CN101622536A - 测定纸料中疏水有机颗粒的方法 - Google Patents
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Abstract
本发明涉及一种测定纸料滤液中疏水有机颗粒浓度的方法。在该方法中，所述疏水有机颗粒用荧光染料标记，并激发所述颗粒使其发光。检测所标记颗粒发出的光并根据所述荧光强度测定所述颗粒的质量浓度。本发明还涉及所述方法用于测定通过滤水器排出的纸料滤液中疏水有机颗粒总浓度的用途。
Description
本发明涉及一种测定纸料滤液中疏水有机颗粒的方法。
在纸张的生产中，值得关注的是例如分析纸料中污染物颗粒的粒度分布及含量。污染物颗粒通常是疏水的并且发粘的。它们来自例如回收的废纸，并在造纸过程中沉积在机器中。为抑制或消除所述污染物对造纸的不利影响，将固定剂计量加入所述纸料中。这确保污染物结合于纤维素纤维，并极大限度地避免了其在机器中沉积。各种情况下所需固定剂的量则借助于对纸料或白水中污染物颗粒的分析测定。
已知多种测定纸料中污染物颗粒的粒度分布的方法。利用常规测定方法，例如在R.Wilken和J.Strauss，“Grundlegende Untersuchungen überklebende Verunreinigungen im wiederverwendeten Altpapier”，Mitteilungen aus dem Papiertechnischen Institut der PapiertechnischenStiftung，volume 11-12(1984)，第292页之后中所综述的X射线微量分析、红外分光光度法或凝胶渗透色谱法，可在实验室中测定污染物颗粒的种类，即它们的化学组成。还可获得有关浓度和颗粒粒度分布的定性信息。然而，这些方法都具有缺点：它们相当费时费力，因此不适于直接监测生产周期中的污染物变化和添加剂对污染物颗粒与纸料结合的效果。
另一种测定污染物颗粒的颗粒粒度分布的方法记载于 T.
P.Lorencak，A.Gierulski，H.Eipel和D.Horn，“A new laser-optical methodfor counting colloidally dispersed pitch”，Nordic Pulp and Paper ResearchJournal，volume 9(1994)，no.1，第26页之后。在此方法中，污染物颗粒用荧光染料染色并通过流体动力学聚流(hydrodynamic focusing)而分离。然后，将激光投射到含有所述被分离的污染物颗粒的样品中并记录由这些颗粒发射的荧光。从而可从所述荧光信号的强度得出所述颗粒的粒度分布。
WO 92/11534公开了一种测定纸料中树脂颗粒的数量和大小的测量方法：首先制备纸料悬浮液，通过过滤从中分离一种用荧光染料标记的树脂颗粒，然后分离并通过激发使其发射荧光，再检测所述荧光信号并对该信号进行评估以用于对所述树脂颗粒计数和大小测定。所用的荧光染料是N-(正丁基)-4-(正丁基氨基)萘酰亚胺。
EP-A 0 856 731公开了一种测定单个样品中至少两种颗粒类型(Ak)的荧光颗粒(Ti)的粒度分布的方法，所述颗粒(Ti)在所述样品中被分离并且光线沿预定投射方向投射到所述样品中，
测量每种颗粒(Ti)的至少一个散射光强度值(S(Ti))和至少一个荧光光强度值(F(Ti))，
所述颗粒(Ti)基于其在三维空间(R)的区域(Bk)内的值对(S(Ti)，F(Ti))的位置各自对应于一种颗粒类型(Ak)，所述位置由所述散射光强度值(S(Ti))、荧光强度值(F(Ti))和所述值对(S(Ti)，F(Ti))的频率限定，其中对应于颗粒类型(Ak)，每个区域(Bk)具有至少一个所述空间(R)中值对(S(Ti)，F(Ti))频率的局部最大值，
测定每种颗粒类型(Ak)的荧光强度值(F(Ti))的相对频率，
每种颗粒类型(Ak)的相对颗粒粒度分布由所述相应颗粒类型(Ak)的荧光强度值(F(Ti))的相对频率计算出，
借助区域(Bk)在所述三维空间(R)中的位置，各个颗粒类型(Ak)的相对颗粒粒度分布被相对于彼此标准化，从而形成所有颗粒类型(Ak)的颗粒(Ti)的共同相对颗粒粒度分布(common relative particle size distribution)，所述位置由所述散射光强度值(S(Ti))、荧光强度值(F(Ti))和所述值对(S(Ti)，F(Ti))的频率限定。
此方法特别用于测定纸料中或造纸机白水中疏水污染物颗粒的颗粒粒度分布，并用于通过产生对应于或分配给所述共同相对颗粒粒度分布的控制信号并基于该控制信号测定所需固定剂的量从而控制向纸料中固定剂的计量加入。
WO 06/122921公开了一种测定纸料中天然的和/或合成的施胶剂(size)的施胶剂浓度、颗粒大小和颗粒粒度分布的方法：将包含所述施胶剂颗粒的样品用荧光染料染色，将样品中的颗粒分离，将光线投射到样品上，且检测样品发射的散射光和/或荧光并评估接收的信号。该方法用于测定造纸过程中纸料或造纸机白水中的反应性施胶剂的颗粒粒度分布。
在上述方法中，待测定的颗粒总是被分离的。然而，各种颗粒的计数成本较高。
本发明的目的是提供另一种测量纸料滤液中疏水性颗粒质量浓度的测定方法。
根据本发明，此目的可通过一种测定纸料滤液中疏水有机颗粒的浓度的方法实现，其中所述疏水有机颗粒用荧光染料标记，然后激发所述颗粒使其发光，检测所标记颗粒发出的光并由所述荧光强度确定所述颗粒的质量浓度。
疏水有机颗粒是，例如，纸料中存在的细碎污染物如胶粘物、白树脂(white pitch)和树脂，以及施胶剂。所述污染物大体上包括分散的疏水物质，其为例如纸张涂料的粘合剂残余物或为胶粘剂。所述污染物的颗粒大小为例如0.5-100μm。
合适的施胶剂是天然的和/或合成的施胶剂，如反应性施胶剂、松香施胶剂、改性的松香施胶剂或具有胶粘作用的聚合物分散体。所述施胶剂为分散在水中并且颗粒大小为例如0.5-100μm、优选为1μm-20μm的化合物。
最重要的纸用反应性施胶剂为烷基双烯酮(AKD)和烯基琥珀酸酐。它们用作生产纸张、纸板和卡纸板的工程施胶剂(masseleimungsmittel)。这些物质基本上是C14-至C22-烷基双烯酮，如十八烷基双烯酮、十六烷基双烯酮、二十二烷基双烯酮、油基双烯酮以及所述双烯酮的混合物。它们例如通过在阳离子淀粉和阴离子分散剂的存在下、在剪切力作用下于水中乳化而制备，参见US 3,223,544和US 3,130,118。由于阳离子淀粉相对阴离子分散剂过量，这样制备的AKD分散体具有阳离子电荷。
烷基双烯酮也可与其他施胶剂一起使用。例如WO 94/05855公开了将烷基双烯酮分散于由被消化的阳离子淀粉的水悬浮液和细碎聚合物水分散体(其为一种纸用施胶剂)形成的混合物中。得到的混合物被用作纸用施胶剂。此外，水性阴离子AKD分散体也是已知的，并且其可通过例如将AKD在作为惟一稳定剂的阴离子分散剂的存在下分散于水中获得，参见WO 00/23651。
聚合物施胶剂在例如JP-A 58/115 196、EP-B 0257 412和EP-B 0 276770中有所记载。它们基本为在淀粉或降解淀粉的存在下制备的共聚物水性分散体。合适的共聚物为，例如，苯乙烯和/或丙烯腈与丙烯酸酯的共聚物。
烯基琥珀酸酐同样用作工业上生产纸和纸产品的工程施胶剂。这种施胶剂的实例为4-、5-、6-、7-和8-十六烯基琥珀酸酐异构体、癸烯基琥珀酸酐、辛烯基琥珀酸酐、十二碳烯琥珀酸酐和正十六碳烯基琥珀酸酐，同样参见C.E.Farley和R.B.Wasser，The Sizing of Paper，Second Edition，(3)，Sizing With Alkenyl Succinic Anhydride，TAPPI PRESS，1989，ISBN0-89852-051-7。
合适的天然施胶剂为松香施胶剂和经化学改性的松香施胶剂，参见E.Strazdins，Chapter 1，“Chemistry and Application of Rosin Size”于W：F.Reynolds(Ed.)，“The Sizing of Paper”，Second Edition，Tappi Press(Atlanta，USA)，1989，第1至31页(ISBN 0-89852-051-7)。
用于疏水颗粒的整体定量测定的测量在例如荧光分光光度计中进行。本研究使用Hitachi荧光分光光度计(Hitachi F4010)。具有低固有吸光度的透明样品优选以90度放置测量，其中激发光线垂直于放置待测样品的小孔的孔壁入射。所发出的光线以与所述激发光线成90度的角度测量。为研究混浊溶液和分散体，选择正面放置，其中所述激发光线以例如45度投射在所述孔壁上且反射光线以与所述激发光线成90度的角度从样品发出并被分析。所述反射光线是孤立的。
将包含污染物和/或施胶剂的样品用至少一种荧光染料染色。合适的染料的实例为：
N-(正丁基)-4-(正丁基氨基)-萘酰亚胺(Fluorol 7GA)，
Color Index(C.l.)40662号染料(Celluflor)，
C.l.45400号染料(Eosin B)，
3，3-乙氧基二碳花青碘，
8-羟基-1，3，6-三磺酸芘的三钠盐，
6-硝基-1，3，3-三甲基-[2H]-1-苯并吡喃-2，2-吲哚(Merocyanin 540)，
2-[6-(二乙基氨基)-3-二乙基亚氨基-3H-呫吨-9-基)苯甲酸(若丹明B)。
特别优选使用的荧光染料为N-(正丁基)-4-(正丁基氨基)萘酰亚胺。
纸料滤液中还存在纤维素纤维以及如果合适无机颜料。这些物质不被所述荧光染料染色，从而不会干扰测量。用荧光染料标记所述污染物和施胶剂所需要的作用时间为，例如，2-14分钟、优选2-5分钟。为了简化分析方法并获得可重复的结果，具体指定某一反应时间如5分钟作为染色时长是有利的。
优选使用至少一种荧光染料的乙醇溶液对待测样品进行染色。溶解于乙醇中的荧光染料的浓度为，例如，10-40mg/l。所述污染物和/或施胶剂的浓度为，例如，0-20mg/l。
对多种聚合物颗粒(市售可得的已知可作为纸张涂料粘合剂的聚合物分散体，例如S360D和D718，被用于此目的)的研究表明在聚合物颗粒的质量浓度和所测荧光强度之间存在线性关系。在污染物和/或施胶剂的浓度为0-0.1g/l的范围内，可通过上述至少一种荧光染料的标记并借助于如此标记的颗粒的荧光强度的测定进行污染物和/或施胶剂的定量质量分析。在所述浓度范围中，在聚合物颗粒的质量浓度和所述荧光强度之间实际存在线性关系。如此，可快速获得聚合物颗粒总质量的定量分析。然而，在不同聚合物颗粒之间进行区分是不可能的。
本发明的测量方法特别适用于快速试验以测定操作助剂的效力。因此所述测量方法用于测定由滤水器(wire)排出得到的纸料滤液中疏水有机颗粒的总浓度。其特别适于用作造纸过程中的在线测量方法。
借助于此测量方法，可实现例如对正在进行的造纸过程中添加污染物控制剂和/或施胶剂的控制。一种已知的污染物控制剂为，例如，水解程度例如为60-95％的水解聚乙烯甲酰胺。其在抄纸(sheet formation)前作为固定剂加入到所述纸料中。如果在正在进行的造纸过程中对白水进行分析，可借助本发明的测量方法测定其中的污染物浓度，并可调整部分水解的聚乙烯甲酰胺向纸料中的计量加入从而使所述白水中的污染物含量尽可能低。所述污染物被，例如，所添加到纤维素纤维中的部分水解的聚乙烯甲酰胺结合。
实施例
一种包含8g/l的TMP纸浆和0.16g/l
D718(一种基于苯乙烯和丁二烯的粘合剂的水分散体)的胶粘体系用作示范物质，其通过先将500ml此混合物置于烧杯中并加入5ml水解程度为83％且K值为61的水解聚乙烯甲酰胺作为固定剂制备。所述K值根据H.Fikentscher，Cellulose-Chemie，volume 13，58-64和71-74(1932)，在温度为25℃且聚合物浓度为0.5重量％的浓度为5％的氯化钠水溶液中测定。在所述固定剂作用于所述纸料5分钟后，将混合物在一个动态滤水保留仪(dynamicdrainage jar)中形成纸张并排出，收集前100ml滤液。将1ml荧光染料N-(正丁基)-4-(正丁基氨基)萘酰亚胺(7GA)的乙醇溶液加入到25ml所述滤液中，将样品充分混合并在染色5分钟后用荧光分光光度计(Hitachi F4010)以正面放置测定。其中激发间隙和发射间隙的间隙宽度都为5nm。所述入射光的波长为442nm，并在500nm下测量荧光强度。评估根据之前得到的浓度为0至0.05g/l的
D718所对应的胶粘体系的校准曲线进行。测得滤液中胶粘部分为浓度为0.01g/l的
D718。此数值对应的
D718的保留量占TMP纸浆的93.7％。
Claims (5)
1.一种测定纸料滤液中疏水有机颗粒浓度的方法，其中所述疏水有机颗粒用荧光染料标记，然后激发所述颗粒使其发光，检测所标记颗粒发出的光并由所述荧光强度确定所述颗粒的质量浓度。
2.权利要求1的方法，其中所用荧光染料为N-(正丁基)-4-(正丁基氨基)萘酰亚胺。
3.权利要求1或2的方法用于测定通过滤水器排出的纸料滤液中疏水有机颗粒总浓度的用途。
4.权利要求1或2的方法用作造纸过程中在线测量方法的用途。
5.权利要求4的用途，其中所述测量方法用于在正在进行的造纸过程中控制污染物控制剂和/或施胶剂的添加。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104515757A (zh) * | 2013-09-29 | 2015-04-15 | 艺康美国股份有限公司 | 利用荧光染料控制疏水性污染物的方法 |
| CN107615042A (zh) * | 2015-06-26 | 2018-01-19 | 栗田工业株式会社 | 树脂分析方法以及树脂处理方法 |
| CN110914496A (zh) * | 2017-06-30 | 2020-03-24 | 凯米拉公司 | 纸浆质量监测 |
| CN113330291A (zh) * | 2018-12-28 | 2021-08-31 | 凯米拉公司 | 纸浆工艺中的疏水性组分的监测和控制 |
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| US20090260767A1 (en) * | 2003-04-14 | 2009-10-22 | Every Penny Counts, Inc. | Use of hydrophobic dyes to monitor hydrophobic contaminants in a papermaking process |
| US20130078730A1 (en) * | 2011-09-23 | 2013-03-28 | Michael J. Murcia | Method for monitoring and control of a wastewater process stream |
| US20100236732A1 (en) * | 2009-03-17 | 2010-09-23 | Alessandra Gerli | Use of fluorescence to monitor hydrophobic contaminants in a papermaking process |
| US9562861B2 (en) * | 2011-04-05 | 2017-02-07 | Nalco Company | Method of monitoring macrostickies in a recycling and paper or tissue making process involving recycled pulp |
| US10139385B2 (en) * | 2013-08-12 | 2018-11-27 | Ecolab Usa Inc. | Method of tracing chemical quantities using encapsulated fluorescent dyes |
| KR101960350B1 (ko) * | 2015-06-17 | 2019-03-20 | 주식회사 엘지화학 | 폴리프로필렌 수지 조성물 및 이로 피복된 케이블 |
| EP3714256B1 (en) | 2017-11-21 | 2023-07-26 | Solenis Technologies, L.P. | Method of measuring hydrophobic contaminants in a pulp slurry or a papermaking system |
| DE102020007953A1 (de) | 2020-12-29 | 2022-06-30 | Wasiliki Tsalastra-Greul | Verfahren zur Bestimmung des Kunststoffpartikelgehalts mit hydrophobem Farbstoff |
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| US12284A (en) * | 1855-01-23 | Fibe-engine | ||
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| NL131880C (zh) * | 1958-12-24 | |||
| US3223544A (en) * | 1963-03-19 | 1965-12-14 | American Cyanamid Co | Manufacture of cationic paper sizing ketene dimer emulsions |
| DE4040463A1 (de) * | 1990-12-18 | 1992-06-25 | Basf Ag | Messverfahren zur bestimmung von harzteilchen in papierstoffen |
| EP0703451A3 (en) * | 1994-09-26 | 1998-07-29 | Nalco Chemical Company | Monitoring process fluids in papermaking systems |
| US6372085B1 (en) * | 1998-12-18 | 2002-04-16 | Kimberly-Clark Worldwide, Inc. | Recovery of fibers from a fiber processing waste sludge |
| WO2003020808A1 (de) * | 2001-09-03 | 2003-03-13 | Basf Aktiengesellschaft | Verstärkung der wirkung von optischen aufhellern mit hilfe von polymeren |
| US20060246595A1 (en) * | 2005-05-02 | 2006-11-02 | Banks Rodney H | Method for using an all solid-state fluorometer in monitoring and controlling chemicals in water |
| MX2008009237A (es) * | 2006-01-18 | 2008-09-22 | Cascades Canada Inc | Metodo para medir contaminantes hidrofobicos en la pulpa de papel. |
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| CN104515757A (zh) * | 2013-09-29 | 2015-04-15 | 艺康美国股份有限公司 | 利用荧光染料控制疏水性污染物的方法 |
| CN107615042A (zh) * | 2015-06-26 | 2018-01-19 | 栗田工业株式会社 | 树脂分析方法以及树脂处理方法 |
| TWI689718B (zh) * | 2015-06-26 | 2020-04-01 | 日商栗田工業股份有限公司 | 樹脂分析方法及樹脂處理方法 |
| CN110914496A (zh) * | 2017-06-30 | 2020-03-24 | 凯米拉公司 | 纸浆质量监测 |
| US11692312B2 (en) | 2017-06-30 | 2023-07-04 | Kemira Oyj | Pulp quality monitoring |
| CN113330291A (zh) * | 2018-12-28 | 2021-08-31 | 凯米拉公司 | 纸浆工艺中的疏水性组分的监测和控制 |
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| ATE553375T1 (de) | 2012-04-15 |
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