CN101983924B - A method for preparing calcium carbonate with controllable morphology from calcium sulfate - Google Patents
A method for preparing calcium carbonate with controllable morphology from calcium sulfate Download PDFInfo
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 84
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims abstract description 48
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 6
- 239000011575 calcium Substances 0.000 abstract description 6
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000012876 topography Methods 0.000 abstract 4
- 235000011132 calcium sulphate Nutrition 0.000 abstract 2
- 239000001175 calcium sulphate Substances 0.000 abstract 2
- 239000000376 reactant Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 6
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 4
- 238000009776 industrial production Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 208000010444 Acidosis Diseases 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007950 acidosis Effects 0.000 description 1
- 208000026545 acidosis disease Diseases 0.000 description 1
- 239000000729 antidote Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 208000000718 duodenal ulcer Diseases 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明属于无机盐材料技术领域，涉及一种形貌可控碳酸钙的制备方法。The invention belongs to the technical field of inorganic salt materials, and relates to a method for preparing calcium carbonate with controllable morphology.
背景技术 Background technique
碳酸钙作为一种重要的无机非金属矿物材料，在工业上被广泛用作涂料、造纸、橡胶、油墨、塑料等行业的填料，有机合成、冶金、玻璃、陶瓷、医药、食品、化妆品等的制造原料，还可用于工业废水处理、胃与十二指肠溃疡病的酸抑制、酸中毒的解毒剂、含SO2消除剂等，是一种非常重要的无机化工产品。Calcium carbonate, as an important inorganic non-metallic mineral material, is widely used in industry as a filler in coatings, papermaking, rubber, ink, plastics and other industries, as well as in organic synthesis, metallurgy, glass, ceramics, medicine, food, cosmetics, etc. It can also be used as a raw material for industrial wastewater treatment, acid inhibition for gastric and duodenal ulcer disease, antidote for acidosis, and SO2- containing scavenger, etc. It is a very important inorganic chemical product.
形貌可控制备碳酸钙的研究吸引着许多科研工作者的关注，目前采用的合成方法主要有两种：碳化法和沉淀法。碳化法是采用石灰石煅烧、石灰消化得到氢氧化钙，再在氢氧化钙中通入CO2进行碳化、分离、干燥等工艺制取碳酸钙。以碳化法制备碳酸钙是大规模工业生产常采用的方法，但是采用该方法存在形貌难以控制的问题，所以目前对碳酸钙的形貌可控制备主要采用沉淀法。沉淀法是采用水溶性钙盐与水溶性碳酸盐在适当的工艺条件下进行反应。研究较多的是在体系中引入表面活性剂或者高聚物等或者与游离钙离子络合，或者在溶液中形成一定的结构从而影响碳酸钙的形核和生长过程，获得不同形貌的碳酸钙。本发明试图用微溶于水的硫酸钙做为钙源，以N，N-二甲基甲酰胺或无水乙醇为溶剂分散钙源，形成硫酸钙悬浮液，避免传统沉淀法中直接采用可溶性的钙盐；在此基础上引入碳酸盐，随着加入碳酸盐水溶液中水量的增加，使硫酸钙缓慢溶解析出钙离子，与碳酸根离子结合形成碳酸钙粉体，通过控制反应条件来控制碳酸钙的形貌。对于硫酸钙反应不完全的情况，该工艺过程获得的是碳酸钙和硫酸钙的混合物，将该混合物溶于适量去离子水中搅拌一定时间即可溶解硫酸钙，获得单相碳酸钙。本工艺不需加入表面活性剂和聚合物，能够简化制备工艺，节约成本，在工业化生产中具有重要的现实作用。The research on the preparation of calcium carbonate with controllable morphology has attracted the attention of many researchers. Currently, there are two main synthesis methods: carbonization and precipitation. The carbonization method uses limestone calcination and lime digestion to obtain calcium hydroxide, and then passes CO2 into the calcium hydroxide for carbonization, separation, and drying to prepare calcium carbonate. The preparation of calcium carbonate by carbonization is a method commonly used in large-scale industrial production, but there is a problem that the morphology is difficult to control by this method, so the precipitation method is mainly used for the preparation of calcium carbonate with controllable morphology. The precipitation method is to use water-soluble calcium salt and water-soluble carbonate to react under appropriate process conditions. More research is to introduce surfactants or polymers into the system or complex with free calcium ions, or form a certain structure in the solution to affect the nucleation and growth process of calcium carbonate, and obtain carbonates with different shapes. calcium. The present invention attempts to use slightly water-soluble calcium sulfate as the calcium source, and uses N,N-dimethylformamide or dehydrated alcohol as the solvent to disperse the calcium source to form a calcium sulfate suspension, avoiding the direct use of soluble calcium sulfate in the traditional precipitation method. Calcium salt; on this basis, carbonate is introduced, and as the amount of water added to the carbonate aqueous solution increases, calcium sulfate slowly dissolves and separates calcium ions, and combines with carbonate ions to form calcium carbonate powder. By controlling the reaction conditions to Control the morphology of calcium carbonate. For the case of incomplete reaction of calcium sulfate, the process obtains a mixture of calcium carbonate and calcium sulfate, which is dissolved in an appropriate amount of deionized water and stirred for a certain period of time to dissolve calcium sulfate and obtain single-phase calcium carbonate. The process does not need to add surfactants and polymers, can simplify the preparation process, save costs, and has an important practical role in industrial production.
发明内容 Contents of the invention
本发明的目的在于提供一种以硫酸钙为钙源制备形貌可控碳酸钙的方法。将微溶于水的硫酸钙粉末分散在N，N-二甲基甲酰胺或无水乙醇中形成硫酸钙悬浮溶液，加入浓度为0.01mol/L-0.9mol/L的碳酸盐溶液20-80℃反应1-12h，将产物离心并分散到50-1000mL去离子水中，搅拌1-8h后离心洗涤处理得到形貌可控的单相碳酸钙粉末。所提供的方法简单，操作方便，所用的原料廉价易得，是一种适于工业化生产的制备方法。具体步骤是：The object of the present invention is to provide a method for preparing calcium carbonate with controllable morphology using calcium sulfate as a calcium source. Disperse the slightly water-soluble calcium sulfate powder in N,N-dimethylformamide or absolute ethanol to form a calcium sulfate suspension solution, and add a carbonate solution with a concentration of 0.01mol/L-0.9mol/L for 20- React at 80°C for 1-12h, centrifuge and disperse the product into 50-1000mL deionized water, stir for 1-8h, and then centrifuge and wash to obtain a single-phase calcium carbonate powder with controllable morphology. The provided method is simple, convenient to operate, and the raw materials used are cheap and easy to obtain, and is a preparation method suitable for industrial production. The specific steps are:
(1)将新鲜制备的硫酸钙粉末磁力搅拌分散于50mL N，N-二甲基甲酰胺或无水乙醇中形成悬浮溶液；(1) The freshly prepared calcium sulfate powder is magnetically stirred and dispersed in 50mL N, N-dimethylformamide or absolute ethanol to form a suspension solution;
(2)快速加入50mL浓度为0.01mol/L-0.9mol/L的碳酸氢钠或碳酸钠溶液，20-80℃搅拌反应1-12h；(2) Quickly add 50mL of sodium bicarbonate or sodium carbonate solution with a concentration of 0.01mol/L-0.9mol/L, and stir at 20-80°C for 1-12h;
(3)将沉淀离心并转移至烧杯中，加入50-1000mL去离子水，在室温下磁力搅拌1-8h；(3) Centrifuge the precipitate and transfer it to a beaker, add 50-1000mL deionized water, and stir magnetically at room temperature for 1-8h;
(4)将液相体系中的产物进行分离，对分离出的产物进行洗涤和干燥处理，即得碳酸钙粉体。(4) Separating the product in the liquid phase system, washing and drying the separated product to obtain calcium carbonate powder.
与现有技术相比，本发明的优点在于：Compared with the prior art, the present invention has the advantages of:
(1)本发明通过选用微溶于水的硫酸钙取代易溶于水的硝酸钙或氯化钙为钙源，首先将其分散于N，N-二甲基甲酰胺或无水乙醇中形成悬浮溶液，通过水量的增加促使硫酸钙的缓慢溶解释放出钙离子来参与反应形成碳酸钙。(1) The present invention replaces calcium nitrate or calcium chloride easily soluble in water by selecting slightly soluble calcium sulfate as the calcium source, first dispersing it in N,N-dimethylformamide or dehydrated alcohol to form Suspended solution, the slow dissolution of calcium sulfate is promoted by the increase of water to release calcium ions to participate in the reaction to form calcium carbonate.
(2)所制备的碳酸钙晶相纯度高、形貌控制比较均匀。随反应条件的改变形貌呈现多样性，包括梭形、球形和棒状等。(2) The crystal phase of the prepared calcium carbonate has high purity and relatively uniform shape control. With the change of reaction conditions, the morphology presents diversity, including fusiform, spherical and rod-shaped, etc.
(3)反应原料简单且廉价易得，不需要添加表面活性剂或者络合剂，制备方法简单，反应条件易于控制，不需要复杂昂贵的设备，易于实现工业化生产。(3) The reaction raw materials are simple, cheap and easy to obtain, no surfactant or complexing agent needs to be added, the preparation method is simple, the reaction conditions are easy to control, no complicated and expensive equipment is required, and industrial production is easy to realize.
附图说明 Description of drawings
图1、实施例1制备的碳酸钙的X射线粉末衍射(XRD)图谱。The X-ray powder diffraction (XRD) spectrum of the calcium carbonate that Fig. 1, embodiment 1 prepares.
图2、实施例1制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photograph of the calcium carbonate that Fig. 2, embodiment 1 prepares.
图3、实施例2制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photo of the calcium carbonate that Fig. 3, embodiment 2 prepares.
图4、实施例3制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photo of the calcium carbonate that Fig. 4, embodiment 3 prepare.
图5、实施例4制备的碳酸钙的X射线粉末衍射(XRD)图谱。The X-ray powder diffraction (XRD) spectrum of the calcium carbonate that Fig. 5, embodiment 4 prepares.
图6、实施例4制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photograph of the calcium carbonate that Fig. 6, embodiment 4 prepares.
图7、实施例5制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photo of the calcium carbonate that Fig. 7, embodiment 5 prepares.
图8、实施例6制备的碳酸钙的扫描电镜(SEM)照片。The scanning electron microscope (SEM) photo of the calcium carbonate that Fig. 8, embodiment 6 prepares.
以下结合附图和具体实施方式对本发明作进一步说明，但本发明的保护范围不仅限于下述实施方式。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, but the scope of protection of the present invention is not limited to the following embodiments.
具体实施方式 Detailed ways
实施例1Example 1
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mL N，N-二甲基甲酰胺中，温度为35℃；将50mL0.06mol/L NaHCO3溶液快速倒入悬浮液中，35℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图1为X射线粉末衍射结果，表明其为单相的碳酸钙。从图2的扫描电子显微镜照片可以看出其为梭形和花状的混合形貌。Disperse the freshly prepared calcium sulfate precursor with magnetic stirring in 50 mL of N,N-dimethylformamide at 35 °C; quickly pour 50 mL of 0.06 mol/L NaHCO 3 solution into the suspension, and stir at 35 °C for reaction 4 hours; centrifuge the precipitate and transfer it to a beaker, add 200ml of distilled water, and stir magnetically at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 1 is X-ray powder diffraction result, shows that it is the calcium carbonate of single phase. From the scanning electron micrograph in Figure 2, it can be seen that it is a mixture of fusiform and flower-shaped.
实施例2Example 2
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mL N，N-二甲基甲酰胺中，温度为35℃；将50mL0.18mol/L NaHCO3溶液快速倒入悬浮液中，35℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图3为其扫描电子显微镜照片，可以清楚的看出其主要为梭形碳酸钙。Disperse the freshly prepared calcium sulfate precursor with magnetic stirring in 50 mL of N,N-dimethylformamide at 35 °C; quickly pour 50 mL of 0.18 mol/L NaHCO 3 solution into the suspension, and stir at 35 °C for reaction 4 hours; centrifuge the precipitate and transfer it to a beaker, add 200ml of distilled water, and stir magnetically at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 3 is its scanning electron micrograph, and it can be clearly seen that it is mainly fusiform calcium carbonate.
实施例3Example 3
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mL N，N-二甲基甲酰胺中，温度为35℃；将50mL0.06mol/L NaHCO3溶液快速倒入悬浮液中，60℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图4为其扫描电子显微镜照片，可以清楚的看出其主要为球形碳酸钙。Disperse the freshly prepared calcium sulfate precursor with magnetic stirring in 50 mL of N,N-dimethylformamide at 35 °C; quickly pour 50 mL of 0.06 mol/L NaHCO 3 solution into the suspension, and stir at 60 °C for reaction 4 hours; centrifuge the precipitate and transfer it to a beaker, add 200ml of distilled water, and stir magnetically at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 4 is its scanning electron micrograph, and it can be clearly seen that it is mainly spherical calcium carbonate.
实施例4Example 4
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mL N，N-二甲基甲酰胺中，温度为35℃；将50mL0.06mol/LNa2CO3溶液快速倒入悬浮液中，35℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图5为X射线粉末衍射结果，表明其为单相的碳酸钙。从图6的扫描电子显微镜照片可以看出其为棒状形貌。Disperse the freshly prepared calcium sulfate precursor with magnetic stirring in 50 mL of N,N-dimethylformamide at 35 °C; quickly pour 50 mL of 0.06 mol/L Na 2 CO 3 solution into the suspension, and stir at 35 °C for reaction 4 hours; centrifuge the precipitate and transfer it to a beaker, add 200ml of distilled water, and stir magnetically at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 5 is X-ray powder diffraction result, shows that it is the calcium carbonate of single phase. It can be seen from the scanning electron microscope photo in Figure 6 that it has a rod-like morphology.
实施例5Example 5
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mLN，N-二甲基甲酰胺中，温度为35℃；将50mL0.12mol/LNa2CO3溶液快速倒入悬浮液中，35℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图7为其扫描电子显微镜照片，可以清楚的看出其主要为片层堆叠形成的碳酸钙颗粒。Disperse the freshly prepared calcium sulfate precursor with magnetic stirring in 50 mL of N,N-dimethylformamide at 35 °C; quickly pour 50 mL of 0.12 mol/L Na 2 CO 3 solution into the suspension, and stir at 35 °C for reaction 4 hours; centrifuge the precipitate and transfer it to a beaker, add 200ml of distilled water, and stir magnetically at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 7 is its scanning electron micrograph, and it can be clearly seen that it is mainly calcium carbonate particles formed by lamellar stacking.
实施例6Example 6
将新鲜制备的硫酸钙前驱物磁力搅拌分散在50mL无水乙醇中，温度为35℃；将50mL0.12mol/L Na2CO3溶液快速倒入悬浮液中，60℃搅拌反应4小时；将沉淀离心并转移至一烧杯中，加入200ml蒸馏水，在室温下磁力搅拌3小时；对分离出的产物进行离心、洗涤和干燥处理，即得碳酸钙粉体。图8为其扫描电子显微镜照片，可以清楚的看出其主要为球形碳酸钙粉体。The freshly prepared calcium sulfate precursor was magnetically stirred and dispersed in 50mL of absolute ethanol at a temperature of 35°C; quickly poured 50mL of 0.12mol/L Na 2 CO 3 solution into the suspension, and stirred at 60°C for 4 hours; Centrifuge and transfer to a beaker, add 200ml of distilled water, and magnetically stir at room temperature for 3 hours; centrifuge, wash and dry the separated product to obtain calcium carbonate powder. Fig. 8 is its scanning electron micrograph, and it can be clearly seen that it is mainly spherical calcium carbonate powder.
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