CN106751560A - Polybutylene terephthalate material-reinforced basalt fiber special-purpose infiltrating agent and preparation method thereof - Google Patents

Polybutylene terephthalate material-reinforced basalt fiber special-purpose infiltrating agent and preparation method thereof Download PDF

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CN106751560A
CN106751560A CN 201611072796 CN201611072796A CN106751560A CN 106751560 A CN106751560 A CN 106751560A CN 201611072796 CN201611072796 CN 201611072796 CN 201611072796 A CN201611072796 A CN 201611072796A CN 106751560 A CN106751560 A CN 106751560A
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basalt fiber
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德阳力久云智知识产权运营有限公司
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUSE OF INORGANIC OR NON-MACROMOLECULAR ORGANIC SUBSTANCES AS COMPOUNDING INGREDIENTS
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
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    • C08K7/10Silicon-containing compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUSE OF INORGANIC OR NON-MACROMOLECULAR ORGANIC SUBSTANCES AS COMPOUNDING INGREDIENTS
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUSE OF INORGANIC OR NON-MACROMOLECULAR ORGANIC SUBSTANCES AS COMPOUNDING INGREDIENTS
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUSE OF INORGANIC OR NON-MACROMOLECULAR ORGANIC SUBSTANCES AS COMPOUNDING INGREDIENTS
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUSE OF INORGANIC OR NON-MACROMOLECULAR ORGANIC SUBSTANCES AS COMPOUNDING INGREDIENTS
    • C08K9/00Use of pretreated ingredients
    • C08K9/08Ingredients agglomerated by treatment with a binding agent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds

Abstract

The invention discloses a polybutylene terephthalate material-reinforced basalt fiber special-purpose infiltrating agent and a preparation method thereof. The infiltrating agent comprises, by weight, 40 to 60 parts of a film-forming agent, 5 to 15 parts of a coupling agent, 1 to 5 parts of a lubricant, 10 to 20 parts of a modifier and 30 to 50 parts of a solvent. The modifier comprises hypophosphite, strong base and maleate according to a mass ratio of 2-4: 1-3: 4-6. The modifier modifies the fiber surfaces in infiltration so that fiber surface roughness is improved and a lot of active groups are grafted and thus chemical bonding and mechanical riveting ability of the basalt fibers and butylene terephthalate material are improved, compatibility of the basalt fibers and butylene terephthalate material is improved and use of the basalt fibers in the field of polybutylene terephthalate enhancement is promoted.

Description

一种聚对苯二甲酸丁二醇酯材料増强玄武岩纤维专用浸润剂及其制备方法 A poly basalt fiber strong wetting agents and specific method for preparing polybutylene terephthalate material zo

技术领域 FIELD

[0001] 本发明涉及玄武岩纤维浸润剂领域,具体涉及一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂及其制备方法。 [0001] The present invention relates to the field of basalt fiber sizes, particularly relates to basalt fiber special wetting agent and a process for preparing poly (butylene terephthalate) reinforcing material.

背景技术 Background technique

[0002] 玄武岩纤维是一种新出现的新型无机环保绿色高性能纤维材料,是未来我国重点发展的四大高性能纤维之一,它是由二氧化硅、氧化铝、氧化钙、氧化铁和二氧化钛等氧化物组成的玄武岩石料在高温熔融后,通过纺丝工艺制备而成的。 [0002] Basalt fiber is a new type of environmentally friendly green high performance inorganic fiber material an emerging, is one of four high-performance fiber future focus on the development of our country, which is composed of silica, alumina, calcium oxide, iron oxide and basalt titania oxides in the high temperature melting, prepared from by a spinning process. 玄武岩连续纤维不仅稳定性好,而且还具有电绝缘性、抗腐蚀、抗燃烧、耐高温等多种优异性能,而且,玄武岩纤维的生产工艺产生的废弃物少,对环境污染小,产品废弃后可直接转入生态环境中,无任何危害,因而是一种名副其实的绿色、环保材料。 Basalt fiber is not only stable, but also has an electrically insulating property, corrosion resistance, burning, and other excellent high temperature performance, and, less waste basalt fiber produced by the process of production, environmental pollution, the waste products It can be transferred directly to the ecological environment, without any harm, so it is a truly green, environmentally friendly materials. 玄武岩连续纤维已在纤维增强复合材料、摩擦材料、造船材料、隔热材料、汽车行业、高温过滤织物以及防护领域等多个方面得到了广泛的应用。 Basalt continuous fiber has a fiber-reinforced composite material, a plurality of friction material aspects, shipbuilding material, heat insulating materials, automobile industry, the field of high temperature filtration fabrics and protection have been widely applied.

[0003] 聚对苯二甲酸丁二醇酯(简称PBT)又名聚四亚甲基对苯二甲酸酯,是通过对苯二甲酸和1,4_ 丁二醇缩聚制成的聚酯。 [0003] Poly (butylene terephthalate) (abbreviation PBT), also known as polytetramethylene terephthalate, a polyester produced by polycondensation of terephthalic acid and butanediol 1,4_. 最重要的热塑性聚酯,五大工程塑料之一,具有耐热性好、韧性好、耐疲劳,自润滑、低摩擦系数等优点;但由于聚对苯二甲酸丁二醇酯中酯基活泼性好,导致聚对苯二甲酸丁二醇酯材料存在不耐强酸、强碱,可燃,高温下分解的缺陷,因此,在使用时多不使用纯的聚对苯二甲酸丁二醇酯材料,聚对苯二甲酸丁二醇酯材料需要进行阻燃、耐腐蚀、耐高温等增强复合改性处理后才能进行应用。 The most important thermoplastic polyester, one of the five engineering plastics having good heat resistance, good toughness, fatigue resistance, self-lubricating, low friction coefficient and the like; ester-based but because polyethylene terephthalate in an inert good, resulting in the presence of poly intolerance acid, alkali polybutylene terephthalate material, flammable, high temperature decomposition of defect, and therefore, do not use multi-pure polybutylene terephthalate material in use, poly (butylene terephthalate) material needs to be flame retardant, corrosion, temperature and other reinforced composite to be modified after the application process. 现今对聚对苯二甲酸丁二醇酯材料的纤维增强改性主要采用玻璃纤维材料进行改性处理,改性效果显著,但玻璃纤维生产成本高、环境污染大,严重限制了复合聚对苯二甲酸丁二醇酯材料的应用,开发一种成本低廉、绿色环保、性能优异的新型纤维材料替代玻璃纤维对聚对苯二甲酸丁二醇酯材料进行改性处理的问题急需得到解决。 Nowadays poly (butylene terephthalate) fiber material is glass fiber reinforced modified main materials modification, modification effect is remarkable, but the high production costs of glass fibers, environment pollution, severely limits the composite polyparaphenylene acid glycol ester materials use to develop a low-cost, excellent in environmental protection, the performance of the new fiber material instead of glass fibers of polyethylene terephthalate, polybutylene terephthalate material modification of issues need to be resolved. 因而,可以预见,将无毒、无污染、来源广泛、性能优异、稳定好的玄武岩纤维用于聚对苯二甲酸丁二醇酯材料的增强必将是今后提高聚对苯二甲酸丁二醇酯材料性能的新趋势。 Accordingly, it is anticipated, will be non-toxic, wide variety of sources, excellent performance, good stability for the basalt fiber reinforced poly (butylene terephthalate) material will improve future polybutylene terephthalate new trends in material properties ester. 但由于现有玄武岩纤维自身结构和性能稳定,纤维表面光滑、表面活性位点少,造成玄武岩纤维在改性过程中难以与聚对苯二甲酸丁二醇酯材料化学键合和机械铆合形成统一的、稳定的整体,即玄武岩纤维在聚对苯二甲酸丁二醇酯材料中是独立存在,对聚对苯二甲酸丁二醇酯材料的改性增强作用相对较弱,增强效果不甚理想,玄武岩纤维添加量少。 However, since the conventional basalt fiber stabilizing its structure and properties, a smooth fiber surface, less surface active sites, resulting in difficult to form a uniform basalt fiber with polyethylene terephthalate material, chemical bonding and mechanical riveting in the modification process , stable overall, i.e. in the basalt fiber material polyethylene terephthalate, polybutylene terephthalate is present independently, poly (butylene terephthalate) modified reinforcement material is relatively weak, the effect is not enhanced over the , add less basalt fiber.

[0004] 浸润剂作为纤维生产过程中用到的最重要的辅助试剂,不仅能对纤维进行物理包覆,增加纤维韧性和润滑性,还能对纤维表面进行化学处理,增加纤维功能性,因此,采用浸润剂对纤维材料进行改性处理,即将纤维的生产和改性合二为一,节简化了生产步骤,节约了生产成本,缩短了生产周期,还能赋予纤维新的性能以满足纤维在不同领域、不同环境中的应用,因此,利用专用浸润剂在玄武岩纤维生产过程中对玄武岩纤维表面进行改性以提高玄武岩纤维与聚对苯二甲酸丁二醇酯材料的相容性是可行的,有利于促进玄武岩纤维在聚对苯二甲酸丁二醇酯材料增强领域中的推广应用。 [0004] The wetting agent as the fiber production process used in the most important auxiliary agents, not only physically coating the fibers, increasing the fiber tenacity and lubricity, but also for chemical treatment of the fiber surface, to increase fiber function, and therefore , wetting agent employed for modification of the fibrous material, production and modification coming into one fiber, simplifying the production step of the section, saving production costs and shorten the production cycle, but also to impart new properties to meet fiber fibers in different areas of applications in different environments, and therefore, the use of special wetting agents basalt fiber surface is modified basalt fiber production process in order to improve the compatibility of the basalt fiber with polyethylene terephthalate material is feasible is conducive to facilitate the deployment of the basalt fiber material is polyethylene terephthalate reinforced areas.

发明内容 SUMMARY

[0005] 本发明的目的在于克服现有玄武岩纤维浸润剂不能提高玄武岩纤维与聚对苯二甲酸丁二醇酯材料相容性的缺陷,提供一种聚对苯二甲酸丁二醇酯增强玄武岩纤维专用浸润剂及其制备方法;本发明浸润剂中含有改性剂,通过改性剂在浸润的同时对纤维表面进行改性,使纤维表面粗糙度增加并接枝大量活性基团,从而提高玄武岩纤维与聚对苯二甲酸丁二醇酯材料之间的化学键合和机械铆合能力,提高了玄武岩纤维与聚对苯二甲酸丁二醇酯材料的相容性,促进了玄武岩纤维在聚对苯二甲酸丁二醇酯材料增强领域中的推广应用。 [0005] The object of the present invention is to overcome the conventional basalt fiber sizes can increase defects basalt fiber with polyethylene terephthalate compatibility of the material, there is provided a reinforced polyethylene terephthalate basalt fiber special wetting agent and preparation method thereof; wetting agent of the present invention contains a modifier by the modifier while wetted fiber surface modification, that the fiber surface roughness increases and a large number of graft-active groups, thereby increasing the basalt fiber and poly mechanical staking and chemical bonding capability between the polybutylene terephthalate materials, basalt fiber improves the compatibility with the poly (butylene terephthalate) materials, basalt fiber in promoting poly application in the field of polyester material reinforced polybutylene terephthalate.

[0006] 为了实现上述发明目的,本发明提供了一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,包括以下重量份组分:40-60份的成膜剂、5-15份的偶联剂、1-5份润滑剂、10-20份的改性剂、30-50份的溶剂。 [0006] In order to achieve the above object, the present invention provides a polybutylene terephthalate ester basalt fiber reinforcing material special wetting agents, comprising by weight parts of the following components: 40-60 parts of a film-forming agent, 5 15 parts coupling agent, 1-5 parts lubricant, 10-20 parts of a modifying agent, 30-50 parts of a solvent.

[0007] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的改性剂包括次磷酸盐:强碱:顺丁烯二酸盐按质量比2-4:1-3:4-6混合而成的混合物;所述改性剂组成能快速对玄武岩纤维表面腐蚀、活化,形成粗糙表面,并接枝大量活性基团,使纤维表面形成大量活性位点和活性基团,从而使玄武岩纤维能与聚对苯二甲酸丁二醇酯进行化学键合和机械铆合;所述的机械铆合是指基体材料通过收缩应力包紧粗糙表面的纤维而产生的摩擦结合;优选的,所述的改性剂包括次磷酸盐:强碱:顺丁烯二酸盐按质量比3:2:5 混合而成的混合物。 [0007] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein the modifiers include hypophosphites: alkali: maleate ratio by mass 2-4 : 1-3: 4-6 are mixed mixture; the modifier composition rapid corrosion of the surface of basalt fiber, activated, form a rough surface, a large number of reactive groups and the grafting, the fibers forming the surface of a large number of active sites and a reactive group, such that the basalt fiber can be polyethylene terephthalate, polybutylene terephthalate and chemical bonding and mechanical staking; riveting machine according to the matrix material by means gripping the contraction stress of the roughened surface fibers generated frictional engagement; preferably, the hypophosphite modifiers include: alkali: a mixture obtained by mixing 5: 2: 3 in mass ratio maleate.

[0008] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的次磷酸盐为二甲基次磷酸盐、乙基甲基次磷酸盐、甲基正丙基次磷酸盐、甲烷二甲基次磷酸盐、苯-1,4-二甲基次磷酸盐、甲基苯基次磷酸盐或二苯基次磷酸盐的一种或多种。 [0008] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein said hypophosphite is dimethyl phosphinate, ethyl methyl phosphinate, methyl n-propyl hypophosphite group, one or more hypophosphites dimethyl methane, benzene-1,4-dimethyl hypophosphite, phosphinate or methylphenyl diphenyl phosphate.

[0009] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的强碱为氢氧化钠、氢氧化钾中的一种或两种。 [0009] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein the strong base is sodium hydroxide, potassium hydroxide or both.

[0010] 述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的顺丁烯二酸盐为顺丁烯二酸钠、顺丁烯二酸钾中的一种或两种。 [0010] said one polyethylene terephthalate basalt fiber reinforcing material-specific sizing, wherein said maleate salt is sodium maleate, potassium maleate in a species or both.

[0011] 一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,在改性剂中各组分的共同作用下,具有能快速对玄武岩纤维表面腐蚀形成粗糙表面并在纤维表面接枝大量能与聚对苯二甲酸丁二醇酯化学键接的活性基团的作用,从而使玄武岩纤维在经过该浸润剂的处理后,不仅具有更好的韧性和润滑性,有利于玄武岩纤维的后期加工,还能提高玄武岩纤维与聚对苯二甲酸丁二醇酯进行化学键合和机械铆合的能力,即提高了玄武岩纤维与聚对苯二甲酸丁二醇酯的相容性;本发明浸润剂促进了玄武岩纤维在聚对苯二甲酸丁二醇酯材料增强领域中的广泛应用。 [0011] A polyethylene terephthalate basalt fiber reinforcing material-specific sizing, the modifier in the joint action of each component, the fiber surface having a quickly basalt fiber surface and etched to form a rough surface large effect can be grafted with reactive groups of the poly (butylene terephthalate) chemical bonding, so that the treated basalt fibers after wetting agent, not only has better toughness and lubricity conducive basalt fiber post-processing, but also improve the ability of basalt fiber and poly (butylene terephthalate) chemical bonding and mechanical riveting, i.e. basalt fiber improves the compatibility with the poly (butylene terephthalate); and present sizing invention facilitates the basalt fiber in the widely used polyethylene terephthalate reinforcing material in the art.

[0012] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的成膜剂为聚丙烯酸酯乳液;成膜剂能很好的在玄武岩纤维表面形成膜结构,增加玄武岩纤维韧性,并能提高玄武岩纤维与聚对苯二甲酸丁二醇酯材料的相容性。 [0012] The one polyethylene terephthalate basalt fiber reinforcing material-specific sizing, wherein said film-forming agent is a polyacrylate emulsion; good film formers can be formed in the film structure of the surface of the basalt fiber , increasing the toughness of basalt fiber, the basalt fiber can be improved and compatibility with polyethylene terephthalate material.

[0013] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的偶联剂为含有酯基、烃基、羧基中一种或多种基团的改性硅烷偶联剂;该硅烷偶联剂既能与玄武岩纤维中硅原子偶联,又能与聚对苯二甲酸丁二醇酯材料偶联,偶联效果最好。 [0013] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein the coupling agent containing an ester group, a hydrocarbon group-modified silane, one or more carboxyl groups coupling; both the silane coupling agent and a silicon atom-coupled basalt fiber, but is preferably poly (butylene terephthalate) materials coupling, the coupling effect.

[0014] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的润滑剂为硬脂酸甲酯和硬脂酸锌中的一种。 [0014] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein the lubricant is zinc stearate, and methyl stearate.

[0015] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其中所述的溶剂为乙醇的水溶液;所述乙醇的水溶液中乙醇与水的体积比为1-3:1;优选的,乙醇的水溶液中乙醇与水的体积比为2:1。 [0015] The one polyethylene terephthalate basalt fiber reinforcing material special wetting agent, wherein the solvent is an aqueous ethanol; the volume ratio of the aqueous ethanol is ethanol and water 1-3: 1; preferably, aqueous ethanol in a volume ratio of ethanol to water is 2: 1.

[0016] 优选的,一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,包括以下重量份组分:50份的成膜剂、10份的偶联剂、3份润滑剂、15份的改性剂、40份的溶剂。 [0016] Preferably, a poly (butylene terephthalate) basalt fiber reinforcing material special wetting agents, comprising by weight parts of the following components: 50 parts of a film-forming agent, 10 parts coupling agent, 3 parts of a lubricant , 15 parts of a modifier, 40 parts of a solvent.

[0017] 为了实现上述发明目的,进一步的,本发明提供了一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的制备方法,包括以下步骤: (1) 将改性剂用溶剂溶解形成混合溶液A;将成膜剂用溶剂溶解后加入偶联剂和润滑剂形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0017] In order to achieve the above object, further, the present invention provides a method for preparing poly basalt fibers special wetting agent polybutylene terephthalate reinforcement material, comprising the steps of: (1) with the modifying agent a solvent is dissolved to form a mixed solution; coupling agent and a lubricant to form a mixed solution B after the film former dissolved in a solvent; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C ; (3) the mixed solution obtained in step 2 C defoaming treatment to obtain polyethylene terephthalate basalt fiber reinforcing material-specific sizing.

[0018] 上述一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的制备方法,其中步骤3所述的消泡处理为物理消泡;避免杂质的引入或副反应的发生。 [0018] The method of preparing a poly basalt fibers special wetting agent material reinforced polybutylene terephthalate, defoaming 3 wherein said step of processing physical defoaming; avoid the introduction of impurities or side reaction.

[0019] —种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的制备方法,将改性剂的稀释溶解与成膜剂、偶联剂、润滑剂的混合溶解分开处理,避免改性剂在稀释溶解时放出的大量热导致副反应的产生,且生产条理清晰、简洁;本发明方法简单、可靠,适合聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的大规模、工业化生产。 [0019] - enhancing seed polymerization method of preparing dedicated basalt fiber wetting agent polybutylene terephthalate material dissolved processed separately diluted with dissolution modifying film former coupling agent is mixed, a lubricant, to avoid modifier dissolves upon dilution released a large number of side reactions due to heat generation, and the production of clear, concise; method of the present invention is simple, reliable, and suitable for polyethylene terephthalate basalt fiber reinforcing material of a large specific sizing scale industrial production.

[0020] 与现有技术相比,本发明的有益效果: 1、本发明聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂能快速对玄武岩纤维表面腐蚀,形成粗糙表面,提高了玄武岩纤维与聚对苯二甲酸丁二醇酯材料之间的机械铆合能力。 [0020] Compared with the prior art, the beneficial effects of the present invention are: 1, the present invention is polyethylene terephthalate, polybutylene terephthalate basalt fiber reinforcing material-specific sizing rapid corrosion of the basalt fiber surface, forming a rough surface, improved basalt fiber mechanical riveting poly (butylene terephthalate) capability between materials.

[0021] 2、本发明聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂浸润能快速在纤维表面接枝大量能与聚对苯二甲酸丁二醇酯化学键接的活性基团,提高了玄武岩纤维与聚对苯二甲酸丁二醇酯材料之间的化学键接能力。 [0021] 2, the present invention is polyethylene terephthalate basalt fiber reinforcing material-specific sizing infiltration can rapidly and a large number of graft polymerizable reactive groups butylene terephthalate chemically bonded surface of the fiber, basalt fiber improves the ability to chemically bond with the poly (butylene terephthalate) material between.

[0022] 3、本发明聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂能提高玄武岩纤维与聚对苯二甲酸丁二醇酯材料之间的相容性,促进了玄武岩纤维在聚对苯二甲酸丁二醇酯材料增强领域中的广泛应用。 [0022] 3, the present invention is polyethylene terephthalate, polybutylene terephthalate dedicated basalt fiber reinforcing material to improve wetting agent compatibility between the basalt fiber material polybutylene terephthalate, basalt fibers promoted wide range of applications of polyethylene terephthalate, polybutylene terephthalate reinforcing material.

[0023] 4、本发明聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的制备方法简单、可靠,适合聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的大规模、工业化生产。 [0023] 4, the present invention is prepared basalt fiber reinforced polyethylene specific sizing simple, reliable, polyethylene terephthalate suitable reinforcing material basalt fiber mass dedicated infiltrant material polybutylene terephthalate ,Industrial production.

具体实施方式 detailed description

[0024] 下面结合试验例及具体实施方式对本发明作进一步的详细描述。 [0024] The following examples and binding assay specific embodiments of the present invention will be further described in detail. 但不应将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明内容所实现的技术均属于本发明的范围。 However, this should not be understood that the present invention relating to the above-described range limited to the following examples, all based on the teachings of the present invention are achieved within the scope of the present invention.

[0025] 实施例I (1) 将15重量份含有二甲基次磷酸钠:氢氧化钠:顺丁烯二酸钠按质量比3: 2: 5混合而成的改性剂用10重量份的乙醇和10重量份的水溶解形成混合溶液A;将50重量份的聚丙烯酸酯乳液用10重量份的乙醇和10重量份的水溶解后加入10重量份的硅烷偶联剂和3重量份的硬脂酸甲酯形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0025] Example I (1) comprising 15 parts by weight of dimethyl sodium hypophosphite: 5 modifiers are mixed with 10 parts by weight: sodium hydroxide: sodium maleate mass ratio 3: 2 10 parts by weight of ethanol and water dissolved to form a mixed solution a; 50 parts by weight of the polyacrylate emulsion with 10 parts by weight of ethanol and 10 parts by weight of water were dissolved 10 parts by weight of a silane coupling agent and 3 parts by weight of methyl stearate to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (. 3) step 2 the resulting mixed solution was defoamed handled C polyethylene terephthalate, polybutylene terephthalate basalt fiber reinforcing material-specific sizing.

[0026] 实施例2 (1) 将10重量份含有苯-1,4-二甲基次磷酸钾:氢氧化钾:顺丁烯二酸钾按质量比4:3:6 混合而成的改性剂用5重量份的乙醇和5重量份的水溶解形成混合溶液A;将60重量份的聚丙烯酸酯乳液用20重量份的乙醇和10重量份的水的溶剂溶解后加入15重量份的硅烷偶联剂和1重量份的硬脂酸锌形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0026] Example 2 (1) comprising 10 parts by weight 1,4-dimethyl-benzyl potassium hypophosphite: Potassium hydroxide: potassium maleic mass ratio 4: 3: 6 mixture of the modified agent with 5 parts by weight of ethanol 5 parts by weight of water and dissolved to form a mixed solution as a; 60 parts by weight of a polyacrylate emulsion after 20 parts by weight of ethanol and 10 parts by weight of water were added 15 parts by weight of solvent to dissolve the a silane coupling agent and 1 part by weight of zinc stearate to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (3) obtained in step 2 defoaming treatment to obtain a mixed solution C polyethylene terephthalate basalt fiber reinforcing material-specific sizing.

[0027] 实施例3 (1) 将20重量份含有乙基甲基次磷酸钠:氢氧化钠:顺丁烯二酸钾按质量比2:1:4混合而成的改性剂用10重量份的乙醇和10重量份的水溶解形成混合溶液A;将40重量份的聚丙烯酸酯乳液用20重量份的乙醇和10重量份的水溶解后加入5重量份的硅烷偶联剂和5重量份的硬脂酸甲酯形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0027] Example 3 (1) containing 20 parts by weight of methyl ethyl hypophosphite: sodium hydroxide: potassium maleic mass ratio 2: 1: 4 mixed with 10 wt modifier parts ethanol and 10 parts by weight of water dissolved to form a mixed solution a; silane coupling agent 40 parts by weight of the polyacrylate emulsion with 20 parts by weight of ethanol 10 parts by weight of water and dissolved by adding 5 parts by weight and 5 wt. parts of methyl stearate to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (. 3) step 2 the resulting mixed solution was defoamed C the poly (butylene terephthalate) basalt fiber reinforcing material-specific sizing.

[0028] 对比例1 (1) 将50重量份的聚丙烯酸酯乳液用20重量份的乙醇和20重量份的水溶解后加入10重量份的硅烷偶联剂和3重量份的硬脂酸甲酯形成混合溶液; (2) 将步骤1得到的混合溶液消泡处理得浸润剂。 [0028] Comparative Example 1 (1) adding 10 parts by weight 50 parts by weight of the polyacrylate emulsion with 20 parts by weight of ethanol and 20 parts by weight of a silane coupling agent dissolved in water and 3 parts by weight of methyl stearate ester to form a mixed solution; (2) mixing the solution of step 1 was defoamed handled wetting agent.

[0029] 对比例2 (1) 将15重量份含有二甲基次磷酸钠:氢氧化钠:顺丁烯二酸钠按质量比3:5:5混合而成的改性剂用10重量份的乙醇和10重量份的水溶解形成混合溶液A;将50重量份的聚丙烯酸酯乳液用10重量份的乙醇和10重量份的水溶解后加入10重量份的硅烷偶联剂和3重量份的硬脂酸甲酯形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0029] Comparative Example 2 (1) comprising 15 parts by weight of dimethyl sodium hypophosphite: 5 modifiers are mixed with 10 parts by weight: sodium hydroxide: sodium maleate mass ratio of 3: 5 10 parts by weight of ethanol and water dissolved to form a mixed solution a; 50 parts by weight of the polyacrylate emulsion with 10 parts by weight of ethanol and 10 parts by weight of water were dissolved 10 parts by weight of a silane coupling agent and 3 parts by weight of methyl stearate to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (. 3) step 2 the resulting mixed solution was defoamed handled C polyethylene terephthalate, polybutylene terephthalate basalt fiber reinforcing material-specific sizing.

[0030] 对比例3 (1)将15重量份含有二甲基次磷酸钠:氢氧化钠:顺丁烯二酸钠按质量比5:2:5混合而成的改性剂用10重量份的乙醇和10重量份的水溶解形成混合溶液A;将50重量份的聚丙烯酸酯乳液用10重量份的乙醇和10重量份的水溶解后加入10重量份的硅烷偶联剂和3重量份的硬脂酸甲酯形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 [0030] Comparative Example 3 (1) comprising 15 parts by weight of dimethyl sodium: sodium hydroxide: sodium maleate mass ratio of 5: 2: 5 are mixed with 10 parts by weight of modifier 10 parts by weight of ethanol and water dissolved to form a mixed solution a; 50 parts by weight of the polyacrylate emulsion with 10 parts by weight of ethanol and 10 parts by weight of water were dissolved 10 parts by weight of a silane coupling agent and 3 parts by weight of methyl stearate to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (. 3) step 2 the resulting mixed solution was defoamed handled C polyethylene terephthalate, polybutylene terephthalate basalt fiber reinforcing material-specific sizing.

[0031] 将上述实施例卜3和对比例1-3中所制备得到的浸润剂分别用于浸润同种玄武岩纤维,将得到的玄武岩纤维进行性能测试和聚对苯二甲酸丁二醇酯塑料(拉伸强度78MPa, 缺口冲击强度60J/m,热变形温度58°C)增强(玄武岩纤维用量为聚对苯二甲酸丁二醇酯质量的30%)实验,记录实验结果,记录数据如下: [0031] The embodiment described above and Bu 3 prepared in Comparative Example 1-3 were obtained infiltrant for infiltrating isotype basalt fiber, the resultant basalt fiber and performance testing of polybutylene terephthalate plastic (78MPa tensile strength, notched impact strength of 60J / m, the heat distortion temperature 58 ° C) reinforcing (basalt fiber in an amount of 30% polyethylene terephthalate by mass) of the experiment, the experimental results recorded data is recorded as follows:

Figure CN106751560AD00071

对上述实验数据分析可知,实施例1-3中采用本发明技术方案得到浸润剂对玄武岩纤维进行浸润处理,得到的玄武岩纤维拉申强度和断裂伸长率好,与聚对苯二甲酸丁二醇酯相容性好,对聚对苯二甲酸丁二醇酯塑料增强效果显著;而对比例1中浸润剂没有添加改性剂,即为常规浸润剂,用该浸润剂处理后的玄武岩纤维为常规玄武岩纤维,该玄武岩纤维与聚对苯二甲酸丁二醇酯材料之间的相容性差,对聚对苯二甲酸丁二醇酯材料增强作用显著减弱;对比例2中没有采用本发明中所保护的改性剂组分配比用量,氢氧化钠用量过大,浸润剂对玄武岩纤维表面侵蚀过渡,对玄武岩纤维结构造成破坏,导致玄武岩纤维的拉伸强度和断裂伸长率显著降低,从而对聚对苯二甲酸丁二醇酯纤维的增强作用也显著下降;对比例3中没有采用本发明中所保护的改性剂组分配比用 Analyzing the data from the above experiment, Examples 1-3 of the present invention obtained using the techniques of the infiltrant for infiltrating process basalt fiber, basalt fiber to obtain good tensile strength and elongation application, and polybutylene terephthalate good compatibility alcohol esters, poly (butylene terephthalate) plastic reinforcement effect is remarkable; Comparative Example 1 while wetting agent is not added modifiers, i.e. conventional wetting agents, the treated basalt fibers with the sizing conventional basalt fiber, the basalt fiber and compatibility between polyethylene terephthalate material difference, poly (butylene terephthalate) materials enhancement was significantly reduced; not used in Comparative Example 2 of the present invention modifier group protected distribution ratio of the amount of sodium hydroxide used is too large, the erosion infiltrant transition basalt fiber surface, damage to the basalt fiber structure, resulting in tensile strength and elongation at break is significantly lower basalt fiber, poly thereby enhancing effect was also significantly decreased the polybutylene terephthalate fibers; Comparative Example 3 does not use the modifier group assignment in the present invention than with the protected 量,二甲基次磷酸钠用量过大,浸润剂对玄武岩纤维表面活化作用减弱,玄武岩纤维表面接枝的活性基团少,与聚对苯二甲酸丁二醇酯材料的化学键合能力差,对聚对苯二甲酸丁二醇酯材料增强作用显著减弱。 The amount of sodium hypophosphite with excessive dimethyl, wetting agents basalt fiber surface activating effect of weakening, basalt fiber surface graft less active group, the chemical bond with the poly (butylene terephthalate) material is poor, poly (butylene terephthalate) materials enhancement significantly reduced.

Claims (10)

  1. 1. 一种聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂,其特征在于,包括以下重量份组分:40-60份的成膜剂、5-15份的偶联剂、1-5份润滑剂、10-20份的改性剂、30-50 份的溶剂;所述改性剂包括质量比为2-4:1-3:4-6的次磷酸盐,强碱,顺丁烯二酸盐。 A polyethylene terephthalate basalt fiber reinforcing material special wetting agent, characterized in that it comprises by weight parts of the following components: 40-60 parts of a film-forming agent, 5-15 parts of coupling agent, 1-5 parts lubricant, 10-20 parts of a modifying agent, 30-50 parts of a solvent; the modifier comprises a mass ratio of 2-4: 1-3: 4-6 hypophosphite, alkali , maleate.
  2. 2. 根据权利要求1所述的浸润剂,其特征在于,所述改性剂包括质量比为3:2:5的次磷酸盐、强碱、顺丁烯二酸盐。 The wetting agent according to claim 1, wherein the modifier comprises a mass ratio of 3: hypophosphites, alkali, maleate of 5: 2.
  3. 3. 根据权利要求1所述的浸润剂,其特征在于,包括以下重量份组分:50份的成膜剂、10 份的偶联剂、3份润滑剂、15份的改性剂、40份的溶剂。 Wetting agent according to claim 1, characterized in that the parts comprising the following components by weight: 50 parts of a film-forming agent, 10 parts coupling agent, 3 parts of a lubricant, 15 parts modifier, 40 parts of a solvent.
  4. 4. 根据权利要求1所述的浸润剂,其特征在于,所述次磷酸盐为二甲基次磷酸盐、乙基甲基次磷酸盐、甲基正丙基次磷酸盐、甲烷二甲基次磷酸盐、苯-1,4-二甲基次磷酸盐、甲基苯基次磷酸盐或二苯基次磷酸盐的一种或多种。 Wetting agent according to claim 1, wherein said hypophosphite is dimethyl phosphinate, ethyl methyl phosphinate, methyl-n-propyl phosphate, dimethyl methane hypophosphites, one or more benzene-1,4-dimethyl hypophosphite, phosphinate or methylphenyl diphenyl phosphate.
  5. 5. 根据权利要求1所述的浸润剂,其特征在于,所述强碱为氢氧化钠、氢氧化钾中的一种或两种。 Wetting agent according to claim 1, wherein the strong base is sodium hydroxide, potassium hydroxide or both.
  6. 6. 根据权利要求1所述的浸润剂,其特征在于,所述成膜剂为聚丙烯酸酯乳液。 The wetting agent according to claim 1, wherein said film-forming agent is a polyacrylate emulsion.
  7. 7. 根据权利要求1所述的浸润剂,其特征在于,所述偶联剂为含有酯基、烃基、羧基中一种或多种基团的改性硅烷偶联剂。 The wetting agent according to claim 1, wherein said coupling agent is an ester group, a hydrocarbon group, a carboxyl group-modified silane coupling agent is one or more groups containing.
  8. 8. 根据权利要求1所述的浸润剂,其特征在于,所述润滑剂为硬脂酸甲酯和硬脂酸锌中的一种。 Wetting agent according to claim 1, wherein the lubricant is zinc stearate, and methyl stearate.
  9. 9. 根据权利要求1所述的浸润剂,其特征在于,所述溶剂为乙醇的水溶液。 Wetting agent according to claim 1, wherein said aqueous solvent is ethanol.
  10. 10. —种权利要求1所述聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂的制备方法,其特征在于,包括以下步骤: (1) 将改性剂用溶剂溶解形成混合溶液A;将成膜剂用溶剂溶解后加入偶联剂和润滑剂形成混合溶液B; (2) 将步骤1得到的混合溶液A加入到混合溶液B中混合均匀形成混合溶液C; (3) 将步骤2得到的混合溶液C消泡处理得聚对苯二甲酸丁二醇酯材料增强玄武岩纤维专用浸润剂。 10. - kind of claim 1 polyethylene terephthalate, polybutylene terephthalate material prepared basalt fiber reinforcement sizing dedicated, characterized by comprising the steps of: (1) dissolving the modifying agent with a solvent to form a mixed solution of a; the solvent for dissolving the film former coupling agent and a lubricant to form a mixed solution B; (2) obtained in step 1 a mixed solution was added to the mixed solution B are mixed uniformly to form a mixed solution C; (3) the step C 2 resulting mixed solution was defoamed handled polyethylene terephthalate basalt fiber reinforcing material-specific sizing.
CN 201611072796 2016-11-29 2016-11-29 Polybutylene terephthalate material-reinforced basalt fiber special-purpose infiltrating agent and preparation method thereof CN106751560A (en)

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* Cited by examiner, † Cited by third party
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JPS6335440A (en) * 1986-07-31 1988-02-16 Dainippon Ink & Chem Inc Agent for treating glass fiber
CN1143943A (en) * 1994-03-14 1997-02-26 Ppg工业公司 Glass fibre sizing and sized glass fibers and polyolefin reinforcing articles
JP2002339246A (en) * 2000-03-07 2002-11-27 Sanyo Chem Ind Ltd Bundling agent for inorganic fiber
US20020051888A1 (en) * 2000-09-08 2002-05-02 Shobha Murari Finish for glass fabrics used for reinforcing epoxy structures
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