CN1238600C - Method for recycling pulp rejects - Google Patents
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- CN1238600C CN1238600C CNB02809641XA CN02809641A CN1238600C CN 1238600 C CN1238600 C CN 1238600C CN B02809641X A CNB02809641X A CN B02809641XA CN 02809641 A CN02809641 A CN 02809641A CN 1238600 C CN1238600 C CN 1238600C
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/01—Waste products, e.g. sludge
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Abstract
Description
技术领域
本发明涉及对纸张、纸板和卡片制备过程中的除渣器排出物的再循环方法，以及所述再循环的除渣器排出物在造纸的纸浆中或造纸工业涂布浆液中的用途。The present invention relates to a process for the recycling of cleaner effluent from paper, board and card making processes and the use of said recycled cleaner effluent in pulp for papermaking or in coating slips for the paper industry.
背景技术 Background technique
在纸张制备中，还将原料(即木浆、木材、精细的草浆或破布浆)与再浆化的半成品纸浆、填料和颜料混合，以便取得密实的表面并因此改善纸张的性能，尤其是白度、不透明和适印性。In paper production, raw materials (i.e. wood pulp, wood, fine straw or rag pulp) are also mixed with repulped semi-finished pulp, fillers and pigments in order to obtain a dense surface and thus improve the properties of the paper, especially are whiteness, opacity and printability.
几乎所有的纸张，尤其是印刷纸和书写纸均掺有填料，这些填料提供均匀的成形、改善的柔软度、白度和触觉等。这些填料，通常称为“灰分”，这是因为在燃烧分析中它们以灰分的形式保留，其被添加至纤维悬浮液中或在涂布步骤中施用。Almost all papers, especially printing and writing papers, incorporate fillers that provide uniform formation, improved softness, whiteness, and tactility, among others. These fillers, often referred to as "ash" because they remain in the form of ash in combustion analysis, are added to the fiber suspension or applied during the coating step.
非涂布纸包含高达35重量％的填料，涂布纸包含25-50重量％的填料。填料的用量主要取决于纸张预定的用途。高加填纸具有较低的强度和较差的施胶性能。Uncoated papers contain up to 35% by weight of fillers, coated papers contain 25-50% by weight of fillers. The amount of filler depends mainly on the intended use of the paper. Highly filled papers have lower strength and poorer sizing properties.
在纸浆中的填料含量通常在5-35重量％之间，并且由原始颜料或再循环的涂布颜料组成，所述再循环的涂布颜料可以得自涂布残余物或涂布排出物。除了对增白纸张很重要的填料白度之外，填料粒径也起着重要的作用，这是因为粒径对纸张的加填效率和物理性能特别是孔隙性有着很大的影响。添加至纤维悬浮液中的填料约有20-80％保留在纸张中。The filler content in the pulp is generally between 5 and 35% by weight and consists of virgin pigments or recycled coating pigments which may be obtained from coating residues or coating effluents. Besides filler whiteness, which is important for whitening paper, filler particle size also plays an important role, because particle size has a great influence on paper filling efficiency and physical properties, especially porosity. About 20-80% of the filler added to the fiber suspension remains in the paper.
以消耗量为衡量标准，现今作为填料和涂布颜料下列产品是相当重要的：高岭土、碳酸钙、沉淀碳酸钙(PCC)、人造硅酸铝和水合氧化物、二氧化钛、缎光白、滑石和硅酸钙。In terms of consumption, the following products are today of considerable importance as fillers and coating pigments: kaolin, calcium carbonate, precipitated calcium carbonate (PCC), artificial aluminum silicates and hydrated oxides, titanium dioxide, satin white, talc and calcium silicate.
在涂覆涂布浆液并干燥后，用刮刀将纸张修平。由此获得的所谓的除渣器(cleaner)排出物(也称为涂布排出物)主要由矿物和纤维组成，并且其还可以占到所生产纸张总量的1-4％。在大多数情况下，它们抛弃在垃圾场。因此，已有人建议使用螺旋挤压机对除渣器排出物进行压缩和压实，以便减小其体积。然而，所获得的待处理的除渣器排出物的总量却没有减少。After the coating slurry is applied and dried, the paper is smoothed with a doctor blade. The so-called cleaner effluent (also called coating effluent) thus obtained consists mainly of minerals and fibers, and it can also account for 1-4% of the total paper produced. In most cases, they end up in landfills. Therefore, it has been proposed to use a screw extruder to compress and compact the cleaner effluent in order to reduce its volume. However, there is no reduction in the total amount of cleaner effluent obtained to be processed.
在过去，对除渣器排出物进行处理的另一种可能的情况是利用离心除渣器对其进行部分处理，以便一方面分离纤维和/或涂布颜料和填料，另一方面至少部分地将它们重新利用。Another possibility in the past for the treatment of the cleaner effluent was to partially treat it with a centrifugal cleaner in order to separate fibers and/or to coat pigments and fillers on the one hand and at least partially Repurpose them.
因此，本发明的目的是提供一种除渣器排出物特别是离心除渣器的排出物的新的环境友好的处理方案，并使其能够尽可能完全地再循环。It is therefore an object of the present invention to provide a new environmentally friendly treatment solution for cleaner effluents, in particular centrifugal cleaner effluents, and to enable as complete a recycling as possible.
特别是，本发明的目的在于提供一种对除渣器排出物进行再循环的方法，该方法同时还可以节省能源成本和原料成本、运输费用以及倾倒成本。In particular, the object of the present invention is to provide a method for recycling the effluent from a cleaner which simultaneously saves energy and raw material costs, transport costs and dumping costs.
根据本发明，在纸张、纸板和卡片的制备过程中，通过对除渣器排出物、尤其是离心除渣器排出物的再循环方法实现了上述目的，所述方法的特征在于：将包含纤维、涂布颜料和/或填料的除渣器排出物研磨至希望的粒径分布，任选地添加水、涂布颜料、新鲜填料和/或填料浆液；并作为原料用于纸浆和/或涂布浆液。According to the invention, the above-mentioned objects are achieved by a process for the recycling of effluent from a cleaner, in particular from a centrifugal cleaner, during the production of paper, board and card, said method being characterized in that the fibers containing , coating pigments and/or fillers are ground to the desired particle size distribution, optionally with the addition of water, coating pigments, fresh fillers and/or filler slurries; and used as raw material for pulp and/or coating Cloth slurry.
除渣器排出物(通常为固体)包含有价值的原料，其通过本发明的方法能够回收，并且在研磨之后能够再循环至造纸的各个过程中。尤其是从制备涂布纸或卡片的造纸厂得到的除渣器排出物包含大量涂布颜料絮片体。涂层的厚度越厚，通过现有技术的技术回收絮片体就越困难。双面涂布级或涂布卡片级在本发明中可以作为具体的例子提及。造纸工业的另一类是SC-纸张的生产工厂，其通过除渣器排出物丢失大量的填料。The cleaner effluent, usually solid, contains valuable raw material which can be recovered by the process of the present invention and, after grinding, can be recycled to the various processes of papermaking. Especially the cleaner effluent from a paper mill producing coated paper or card contains a large amount of coating pigment flakes. The thicker the coating, the more difficult it is to recover the flakes by prior art techniques. Double-side coated grades or coated card grades may be mentioned as specific examples in the present invention. Another category in the paper industry is SC-paper production plants, which lose large amounts of filler through the cleaner effluent.
现在，借助本发明，对除渣器排出物进行研磨，并且任选地将其与水、涂布颜料、填料和/或填料浆液混合。然后将除渣器排出物浆液或研磨的粉末再循环至造纸过程中，用作纸浆和/或涂布浆液。Now, with the present invention, the cleaner effluent is ground and optionally mixed with water, coating color, filler and/or filler slurry. The cleaner effluent slurry or ground powder is then recycled to the papermaking process for use as pulp and/or coating slurry.
在对除渣器排出物进行仔细监测时，可以发现填料成分、涂布颜料絮片体、纤维悬浮液残留物(如纤维团块或碎块)，以及外来杂质(例如沙子)。Filler components, coating pigment flakes, fiber suspension residues such as fiber clumps or pieces, and foreign matter such as sand can be found when carefully monitoring the cleaner effluent.
在对除渣器排出物进行研磨之后，除渣器排出物的粒子大小分布基本上与涂布颜料、填料或填料/颜料浆液的原始分布相同。因此，通过本发明，能够回收除渣器排出物总量的95％以上，甚至全部回收，并再循环至生产过程中。After milling the cleaner effluent, the particle size distribution of the cleaner effluent is substantially the same as the original distribution of the coated pigment, filler or filler/pigment slurry. Therefore, by means of the present invention, more than 95% or even all of the total effluent from the cleaner can be recovered and recycled to the production process.
例如，将根据本发明处理的除渣器排出物用作填料，借此使新鲜填料或颜料的消耗量明显降低。For example, the cleaner effluent treated according to the invention is used as filler, whereby the consumption of fresh filler or pigment is significantly reduced.
根据本发明，对除渣器排出物的研磨优选安排在通常的离心除渣器的若干阶段中最后一段的下游的离心除渣器系统中。从该增加的除渣器系统得到的浆料被再循环至先前的阶段中，并使残余量的除渣器排出物形成最终的排出物。According to the invention, the grinding of the cleaner effluent is preferably arranged in a centrifugal cleaner system downstream of the last of several stages of a conventional centrifugal cleaner. Slurry from this added cleaner system is recycled to the previous stage and the residual amount of cleaner effluent forms the final effluent.
在现存的除渣器系统中，最简单的应用范围包括：在倒数第二的除渣器阶段后面安排研磨，并将最后的净化过程用作最终阶段。In existing cleaner systems, the simplest scope of application consists of arranging grinding after the penultimate cleaner stage and using the final cleaning process as the final stage.
当进行本发明的方法时，业已发现，涂布颜料絮片体的粒径分布已经得到改良，并且已经达到颜料颗粒的初始分布。这可由细小颗粒，尤其是从不同分布的细小颗粒的量看出。纤维结被提取出并明显地得到了精制。When carrying out the method of the present invention, it has been found that the particle size distribution of the coated pigment flakes has been improved and the original distribution of pigment particles has been achieved. This can be seen from the amount of fine particles, especially from the different distribution of fine particles. Fibrous knots are extracted and visibly refined.
在造纸中，对于纸浆或涂布浆液的制备，通常采用粉末形式或固体含量优选30-85重量％的浓缩浆液形式的填料和涂布颜料。新鲜的填料和颜料通常由厂家以浆液或粉末(具备希望的白度和粒度分布)的形式提供。In papermaking, fillers and coating pigments are generally employed in powder form or in the form of concentrated slurries with a solids content of preferably 30-85% by weight for the preparation of pulp or coating slurries. Fresh fillers and pigments are usually supplied by the manufacturer in the form of slurries or powders (with the desired whiteness and particle size distribution).
在除渣器排出物处理过程中，肯定要分离并丢掉由碎块、砂粒及其他杂质组成的粗杂质成分。为此，通常采用多级离心式除渣器。如此获得的筛余物由纤维、填料、颜料、细砂、黑色颗粒和填料和颜料的聚集体、或颜料、纤维和填料组成。″填料″通常表示在纸浆中使用的细颗粒；″颜料″表示在涂料中使用的细颗粒。During cleaning effluent treatment, it is imperative to separate and discard the coarse foreign matter component consisting of debris, grit and other impurities. For this reason, multistage centrifugal slag cleaners are usually used. The sieve thus obtained consists of fibers, fillers, pigments, fine sand, black particles and aggregates of fillers and pigments, or pigments, fibers and fillers. "Filler" generally means fine particles used in pulp; "pigment" means fine particles used in paint.
显而易见的可用于分离除渣器排出物中不希望的内含物的已知方法是：絮凝和沉积、过滤、筛选和/或离心分离。在这种情况下，通常存在不同颜料的混合物，其中经常包含高岭土、碳酸钙和滑石。在分离过程中，由于絮凝和电荷逆转，经常形成聚集体；根据本发明现在可以对它们进行研磨。The obvious known methods that can be used to separate the unwanted content in the cleaner effluent are: flocculation and sedimentation, filtration, screening and/or centrifugation. In this case, there is usually a mixture of different pigments, which often contain kaolin, calcium carbonate and talc. During separation, aggregates are often formed due to flocculation and charge reversal; they can now be ground according to the invention.
根据本发明，可以使用常用的干式研磨机或湿式研磨机，尤其是例如具有700-5000L或更大容量的搅拌球磨机(agitator ball mill)，能够连续或不连续地将其研磨成粉末或浆液。所用研磨介质，优选是研磨球，尤其是具有1-4毫米直径的研磨球。According to the present invention, it is possible to use conventional dry or wet mills, especially agitator ball mills, for example with a capacity of 700-5000 L or more, capable of grinding continuously or discontinuously into powder or slurry . The grinding media used are preferably grinding balls, especially grinding balls with a diameter of 1-4 mm.
为进行处理，通常使用用于分离杂质(球状破碎物、分离材料、铁锈等等)的筛，优选弧形筛(sieve bends)。在研磨过程中，使用激光测量仪来测量和控制研磨的细度，并使用计算机对搅拌球磨机进行控制。For the treatment, sieves, preferably sieve bends, are generally used for separating impurities (spheroidal crush, separated material, rust, etc.). During the grinding process, a laser measuring instrument is used to measure and control the grinding fineness, and a computer is used to control the stirring ball mill.
因此，为制备新的涂布浆液，或者还任选地将其用于纸浆，需要通过本身已知的方法来提高白度。优选对聚集体进行解离，这些聚集体通过形成刀口痕纹在刮刀处对涂布浆液的流动性产生负面影响，并由此对涂层产生负面影响。在研磨过程中分散助剂、填料和颜料的使用将降低这些材料的总消耗。Therefore, in order to prepare new coating slips, or optionally also use them for pulp, it is necessary to increase the brightness by methods known per se. Preference is given to dissociating aggregates which, by forming knife-edge marks, have a negative effect on the flowability of the coating slip and thus on the coating at the doctor blade. The use of dispersing aids, fillers and pigments in the milling process will reduce the overall consumption of these materials.
在除渣器排出物中，填料和/或颜料与纤维的比例可在大范围内变化。根据本发明，特别优选的是使用任选地富含填料和/或涂布颜料的除渣器排出物，以固体含量计，所述浓度范围在5-90重量％之间，特别是在30-70重量％之间。因此，纤维含量，或填料和/或涂布颜料的含量可以很大范围内改变，例如在1-99重量％或在99-1重量％之间，特别是在30-70重量％之间。在本发明中“富含”尤其包含添加新鲜的填料和/或新鲜的颜料。The filler and/or pigment to fiber ratio in the cleaner effluent can vary widely. According to the invention, it is particularly preferred to use the cleaner effluent, optionally enriched with fillers and/or coating pigments, in a concentration range between 5 and 90% by weight, in particular at 30%, based on the solids content. -70% by weight. Thus, the fiber content, or the filler and/or coating pigment content can vary widely, for example between 1-99% by weight or between 99-1% by weight, especially between 30-70% by weight. "Enriched" in the context of the present invention includes especially the addition of fresh fillers and/or fresh pigments.
因此，根据本发明，优选在研磨之前、之后和/或期间，将高岭土、天然或沉淀碳酸钙、人造或天然硅酸铝和氧化物水合物、二氧化钛、缎光白、白云石、云母、金属絮片体(特别是铝的絮片体)、皂土、金红石、氢氧化镁、石膏、层状硅酸盐、滑石、硅酸钙及其他岩石和泥土用作新鲜的颜料和/或新鲜的填料。Therefore, according to the invention, kaolin, natural or precipitated calcium carbonate, artificial or natural aluminum silicates and oxide hydrates, titanium dioxide, satin white, dolomite, mica, metal Flakes (especially of aluminum), bentonite, rutile, magnesium hydroxide, gypsum, phyllosilicates, talc, calcium silicates and other rocks and earths used as fresh pigments and/or fresh filler.
所述新鲜的颜料或新鲜的填料优选是，在除渣器排出物和任选的常用研磨助剂和/或分散助剂存在下，以粉末、包含含水新鲜颜料和/或新鲜填料的浆液的形式使用，从而给出固体含量例如在30-85重量％之间，尤其是在40-75重量％之间的浆液。在根据本发明的优选方法中常用研磨助剂和/或分散助剂添加至固体含量为30-85重量％的浆液中。The fresh pigment or fresh filler is preferably in the form of a powder, a slurry comprising aqueous fresh pigment and/or fresh filler in the presence of the cleaner discharge and optionally customary grinding aids and/or dispersing aids form to give a slurry with a solids content of, for example, between 30-85% by weight, especially between 40-75% by weight. In the preferred process according to the invention customary grinding aids and/or dispersing aids are added to slurries having a solids content of 30-85% by weight.
以除渣器排出物计，优选纤维、涂布颜料和/或填料(再循环的或新鲜的)的添加量为1-100重量％。在根据本发明的优选方法中以除渣器排出物计，所述常用的研磨助剂和/或分散助剂的添加量为1-100重量％。Fibers, coating colors and/or fillers (recycled or fresh) are preferably added in an amount of 1 to 100% by weight, based on the cleaner effluent. In a preferred method according to the invention, the customary grinding aids and/or dispersing aids are added in an amount of 1 to 100% by weight, based on the cleaner discharge.
特别优选的是添加水，以便将根据本发明研磨的除渣器排出物用于纸浆流的稀释浆液中。优选使用固体含量为5-50重量％，尤其是为10-20重量％的浆液。因此，在本发明优选的实施方案中，以固体含量计，在1-1000重量％，尤其是100-1000重量％的水的存在下进行研磨。It is particularly preferred to add water in order to use the cleaner effluent ground according to the invention in the dilute slurry of the pulp flow. Preference is given to using slurries with a solids content of 5-50% by weight, especially 10-20% by weight. Therefore, in a preferred embodiment of the invention, grinding is carried out in the presence of 1 to 1000% by weight, especially 100 to 1000% by weight of water, based on the solids content.
优选将除渣器排出物研磨成具有下面粒度分布的浆液或粉末：The cleaner effluent is preferably ground to a slurry or powder having the following particle size distribution:
10-99重量％的颗粒＜1微米，尤其是10-99% by weight of particles < 1 micron, especially
10-95重量％的颗粒＜1微米，10-95% by weight of particles < 1 micron,
其中分别以等效直径计。Among them, the equivalent diameters are used respectively.
根据EP 0 625 611 A1，涂布颜料的粒度分布是已知的，其优选还通过本发明方法进行调节。因此，根据本发明，特别优选将除渣器排出物研磨成具有下面粒度分布的浆液或粉末：The particle size distribution of coating pigments is known from EP 0 625 611 A1, which is preferably also adjusted by the method of the invention. Therefore, according to the invention it is particularly preferred to grind the cleaner effluent to a slurry or powder having the following particle size distribution:
A)95-100重量％的颗粒＜10微米；A) 95-100% by weight of particles < 10 microns;
B)50-100重量％的颗粒＜2微米，尤其是50-95重量％的颗粒＜2微米；B) 50-100% by weight of particles < 2 microns, especially 50-95% by weight of particles < 2 microns;
C)27-95重量％的颗粒＜1微米，尤其是27-75重量％的颗粒＜1微米；和C) 27-95% by weight of particles < 1 micron, especially 27-75% by weight of particles < 1 micron; and
D)0.1-55重量％的颗粒＜0.2微米，尤其是0.1-35重量％的颗粒＜0.2微米；D) 0.1-55% by weight of particles < 0.2 microns, especially 0.1-35% by weight of particles < 0.2 microns;
其中均以颗粒的等效直径计。根据本发明，优选除渣器排出物的研磨在干式研磨机或湿式研磨机中，尤其是在垂直的搅拌球磨机中进行。All of them are calculated by the equivalent diameter of the particles. According to the invention, the grinding of the cleaner effluent is preferably carried out in dry or wet mills, especially in vertical agitated ball mills.
另外，根据本发明，白度和粒度分布可能有大的变动，其特别是可通过研磨方式和时间来加以控制。因此，有可能就地将相对粗的新鲜的填料和水与大量的除渣器排出物混合，以便在研磨之后将该浆液引入纸浆中。同样地，有可能使用少量除渣器排出物，并与新鲜的颜料就地进行精细的研磨，然后将其用作涂布颜料，尤其是预涂层。In addition, according to the invention, large variations in whiteness and particle size distribution are possible, which can be controlled in particular by the type and time of grinding. Thus, it is possible to mix relatively coarse fresh filler and water in situ with a large volume of cleaner effluent in order to introduce this slurry into the pulp after grinding. Likewise, it is possible to use a small amount of cleaner effluent and finely grind it in situ with fresh pigment, which can then be used as coating pigment, especially pre-coat.
正如例如由EP0 625 611 A1已知的那样，尽管根据本发明，在除渣器排出物混合和研磨期间，可以使用本身已知的润湿剂、稳定剂、研磨助剂和分散助剂，但其所需量与现有技术相比明显减少。除渣器排出物中已经含有一定量的根据本发明循环至造纸过程中的所述制剂。As is known, for example, from EP 0 625 611 A1, although according to the invention during mixing and grinding of the cleaner effluent it is possible to use wetting agents, stabilizers, grinding aids and dispersing aids known per se, Its required amount is significantly reduced compared with the prior art. The cleaner effluent already contains a certain amount of said formulation which is recycled to the papermaking process according to the invention.
根据本发明获得的粉末或浆液特别适用于造纸工业，尤其是用于制备纸张涂层的涂料或用于纸浆。当纤维含量较低时，根据本发明研磨的除渣器排出物优选用于涂布浆液中，而当纤维含量高时，优选用于纸浆中。根据本发明，在筛上获得了良好的留着率(retention)。特别优选的是，将根据本发明研磨的除渣器排出物用于制备胶版纸。另外，根据本发明的浆液还适合于制备用于轻质涂布纸、尤其是高涂布速度的涂布浆液，和用于制备轮转(rotary)胶版纸、特别是用于制备轻质涂布的轮转胶版纸、卡片和特种纸(如标签、壁纸、硅酮基纸张、自-拷贝纸张)的涂层，以及用于凹版印刷纸。因此，根据本发明获得的涂布颜料浆液特别适用于单张(sheet-fed)胶版纸，尤其是用于单张胶版纸的单涂层、单张胶版纸的双涂层：单张胶版纸预涂层和单张胶版纸顶涂层；用于轮转胶版纸，尤其是用于LWC轮转胶版纸单涂层、轮转胶版纸的双涂层：轮转胶版纸预涂层和轮转胶版纸顶涂层；用于凹版印刷纸，尤其是用于LWC凹版印刷纸单涂层、LWC凹版印刷纸双涂层：凹版印刷纸预涂层和凹版印刷纸顶涂层；用于卡片，尤其是卡片双涂层：卡片预涂层和卡片顶涂层；以及用于特种纸，尤其是用于标签和软包装。The powders or slurries obtained according to the invention are particularly suitable for use in the paper industry, especially for the preparation of coatings for paper coatings or for pulp. The cleaner effluent ground according to the invention is preferably used in coating slurries when the fiber content is low and in paper pulp when the fiber content is high. According to the invention, a good retention on the sieve is obtained. It is particularly preferred to use the cleaner effluent ground according to the invention for the production of offset paper. In addition, the size according to the invention is also suitable for the preparation of coating slips for light weight coated paper, especially for high coating speeds, and for the production of rotary offset paper, especially for the production of light weight coated Coating of web-offset paper, card and specialty paper (such as labels, wallpaper, silicone-based paper, self-copying paper), as well as for gravure printing paper. Therefore, the coating pigment slurry obtained according to the present invention is particularly suitable for use in sheet-fed offset paper, especially for single-coating of sheet-fed offset paper, double-coating of sheet-fed offset paper: sheet-fed offset paper Pre-coating and sheetfed topcoat; for web-offset, especially for LWC web-offset single-coat, web-offset double-coating: web-offset pre-coating and web-offset topcoat Layer; for gravure paper, especially for LWC gravure paper single coat, LWC gravure paper double coat: gravure paper pre-coat and gravure paper top coat; for cards, especially card double Coatings: Card pre-coats and card top coats; and for specialty papers, especially for labels and flexible packaging.
该方法给使用本发明制备的颜料浆液提供了机会，而且不使原纸、涂料的质量，尤其是用其制得的最终产品的质量受到损失。This method offers the opportunity to use the pigment slurries prepared according to the invention without compromising the quality of the base paper, the coating and especially the quality of the final product produced therewith.
在下文中，为了进行说明，给出了可根据本发明获得的一些涂布配方(所有数值转换成固体的重量份数(atro/活性成分))。填料和/或颜料浆液的用量可部分或全部地被相应用量的根据本发明研磨的除渣器排出物所替代。In the following, for illustration, some coating formulations obtainable according to the invention are given (all values converted into parts by weight of solids (atro/active ingredient)). The amount of filler and/or pigment slurry can be partially or completely replaced by a corresponding amount of cleaner effluent ground according to the invention.
1.单张(sheet-fed)胶版纸1. Sheet-fed offset paper
1.1单张(sheet-fed)胶版纸单涂层1.1 Sheet-fed offset paper single coating
70重量份的市售CaCO3(90型)70 parts by weight of commercially available CaCO 3 (type 90)
30重量份的市售粘土(优质，例如US No.1)30 parts by weight of commercially available clay (high quality, such as US No.1)
11重量份的市售乳液(丙烯酸酯)11 parts by weight of commercially available emulsion (acrylate)
0.6重量份的市售羧甲基纤维素(CMC)0.6 parts by weight of commercially available carboxymethylcellulose (CMC)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
0.5重量份的市售硬脂酸钙0.5 parts by weight of commercially available calcium stearate
固体含量： 64％Solid content: 64%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
1.2单张(sheet-fed)胶版纸双涂层1.2 Single (sheet-fed) offset paper double-coated
1.2.1单张(sheet-fed)胶版纸预涂层1.2.1 Sheet-fed offset paper pre-coating
100重量份的市售CaCO3(75或60型)100 parts by weight of commercially available CaCO 3 (type 75 or 60)
10重量份的市售乳液10 parts by weight of commercially available emulsion
4重量份的市售淀粉(天然或氧化的玉米或马铃薯淀粉)4 parts by weight commercially available starch (native or oxidized corn or potato starch)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
固体含量： 66％Solid content: 66%
布氏粘度(100/分)： 1100mPa.sBrookfield viscosity (100/min): 1100mPa.s
PH值： 9.0PH value: 9.0
1.2.2单张(sheet-fed)胶版纸顶涂层1.2.2 Sheet-fed offset paper top coat
70重量份的市售CaCO3(90型)70 parts by weight of commercially available CaCO 3 (type 90)
30重量份的市售粘土(优质，例如US No.1)。30 parts by weight of commercially available clay (high quality, such as US No.1).
10重量份的市售乳液(丙烯酸酯)10 parts by weight of commercially available emulsion (acrylate)
0.6重量份的市售羧甲基纤维素(CMC)0.6 parts by weight of commercially available carboxymethylcellulose (CMC)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
0.7重量份的市售硬脂酸钙0.7 parts by weight of commercially available calcium stearate
固体含量： 64％Solid content: 64%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
2.轮转胶版纸2. Rotary offset paper
2.1LWC轮转胶版纸单涂层2.1 LWC web offset paper single coating
50重量份的市售CaCO3(90型)50 parts by weight of commercially available CaCO 3 (type 90)
50重量份的市售粘土(优质/英国粘土)50 parts by weight commercially available clay (premium/English clay)
2重量份的市售淀粉(天然或氧化的玉米或马铃薯淀粉)2 parts by weight commercially available starch (native or oxidized corn or potato starch)
12重量份的市售乳液(XSB)12 parts by weight of commercially available emulsion (XSB)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.7重量份的市售增亮剂(任选的)0.7 parts by weight of commercial brightener (optional)
0.5重量份的市售硬脂酸钙0.5 parts by weight of commercially available calcium stearate
固体含量： 62％Solid content: 62%
布氏粘度(100/分)： 1400mPa.sBrookfield viscosity (100/min): 1400mPa.s
PH值： 8.5PH value: 8.5
2.2轮转胶版纸双涂层2.2 Rotary offset paper double coating
2.2.1轮转胶版纸预涂层2.2.1 Web offset paper pre-coating
100重量份的市售CaCO3(75或60型)100 parts by weight of commercially available CaCO 3 (type 75 or 60)
4重量份的市售淀粉(天然或氧化的玉米或马铃薯淀粉)4 parts by weight commercially available starch (native or oxidized corn or potato starch)
12重量份的市售乳液(XSB)12 parts by weight of commercially available emulsion (XSB)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
固体含量： 66％Solid content: 66%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 9.0PH value: 9.0
2.2.2轮转胶版纸顶涂层2.2.2 Web offset paper top coat
60重量份的市售CaCO3(95型)60 parts by weight of commercially available CaCO 3 (type 95)
40重量份的市售粘土(优质/英国粘土)40 parts by weight commercially available clay (premium/English clay)
10重量份的市售乳液(XSB)10 parts by weight of commercially available emulsion (XSB)
0.6重量份的市售羧甲基纤维素0.6 parts by weight of commercially available carboxymethylcellulose
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
0.5重量份的市售硬脂酸钙0.5 parts by weight of commercially available calcium stearate
固体含量： 64％Solid content: 64%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
3.凹版印刷纸3. Gravure printing paper
3.1LWC凹版印刷纸单涂层3.1 LWC gravure printing paper single coating
70重量份的市售粘土(普通/英国粘土)70 parts by weight of commercially available clay (common/English clay)
30重量份的市售滑石30 parts by weight of commercially available talc
5.0重量份的市售乳液(丙烯酸酯粘合剂)5.0 parts by weight of commercially available emulsion (acrylate adhesive)
0.2重量份的市售增稠剂(合成的)0.2 parts by weight of commercially available thickeners (synthetic)
1.0重量份的市售硬脂酸钙1.0 parts by weight of commercially available calcium stearate
固体含量： 58％Solid content: 58%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
3.2版印刷纸双涂层3.2 printing paper double coating
3.2.1凹版印刷纸预涂层3.2.1 Gravure printing paper pre-coating
100重量份的市售CaCO3(75型)100 parts by weight of commercially available CaCO 3 (type 75)
6.0重量份的市售乳液(丙烯酸酯粘合剂)6.0 parts by weight of commercially available emulsion (acrylate adhesive)
0.3重量份的市售增稠剂(合成的)0.3 parts by weight of commercially available thickener (synthetic)
0.5重量份的市售硬脂酸钙0.5 parts by weight of commercially available calcium stearate
固体含量： 66％Solid content: 66%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 9.0PH value: 9.0
3.2.2凹版印刷纸顶涂层3.2.2 Gravure paper top coating
85重量份的市售粘土(英国粘土)85 parts by weight of commercially available clay (English clay)
15重量份的市售粘土(煅烧粘土)15 parts by weight of commercially available clay (calcined clay)
5.0重量份的市售乳液(丙烯酸酯粘合剂)5.0 parts by weight of commercially available emulsion (acrylate adhesive)
0.2重量份的市售增稠剂(合成的)0.2 parts by weight of commercially available thickeners (synthetic)
0.8重量份的市售硬脂酸钙0.8 parts by weight of commercially available calcium stearate
固体含量： 57％Solid content: 57%
布氏粘度(100/分)： 1300mPa.sBrookfield viscosity (100/min): 1300mPa.s
PH值： 8.5PH value: 8.5
4.卡片4. Cards
4.1卡片双涂层4.1 Card Double Coating
4.1.1卡片预涂层4.1.1 Card pre-coating
100重量份的市售CaCO3(75型)100 parts by weight of commercially available CaCO 3 (type 75)
3重量份的市售淀粉(天然或氧化的玉米或马铃薯淀粉)3 parts by weight commercially available starch (native or oxidized corn or potato starch)
14重量份的市售乳液(XSB)14 parts by weight of commercially available emulsion (XSB)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.5重量份的市售增亮剂(任选的)0.5 parts by weight of commercial brightener (optional)
固体含量： 66％Solid content: 66%
布氏粘度(100/分)： 1000mPa.sBrookfield viscosity (100/min):
PH值： 9.0PH value: 9.0
4.1.2纸板顶涂层4.1.2 Cardboard top coat
50重量份的市售CaCO3(90型)50 parts by weight of commercially available CaCO 3 (type 90)
50重量份的市售粘土(优质/英国粘土)50 parts by weight commercially available clay (premium/English clay)
13重量份的市售乳液(丙烯酸酯)13 parts by weight of commercially available emulsion (acrylate)
2重量份的市售助粘合剂(丙烯酸酯)2 parts by weight of commercially available auxiliary binder (acrylate)
0.8重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.8 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.6重量份的市售硬脂酸钙0.6 parts by weight of commercially available calcium stearate
固体含量： 60％Solid content: 60%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
5.特种纸5. Specialty paper
5.1.标签5.1. Labels
70重量份的市售粘土(普通/英国粘土)70 parts by weight of commercially available clay (common/English clay)
10重量份的市售二氧化钛(金红石)10 parts by weight of commercially available titanium dioxide (rutile)
20重量份的市售CaCO3(90型)20 parts by weight of commercially available CaCO 3 (type 90)
16重量份的市售乳液(XSB)16 parts by weight of commercially available emulsion (XSB)
0.5重量份的市售硬化剂(EH)(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.5 parts by weight of commercially available hardener (EH) (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.6重量份的市售硬脂酸钙0.6 parts by weight of commercially available calcium stearate
固体含量： 60％Solid content: 60%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
5.2软包装5.2 Flexible packaging
80重量份的市售粘土(普通/英国粘土)80 parts by weight of commercially available clay (common/English clay)
20重量份的市售CaCO3(90型)20 parts by weight of commercially available CaCO 3 (type 90)
14重量份的市售乳液(丙烯酸酯)14 parts by weight of commercially available emulsion (acrylate)
0.8重量份的市售羧甲基纤维素0.8 parts by weight of commercially available carboxymethylcellulose
0.5重量份的市售硬化剂(脲醛树脂、三聚氰胺甲醛树脂、环氧树脂)0.5 parts by weight of commercially available hardener (urea-formaldehyde resin, melamine-formaldehyde resin, epoxy resin)
0.6重量份的市售增亮剂(任选的)0.6 parts by weight of commercial brightener (optional)
1.0重量份的市售硬脂酸钙1.0 parts by weight of commercially available calcium stearate
固体含量： 58％Solid content: 58%
布氏粘度(100/分)： 1200mPa.sBrookfield viscosity (100/min): 1200mPa.s
PH值： 8.5PH value: 8.5
实施例Example
将从现有技术的市售造纸机的方法得到的除渣器排出物在15重量％的悬浮液中研磨成粒径＜10微米的浆液，并添加至纸浆流中。Cleaner effluent obtained from a prior art commercial paper machine process was ground to a particle size <10 micron slurry in a 15% by weight suspension and added to the pulp stream.
在研磨装置与根据本发明研磨的除渣器排出物连通之后不久，便可使纸张中灰分增加。The ash content of the paper can be made shortly after the grinding device is connected to the cleaner discharge ground according to the present invention.
由于所述灰分含量增加，因此可减少填料的剂量。由研磨装置，大约以16-18L/min的流量将由研磨的除渣器排出物组成的颜料浆液供至纸浆池(pulp chest)。为将灰分含量保持在预定的恒定值，新鲜填料的用量可从10L/h降至6.0L/h。Due to the increased ash content, the dosage of fillers can be reduced. The pigment slurry consisting of the ground cleaner effluent is fed to the pulp chest from the grinding unit at a flow rate of approximately 16-18 L/min. To keep the ash content at a predetermined constant value, the amount of fresh filler can be reduced from 10L/h to 6.0L/h.
在试验期间，研磨装置的运行没有问题。浆流的灰分含量在通常范围内改变。开始时留着率稍有下降，但在实验过程中将增加至通常值。所节省的新鲜颜料浆液的量约为240L/h。During the test period, the milling device operated without problems. The ash content of the slurry stream varies within a typical range. Retention will drop slightly at first, but will increase to normal values over the course of the experiment. The amount of fresh pigment slurry saved is about 240 L/h.
约10小时的试运行表明：通过本发明的方法，在不损失留着率的情况下，能够再次将处理过的除渣器排出物作为填料用于纸浆中。A test run of about 10 hours showed that the treated cleaner effluent can be used again as filler in pulp by the method of the invention without loss of retention.
有关除渣器排出物浆液组分的说明：A note about the composition of the cleaner effluent slurry:
固体含量：约24.0％Solid content: about 24.0%
颜料比例：约85.0％，以固体含量计Pigment ratio: about 85.0%, based on solid content
纤维比例：约15.0％，以固体含量计Fiber ratio: about 15.0%, based on solid content
Claims (12)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10122331.5 | 2001-05-08 | ||
| DE10122331A DE10122331B4 (en) | 2001-05-08 | 2001-05-08 | Process for recycling and use of rejects |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1524145A CN1524145A (en) | 2004-08-25 |
| CN1238600C true CN1238600C (en) | 2006-01-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB02809641XA Expired - Fee Related CN1238600C (en) | 2001-05-08 | 2002-01-24 | Method for recycling pulp rejects |
Country Status (25)
| Country | Link |
|---|---|
| US (1) | US20040168783A1 (en) |
| EP (1) | EP1313917B1 (en) |
| JP (1) | JP4463480B2 (en) |
| KR (1) | KR100778426B1 (en) |
| CN (1) | CN1238600C (en) |
| AT (1) | ATE266768T1 (en) |
| AU (1) | AU2002235867B2 (en) |
| BG (1) | BG108226A (en) |
| BR (1) | BR0209390A (en) |
| CA (1) | CA2443065C (en) |
| CZ (1) | CZ20033036A3 (en) |
| DE (2) | DE10122331B4 (en) |
| DK (1) | DK1313917T3 (en) |
| ES (1) | ES2201949T3 (en) |
| HU (1) | HUP0400018A3 (en) |
| MX (1) | MXPA03009321A (en) |
| NO (1) | NO20034968D0 (en) |
| PL (1) | PL206622B1 (en) |
| PT (1) | PT1313917E (en) |
| SI (1) | SI1313917T1 (en) |
| SK (1) | SK286317B6 (en) |
| TR (1) | TR200401126T4 (en) |
| UA (1) | UA74639C2 (en) |
| WO (1) | WO2002090651A1 (en) |
| ZA (1) | ZA200307798B (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19627523C1 (en) * | 1996-07-09 | 1997-10-23 | Alpha Calcit Fuellstoff Gmbh | Preparation of filler or pigment coating material for paper, pulp or board from waste sludge |
| EP2014830A1 (en) | 2007-06-22 | 2009-01-14 | Alpha Calcit Füllstoff Gesellschaft mbH | Manufacturing of coating colour dispersions |
| CN103835182B (en) | 2008-04-03 | 2018-11-16 | 英文蒂亚有限责任公司 | The coating composition of printing |
| PT2236545E (en) | 2009-03-30 | 2014-11-06 | Omya Int Ag | Process for the production of nano-fibrillar cellulose gels |
| EP3617400B1 (en) | 2009-03-30 | 2022-09-21 | FiberLean Technologies Limited | Use of nanofibrillar cellulose suspensions |
| GB0908401D0 (en) | 2009-05-15 | 2009-06-24 | Imerys Minerals Ltd | Paper filler composition |
| FI20095692A0 (en) | 2009-06-18 | 2009-06-18 | Upm Kymmene Oyj | Paper product and process for making it |
| EP2386683B1 (en) | 2010-04-27 | 2014-03-19 | Omya International AG | Process for the production of gel-based composite materials |
| PT2386682E (en) | 2010-04-27 | 2014-05-27 | Omya Int Ag | Process for the manufacture of structured materials using nano-fibrillar cellulose gels |
| FI124324B (en) * | 2010-10-18 | 2014-06-30 | Ekokem Palvelu Oy | Treatment of wood containing fraction |
| GB201019288D0 (en) | 2010-11-15 | 2010-12-29 | Imerys Minerals Ltd | Compositions |
| CA2824076A1 (en) | 2012-08-21 | 2014-02-21 | University Of New Brunswick | System and method for reclaiming rejects in sulfite pulping |
| CN104250942B (en) * | 2013-06-25 | 2016-08-24 | 立诚包装有限公司 | Middle-size and small-size packaging paper plant mud reuse technology |
| WO2017064559A1 (en) | 2015-10-14 | 2017-04-20 | Fiberlean Technologies Limited | 3d-formable sheet material |
| US11846072B2 (en) | 2016-04-05 | 2023-12-19 | Fiberlean Technologies Limited | Process of making paper and paperboard products |
| EP3828339B1 (en) | 2016-04-05 | 2023-11-29 | FiberLean Technologies Limited | Paper and paperboard products |
| PL3445900T3 (en) | 2016-04-22 | 2022-07-11 | Fiberlean Technologies Limited | Fibres comprising microfibrillated cellulose and methods of manufacturing fibres and nonwoven materials therefrom |
| CN110694348B (en) * | 2019-10-28 | 2021-08-20 | 海南金海浆纸业有限公司 | System and method for dissociating waste residues of papermaking coating |
Family Cites Families (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4115187A (en) * | 1970-03-31 | 1978-09-19 | Welwyn Hall Research Association | Agglomerated fillers used in paper |
| DE3116905C2 (en) * | 1981-04-29 | 1986-06-26 | J.M. Voith Gmbh, 7920 Heidenheim | Process for waste paper processing and device for carrying out the process |
| DE3148749C2 (en) * | 1981-12-09 | 1984-09-27 | Steinbeis Papier GmbH, 7121 Gemmrigheim | Papers, preferably for sheet-fed printing, made from recycled waste paper, and processes for their production |
| DE3414460A1 (en) * | 1983-12-16 | 1985-10-24 | J.M. Voith Gmbh, 7920 Heidenheim | Arrangement for reprocessing scrap paper |
| DE3345548C2 (en) * | 1983-12-16 | 1986-09-18 | J.M. Voith Gmbh, 7920 Heidenheim | Process and arrangement for processing waste paper |
| EP0183863B2 (en) * | 1984-12-03 | 1991-10-23 | Steinbeis Temming Papier GmbH & Co. | Format paper with a low dust content, process for its manufacture and its use |
| FI85041C (en) * | 1989-01-16 | 1992-02-25 | Enso Gutzeit Oy | Method of bringing pulp onto a paper machine's wire |
| DE4037230A1 (en) * | 1990-11-23 | 1992-05-27 | Voith Gmbh J M | METHOD AND SYSTEM FOR THE PROCESSING OF WASTE PAPER |
| DE4042221A1 (en) * | 1990-12-29 | 1992-07-02 | Pwa Industriepapier Gmbh | FIBER FIBER COMPONENT FOR THE PRODUCTION OF PAPER, WITH THIS PRODUCED PAPER AND THE USE THEREOF AND METHOD FOR THE PRODUCTION OF FIBER COMPONENT AND PAPER |
| US5139652A (en) * | 1990-12-31 | 1992-08-18 | A. Ahlstrom Corporation | Centrifugal cleaner |
| US5390860A (en) * | 1992-05-15 | 1995-02-21 | Tetra Laval Holdings & Finance Sa | Method and apparatus for separating paper fiber and plastics from mixed waste materials and products obtained thereby |
| DE4312463C1 (en) * | 1993-04-16 | 1994-07-28 | Pluss Stauffer Ag | CaCO3 3 -Talkum coating pigment slurry, process for its preparation and its use |
| FI97736C (en) * | 1995-03-07 | 1997-02-10 | Ahlstrom Machinery Oy | Processes and devices for treating filler-containing material, e.g. recycled |
| DE19627523C1 (en) * | 1996-07-09 | 1997-10-23 | Alpha Calcit Fuellstoff Gmbh | Preparation of filler or pigment coating material for paper, pulp or board from waste sludge |
| US6164572A (en) * | 1996-07-26 | 2000-12-26 | Tudahl; Daniel L. | Apparatus and method for recycling gypsum wallboard |
| DE19631150B4 (en) * | 1996-08-01 | 2007-04-19 | Süd-Chemie AG | Process for the removal of printing inks (deinking) of cellulosic print substrates |
| US5882475A (en) * | 1997-03-26 | 1999-03-16 | Ahlstrom Machinery Inc. | Method of recovering fibers from a reject stream generated in a wastepaper treating process |
| FI108779B (en) * | 1999-11-24 | 2002-03-28 | Megatrex Oy | Process for processing filler-containing reject flows at a paper or cardboard factory and using a device |
-
2001
- 2001-05-08 DE DE10122331A patent/DE10122331B4/en not_active Expired - Lifetime
-
2002
- 2002-01-24 AT AT02702307T patent/ATE266768T1/en active
- 2002-01-24 HU HU0400018A patent/HUP0400018A3/en unknown
- 2002-01-24 EP EP02702307A patent/EP1313917B1/en not_active Revoked
- 2002-01-24 JP JP2002587701A patent/JP4463480B2/en not_active Expired - Fee Related
- 2002-01-24 PL PL366987A patent/PL206622B1/en unknown
- 2002-01-24 CA CA002443065A patent/CA2443065C/en not_active Expired - Fee Related
- 2002-01-24 PT PT02702307T patent/PT1313917E/en unknown
- 2002-01-24 CN CNB02809641XA patent/CN1238600C/en not_active Expired - Fee Related
- 2002-01-24 DK DK02702307T patent/DK1313917T3/en active
- 2002-01-24 DE DE50200434T patent/DE50200434D1/en not_active Revoked
- 2002-01-24 UA UA20031110032A patent/UA74639C2/en unknown
- 2002-01-24 WO PCT/EP2002/000699 patent/WO2002090651A1/en not_active Ceased
- 2002-01-24 BR BR0209390-1A patent/BR0209390A/en not_active Application Discontinuation
- 2002-01-24 SI SI200230016T patent/SI1313917T1/en unknown
- 2002-01-24 TR TR2004/01126T patent/TR200401126T4/en unknown
- 2002-01-24 KR KR1020037014058A patent/KR100778426B1/en not_active Expired - Fee Related
- 2002-01-24 AU AU2002235867A patent/AU2002235867B2/en not_active Ceased
- 2002-01-24 MX MXPA03009321A patent/MXPA03009321A/en active IP Right Grant
- 2002-01-24 CZ CZ20033036A patent/CZ20033036A3/en unknown
- 2002-01-24 SK SK1356-2003A patent/SK286317B6/en not_active IP Right Cessation
- 2002-01-24 ES ES02702307T patent/ES2201949T3/en not_active Expired - Lifetime
- 2002-01-24 US US10/476,620 patent/US20040168783A1/en not_active Abandoned
-
2003
- 2003-10-03 BG BG108226A patent/BG108226A/en unknown
- 2003-10-06 ZA ZA200307798A patent/ZA200307798B/en unknown
- 2003-11-07 NO NO20034968A patent/NO20034968D0/en not_active Application Discontinuation
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Granted publication date: 20060125 Termination date: 20120124 |