CN101679115B - 用于从二水硫酸钙生产α-半水硫酸钙的方法 - Google Patents

用于从二水硫酸钙生产α-半水硫酸钙的方法 Download PDF

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CN101679115B
CN101679115B CN2008800173554A CN200880017355A CN101679115B CN 101679115 B CN101679115 B CN 101679115B CN 2008800173554 A CN2008800173554 A CN 2008800173554A CN 200880017355 A CN200880017355 A CN 200880017355A CN 101679115 B CN101679115 B CN 101679115B
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autoclave
method described
water
stirring
calcium
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CN101679115A (zh
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雷恩哈德·耶格尔
阿尔佛雷德·布罗斯格
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Grenzebach BSH GmbH
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Grenzebach BSH GmbH
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    • C04B11/032—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained for the wet process, e.g. dehydrating in solution or under saturated vapour conditions, i.e. to obtain alpha-hemihydrate
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Abstract

公开了用于从钙二水化物生产α-半水硫酸钙的方法。所述方法具有下列特征：a)搅拌的高压釜(1)负载钙二水化物；b)搅拌的高压釜(1)间接加热；c)水以可控方式加入并混合；d)通过固定在搅拌的高压釜(1)的桨叶和/或驱动轴(16)的移动链(3)，防止原料粘附在反应室表面；e)当内部达到一定压力时，通过间隔或者连续排出蒸汽的方式调节反应室内的压力，蒸汽通过离心分离器(17)和控制阀(18)引导；f)递送冷空气用于残余干燥目的；g)去除工艺材料。还公开了用于开展所述方法的相应设备。

Description

用于从二水硫酸钙生产α-半水硫酸钙的方法
技术领域
本发明涉及生产α-半水硫酸钙的方法，尤其是从二水硫酸钙α-半水硫酸钙的方法。
背景技术
石膏是化合物二水硫酸钙(CaSO4·2H2O)的矿物学名称。
通过供给热能，石膏从其每一分子单元的化学结合的结晶水中损失11/2个分子，并且因此二水硫酸钙转变成半水硫酸钙CaSO4·0.5H2O。
存在两种技术形式的半水硫酸钙，并且在实践中经常将它们区分为α和β型，但是根据化学矿物学它们是相同的。如果在大气压下供给热能，得到β型半水硫酸钙。此烧制产物颗粒具有高的固有孔隙率并且由包含众多的个体微晶。由于高的表面面积，包含该半水化物的粘合剂在加工过程中需水量高，并且这导致水-石膏系数为约0.6-1.0(通过计量定量测定；根据EN 13279-1测试；2005年9月)。这意味着在加工过程中得到低强度值。β型是熟石膏的主要成分，熟石膏是用于生产石膏灰泥和石膏板的极其重要的粘合剂。
本发明涉及生产另一种形式的半水硫酸钙，即α型。
该α型半水硫酸钙从过饱和水溶液中，特别地从酸和盐电解质的溶液中或者在高压釜的高的温度下和高蒸汽压力下产生。这些转变通常使用对所生产晶体形态学具有期望影响的添加剂开展。
与β型相比，α型提供良好成型的个体晶体，其在研磨后产生水-石膏系数约0.3至0.5的粘合剂。这导致在使用过程中产生相当更高的强度值。如此的粘合剂用于例如牙科中。
如果α-半水硫酸钙从水溶液或电解质溶液中结晶，则使用术语“湿法”。在使用水溶液的湿法中，在“中性”操作和“酸性”操作之间是有区别的。在中性操作中，大致pH中性的石膏诸如天然石膏或FGD石膏被转变，而无需设定pH值(见例如GB 563 019)，然而在酸性操作中有意地使用硫酸将pH值设置成大约2至3，在其中通常使用酸性启动石膏诸如磷石膏(DE 11 57 128 A1)。相反，如果α-半水硫酸钙在蒸汽负载的高压釜中生产，则使用术语“干法”(见例如US 1 901 051)。
从电解质溶液生产α-半水硫酸钙(US 2 616 128)在工业上尚未成功，因为在装置上发生相当大的腐蚀。此外，需要在干燥之前开展的过滤脱水、滤饼洗涤和废水处理的过程工业步骤遭遇到无法克服的困难。此外，由于置入二水硫酸钙导致不可避免地出现材料粘附和结垢的情况。
在“干法”中，具有高纯度和致密晶体微结构的粗天然石膏片堆在架装推车上或者多孔钢笼中并且在蒸汽负载的高压釜中加热。为了实现甚至在核心区也达到高程度转变，有必要将石膏留在加压的蒸汽压下达几小时的时间。同样的原理应用于“干法”中，在其中最初精细粉碎的石膏被压成石坯，然后如上所述在加压的蒸汽里经加热处理(见例如DE 38 19 652C3)。
根据DE 0937276 C、DE 4217978 A1和EP 0572781 B1，用于干法或半干法的另一种方法提供水平(否则垂直)搅拌器高压釜。根据DE 093 7276C，从石膏中产生的最初的结晶水形成了搅拌器高压釜中的压力，如果适当，通过所出现的渗吸水辅助(一直到大约3％)。使用颗粒材料，并且可以在转筒中开展干燥。
根据DE 4217978 A1和EP 0572 781 B1，精细粉碎的材料在水平搅拌器高压釜中转变，不加或者加入极少量的带有或不带有添加剂的水。干燥可以在高压釜或下游设备中开展。
EP 0572 781 B1的权利要求1请求保护用于使用干法从二水硫酸钙生产α-半水硫酸钙的方法，其中精细颗粒状原材料被负载，并且在压力、温度和蒸汽作用下转变，该方法特征在于材料使用外部驱动的混合设备在固定式反应器内部混合或者使用固定的或可移动的混合设备在旋转反应器内部混合，并且特征在于反应器内材料的温度被连续地测量并依照预选的时间曲线进行控制。
此外，从属权利要求本质上请求保护负载具有特定比例的表面湿度和/或具有降低的结晶水比例的原材料，加入添加剂，依据预选时间曲线控制压力，撤出蒸汽并且混合空气以及提供单独的下游干燥设备。
说明书还涉及预期防止凝聚的适当设计的混合工具(第4列，第15-19行)。然而，关于这方面的相应的详细公开在EP 0572 781 B1中找不到。
迄今为止，根据该公开不可能成功地操作设备。由于无法克服的技术难题，在试验操作两年后模型设备被取下。
对相应专利的撤销在1998年07月23日具有法律效力。
发明内容
因此，根据本发明的方法基于说明用于从钙二水化物生产α-半水硫酸钙的方法和设备的这样一个目标，其显示了成本低廉和技术可靠方式下的效果，同时节省能源。
该目标通过如权利要求1中所述的方法和如权利要求11中所述的设备实现。
这些方法和相应的设备在下面更加详细描述。
附图说明
图1显示根据本发明的搅拌器高压釜，图2显示根据本发明的带有外围设备的搅拌器高压釜。
具体实施方式
如图1所示，在其底架(2)上的搅拌器高压釜(1)主要区别在于其具有悬挂在搅拌器区(5)反应室内的链(3)。
在这里，改造在实践中通常间接加热的、水平桨叶干燥器，使得可移动钢链(3)已经固定在通过驱动轴(16)驱动的旋转搅拌元件中间。这些钢链(3)与高压釜(1)的较低顶点内的底部接触。负重的钢链(3)还环绕在中心搅拌轴周围，使得它们可以在桨叶元件之间自由移动。重力意味着钢链总是向下垂直悬挂并且剥去从旋转中心搅拌器轴和从对材料积累敏感的设备的其它内部部分形成的任何材料积累。
此外，经过超声使得它能够促进匀化过程并减少材料粘附。
在设备内部部分上的能阻止材料粘附发生并且对转变过程无作用的特殊的额外涂层具有相似的效果。
根据本发明，源于重力剥掉不期望的材料积累的链元件的效果可以通过在边缘安装或多或少的重体进一步提高，诸如代替各个链元件的或者除各个链元件之外的立方体或相似的柏拉图体。
以蒸汽形式的工艺加热通过搅拌器高压釜内套层(6)和外套层之间的蒸汽进料口(15)提供。此处产生的冷凝物通过冷凝物排放口(4)排出。
同样，中心搅拌器(5)通过蒸汽进料口(8)加热，对于产生的冷凝物可以通过冷凝物流出口(7)流出。
然而，根据本发明，还可以通过其它能量载体提供所需的工艺加热。在这里可以想到的是太阳能、风能或原子过程中产生的余热。在任何可以想到的方式中得到的电能主要通过微波供给工艺所涉及的部件。
工艺中需要的压缩空气通过压缩空气进料口(9)提供。这排放掉残留水份。由于所提供的压缩空气是冷的，加热后它可以吸收大量残留水份。
原材料通过原材料入口(14)提供。
普遍公知，精细的颗粒固体物质在与水或其它液体混合后倾向于沉积在接触表面上。因此，在高压釜外面不可能将用于调整最佳表面水份所需要的水混合到当中，因为由于堵塞会停止向高压釜装载材料。因此，有必要向已经存在于高压釜中的移动的二水硫酸钙喷射水。
因此，工艺所需要的水通过喷射嘴(13)供给。
在二水硫酸钙转变并结晶形成α-半水硫酸钙之后，材料留在高压釜内。
此外，热能供应至高压釜的双套层内，而反应室内的压力不断降低。结果，在所加热的双套层和反应室之间的饱和温度的差异增加，并且这导致增加能量流，并因此导致加速干燥。干燥过程简单地通过将压缩空气吹入反应室完成。加热的压缩空气具有从α-半水硫酸钙吸收残留水份的巨大潜能。
完全干燥的α-半水硫酸钙从反应室排空，并且然后可以从出口(10)排出。
工艺蒸汽通过开口(12)去除，并且可以通过检查口(11)检查设备。
图2显示对于本发明搅拌器高压釜的最佳操作所需要的额外装置。
由此，工艺蒸汽出口(12)通往蒸汽旋风分离器并且充当蒸汽闸，在图2中蒸汽旋风分离器通过参考数字(17)指示。
旋风分离器在化学中用于离心分离粉尘。旋风分离器是圆筒状设备，其在下部区域逐渐锥形化。待去除粉尘的原气从上面切向流入旋风分离器内并且通过旋风分离器壁强力进入回路中。这产生旋转气膜振荡。伴随旋转的粉尘颗粒通过离心力被掷向壁，絮结形成团块并向下落在壁上，使用星形轮将它们从旋风分离器壁上去除。
气膜振荡以在设备上旋转方式向下移动进入变窄部分，降低了工艺中的循环直径。由于它不能从设备的底部逃出，它倾斜在设备的底板上并且以顶部直径减小的旋转方式隆起，在这里通过浸渍管使它们离开旋风分离器。
在图2中所示的情况下，蒸汽旋风分离器(17)用于清洁所产生的粉尘工艺蒸汽。在该阶段，清洁效率高达95％。在蒸汽旋风分离器中产生的粉尘通常是α-半水硫酸钙核，它可以通过所示的返回口(20)返回至高压釜(1)。然后其余的粉尘使用文丘里涤气器(19)去除，并且同样可以返回到整个工艺中。
工艺水泵(23)从水进料器(22)取得水并通过喷射嘴(13)向搅拌的高压釜(1)供应水。在冷凝器(21)和工艺水冷却器(24)中存在的水再返回到工艺中。工艺蒸汽通过控制阀(18)排出。
管线的相应路线基本上通过功能确定。
影响晶体生长的添加剂的加入没有更详细地显示。可以使用根据现有技术已知用于该工艺的所有添加剂。
根据本发明的方法和根据本发明的设备保证了在节约能源的同时以操作上可靠方式从钙二水化物生产高质量的α-钙半水化物。
此种设备的总体效率可以通过根据工艺技术学同时操作和连接多个本发明设备而进一步提高。参考数字列表
(1)搅拌器高压釜
(2)底架
(3)链
(4)冷凝物排放口(套层加热)
(5)搅拌器(加热的)
(6)内套层
(7)冷凝物流出口(搅拌器加热)
(8)蒸汽进料口(搅拌器加热)
(9)压缩空气进料口
(10)α-半水硫酸钙出口
(11)检查口
(12)工艺蒸汽出口
(13)喷射嘴
(14)原材料入口
(15)蒸汽进料口(套层加热)
(16)驱动轴(搅拌器)
(17)蒸汽旋风分离器
(18)控制阀，促动阀
(19)文丘里涤气器
(20)α核返回口
(21)冷凝器
(22)水进料器
(23)工艺水泵
(24)工艺水冷却器

Claims (13)

1.用于从钙二水化物生产α-半水硫酸钙的方法，所述方法包含下列特征：
a)搅拌的高压釜(1)负载二水硫酸钙，
b)搅拌的高压釜(1)间接加热，
c)水以可控方式加入并混合，
d)通过移动固定在搅拌的高压釜(1)的桨叶和/或驱动轴(16)的链(3)，防止材料粘附在反应室表面，
e)当内部达到特定压力时，通过间隔或者连续排出蒸汽调节反应室内的压力，蒸汽通过旋风分离器(17)和促动阀(18)引导，
f)供给冷空气用于残余干燥，和
g)去除工艺材料。
2.如权利要求1中所述的方法，特征在于
a)加入α-半水硫酸钙形式的核，和
b)可控加入和混合溶于水的添加剂。
3.如权利要求1或2中所述的方法，特征在于文丘里涤气器(19)连接在旋风分离器(17)的下游。
4.如权利要求3中所述的方法，特征在于沉积在旋风分离器(17)和/或文丘里涤气器内的材料再利用用于生产α-半水硫酸钙。
5.如权利要求1或2中所述的方法，特征在于搅拌的高压釜(1)使用研磨的天然石膏、烟气脱硫石膏或其他精细粉碎的合成石膏负载。
6.如权利要求1或2中所述的方法，特征在于搅拌的高压釜(1)用化石能量载体、太阳能、风能或残余原子热加热。
7.如权利要求2中所述的方法，特征在于核以直至二水硫酸钙质量的5％的程度加入。
8.如权利要求1或2中所述的方法，特征在于水以直至二水硫酸钙质量的20％的程度加入。
9.如权利要求8中所述的方法，特征在于水以通过均一或非均一分布在搅拌的高压釜(1)周围的喷射嘴(13)引入的可控方式加入。
10.如权利要求1或2中所述的方法，特征在于多个搅拌的高压釜(1)通过工艺技术学联合操作。
11.用于在搅拌的高压釜(1)中从钙二水化物生产α-半水硫酸钙的设备，所述设备包含下列特征：
a)搅拌的高压釜(1)具有两个壁并且被间接加热，用于搅拌所负载材料的装置(5)是可加热的，
b)分布在搅拌的高压釜(1)套层上的喷射嘴(13)被设计，使得水和溶于水的添加剂可以通过它们引入，
c)松弛悬挂的链(3)固定在搅拌器(5)区域，和
d)旋风分离器(17)和文丘里涤气器(19)连接在搅拌的高压釜(1)下游。
12.如权利要求11中所述的设备，特征在于沉积在旋风分离器(17)和文丘里涤气器(19)内的材料返回至搅拌的高压釜(1)。
13.如权利要求11和12任一中所述的设备，特征在于多个高压釜(1)联合操作。
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