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Alternative TitleConversion and Products (Sodium Percarbonate and Magnesium Borate Whisker) Development of Boron Resources
Thesis Advisor张懿  ;  李平
Degree Grantor中国科学院研究生院
Degree Discipline化学工艺
Keyword低品位硼镁矿   亚熔盐   偏硼酸钠   过硼酸钠   硼酸镁晶须
Abstract依托亚熔盐平台技术,以我国硼矿藏中占总储量58 %的硼铁矿浮选后的低品位硼镁矿为切入点,基于低品位硼镁矿B2O3含量低、Mg/B比高的特点,在引入亚熔盐体系,发挥其处理低品位难处理矿优势的基础之上,走特色产品路线,与后续硼化工主要产品之一过硼酸钠(NaBO3·4H2O)的制备和高新材料硼酸镁(Mg2B2O5)晶须的制备相结合,实现低品位硼镁矿高效清洁转化和硼产品工程化。 本论文在以下几个方面取得了进展: (1)采用钠系亚熔盐介质(高浓度NaOH溶液体系)处理低品位硼镁矿产生的偏硼酸钠(NaBO2)为原料,直接与H2O2反应,一步法制备出NaBO3·4H2O,系统研究了原料配比、反应时间、反应温度、液固比等对NaBO3·4H2O产品性能的影响,确定了最优制备工艺条件。在此基础上,针对新一代高性能NaBO3·4H2O在产品性能方面的需求(砂状、堆积密度大、氧稳定性高),解决的关键是增大产品粒度和降低产品放氧;因此通过加入添加剂控制NaBO3晶面生长方向,调控其生长成具有一定形貌的小颗粒,再引入大分子控制临界胶束浓度促使小颗粒聚集成大颗粒,大颗粒通过包覆后抑制其放氧,从而制备高性能NaBO3·4H2O。 (2)以NaBO3·4H2O制备小试试验为基础,开展了由NaBO2制备NaBO3·4H2O的2~5 L反应器扩大试验,以研究原材料、溶液循环、杂质等对NaBO2与H2O2反应合成NaBO3·4H2O产品的影响。实验系统考察了溶液循环次数、杂质、原材料等因素对NaBO3·4H2O制备的影响,确定了扩大试验优化制备工艺。 (3)以硼砂(Na2B4O7?10H2O)和MgCl2?6H2O为原料,利用高温-助熔剂-湿法工艺合成了高品质的Mg2B2O5晶须产品,系统研究了助熔剂的选择、硼镁物质的量比、助熔剂添加量、煅烧温度及煅烧时间对晶须品质的影响,并对Mg2B2O5晶须的生长机理进行了研究。
Other AbstractBased on the platform of sub-molten salt technology, low grade ascharite ore obtained after flotation of paigeite which possess 58 % of the total boron mineral deposits in our country, which has the characteristics of low content of B2O3 and high mass ratio of Mg/B, was dealed with sub-molten salt system to obtain sodium metaborate (NaBO2). The NaBO2 reacted with H2O2 to produce NaBO3?4H2O as one of the main product in the boron chemical process. Combined with the preparation of momentive magnesium borate with high value, realized the effective clean conversion of low grade ascharite ore and industrialization of boron products. This paper made progressive results in the following respects: (1) Sodium sub-molten salt medium (high concentration of NaOH solution system) was adopted to directly handle low grade ascharite ore to get NaBO2 as the raw material which then reacted with H2O2 to make NaBO3·4H2O. The influence of raw material, reaction time, reaction temperature and solid-liquid ratio on the performance of NaBO3·4H2O was systematically studied and the optimal preparation process conditions were determined. On this basis, annexing agent was added to control crystal growth direction, macromolecular was introduced to control critical micelle concentration to prompt small particles gathered into larger particles, and the larger particles could inhibit oxygen evolving after coated then got high performance NaBO3·4H2O due to the requirements of the high performance NaBO3·4H2O product (sandy shape, high bulk density and high oxygen stability). (2) Pilot test in preparing NaBO3·4H2O by NaBO2 was conducted on the basis of bench-scale test on preparing NaBO3·4H2O. Experimental apparatus was expanded from 0.2 L to 2~5 L. The object was to discover the influence of raw materials, solution cycles and impurities on the synthesis reaction of NaBO2 and H2O2 to make NaBO3·4H2O product, which could further provide technological base for realizing industrialized production of sodium perborate. In the pilot test, the influence of solution cycle times, impurities and raw materials on the NaBO3·4H2O product synthesis were observed, and the optimum preparation conditions for pilot test were determined. (3) Na2B4O7?10H2O and MgCl2?6H2O were taken as raw material to synthesize magnesium borate whisker product with high quality based on high temperature-flux-wet process. The influence of the selection of flux, the molar ratio of boron and magnesium, flux content, calcination temperature and calcination time on the quality of whisker were systematically studied, and the growth mechanism of magnesium borate whisker was discussed.
Document Type学位论文
Recommended Citation
GB/T 7714
张文静. 硼资源转化及其产品(过硼酸钠和硼酸镁晶须)开发[D]. 中国科学院研究生院,2014.
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