CN102834356A - 得到沉淀碳酸钙的方法 - Google Patents
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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 132
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- 239000000725 suspension Substances 0.000 claims abstract description 12
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims description 71
- 239000000463 material Substances 0.000 claims description 13
- 239000000123 paper Substances 0.000 claims description 12
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 7
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- 239000003795 chemical substances by application Substances 0.000 claims description 5
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- 235000013305 food Nutrition 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000976 ink Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 abstract description 31
- 235000011116 calcium hydroxide Nutrition 0.000 abstract description 31
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract description 17
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 abstract description 6
- 229910001866 strontium hydroxide Inorganic materials 0.000 abstract description 6
- 239000007900 aqueous suspension Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 description 44
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 18
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- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
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- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 6
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- 229910001631 strontium chloride Inorganic materials 0.000 description 4
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- 229910021532 Calcite Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
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- 238000003756 stirring Methods 0.000 description 2
- 150000003438 strontium compounds Chemical class 0.000 description 2
- 229910001427 strontium ion Inorganic materials 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 229910003514 Sr(OH) Inorganic materials 0.000 description 1
- 229910004116 SrO 2 Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-O oxonium Chemical compound [OH3+] XLYOFNOQVPJJNP-UHFFFAOYSA-O 0.000 description 1
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- 239000004575 stone Substances 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
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Abstract
本发明提供一种用于制备沉淀碳酸钙产物的方法。该方法包括以下步骤:通过在碳酸化之前或在碳酸化期间以基于Ca(OH)2之摩尔数计0.005至0.030摩尔呈Sr(OH)2形式之Sr存在下使Ca(OH)2悬浮液碳酸化来制备沉淀碳酸钙晶种的水性悬浮液;通过在以干重计0.5%至5%沉淀碳酸钙晶种存在下使Ca(OH)2浆液碳酸化来形成沉淀碳酸钙产物之水性悬浮液,其中沉淀碳酸钙晶种之D50小于沉淀碳酸钙产物之D50,且沉淀碳酸钙晶种之文石多型变体含量大于或等于沉淀碳酸钙产物的文石多型变体含量。
Description
发明领域
本发明涉及一种用于产生沉淀碳酸钙且尤其具有增加的重量百分比之文石晶体多型变体的沉淀碳酸钙产物的方法。
发明背景
近年来,碳酸钙已在许多领域中得到广泛使用。举例而言,碳酸钙为纸张、塑料、油漆及涂料行业中最广泛使用的矿物质之一,其用作填料且因其色彩为白色而用作涂布颜料。在造纸业中,碳酸钙因其高亮度、不透明度及光泽而有价值,且通常用作填料以制造光亮的不透明纸张。此外,碳酸钙在油漆中常用作增量剂,且亦在黏着剂及密封剂中用作填料。高等级碳酸钙亦已在医药制剂中得到使用。
已知碳酸钙以三种类型的晶体多型变体的形式存在:方解石、文石及球霰石。方解石为最常见的晶体多型变体,其被视为碳酸钙之最稳定晶体形式。文石较为少见,其具有离散或丛集之针状斜方晶体结构。球霰石为最罕见的碳酸钙多型变体,且一般不稳定。
在此三种形式中,文石因其提供增强之纸张松厚度(paper bulk)及不透明度的针形晶体结构而尤其适用于许多应用,诸如无机填料或纸面涂料。因此,对具有显著文石晶体含量的碳酸钙的需要已经大大增加。
一般而言,一种商业上产生碳酸钙的方式为通过锻烧粗碳酸钙而得到生石灰。接着添加水以产生氢氧化钙之水性悬浮液(“石灰乳”),且向此浆液中再引入二氧化碳以使碳酸钙沉淀。此方法之产物称为沉淀碳酸钙(“PCC”)。所得碳酸钙水性悬浮液或浆液可按原样使用或经进一步处理(亦即脱水、研磨等)以形成干产物。视所使用之确切反应条件而定,沉淀反应能够产生三种多型变体(方解石、文石及球霰石)中之每一者。
用于产生具有增加的文石晶体含量的PCC产物的先前技术方法一般采取许多途径。在第一种途径中,已开发出在碳酸化期间使用诸如锶盐之添加剂来促进文石晶体产生,从而形成PCC的方法。举例而言,GB 2145074A揭示一种通过在碳酸化期间添加氯化锶(SrCl2)以充当形成文石晶体之试剂来产生沉淀的文石碳酸钙的方法。
使用锶化合物作为碳酸化过程之添加剂以供制备PCC亦揭示于以下日本专利公开案之PCC生产方法中:JP63260815、JP59223225、JP5116936及JP1018911。
在第二种途径中,方法已利用文石晶种来增加文石晶体形成。举例而言,GB 941900A教示一种通过在碳酸化期间引入碳酸钠溶液来产生文石碳酸钙的方法。该参考文献建议向所揭示之方法中添加文石晶种可加速文石晶体的产生。
上文所论述之生产方法已显示或多或少地增加PCC产物的总文石晶体含量。然而,这些方法一般不能产生总文石含量大于60%的PCC。
因此,需要一种用于产生含有增加量的文石多型变体的沉淀PCC的低成本方法。
发明概述
本发明提供一种产生低成本的包含PCC的物质的方法,其中在包含PCC的物质中,相对于PCC大于60%且优选大于70%为文石多型变体。在其一般形式中,本发明通过利用两阶段制造方法来实现这些需求。在第一阶段中,可通过在碳酸化之前每摩尔Ca(OH)20.005至0.030摩尔或更优选0.01至0.02摩尔呈Sr(OH)2形式之锶存在下使Ca(OH)2悬浮液碳酸化来形成沉淀碳酸钙晶种的水性悬浮液。在第二阶段中,通过在以干重计0.5%至5%沉淀碳酸钙晶种存在下使Ca(OH)2浆液碳酸化来形成沉淀碳酸钙产物的水性悬浮液。沉淀碳酸钙晶种之D50可小于沉淀碳酸钙产物之D50,且沉淀碳酸钙晶种之文石多型变体含量可大于或等于沉淀碳酸钙产物的文石多型变体含量。如以下实施例中将论述,此两阶段方法之产物解决了先前PCC生产方法的不足且最终产物中文石多型变体的总重量百分比得到期望的增加。
本发明亦提供一种由本发明方法制备的沉淀碳酸钙产物。
此外,本发明提供一种包含本发明之沉淀碳酸钙产物的物质。该物质可包括例如需要包括碳酸钙作为填料之产品,诸如纸张、纸制品、油墨、油漆、涂料、塑料、黏着剂、建筑产品、食品及医药产品。
最后,本发明之沉淀碳酸钙产物系针对使用该产物来制造需要使用文石PCC作为填料的物质。
本发明之其他目的将自以下描述显而易见。
发明详述
如上文所论述,PCC典型地通过熟石灰碳酸化来制造。在此方法中,首先锻烧(加热)粉碎的碳酸钙以形成石灰(CaO)及二氧化碳气体(CO2)。此反应展示于反应(1)中:
(1)CaCO3→CaO+CO2
接着用水使石灰熟化以形成氢氧化钙(Ca(OH)2)或石灰乳,其展示于反应(2)中:
(2)CaO+H2O→Ca(OH)2
最后,将氢氧化钙与二氧化碳(通常在锻烧步骤期间捕获)组合以使碳酸钙沉淀。此碳酸化步骤展示于反应(3)中:
(3)Ca(OH)2+CO2→CaCO3+H2O
根据本发明,以两阶段方法制备沉淀碳酸钙产物。在第一阶段中,通过在碳酸化之前基于Ca(OH)2之摩尔数为0.005至0.030摩尔或更优选0.01至0.02摩尔呈Sr(OH)2形式之锶存在下使Ca(OH)2悬浮液碳酸化来制备沉淀碳酸钙晶种之水性悬浮液(或浆液)。可经由Ca(OH)2悬浮液之石灰引入Sr(OH)2,或更优选可通过在熟化和/或碳酸化期间添加包含SrO的矿物质而原位形成Sr(OH)2。若通过添加包含SrO的矿物质而原位形成Sr(OH)2,则优选可通过锻烧包含SrCO3的矿物质或粗菱锶矿原料石而得到包含SrO的矿物质。
本发明之沉淀碳酸钙晶种的特征为文石多型变体含量大于或等于第二阶段中所产生之沉淀碳酸钙产物的文石多型变体含量。具体地,在本发明方法中,沉淀碳酸钙晶种之水溶液可具有以干重计大于85%、优选为90%或最优选为95%的文石多型变体含量。如本文所述之干重百分比通过X射线衍射分析(XRD)来测定。
在制造方法之第一阶段期间所产生之沉淀碳酸钙晶种的另一特征为D50小于沉淀碳酸钙产物的D50。D50尺寸定义为如下尺寸:在该尺寸下以累积体积分数计50%之产物小于该尺寸。使用MicrometricsSedigraphTM 5100量测粒径。
在本发明之范围内,晶种产生过程可进行其他处理步骤,诸如进行脱水、分散和/或研磨。在优选实施方案中,可进一步处理沉淀碳酸钙晶种之水性悬浮液以得到小于或等于0.1至0.3μm之D50及10至30m2/g之BET SSA。使用TriStar 3000,通过根据BET程序量测干燥样品上之氮吸附来量测BET或表面积。
关于研磨,可对所述方法的第一阶段中所得之PCC晶种进行干式研磨和/或湿式研磨。湿式研磨是指在液体介质(例如浆液)中研磨PCC。湿式研磨可在不存在助磨剂或存在助磨剂的情况下进行。可包括一或多种研磨剂,诸如聚丙烯酸钠、聚丙烯酸盐和/或丙烯酸共聚物之盐。干燥可使用任何适合之干燥设备进行,且可包括例如使用诸如蒸发器、快速干燥器、烘箱、喷雾干燥器(诸如由Niro和/或Nara出售之喷雾干燥器)之设备来热干燥和/或在减压下干燥和/或在真空腔室中干燥。
在本发明方法之第二阶段中,通过在以干重计0.5%至5%的自生产方法第一阶段得到之沉淀碳酸钙晶种存在下使Ca(OH)2浆液碳酸化来形成沉淀碳酸钙产物之水性悬浮液。就此而言,可在沉淀碳酸钙产物碳酸化之前将沉淀碳酸钙晶种添加至Ca(OH)2浆液中。或者,可在前四分之一的总碳酸化时间内将沉淀碳酸钙晶种添加至Ca(OH)2浆液中,其中总碳酸化时间包括自碳酸化开始直至电导率最小之时所量测的总时间跨度。
本文所述之方法能够产生沉淀碳酸钙产物,其含有以干重计大于60%且优选以干重计大于70%之文石多型变体含量,如通过XRD分析所测定。此外,第二阶段中所产生之沉淀碳酸钙产物优选具有1至5摩尔/干公吨之总锶量。
可对第二阶段中得到的沉淀碳酸钙产物进行进一步处理,包括例如脱水、分散和/或研磨步骤,以得到具有所要特征之沉淀碳酸钙产物,其亦处于本发明之范围内。优选可对第二阶段中得到之沉淀碳酸钙产物进行额外处理以得到0.35至0.45微米之D50及8至20m2/g之BETSSA。
最后,根据本发明产生之沉淀的文石碳酸钙产物可用于需要使用碳酸钙作为填料的各种物质中。举例而言,沉淀的文石碳酸钙产物可用于医药领域产品(诸如医药)、人类或动物食品、造纸领域(诸如填料或纸面涂料)、水基或非水基油漆、塑料或印刷油墨(例如平板印刷、轮转凹版印刷)中。
初步试验
作为起点,考虑八水合氢氧化锶(Sr(OH)2·8H2O),其目前用作文石-PCC(“A-PCC”)晶种碳酸化之文石促进剂。进行实验室试验以评估替代性的且比Sr(OH)2·8H2O更经济之Sr2+来源。
在第一个试验中,经由在25%w/w乙酸中溶解SrCO3来制备乙酸锶(Sr(CH3COO)2)之26%w/w溶液。随后评估乙酸锶在A-PCC晶种制造中作为Sr(OH)2·8H2O之替代物用作碳酸化添加剂。此碳酸化试验之结果表明,在基于石灰乳相同的Sr2+摩尔添加率下,乙酸锶与Sr(OH)2·8H2O相比效果较差。特别是,XRD分析揭示,当与Sr(OH)2·8H2O添加剂相比时,晶种碳酸化之后文石含量已自97%降至38%。
基于第一个试验之结果,在第二个试验中,在1300℃下将化学纯的沉淀的SrCO3锻烧2小时以得到SrO。在添加2%SrO(干/干CaO)作为熟化添加剂下进行A-PCC晶种碳酸化,得到与使用7.5%Sr(OH)2·8H2O(干/干Ca(OH)2)相同的结果(97%文石)。这些初步试验之结果展示于表1中。使用所述经后处理之A-PCC晶种的A-PCC制造试验亦取得成功且在以下实施例中加以论述。
表1-初步试验,碳酸化
Sr(OH)2·8H2O | [%w/w,基于石灰乳] | 7.5 | |
Sr(CH3COO)2 | [%w/w,基于石灰乳] | 3.0 | |
SSA | [m2/g] | 6.2 | 13.2 |
D50 | [μm] | 2.37 | 0.97 |
文石 | [%] | 38.6 | 97.0 |
晶种中的总Sr | [mol/DMT晶种] | 108.0 | 208.7 |
此外,通过处于技术现状下之X射线衍射对第二个试验中得到之PCC晶种进行矿物学分析。显然,未检测到结晶碳酸锶,此表明所有锶离子皆以外来离子形式并入文石晶格中。此证实在初始晶核生成阶段期间最终沉淀之碳酸锶似乎不会干预晶种形成,而锶离子则会如此。基于这些发现,本领域技术人员将预期用高度可溶性锶盐(诸如SrCl2)会得到最好的结果。然而,如下文进一步论述之结果所表明,SrCl2并不如Sr(OH)2(或向水中添加SrO所得之Sr(OH)2)那样有助于A-PCC晶种形成,尽管氯化锶在水中之溶解度为53.8g/100mL(20℃),而氢氧化锶之溶解度为1.77g/100ml(20℃)。
可通过比较使用单阶段碳酸化方法之先前技术方法与利用两阶段方法之本发明实施例来说明这些结果。这些实施例仅欲作为说明,且不应视为以任何方式限制以下权利要求所界定之本发明范畴。
表2展示由本发明得到的文石百分比相比使用先前技术方法得到的文石百分比的比较。
表2
实施例
实施例1
阶段1:A-PCC晶种
通过将160kg生石灰CaO(例如Mississippi LimeCo.,Ste.Geneviève,Mo供应之生石灰)添加至搅拌反应器中之1,300公升50℃自来水中而使该化合物熟化。熟化前,向CaO中添加通过在1300℃下将化学纯之沉淀SrCO3锻烧2小时而得到之3.2kgSrO。在连续搅拌下使生石灰熟化30分钟,且经由用60℃水稀释将所得氢氧化钙浆液(”石灰乳”)调节至13%固体含量,接着在100μm筛网上过筛。
在配备有通气搅动器(gassing agitator)、用以将二氧化碳/空气气流引导至叶轮的不锈钢碳酸化管和用于监测悬浮液pH值及电导率的探针的1000公升挡板式圆柱形不锈钢反应器中进行A-PCC晶种沉淀。向碳酸化反应器中添加调节至60℃之温度的800公升上述熟化步骤中得到之氢氧化钙悬浮液。接着在1480rpm之浆液搅动下,使6体积%CO2/空气气体以100m3/h之速率向上鼓泡通过浆液15分钟(自开始引入CO2气体时计算)。此后,将气体中之CO2体积分数扩增至24%,且将气体流量扩增至200m3/h。在此速率下维持CO2体积分数及气体流量直至反应结束。在碳酸化期间,不控制反应混合物之温度,且该温度因放热沉淀反应所产生之热而升高。在电导率达到对应于Ca(OH)2全部转化成PCC的最小值之后,再继续通气8分钟,接着停止引入气体。自开始引入气体至电导率最小之时所计算的碳酸化时间为84分钟。接着在45μm筛网上使A-PCC晶种浆液过筛,且回收呈A-PCC晶种之水性浆液形式的过筛产物。如表2之A栏中所示,在添加基于干CaO为2% SrO(对应于基于干石灰乳为1.51%SrO)下A-PCC晶种碳酸化得到具有97.4%文石之A-PCC晶种浆液。
虽然并不需要,但在此实施例中进行A-PCC晶种浆液之后处理。具体地,使该物质脱水并研磨以得到具有17.4m2/gSSA及0.23μm中值直径的粒子。
阶段2:A-PCC产物
以与上述阶段1中所述相同之方式进行熟化及碳酸化,但不添加SrO且在碳酸化之前向石灰乳中添加2.5重量%(基于氢氧化钙之干重计,以干碳酸钙计算)之阶段1中形成的经研磨A-PCC晶种。对最终A-PCC产物进行之测试表明87.7%之产物为文石晶体。此外,如上述阶段1中所述进行后处理,得到具有11.7m2/gSSA及0.41μm中值直径的粒子。
实施例2
阶段1:A-PCC晶种
以与上述实施例1中所述相同之方式进行A-PCC晶种碳酸化,但在熟化之前不向CaO中添加SrO。为形成A-PCC晶种,在碳酸化之前向石灰乳中添加5.0重量%之Sr(OH)2·8H2O(基于氢氧化钙之干重)。如表2之B栏中所示,在添加5.0% Sr(OH)2·8H2O下A-PCC晶种碳酸化得到具有96.1%文石之A-PCC晶种浆液。
虽然并不需要,但在此实施例中进行A-PCC晶种浆液之后处理。具体地,使该物质脱水并研磨以得到具有20.6m2/gSSA及0.22μm中值直径的粒子。
阶段2:A-PCC产物
以与上述阶段1中所述相同之方式进行熟化及碳酸化,但不添加Sr(OH)2·8H2O且在碳酸化之前向石灰乳中添加2.5重量%(基于氢氧化钙之干重,以干碳酸钙计算)之阶段1中形成的经研磨A-PCC晶种。对最终A-PCC产物进行之测试表明77.6%之产物为文石晶体。
实施例3
阶段1:A-PCC晶种
以与上述实施例1中所述相同之方式进行A-PCC晶种碳酸化,但在熟化之前不向CaO中添加SrO。为形成A-PCC晶种,在碳酸化之前向石灰乳中添加7.5重量%之Sr(OH)2·8H2O(基于氢氧化钙之干重)。如表2之C栏中所示,在添加7.5% Sr(OH)2·8H2O下A-PCC晶种碳酸化得到具有97.6%文石之A-PCC晶种浆液。
虽然并不需要,但在此实施例中进行A-PCC晶种浆液之后处理。具体地,使该物质脱水并研磨以得到具有22.5m2/gSSA及0.21μm中值直径的粒子。
阶段2:A-PCC产物
以与上述阶段1中所述相同之方式进行熟化及碳酸化,但不添加Sr(OH)2·8H2O且在碳酸化之前向石灰乳中添加2.5重量%(基于氢氧化钙之干重,以干碳酸钙计算)之阶段1中形成的经研磨A-PCC晶种。对最终A-PCC产物进行之测试表明77.4%之产物为文石晶体。
比较实施例1
以与上述实施例1中所述相同之方式进行A-PCC晶种碳酸化,但在熟化前不向CaO中添加SrO。为形成A-PCC晶种,在碳酸化之前向石灰乳中添加3.5重量%之SrCl2·6H2O(基于氢氧化钙之干重)。如表2之D栏中所示,该方法得到仅具有61.7%文石之A-PCC。如上文所论述,这些结果证实,当以类似添加率(摩尔锶/干公吨A-PCC晶种)添加时,高度可溶性锶盐(诸如SrCl2)不如Sr(OH)2(或向水中添加SrO所得之Sr(OH)2)那样有效,尽管氯化锶在水中之溶解度比氢氧化锶大。
比较实施例2
在单阶段A-PCC方法中,在碳酸化之前向Ca(OH)2中添加0.1%w/wSr(OH)2·8H2O。以与上述实施例1的阶段2中所述相同之方式进行熟化及碳酸化,但不添加A-PCC晶种,而替代地在碳酸化之前向石灰乳中添加0.1%w/wSr(OH)2·8H2O(基于氢氧化钙之干重)。如表2之E栏中可见,所得A-PCC产物仅含有53.8%文石。
比较实施例3
在单阶段A-PCC方法中,在碳酸化之前向Ca(OH)2中添加0.2%w/wSr(OH)2·8H2O。以与上述实施例1的阶段2中所述相同之方式进行熟化及碳酸化,但不添加A-PCC晶种,而替代地在碳酸化之前向石灰乳中添加0.2%w/wSr(OH)2·8H2O(基于氢氧化钙之干重)。如表2之F栏中可见,所得A-PCC产物仅含有46.4%文石。
比较实施例4
在单阶段A-PCC方法中,在碳酸化之前向Ca(OH)2中添加0.07%w/wSrCl2·6H2O。以与上述实施例1的阶段2中所述相同之方式进行熟化及碳酸化,但不添加A-PCC晶种,而替代地在碳酸化之前向石灰乳中添加0.07%w/w SrCl2·6H2O(基于氢氧化钙之干重)。如表2之G栏中可见,所得A-PCC产物仅含有49.8%文石。
利用氢氧化锶产生A-PCC产物的本发明的两阶段方法提供先前由在碳酸化期间仅利用锶化合物作为添加剂的先前技术方法无法得到的高文石产率。实际上,通过在氢氧化锶存在下首先产生A-PCC晶种,可始终得到具有高于60%文石含量的A-PCC产物。此外,与氯化锶相比,使用氢氧化锶显著增加文石晶体生长,同时降低制造成本。
鉴于已详细描述本发明之各种实施方案,各种修改及改良将为本领域技术人员显而易知。因此,本发明实施方案应视为在所有方面皆为说明性而非限制性的,本发明之范畴由随附权利要求所表明,且处于权利要求之等效含义及范围内的所有变化由此欲涵盖在内。
Claims (19)
1.一种用于制备沉淀碳酸钙产物的方法,其包括以下步骤:
(a)通过在碳酸化之前或在碳酸化期间在每摩尔Ca(OH)20.005至0.030摩尔呈Sr(OH)2形式的Sr存在下使Ca(OH)2悬浮液碳酸化来制备沉淀碳酸钙晶种的水性悬浮液;和
(b)通过在以干重计0.5%至5%该沉淀碳酸钙晶种存在下使Ca(OH)2浆液碳酸化来形成沉淀碳酸钙产物的水性悬浮液,
其中该沉淀碳酸钙晶种的D50小于该沉淀碳酸钙产物的D50,且该沉淀碳酸钙晶种的文石多型变体含量大于或等于该沉淀碳酸钙产物的文石多型变体含量。
2.权利要求1的方法,其中在每摩尔Ca(OH)20.01至0.02摩尔Sr的存在下对步骤(a)中Ca(OH)2悬浮液进行碳酸化。
3.权利要求1的方法,其中步骤(a)中的Sr(OH)2通过添加在熟化和/或碳酸化之前或期间所添加的包含SrO的矿物质而原位形成。
4.权利要求3的方法,其中该包含SrO的矿物质通过煅烧包含SrCO3的矿物质而得到。
5.权利要求1-4中任一项的方法,其进一步包括以下步骤:对步骤(a)中制备的沉淀碳酸钙晶种进行脱水、分散或研磨中的一种或多种,以得到D50小于或等于0.1至0.3μm且BET SSA为10至30m2/g之沉淀碳酸钙晶种的水性悬浮液。
6.权利要求1-5中任一项的方法,其中步骤(a)中形成的沉淀碳酸钙晶种的水溶液具有以干重计大于85%之文石多型变体含量。
7.权利要求1-5中任一项的方法,其中步骤(a)中形成的沉淀碳酸钙晶种的水溶液具有以干重计大于90%之文石多型变体含量。
8.权利要求1-5中任一项的方法,其中步骤(a)中形成的沉淀碳酸钙晶种的水溶液具有以干重计大于95%之文石多型变体含量。
9.权利要求1-8中任一项的方法,其中该沉淀碳酸钙晶种在碳酸化之前添加至步骤(b)中的Ca(OH)2浆液中。
10.权利要求1-8中任一项的方法,其中该沉淀碳酸钙晶种在前四分之一的总碳酸化时间内添加至步骤(b)中的Ca(OH)2浆液中。
11.权利要求1-10中任一项的方法,其进一步包括以下步骤:对步骤(b)中得到的沉淀碳酸钙产物进行脱水、分散或研磨中的一种或多种,以得到D50为0.35至0.4微米且BET SSA为8至20m2/g的沉淀碳酸钙产物。
12.权利要求1-11中任一项的方法,其中步骤(b)中得到的沉淀碳酸钙产物具有0.2至15摩尔/干公吨之总锶量。
13.权利要求1-11中任一项的方法,其中步骤(b)中得到的沉淀碳酸钙产物具有1至5摩尔/干公吨之总锶量。
14.权利要求1-13中任一项的方法,其中步骤(b)中得到的沉淀碳酸钙产物含有以干重计大于60%之文石多型变体含量。
15.权利要求1-13中任一项的方法,其中步骤(b)中得到的沉淀碳酸钙产物含有以干重计大于70%之文石多型变体含量。
16.一种沉淀碳酸钙产物,其由权利要求1-15中任一项的方法产生。
17.一种物质,其包含权利要求16的沉淀碳酸钙。
18.权利要求17的物质,其中该物质选自由纸张、纸制品、油墨、油漆、涂料、塑料、黏着剂、建筑产品、食品及医药产品组成的组。
19.权利要求16的沉淀碳酸钙产物的用途,其用于制造选自由纸张、纸制品、油墨、油漆、涂料、塑料、黏着剂、建筑产品、食品及医药产品组成的组的物质。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10003665.6 | 2010-04-01 | ||
EP10003665A EP2371766B1 (en) | 2010-04-01 | 2010-04-01 | Process for obtaining precipitated calcium carbonate |
US34201710P | 2010-04-08 | 2010-04-08 | |
US61/342,017 | 2010-04-08 | ||
PCT/EP2011/054994 WO2011121065A1 (en) | 2010-04-01 | 2011-03-31 | Process for obtaining precipitated calcium carbonate |
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CN107074577A (zh) * | 2014-10-24 | 2017-08-18 | 欧米亚国际集团 | 具有减少的氢氧钙石含量的pcc |
CN107074577B (zh) * | 2014-10-24 | 2019-12-06 | 欧米亚国际集团 | 具有减少的氢氧钙石含量的pcc |
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CN105819483A (zh) * | 2015-01-06 | 2016-08-03 | 上海华明高技术(集团)有限公司 | 含文石晶相的沉淀碳酸钙晶种及其制备方法 |
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