WO2020207242A1 - 一种有机分子诱导制备高纯球形速溶硼酸的方法 - Google Patents

一种有机分子诱导制备高纯球形速溶硼酸的方法 Download PDF

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WO2020207242A1
WO2020207242A1 PCT/CN2020/080988 CN2020080988W WO2020207242A1 WO 2020207242 A1 WO2020207242 A1 WO 2020207242A1 CN 2020080988 W CN2020080988 W CN 2020080988W WO 2020207242 A1 WO2020207242 A1 WO 2020207242A1
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boric acid
temperature
purity
range
instant
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宁桂玲
朱培函
庞洪昌
田朋
叶俊伟
程君
林�源
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Dalian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10—Compounds containing boron and oxygen
    • C01B35/1045—Oxyacids
    • C01B35/1054—Orthoboric acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres

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  • the invention belongs to the technical field of inorganic functional material preparation, and particularly relates to a preparation method of high-purity spherical instant boric acid.
  • Boric acid has been widely used in many fields such as industry, agriculture, medicine, new energy, aerospace and optoelectronic materials due to its unique physical and chemical properties. Because the crystalline morphology of traditional boric acid is usually lamellar, its dissolution rate in water is slow, resulting in a series of problems that affect efficiency and affect operation quality when used in some special occasions such as nuclear power plants. At present, there are very few published literature reports on increasing the dissolution rate of boric acid or the preparation of instant boric acid. The methods commonly used in industry include increasing the dissolution temperature or stirring rate, grinding to form smaller crystal sizes, etc., and these methods are used in some special occasions or fields. Applications are often limited, such as in the fields of biomedicine, instant fertilizers and nuclear power. Some of them have special requirements for temperature, purity or dissolution equipment, which requires instant boric acid. Moreover, the potential demand for high-purity instant boric acid is also increasing, so the development of instant boric acid has important application value.
  • the present invention provides a method for preparing high-purity spherical instant boric acid by using organic molecules to induce crystallization.
  • This method uses high-purity boric acid as the raw material, and the specific purity is determined according to actual needs. It uses lower alcohols, ketones, ethers or acid and water mixtures with carbon less than 4 (ie less than C4) as solvents, and uses the principle of solubility and surface free energy control , Through the method of organic molecule inducing crystallization to adjust the boric acid crystal exposed crystal surface and aggregate particle morphology, and then obtain the spherical instant boric acid product with multi-stage aggregate structure and high active crystal surface exposed.
  • the purpose of the present invention is to provide a method for preparing high-purity spherical instant boric acid on a large scale and at low cost.
  • the method is induced by alcohol and other organic molecules by changing the boric acid concentration in the boric acid solution and the temperature gradient during the cooling crystallization process.
  • An instant spherical boric acid with controllable multi-level aggregate structure and aggregate particle size is obtained. This method solves the problems of easy agglomeration and slow dissolution rate of ordinary flaky boric acid in the past.
  • the technical scheme of the present invention is based on high-purity boric acid as a raw material, and a mixture of lower alcohols, ketones, ethers or acids with water below C4 as the solvent.
  • the mixture can also contain alcohols, ketones, ethers and acids below C4. Two or more. Dissolve boric acid in a hot mixed solution solvent to make it close to saturation, and then control the temperature of the boric acid solution to achieve supersaturation.
  • composition and concentration changes of alcohol and other organic molecules in the solution to expose the surface energy and crystallization of the boric acid saturated solution
  • the surface is adjusted to make the precipitated boric acid crystals form spherical microcrystalline aggregates; the aggregates exhibit porosity, crystalline disorder, and modulability of the exposed crystal surface, thereby increasing the dissolution rate; and after filtering at room temperature, After drying, spherical boric acid without agglomeration is obtained.
  • the method for preparing instant spherical boric acid by induction of organic molecules is characterized by the preparation process, the formulation design of the organic solvent and water content used in the preparation, the selection of the cooling interval, and the control of the cooling rate, which are specifically as follows:
  • Step 1 Add boric acid to a pressure vessel filled with mixed solvents, heat the pressure vessel to a set temperature to completely dissolve the boric acid, stir moderately during this period to speed up the dissolution;
  • the boric acid is high-purity boric acid, and its purity is analytical purity or nuclear power grade purity, which is determined according to application requirements.
  • the setting temperature range is between 40 ⁇ 300°C.
  • the amount of boric acid added is determined according to the solubility of boric acid in the mixed solvent at the set temperature, and the added boric acid is just completely dissolved at the set temperature.
  • the mixed solvent is a mixed liquid of an organic solvent and water, the mass ratio of the two is 0.5-20:80-99.5, and the organic solvent is a mixture of one or more of lower alcohols, ketones, ethers or acids below C4.
  • Step 2 The boric acid solution obtained in step 1 is lowered to room temperature at a cooling rate of 0.2-20°C/min, and the standing time is controlled within the range of 0.2-10 hours to make the precipitated boric acid aggregate complete and stable;
  • Step 3 The suspension slurry obtained in step 2 is filtered and dried at room temperature to obtain a high-purity spherical instant boric acid product;
  • the drying temperature in step 3 above is controlled within the range of 20 ⁇ 110°C.
  • Step 4 The mother liquor after the boric acid is separated continues to be recycled as the dissolving liquid.
  • the beneficial effects of the present invention using the inducing effect of organic molecules such as alcohols, ketones, ethers, acids, etc. on boric acid, by changing the composition of the boric acid solution and regulating the cooling rate of the dissolution-recrystallization process, the spherical instant boric acid can be conveniently obtained. No other additives or special equipment are needed, the preparation process is simple, the material liquid is recycled and used without emissions, and it can be produced on a large scale. The production rate is high and the cost is low.
  • the invention provides a new way for low-cost preparation of instant boric acid, exhibits a competitive advantage in environmental friendliness, etc., and is expected to be used in nuclear power plants or other instant boric acid product fields.
  • Figure 1(a) is an SEM photograph of the boric acid obtained in Example 1 at 20 ⁇ m.
  • Figure 1(b) is an SEM photograph of the boric acid obtained in Example 1 at 20 ⁇ m.
  • Example 2 is the XRD pattern of the boric acid powder prepared in Example 1.
  • Figure 3(a) is an SEM photograph of the boric acid obtained in Example 2 at 50 ⁇ m.
  • Figure 3(b) is an SEM photograph of the boric acid obtained in Example 2 at 5 ⁇ m.
  • the mixed solvent used is a mixture of ethanol and water.
  • the mixed solvent used is a mixed liquid of acetone and water
  • the cooling rate is about 20°C/min
  • the mixed solvent used is a mixed liquid of ether and water
  • the cooling rate is about 0.2°C/min
  • the obtained boric acid powder is spherical and rich in a large number of pore structures; take 3.0 g of the obtained spherical boric acid powder and add it to a beaker containing 97 g of deionized water, magnetic stirring speed 400 rpm, complete dissolution within 60 seconds.
  • the mixed solvent used is a mixed liquid of oxalic acid and water
  • the cooling rate is about 0.2°C/min
  • the mixed solvent used is a mixed liquid of acetone and water
  • the cooling rate is about 20°C/min

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明属于无机功能材料制备技术领域，提供了一种有机分子诱导制备高纯球形速溶硼酸的方法。以分析纯硼酸或工业硼酸为原料，以含碳小于4的低级醇、酮、醚或酸与水混合液为溶剂。将硼酸溶于热的溶剂中，基于溶解度和表面自由能调控原理，再将硼酸溶液降温，利用有机分子诱导结晶的方法调变硼酸结晶裸露晶面和聚集颗粒形貌，使过饱和溶液析出重结晶的硼酸微球。经抽滤、干燥，即可获得无团聚的高纯球形硼酸。通过该法所得速溶球形硼酸粉体操作过程简单，工艺条件易于控制，无需消耗表面活性剂或助剂，物料利用率高，产品纯度高。该法解决了以往普通硼酸溶解速度慢、易结块等问题。

Description

一种有机分子诱导制备高纯球形速溶硼酸的方法 技术领域
本发明属于无机功能材料制备技术领域，特别涉及到一种高纯球形速溶硼酸的制备方法。
 背景技术
硼酸因其独特的物化性质，在工业、农业、医药、新能源、航空航天和光电材料等诸多领域得到广泛应用。由于传统硼酸结晶形貌通常为片层状，其在水中溶解速度缓慢，导致在核电站等一些特殊场合应用时影响效率和影响运行质量等一系列问题。当前关于提高硼酸溶解速度或有关速溶硼酸制备的公开文献报道极少，工业上普遍采用的方法有提高溶解温度或搅拌速率、研磨形成较小结晶尺寸等，而这些方法在一些特殊场合或领域的应用常常受限，如在生物医药、速溶肥料和核电领域等，它们有的对温度、有的纯度或溶解设备等有特殊要求，从而需要速溶性硼酸。而且高纯速溶硼酸的潜在需求也在不断增长，因此速溶硼酸的研制具有重要应用价值。
本发明提出一种利用有机分子诱导结晶制备高纯球形速溶硼酸的方法。该法以高纯硼酸为原料，具体纯度根据实际需求确定，以含碳小于4（即C4以下）的低级醇、酮、醚或酸与水混合液为溶剂，利用溶解度和表面自由能调控原理，通过有机分子诱导结晶的方法调变硼酸结晶裸露晶面和聚集颗粒形貌，进而获得具有多级聚集结构、高活性晶面裸露的球形速溶硼酸产品。制备过程中不引进任何有害杂质，速溶硼酸纯度由原料硼酸纯度决定。制备过程简单，工艺条件易控制，成本低，物料利用率高，具有显著的工业化应用前景。
 技术问题
本发明的目的是提供一种可规模化低成本制备高纯球形速溶硼酸的方法，该法在醇等有机分子诱导下，通过改变硼酸溶解液中硼酸浓度和降温结晶过程中温度梯度，即可获得多级聚集结构和聚集颗粒尺寸可控的速溶球形硼酸。该法解决了以往普通片状硼酸易结块、溶解速度慢等问题。
 技术解决方案
本发明的技术方案是以高纯硼酸为原料，以C4以下的低级醇、酮、醚或酸与水的混合液为溶剂，混合液中可以同时含有C4以下醇、酮、醚及酸中的两种或两种以上。将硼酸溶于热的混合液溶剂中使其接近饱和，再将该硼酸溶液进行控制降温使达到过饱和，利用溶液中醇等有机分子的组成和浓度变化对硼酸饱和液表面能和析晶裸露面进行调控，使析出的硼酸结晶形成球形微晶聚集体；该聚集体表现出多孔性、结晶无序性和裸露晶面调变性，进而使溶解速度得到提高；再在室温下经抽滤、干燥即得到无团聚的球形硼酸。这种有机分子诱导制备速溶球形硼酸的方法，其特征在于制备工艺过程、制备中所用有机溶剂及含水量的配方设计、降温区间选择、降温速率控制，具体如下：
一种有机分子诱导制备高纯球形速溶硼酸的方法，其步骤如下：
步骤1：将硼酸加入装有混合溶剂的压力容器中，将压力容器加热至设定温度使硼酸完全溶解，期间适度搅拌，以加快溶解速度；
所述的硼酸为高纯硼酸，其纯度是分析纯或核电级纯度，根据应用要求确定。
设定温度的范围在40~300℃之间。
硼酸加入量根据设定温度下硼酸在混合溶剂中溶解度大小确定，以设定温度下刚好使加入的硼酸完全溶解。
混合溶剂为有机溶剂与水的混合液，二者的质量比为0.5~20：80~99.5，有机溶剂为在C4以下的低级醇、酮、醚或酸中的一种或两种以上混合。
步骤2：将步骤1得到的硼酸溶解液，按照降温速率0.2~20℃/分钟降至室温，并放置时间控制在0.2~10小时范围使析出的硼酸聚集趋于完全和稳定；
步骤3：将步骤2所得悬浊液浆料，在室温条件下经过滤、干燥，即获得高纯球形速溶硼酸产品；
上述步骤3中所述干燥温度控制在20~110℃范围内。
步骤4：将分离出硼酸后的母液继续作为溶解液循环使用。
 有益效果
本发明的有益效果：利用醇、酮、醚、酸等有机分子对硼酸的诱导效应，通过改变硼酸溶解液组成和调控其溶解-再结晶过程的降温速率可以方便地获得球形速溶硼酸，整个过程无需其它助剂或特殊设备，制备过程简单，料液循环利用无排放，可规模化生产，产率高，成本低，制备过程不引进有害杂质，产品流动性好无结块。本发明为低成本制备速溶硼酸提供了新途径，在环境友好等方面展现出竞争优势，有望用于核电站或其它速溶硼酸产品领域。
 附图说明
图1（a）是20μm下，实施例1所得硼酸的SEM照片。
图1（b）是20μm下，实施例1所得硼酸的SEM照片。
图2是实施例1所制备硼酸粉体的XRD图谱。
图3（a）是50μm下，实施例2所得硼酸的SEM照片。
图3（b）是5μm下，实施例2所得硼酸的SEM照片。
 本发明的实施方式
以下结合附图和技术方案，进一步说明本发明的具体实施方式。
实施例 1
将20 g分析纯硼酸加入装有100 g混合溶剂的压力容器中，其中混合溶剂由乙醇、丙酮和水按上述配方比例配制；加热压力容器使温度达到约140℃得到澄清溶液；再控制降温速率约5℃/分钟，使容器温度降至室温，并在室温下放置约0.5小时，此时溶液中析出大量白色沉淀；将该沉淀进行抽滤，60℃干燥，即可获得疏松的球形多孔硼酸粉体，其形貌如图1所示。所得粉体的X射线衍射图见图2，经分析符合标准卡片JCPDS No. 30-0199；取3.0 g所得球形硼酸，加入装有97 g去离子水的烧杯中，磁力搅拌速度400 rpm, 60秒内即可完全溶解。
所用的混合溶剂为乙醇与水的混合液。
实施例 2
与实施例1的区别条件：（1）所用的混合溶剂为丙酮与水的混合液；
（2）压力容器的温度为300℃；
（3）降温速率约20℃/分钟；
（4）干燥温度为80℃。
实施例 3
与实施例1的区别条件：（1）所用的混合溶剂为乙醚与水的混合液；
（2）压力容器的温度为40℃；
（3）降温速率约0.2℃/分钟；
（4）干燥温度为110℃。
实施例 4
将20 g核电级硼酸加入装有100 g 混合溶剂的压力容器中，其中混合溶剂由冰醋酸、异丙醇和水按上述配方比例配制；加热压力容器使温度达到约120℃得到澄清溶液；再控制降温速率约4℃/分钟，使容器温度降至室温，并在室温下放置约1小时，得到有大量白色沉淀的混合浆料；再将该料浆进行抽滤、干燥，即可得到疏松的硼酸粉体，形貌如图3所示，所得硼酸粉体为球形，而且富含大量孔道结构；取3.0 g所得球形硼酸粉体，加入装有97 g去离子水的烧杯中，磁力搅拌速度400 rpm，60秒以内即完全溶解。
实施例 5
与实施例4的区别条件：（1）所用的混合溶剂为乙二酸与水的混合液；
（2）压力容器的温度为40℃；
（3）降温速率约0.2℃/分钟；
（4）干燥温度为110℃。
实施例 6
与实施例4的区别条件：（1）所用的混合溶剂为丙酮与水的混合液；
（2）压力容器的温度为300℃；
（3）降温速率约20℃/分钟；
（4）干燥温度为80℃。

Claims (8)

  1. 一种有机分子诱导制备高纯球形速溶硼酸的方法，其特征在于，步骤如下：
    步骤1：将硼酸加入装有混合溶剂的压力容器中，将压力容器加热至设定温度使硼酸完全溶解，期间适度搅拌，以加快溶解速度；
    设定温度的范围在40~300℃之间；
    混合溶剂为有机溶剂与水的混合液，二者的质量比为0.5~20：80~99.5，有机溶剂为在C4以下的低级醇、酮、醚或酸中的一种或两种以上混合；
    步骤2：将步骤1得到的硼酸溶解液，降至室温，并放置使析出的硼酸聚集趋于完全和稳定；
    步骤3：将步骤2所得悬浊液浆料，在室温条件下经过滤、干燥，即获得高纯球形速溶硼酸产品；
    步骤4：将分离出硼酸后的母液继续作为溶解液循环使用。
  2. 根据权利要求1所述的方法，其特征在于，所述的硼酸为高纯硼酸，其纯度是分析纯或核电级纯度，根据应用要求确定。
  3. 根据权利要求1或2所述的方法，其特征在于，步骤1中，硼酸加入量根据设定温度下硼酸在混合溶剂中溶解度大小确定，以设定温度下刚好使加入的硼酸完全溶解。
  4. 根据权利要求1或2所述的方法，其特征在于，步骤2中，按照降温速率0.2~20℃/分钟降至室温，并放置时间控制在0.2~10小时范围使析出的硼酸聚集趋于完全和稳定。
  5. 根据权利要求3所述的方法，其特征在于，步骤2中，按照降温速率0.2~20℃/分钟降至室温，并放置时间控制在0.2~10小时范围使析出的硼酸聚集趋于完全和稳定。
  6. 根据权利要求1、2或5所述的方法，其特征在于，步骤3中，干燥温度控制在20~110℃范围内。
  7. 根据权利要求3所述的方法，其特征在于，步骤3中，干燥温度控制在20~110℃范围内。
  8. 根据权利要求4所述的方法，其特征在于，步骤3中，干燥温度控制在20~110℃范围内。
PCT/CN2020/080988 2019-04-10 2020-03-25 一种有机分子诱导制备高纯球形速溶硼酸的方法 Ceased WO2020207242A1 (zh)

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