing agent and continue to knead evenly on the open mill to form flakes, the temperature is not higher than 30°C; (2)将步骤(1)得到的胶料于160-180℃、15Mpa在平板硫化仪下热压4-20min成型;(2) Hot press the rubber compound obtained in step (1) at 160-180°C and 15Mpa for 4-20min under a flat vulcanizer; (3)将步骤(2)压制成型的材料在200℃烘箱下进行二段硫化2h,即可得到陶瓷化阻燃耐火硅橡胶。(3) The material press-molded in step (2) is subjected to two-stage vulcanization in an oven at 200°C for 2 hours to obtain ceramicized flame-retardant and refractory silicone rubber.
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CN108003633A (en) * 2017-12-19 2018-05-08 大连理工常州研究院有限公司 It is a kind of that there is the excellent resistance to Ceramic silicon rubber composition for burning performance
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CN112341820A (en) * 2020-11-30 2021-02-09 北京宇航系统工程研究所 Instantaneous high-temperature-resistant silicone rubber and preparation method thereof
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CN107722535A (en) * 2017-09-25 2018-02-23 江苏奔拓电气科技有限公司 A kind of preparation method of fire-resistant silicon rubber cable
CN108003633A (en) * 2017-12-19 2018-05-08 大连理工常州研究院有限公司 It is a kind of that there is the excellent resistance to Ceramic silicon rubber composition for burning performance
CN108059834A (en) * 2017-12-19 2018-05-22 大连理工常州研究院有限公司 A kind of battery cell case material with fire protecting performance
CN109957248A (en) * 2017-12-22 2019-07-02 洛阳尖端技术研究院 Composition for forming flame retardant silicone rubber and flame retardant silicone rubber
CN109266007A (en) * 2018-09-27 2019-01-25 唐山师范学院 Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber
CN109796870A (en) * 2019-01-07 2019-05-24 上海航天精密机械研究所 Can the porcelainization silicon rubber composite material of resistance to ablation coating and its coating preparation method
CN109880176A (en) * 2019-01-24 2019-06-14 深圳市锦昊辉矿业发展有限公司 Low temperature ceramic polymer matrix composite
CN110982185A (en) * 2019-12-16 2020-04-10 应急管理部天津消防研究所 A fireproof sealing rubber material
CN111627606A (en) * 2020-05-25 2020-09-04 浙江德通科技有限公司 High-flame-retardancy coaxial radio frequency cable and preparation method thereof
CN111471304A (en) * 2020-06-03 2020-07-31 苏州法思特新材料有限公司 Flame-retardant and fire-resistant silicon rubber material and preparation method and application thereof
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CN112152182A (en) * 2020-10-15 2020-12-29 深圳供电局有限公司 Fire protection device for cable intermediate joint, method of manufacture and use
CN112341820A (en) * 2020-11-30 2021-02-09 北京宇航系统工程研究所 Instantaneous high-temperature-resistant silicone rubber and preparation method thereof
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Application publication date: 20170613