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  • Synthesis and application of high temperature resistant boron modified phenolic resin

    Synthesis and application of high temperature resistant boron modified phenolic resin

    Using sodium carbonate as catalyst, the first use of phenol and formaldehyde inwater solution synthesis salicyl alcohol, salicyl alcohol further and boric acidreaction of boron modified PF (phenolic resin); then as indexes to the carbon residue rate, discusses the types of catalyst, phenol, phenol aldehyde thanboron ratio and synthesis of salicyl alcohol reaction time the influence on theproperties of PF modified boron by single factor experiments, and the optimumtechnological conditions of the preparation of boron modified PF. The research results show that: when the reaction time of synthesis salicyl alcohol for 2.0h, n(phenol): n (formaldehyde): n (boric acid): =1 (1.7~2.0): 0.3 and using sodium carbonate as catalyst, 800 C carbon residue of boron modified PF rate (65.88%)relative to the highest, the combination of SiC material made of special shaped Si3N4 and ramming material has good application performance.

    Wang Dongmei, Zhang Yanchang, Yin yuan, Cao Jinli, Li Tianxian, Zhao Xianzeng (Key Laboratory of Henan Province, Henan fine chemical industry,Zhengzhou 450002)

    Keywords: phenolic resin; boric acid; high temperature; modification; heat resistance

    CLC number: TQ323.1 document code: A article number: 1004-2849 (2014) 01-0022-05

    0 foreword

    Widely application of high temperature resistant resin in refractories, abrasives,superhard materials, friction materials, aerospace materials, insulation material and insulation materials and other fields, and the development of these fieldscannot do without high performance of high temperature resistant resin. With the continuous progress of the technology, the traditional high temperature resistant resin has been unable to meet the special requirements in the field of [1-2]. PF(phenolic resin) molecular chain contains a large number of benzene ring, hasstable performance and high mechanical strength advantages, but there are stillgreat brittleness, high water absorption and shrinkage defect rate etc..Therefore, the PF is modified using a variety of techniques to improve theperformance of the strengthened, or some of its aspects, has become one of the important topics in the research field of [3-8].

    Method for improving the heat resistance of PF are mainly alkyl phenol andphenyl phenol modified, rare elements (such as molybdenum, tungsten andorganic boron modified), silicone modified, and other heteroatom containingpolymer materials such as EP (epoxy resin), polyamide and polyimide]copolymerization or blending modification etc.. In the modification, organic boronmodification is one of the most economical method. Therefore, in this study,using sodium carbonate as catalyst, the first use of phenol and formaldehyde inwater solution synthesis salicyl alcohol, salicyl alcohol further and synthesis of boron modified PF boric acid reaction. Through discussing the types of catalyst,phenol, phenol aldehyde than boron ratio and synthesis of saligenol reaction time effects on the performance of the modified resin, preferably a preparationusing the optimum process conditions to meet the requirements of the modified resin, provide effective reference after the sequence of research in this field in order to.

    1 - test part

    1.1 test materials

    Phenol, industrial grade, Beijing Yanshan Petroleum Chemical Industry Group Co., Ltd.; formaldehyde, industrial grade, Wu Shexian County Huayu Oil Co. Ltd;boric acid, analysis of pure, Xi'an Chemical reagent; anhydrous sodium carbonate, hydrochloric acid (HCl), analysis of pure, Luoyang Chemical ReagentFactory; sodium hydroxide (NaOH), analysis of pure, Henan Rui equipment company; calcium hydroxide, analysis of pure, Shanghai Chemical ReagentFactory; barium hydroxide, analysis of pure, Beijing Red Star Chemical Factory;high aluminum material, corundum, silicon carbide (SiC), silicon nitride (Si3N4),asphalt, graphite, industrial grade, commercially available.

    1.2 test instrument

    FTIR-6700 infrared spectrometer, USA company Nicolet; measuring instrument type STA499C heat resistance, the German company Netzsch; softening pointmeasuring instrument type SYD-2806E asphalt, Sino German Albert Instrument Co., Ltd.; electric air blowing drying box, Shanghai Yiheng Scientific Instrument Co. Ltd.; KFTi-Touch sprite generation integrated Carle Fischer titration,metrohm Ltd; TYE-600B pressure testing machine, Wuxi built instrument and Machinery Co Ltd; S116 type sand mixing machine, Shanghai heavy machinefactory foundry.

    1.3 test preparation

    Boron modified [3] 1.3.1 synthesis of high temperature resistant PF

    With an electric mixer in 500mL four neck flask, adding measurement offormaldehyde, phenol and sodium carbonate, oil bath is heated to 70~75 DEG C,the reaction of 2H; and then adding measurement of boric acid, heating to 100~104 Deg. C, return 3H; cooling to 80 DEG C, vacuum dehydration to the required viscosity discharge can be.

    1.3.2 uses a boron modified PF for preparing special Si3N4 combined with SiCmaterials

    To aggregate (Si3N4, SiC) added 3%~8% of boron modified PF (for use as adhesives), grinding and mixing by isostatic pressing technology for preparation of the final product.

    1.3.3 uses a boron modified PF prepared iron runner ramming material

    Ramming material (mainly for trough of blast furnace ironmaking plant) issubjected to a high temperature of over 1500 degrees and molten iron scouringand erosion, subjected to blast furnace slag, so the use of harsh conditions; in addition, ramming material performance directly affects the quality of blast furnace production. Therefore, ramming material used in the main raw materialwith high aluminum material, corundum, SiC, asphalt and graphite etc.. In this study 2% boron modified PF and X% PF as the common thermosetting adhesive(X is a variable), the preparation of (X+2)% thermosetting PF (relative to the totalmaterial quality). First of all, sequentially adding aggregate, adhesive and powderto sand mixing machine, hybrid 10min; to be above the material mixed evenly,weighing and bagging.

    The 1.4 test or characterization

    (1) the carbon residue rate: join the 2~3g sample in 30mL crucible of constant weight, and placed in the oven, drying at 210 deg.c for 2h, in the dryer after cooling to room temperature and 800 DEG C weighing; heat treatment of 7min, in the drying chamber is cooled to room temperature after weighing; finallyaccording to type



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