CN1197411A - 溶液的制备 - Google Patents

溶液的制备 Download PDF

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CN1197411A
CN1197411A CN96197127A CN96197127A CN1197411A CN 1197411 A CN1197411 A CN 1197411A CN 96197127 A CN96197127 A CN 96197127A CN 96197127 A CN96197127 A CN 96197127A CN 1197411 A CN1197411 A CN 1197411A
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I·格雷夫森
K·菲尔普
G·R·罗斯
D·S·托尔森
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Lion True Fiber Co ltd
Lenzing AG
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Abstract

一种由固体制成溶液的方法,包括步骤:(1)先制成一种分散液,它含有(a)一种液体、(b)以粉末状态分散在该液体中的固体、(c)溶解在该液体中的聚合物粘合剂,(2)在将分散液和溶剂混合,务使粉末溶解在溶剂中。这种方法制得的溶液干燥后,由于聚合物粘合剂将粉末颗粒结合起来,就消除了粉尘的形成。本方法特别适用于反应性的织物助剂固体。固体粉末在水性液体中形成的分散液含有低粘度水溶性纤维素醚作为其主要组分,其次要组分为天然多糖胶。

Description

溶液的制备
发明背景
本发明涉及粉末液体中的糊、浆和分散液，具体是有关安全处理固体粉末的方法，特别是在制备这些物质溶液时所用的方法。
人们时常有必要测定和控制固体粉末进入某一过程步骤的流量。已知有一些粉末，特别是含有很高比例细颗粒的粉末，在大气中很容易分散，结果引起形成粉尘的问题。这对于毒性物质来说更是一个问题。人们还知道，有一些固体粉末很容易引燃或爆炸。还知道有一些固体粉末很难处理，例如在用螺杆进料器进行计量时。为便于储藏和运输并解决这些问题，将粉末分散在合适的液体中形成糊、浆或分散液(所有的这些固体/液体混合物在后面统称为分散液)就很方便。这里所用的液体时常就方便地用一种过程用的液体，例如在该过程步骤中或步骤后要在其中加入固体的溶剂(如果需要形成该固体的溶液)或其它某种所需的液体。另外，可用惰性液体或挥发性液体，后者可通过随后的蒸发从步骤中除去。
有一些分散液很难形成，因为固体不易被液体润湿。已知在分散液中加入润湿剂可解决此问题。有一些分散液是不稳定的，在储藏时或当分散液受到剪切力作用(例如在泵送)时，固体和液体相会相互分离。已知在分散液中可加入分散剂来抑制这种分离现象。例如D M Lewis等人在“燃料和着色杂志”(Journal of theSociety of Dyers and Colourists)第111卷，1995年1月/2月，12-18页中，描述了含有分散剂的织物助剂1，3，5-三丙烯酰基六氢-1，3，5-三吖嗪(TAHT)的水性分散液。
然而，这些分散液总有变干的可能。例如泼溅时或在管道和容器中作为残余物存在时都会发生。如果发生这种情况，那么仍会发生处理干粉末时引起的危害。本发明的目的是提供一种防止这类问题产生的方法。
发明内容
本发明提供一种制成固体在溶剂中的溶液的方法，包括步骤：(1)先制成一种分散液，它含有(a)一种液体、(b)以粉末形式分散在液体中的固体、(c)溶解在液体中的聚合物粘合剂，(2)将分散液和溶剂混合，所用的条件是使得粉末溶解在溶剂中。
所用液体通常是挥发性液体，以这类液体为基础的分散液易于变干。液体通常是低粘度的，例如其粘度小于约10mPa·s(10厘泊)。也可用几种液体的混合物。在许多应用中，液体的主要成分可以是水，或者基本上由水组成，在这种情况下聚合物粘合剂用水溶性聚合物。许多适用于本发明的水溶性聚合物粘合剂是此领域中人们已知的。例子包括纤维素醚，例如羧甲基纤维素和烷基纤维素、直链多糖如藻酸钠、黄原胶和瓜耳胶、明胶、聚乙烯醇、聚丙烯酰胺和以丙烯酸为基础的聚合物。聚合物粘合剂可以是成膜聚合物。
制备悬浮液用的液体可以是与溶剂相同的物质或相同的物质混合物。在这种情况下，可以认为在本发明方法的步骤(2)中所需要加的溶剂是再次加的溶剂。应当理解在这种情况下，分散液将含有溶解的固体和分散的固体粉末。这种分散液就容易用溶剂进一步稀释成浓度准确可知的溶液。
人们发现，在液体中相对可溶解的固体以及在处理该分散液的温度范围内在液体中溶解度有显著差别的固体的分散液在储藏时是容易沉积的。这是由于固体在液体中部分溶解和固体又从液体中重新结晶出来的过程所致。固体在液体中的溶解度宜小于50克/升，更佳应小于5克/升。在通常处理分散液采用的温度范围内，固体在液体中的最大和最小溶解度之差最好小于2克/升。
当固体在溶剂中的溶解度相对较低时，本发明的方法特别有价值。当需要控制循环操作液体中溶解固体的浓度时，采用本发明的方法特别有益处。
本发明方法中所用的分散液还可包含一些已知种类的添加剂，例如润湿剂(它有助于形成分散液)和/或分散剂(它可以维持粉末处于分散状态)和/或防沫剂。对于任何一种具体的分散液，通过反复试验可以很容易地选出合适的润湿剂、分散剂和防沫剂。分散剂在分散液中的百分数通常为0.1至5％(重量)。防沫剂如果使用的话，其用量一般很少，通常为分散液的0.005至0.25％即50至500ppm(重量)。在TAHT水性分散液情况下，合适的分散剂的例子包括低起沫的阴离子表面活性剂，如那些以有取代甲基的苯磺酸钠为基的阴离子表面活性剂。磷酸盐化的醇乙氧基化物也是有效的分散剂，但通常它们有较高的起沫作用，因此不大采用。在这种情况下发现通常也不太满意的材料例子，还包括磷酸盐化的醇以及聚丙烯酸氨和聚丙烯酸钠。适用防沫剂的较佳的例子包括非离子型硅烷防沫剂。
本发明方法所用的粉末在分散液中的浓度可以是该具体粉末在分散液中常用的浓度。很容易理解，粉末在分散液中的浓度可根据粉末性质和用于处理粉末的装置等等因素而在很大范围内有所不同。固体在分散液中的百分数通常为20至60％(重量)。
所用粉末的颗粒数均粒度一般小于750微米，时常小于100微米，但通常大于0.1微米。颗粒的数均粒度可以在10至400微米之间。本发明方法所用的颗粒，其长宽比可以很低，特别是也可以很高(最大和最小尺寸之比在2∶1至100∶1范围内，通常在10∶1至100∶1内)，其形状包括扁球形、片形和针形。
粉末通常是会起反应的物质。本发明可用的粉末例子包括各种织物助剂。合适的织物助剂包括可与施加在其上的织物起反应的化学物质。这些起反应的织物助剂通常是将织物放在循环浴中由溶液施加到织物上的，而本发明的方法特别适于生产这些溶液。这些织物助剂中有一些可与溶纺纤维素纤维(lyocell fibre)起反应，提高了这些纤维的耐纤丝化性能，如US-A-5310424中所述，其内容参考结合于本发明。这种织物助剂的一个具体例子是1，3，5-三丙烯酰基六氢-1，3，5-三吖嗪(TAHT)，它的应用在公开的国际专利申请号WO-A-94/09191和WO-A-95/28516以及国际专利申请号PCT/GB/00609(公开日为1996年9月19日)中都有所描述，所有这些内容也都参考结合于本发明中。
本发明的方法也可用于在水性叔胺N-氧化物如N-甲基吗啉N-氧化物溶剂中的纤维素溶液。如US-A--5,413,613中所描述的(参考结合于此)，这种溶液可以是令水从胺氧化物和水的纤维素浆液中蒸发来制得。如在EP-A-0,047,929中描述的，这种溶液中还含有少量的一种或多种热稳定剂。合适的稳定剂包括多酚如棓酸及其酯，包括棓酸丙酯。稳定剂在溶液中的浓度通常为0.01至0.5％(重量)。根据本发明，方便地以控制的速度加入稳定剂并使其溶解在纤维素的浆液或溶液中的方法是将一种分散液加入其中，该分散液含有20至60％(重量)的稳定剂(部分为溶解状态，部分为粉末分散的状态)、约40至80％(重量)的水、0.01至3％(重量)的聚合物粘合剂如水溶性中性纤维素醚(例如甲基纤维素或羟丙基甲基纤维素)。
当粉末是活泼物质时，应仔细选择聚合物粘合剂，因为不难理解，粉末和分散液中或溶液中的聚合物粘合剂起反应通常是不希望的。
本发明方法所用分散液中聚合物粘合剂的最小浓度应使得基本上所有的粉末在分散液干燥时被聚合物粘合剂粘结。容易理解，该浓度与粉末性质以及其在分散液中的浓度有关。聚合物粘合剂的浓度通常并不需要用比实现本发明优点所需的最小浓度更高，需知若采用更高浓度的聚合粘合剂将使工艺成本增加。用反复试验法是很容易测得任一具体情况下聚合物粘合剂所需最小浓度的。发现聚合物粘合剂在分散液中的浓度在0.1至5.0％(重量)范围内，有时在0.5至2.0％(重量)内通常是合适的。发现聚合物粘合剂通常还有起分散液粘度调节剂作用的优点，因此它有助于在悬浮液储藏时维持其中固体处于悬浮状态。也可以采用聚合物粘合剂的混合物。在本发明的一个较佳实施方案中，聚合物粘合剂含有一种成膜聚合物(通常为80至99.9％(重量)，较佳为90至99.9％(重量))作为其主要组分，其次要组分是对于分散固体有良好悬浮性质的聚合物(通常为0.1至20，较佳为0.5至10％(重量))，在此实施方案中还提供了含有这种聚合物混合物作为粘合剂的分散液。在水为基的系统中，溶剂是水性液体，合适的成膜聚合物例如可用水溶性纤维素醚，特别是中性纤维素醚如甲基纤维素和羟丙基甲基纤维素，具有良好悬浮性质的聚合物例如可用中性多糖胶如黄原胶、瓜耳胶和刺槐豆胶。有范围很广的可控溶液粘度的纤维素醚是有市售的。宜采用低粘度的纤维素醚，例如在低剪切条件下测得其2％溶液室温下粘度为1至20mPa·s。具有良好悬浮性质的聚合物，其在低剪切条件下测得1％的室温溶液粘度为1000至10000mPa·s。(应该知道，在商业上水溶性聚合物的粘度通常用这种方法表示)。胶如黄原胶溶液的粘度，甚至在非常低的浓度下，也随着浓度的增加而迅速增加，所以如果单用这种胶则将很难控制粘度。因此，该实施方案提供了良好悬浮性质、成膜性质和易于控制分散液粘度的结合。
如果本发明方法所用的分散液变干后，则很容易收集粉末和聚合物粘合剂的干燥混合物便于进行处理或回收，而此时最大程度地避免了处理游离粉末会引起的危害。根据聚合物粘合剂和其它添加物质的性质，干燥后混合物的形式是多少硬些的或糊状的固体。
本发明的方法特别适用于处理在粉末状态下呈现一种或多种危害性能的固体。这些危害性能包括对动物或植物的急性或慢性毒性、易燃性和易爆性。
本发明用下列一些实施例来描述，若没有其它说明，则份数和百分比均用重量表示。
实施例1
将1份Sollogen HR(Henkel KGaA的表面活性剂商品名称，双(1-甲基乙基)萘磺酸盐)溶解在53份水中。将45份粉末状态的1，3，5-三丙烯酰基六氢-1，3，5-三吖嗪(TAHT)加入此溶液中，用高剪切混合机搅拌混合物约5分钟。然后加入0.005份RD防沫乳剂(Dow Corning Corp.的一种非离子型硅烷防沫剂的商品名称)，同时轻微搅拌破坏产生的泡沫。然后用高剪切混合机搅拌此混合物，所用的条件务使在其中形成旋涡。将1份Courgel T1225(Courtaulds Chemicals(Holdings)Limited的商品名称，它是水溶性聚合物粘合剂的混合物，由99份羟丙基甲基纤维素(其名义2％溶液在低剪切条件下室温测得的粘度为5-6mPa·s)和1份黄原胶组成)缓慢加入旋涡的外缘处。加完后，轻微搅拌此混合物20分钟直至聚合物粘合剂完全溶解。这样得到的分散液可用水稀释形成含有适用于溶纺纤维素纤维的TAHT的水性溶液。这种分散液有良好的储藏稳定性(抗沉积性)。当将分散液样品干燥后，得到的固体很少有粉尘。相反，不含聚合物粘合剂的TAHT在水中的分散液(即不是本发明的)干燥后，将形成细微的粉尘。
实施例2
在用高剪切混合机搅拌条件下，将1.5份Courgel T1225加入52.5份65-75℃的水中。混合物冷却后，Courgel T1225就溶解在水中(Courgel T1225在热水溶解度很小)。在搅拌条件下，将46份TAHT加入冷却的混合物中，然后加入微量硅烷防沫剂。得到的分散液可用水稀释获得TAHT溶液。
实施例3
重复实施例2，不同的是在高剪切搅拌条件下，将Courgel T1225加入17.5份热水中，获得的分散液迅速用35份冷水稀释，然后搅拌，直至聚合物粘合剂溶解并且混合物冷却下来。

Claims (20)

1.一种制成固体在溶剂中的溶液的方法，其特征在于它包括步骤：(1)先制成一种含有(a)一种液体、(b)以粉末状态分散在该液体中的固体、(c)溶解在该液体中的聚合物粘合剂的分散液，(2)将分散液和溶剂混合，条件是使粉末溶解在溶剂中。
2.根据权利要求1所述的方法，其特征在于所用的液体和溶剂是相同的物质或相同的物质混合物。
3.根据权利要求1或2所述的方法，其特征在于固体是反应性的织物助剂。
4.根据权利要求3所述的方法，其特征在于固体是1，3，5-三丙烯酰基六氢-1，3，5-三吖嗪。
5.根据权利要求1、2、3或4所述的方法，其特征在于液体至少含有水作为其主要组分，聚合物粘合剂是水溶性聚合物。
6.根据权利要求1～5任一所述的方法，其特征在于分散液含有0.1至5.0重量百分数的聚合物粘合剂。
7.根据权利要求1～6任一所述的方法，其特征在于粉末由数均粒度为10至400微米的颗粒组成。
8.根据权利要求1～7任一所述的方法，其特征在于聚合物粘合剂是一种成膜聚合物。
9.根据权利要求1～7的任一所述的方法，其特征在于聚合物粘合剂含有80至99.9重量百分数的成膜聚合物和0.1至20重量百分数的天然多糖胶。
10.根据权利要求9所述的方法，其特征在于成膜聚合物是纤维素醚，其2％溶液在低剪切条件下室温测得的粘度为1至20mPa·s。
11.根据权利要求1～10任一所述的方法，其特征在于分散液中固体含量在20至60重量百分数范围内。
12.根据权利要求1～11任一所述的方法，其特征在于粉末由长宽比为2∶1至100∶1的颗粒组成。
13.一种固体粉末在水性液体中的分散液，其特征在于，它含有溶解在其中的聚合物粘合剂，该聚合物粘合剂含有(a)80至99.9重量份数的水溶性纤维素醚，该纤维素醚的2％溶液在低剪切条件及室温下测得的粘度为1至20mPa·s，(b)0.1至20重量份数的天然多糖胶，该多糖胶的1％溶液在低剪切条件和室温下测得的粘度为1000至10000mPa·s。
14.根据权利要求13所述的分散液，其特征在于组分(a)的含量为90至99.5重量百分数，组分(b)的含量为0.5至10重量百分数。
15.根据权利要求13或14所述的分散液，其特征在于水溶性纤维素醚是中性纤维素醚。
16.根据权利要求13至15的任一条所述的分散液，其特征在于天然多糖胶选自黄原胶、瓜耳胶和刺槐豆胶。
17.根据权利要求13至16的任一条所述的分散液，其特征在于聚合物粘合剂在分散液中的含量为0.1至5.0重量百分。
18.根据权利要求13至17的任一条所述的分散液，其特征在于分散液中固体的含量为20至60重量百分数。
19.根据权利要求13至18的任一条所述的分散液，其特征在于固体是反应性的织物助剂。
20.根据权利要求19所述的分散液，其特征在于固体是1，3，5-三丙烯酰基六氢-1，3，5-三吖嗪。
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