Method for determining white pigment in a paper layer

Abstract

The invention relates to a NIR-spectroscopy-based method for determining the amount of white pigment in a paper layer, in particular the amount and type of white pigment in a paper layer.

Description

[0001] Method for determining white pigment in a paper layer

[0002] The present invention relates to a method for determining white pigment in a paper layer, in particular the type and amount of white pigment in a paper layer.

[0003] Description

[0004] In the wood-based materials industry, impregnated papers are used extensively for the surface finishing of wood-based panels. These are essentially decorative papers, overlays, and counter-laminating papers that are pressed onto wood-based panels at high pressure and high temperatures. These coated panels are then used in a wide variety of applications (furniture, interior design, laminate flooring, etc.).

[0005] The quality of the decorative paper used is particularly important when using such coated wood-based panels in the furniture industry. Even the smallest color deviations in the production of front elements can lead to a negative overall impression and thus to complaints.

[0006] Decorative papers are specialty papers for surface finishing of wood-based materials, allowing for a wide variety of designs. In addition to the typical prints of various wood textures, more sophisticated prints featuring geometric shapes or artistic, decorative designs are available.

[0007] To ensure optimal printability, the paper used as the base paper must be smooth and dimensional stable. Furthermore, the paper should be as light in color as possible to achieve the highest possible brilliance. For this reason, designs are preferably printed on light, ideally white, paper.

[0008] For this purpose, white standard papers or base papers, preferably low-gram papers for cost savings, are initially prepared with a base content of white pigmentation. The white pigments are incorporated into the base papers during the manufacturing process.

[0009] Base paper refers to paper that has neither been subjected to sizing in the pulp nor to surface impregnation with a resin or glue. Base paper consists essentially of pulp, pigments (preferably white pigments), fillers, and common additives. Softwood pulp, hardwood pulp, or mixtures of both pulp types can be used to produce base paper.

[0010] A variety of inorganic compounds are used as white pigments. However, the focus remains on titanium dioxide, as it achieves the highest increase in opacity relative to the applied quantity. Other inorganic compounds such as barium sulfate, zinc oxide, or calcium sulfate are sometimes added to reduce costs and / or to modify the color.

[0011] To increase the opacity, these white standard papers or white base papers are treated with pigmented impregnating resins so that their whiteness is further increased by impregnation with resins containing white pigment.

[0012] The addition of pigments to impregnating resins such as urea or melamine resin is not entirely without problems, as the pigments tend to sediment in the impregnation bath. For this reason, the maximum pigment dispersion that can be added to an impregnating resin is approximately 10-20 wt%, with the solids content of the dispersion typically being approximately 50 to 60 wt%. However, even highly effective dispersing agents and very finely ground pigments (particle sizes: 3 to 5 pm) used for the dispersions can at best reduce the effect of sedimentation somewhat but cannot completely prevent it. Sedimentation not only leads to losses of the expensive titanium dioxide but also to a change in the whiteness of the paper. This effect cannot be seen with the naked eye on the impregnation line. Furthermore, it is evident that once sedimentation has begun in the impregnation tank, it continues at an accelerated rate.

[0013] Changes in whiteness can, of course, also occur if errors occur during the formulation and mixing of the pigment-containing impregnating resin. All of this can lead to quality deviations being detected in downstream process steps or, even more seriously, to complaints from customers (furniture factories, etc.). This is less of a problem for products used in the carcass area than for panels used to manufacture front elements. It should also be considered that customers have significantly tightened their guidelines regarding color deviations. The resulting disadvantages are color deviations, pigment loss, and the resulting rising costs due to increased waste and difficult quality control.

[0014] The invention is therefore based on the technical problem of developing a method with which the white pigmentation, or the amount and type of white pigment, in or on a paper used as a printing base can be determined, in order to eliminate quality defects attributable to this parameter. The system technology should not require increased safety standards. Furthermore, the determination should yield the lowest possible error. The determination should be continuous and suitable for automated system control based on this parameter.

[0015] This object is achieved by a method having the features of claim 1.

[0016] Accordingly, a method for determining white pigment in a paper layer, in particular the amount and type of white pigment in a paper layer, is provided. The present method comprises the following steps:

[0017] - Providing several layers of paper, each with different quantitatively defined amounts of white pigment, as reference samples;

[0018] - recording at least one NIR spectrum of each of the reference samples using at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm;

[0019] - Allocation of the different quantitatively defined amounts of white pigment in the reference samples to the recorded NIR spectra of the said reference samples; and

[0020] - Creation of a calibration model for the relationship between the spectral data of the NIR spectra and the corresponding quantitatively defined amounts of white pigment in the reference samples using a multivariate data analysis;

[0021] - Providing at least one sample of a paper layer containing a white pigment to be measured; - Recording at least one NIR spectrum of the impregnated paper layer using the at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; and

[0022] - Determination of the quantitative amount of white pigment introduced into the impregnated paper layer in the sample to be measured by comparing the NIR spectrum recorded for the sample to be measured with the calibration model created from the reference samples.

[0023] Accordingly, a measurement method is provided that allows for the determination of the type and quantity of a white pigment in a paper layer, especially a raw paper layer. The measurement method uses NIR spectroscopy, which allows for the continuous determination of the white pigment contained in a paper layer.

[0024] As already mentioned, the present measurement method now makes it possible to determine the quantity and type of white pigment in a base paper layer. As already defined, the term "base paper" refers to a paper layer that is not (yet) impregnated; i.e., a paper layer that is not impregnated with an impregnating resin, in particular a formaldehyde resin such as melamine, urea, and / or phenol-formaldehyde resin, or other resins such as melamine ether resins, acrylic resins, or epoxy resins, and thus consists solely of bonded cellulose fibers and, if applicable, additives.

[0025] US Pat. No. 5,7953,394 discloses the use of IR spectroscopy to determine the amount of a coating material containing calcium carbonate on a substrate, in particular on a paper layer. However, the described approach for determining the calcium carbonate concentration requires the use of a filter in a wavelength range between 3.9 pm and 4.1 pm, with a wavelength range between 3.6 and 3.85 pm used as the reference range. The present measurement method, in contrast, uses NIR spectroscopy in a specific wavelength range without the use of filters. In addition, a calibration model is created to determine the amount of white pigment.

[0026] US 2007 / 131862A1 describes the use of NIR spectroscopy for the quantitative analysis of resin-wood composites, where the samples to be measured are present as loose, unpressed mixtures. For example, the components resin, wax, polyols, and inorganic hardness are mixed with OSB strands and then measured using NIR spectroscopy, and calibration models are created. Concentrations of various components in a sample of a resin-wood composite are measured simultaneously. The calibration models are then used for the quantitative analysis of unknown resin-wood samples. However, this document does not contain any reference to the use of NIR spectroscopy to measure a white pigment in a paper layer.

[0027] In one embodiment of the present process, the white pigment used in the base paper layers is selected from titanium dioxide, barium sulfate, calcium sulfate, calcium carbonate, and / or zinc oxide, or a mixture thereof. The preferred white pigment is titanium dioxide.

[0028] Accordingly, in one embodiment, a base paper can be used that has a (basic) content of titanium dioxide. Typically, the amounts of titanium dioxide in such a white base paper are between 20 and 40 wt%, preferably between 25 and 35 wt% (based on the total paper weight).

[0029] In the case of the determination of a (single) white pigment in the raw paper layer, a first NIR spectrum is recorded for a raw paper layer without white pigment and another NIR spectrum for a raw paper layer containing a white pigment and the amount and type of white pigment are determined from the difference.

[0030] When determining the combination of different white pigments in the base paper layer, an NIR spectrum is first recorded for a base paper layer containing a first white pigment (e.g., TiO2) and another NIR spectrum is recorded for a base paper layer containing a first (e.g., TiO2) and a second white pigment (e.g., BaSO4 or ZnO). The sum of the values ​​for the paper with the first and second white pigments and the value for the paper with the first (single) white pigment ultimately yields the difference, from which the amount and type of the second white pigment can be determined.

[0031] Determining the type of pigment in a base paper layer is important, for example, because pigments such as zinc oxide or calcium carbonate neutralize hardeners used to cure impregnating resins (with which the base paper layers must be impregnated before further use). This can lead to undercuring of the impregnated paper layers, which cannot be readily explained without knowledge of the pigment composition. The use of lower-quality (cheaper) pigments can also lead to poorer lightfastness results or undesirable interactions when using surface-modifying chemicals in the resin formulation.

[0032] As already indicated above, the whiteness of the base paper is insufficient or inconsistent in certain cases, making the use of this white base paper as a printing base impossible or not advantageous. Accordingly, it is necessary to increase the whiteness of white base paper or white standard paper by impregnating it with a white pigment-containing impregnating resin.

[0033] The amount of white pigment applied to the base paper can also be determined (in addition to the white pigment contained in the base paper) using NIR spectroscopy.

[0034] Accordingly, in one embodiment, a method for determining the amount of white pigment in a paper layer is also provided, wherein the white pigment to be determined is introduced into the paper layer during impregnation of the paper layer with an impregnating resin. The present method comprises the following steps:

[0035] - Impregnating several layers of paper with an impregnating resin, each containing different quantitatively defined amounts of white pigment as reference samples;

[0036] - recording at least one NIR spectrum of each of the reference samples using at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm;

[0037] - Allocation of the different quantitatively defined amounts of white pigment in the reference samples to the recorded NIR spectra of the said reference samples; and

[0038] - Creation of a calibration model for the relationship between the spectral data of the NIR spectra and the corresponding quantitatively defined amounts of white pigment in the reference samples using multivariate data analysis; - Provision of at least one sample of an impregnated paper layer to be measured by impregnating at least one paper layer with an impregnating resin containing white pigment,

[0039] - Recording at least one NIR spectrum of the impregnated paper layer using the at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; and

[0040] - Determination of the quantitative amount of white pigment introduced into the impregnated paper layer in the sample to be measured by comparing the NIR spectrum recorded for the sample to be measured with the calibration model created from the reference samples.

[0041] Accordingly, in one embodiment, a measurement method is provided that allows for determining the amount of a white pigment that is incorporated into or applied to a paper layer together with the impregnating resin during an impregnation process. The measurement method utilizes NIR spectroscopy, which allows for continuous determination of the white pigment applied during the impregnation process.

[0042] According to this embodiment, the NIR measuring head determines the sum of the white pigment already contained in the base paper and the additional white pigment introduced into the base paper through impregnation. The difference is ultimately calculated from the sum and the value for the unpigmented paper.

[0043] As explained in more detail later, calibration grades are created for this process to establish a connection with the spectra determined via NIR. This makes it possible to determine unknown amounts of white pigment, such as titanium dioxide, in or on the paper layer. Furthermore, this calibration can be used to establish process monitoring. This can, for example, provide real-time quality data across the entire web width and enable rapid intervention in the event of deviations.

[0044] This method also makes it possible to analyze competitor products, process complaints more quickly, and support product development. The spectroscopic data can be used to analyze not only the order volume but also fluctuations within the order.

[0045] In one embodiment of the present method, it is provided that the white pigment to be determined is introduced into the paper layer during a core impregnation (or pre-impregnation) of the paper layer.

[0046] The term "core impregnation" or "pre-impregnation" refers to the impregnation of the paper core, whereby the impregnating resin penetrates the paper layer. In this case, the paper layer is completely or partially saturated with the impregnating resin.

[0047] Core impregnation or pre-impregnation occurs in the production of impregnated materials by applying the impregnating resin (in this case, mixed with a white pigment) to a first impregnation tank. After immersion in the impregnation tank, the resin is spread to a defined resin layer using doctor blades or squeegees. The pre-impregnate is then dried in a flotation dryer with hot air (intermediate drying). This may be followed by surface impregnation of the pre-impregnate with further drying. These drying steps each reduce the water content of the paper layer, preferably to 10-20 wt.%. Systems suitable for such impregnations are known. For example, see EP 3075906 B1, which describes an impregnation system consisting of a first impregnation station with a downstream drying station and a second impregnation station with a downstream drying station.

[0048] The determination of the amount of white pigment absorbed by the paper layer during core or pre-impregnation by means of NIR spectroscopy can be carried out after the first impregnation step and drying step (i.e. after pre-impregnation), or after the second impregnation step and drying step (i.e. after surface impregnation), the latter being preferred.

[0049] The present method requires only a single NIR measurement to determine the amount and type of white pigment in or on the paper layer. Another advantage is that the measurement is performed on a continuous paper layer, i.e., the paper layer is not destroyed. According to the present method, reference samples of paper layers are first prepared, each containing different quantitatively defined amounts of white pigment and / or impregnated with an impregnating resin containing different quantitatively defined amounts of white pigment. It is essential that the reference sample be similar to the sample to be measured. Thus, the impregnating resin of the reference sample should have the same composition as the impregnating resin to be measured.The similarity of the sample to be measured and the reference sample can be important, especially when using impregnating resins with additives such as flame retardants, fibers, or other additives.

[0050] At least one NIR spectrum of these reference samples is recorded in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm and / or between 1150 and 1300 nm.

[0051] The known quantitative composition of the base paper layer and / or the impregnating resin (i.e. the known white pigment content) is then assigned to the recorded NIR spectra of these reference samples, i.e. the different quantitatively defined amounts of white pigment in the reference samples are assigned to the recorded NIR spectra of the aforementioned reference samples. A calibration model for the relationship between the spectral data of the NIR spectra of the reference samples and the associated parameter values ​​is created using multivariate data analysis; i.e., for each parameter value of the reference sample, there corresponds an NIR spectrum of the reference sample. The calibration models created for the various parameters are stored in a suitable data storage.

[0052] Subsequently, at least one (raw) paper layer is provided with an unknown amount of white pigment and / or impregnated with an impregnating resin containing white pigment (in an unknown amount), and the (raw) paper layer and / or impregnated paper layer is measured as a sample. For this purpose, at least one NIR spectrum of the sample to be measured is recorded using the at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm and / or between 1150 and 1300 nm. The quantitative amount of white pigment contained in the (raw) paper layer and / or of the white pigment introduced into the impregnated paper layer in the respective sample to be measured can then be determined by comparing the NIR spectrum recorded for the sample to be measured with the calibration model created from the reference samples.

[0053] A comparison and interpretation of the NIR spectra is best performed across the entire recorded spectral range. This is best done using a well-known multivariate data analysis (MDA). Multivariate analysis methods typically examine several statistical variables simultaneously in a well-known manner. To achieve this, these methods typically reduce the number of variables contained in a data set without simultaneously diminishing the information contained therein.

[0054] In this case, the multivariate data analysis is performed using partial least squares regression (PLS), which allows for the creation of a suitable calibration model. The obtained data is preferably evaluated using suitable analysis software, such as SIMCA-P from Umetrics AB or The Unscrambler from CAMO.

[0055] In a further embodiment, spectral data from the NIR spectral range between 1400 nm and 1600 nm, preferably between 1450 and 1550 nm and / or between 1150 and 1300 nm, are used to create the calibration model, which are pretreated by means of suitable mathematical methods and then fed to the multivariate data analysis.

[0056] The significance of a wavelength for predicting the resin ratio from the NIR spectrum is illustrated using the regression coefficients. Regions with large coefficient values ​​have a strong influence on the regression model. Thus, the representation of the regression coefficients in a PLS regression model for determining the amount and type of white pigment shows that the wavelength range between 1450 nm and 1550 nm, with a maximum at 1480-1490 nm, is the most important for calculating the model, as this is where the regression coefficient values ​​are greatest. Although the other ranges in the spectrum have less information content with regard to the NIR measurement, they nevertheless contribute to taking into account or minimizing other information or interfering factors (such as the transparency of the layer, the surface quality of the substrate material, etc.). To eliminate interfering influences (such asDepending on the nature of the substrate surface, the color of the samples, light scattering by solid particles or other additives, etc., it is necessary to process the spectral data using mathematical pretreatment methods (e.g., derivative data pretreatment, standardization according to SNVT (Standard Normal Variate Transformation), multiplicative signal correction (EMSC, Extended Multiplicative Signal Correction, etc.). This removes the baseline effects, which are mainly caused by the different colors of the samples, from the spectra, separates overlapping bands, and takes into account the dependence of light scattering on the substrate surface or on the solid particles in the coating.

[0057] From the pre-treated data, a calibration model is developed using multivariate data analysis, which includes all decors used in the calibration.

[0058] Accordingly, the comparison and interpretation of NIR spectra are preferably carried out in the spectral range between 1450 and 1550 nm using multivariate data analysis (MDA). Multivariate analysis methods typically examine several statistical variables simultaneously in a conventional manner. This involves reducing the number of variables contained in a data set without simultaneously diminishing the information contained therein.

[0059] Titanium dioxide is also preferably used alone as a white pigment to increase the whiteness of the paper ply through impregnation. However, it can also be used in combination with other white pigments, particularly in combination with barium sulfate and / or zinc oxide. Preferred combinations are titanium dioxide and barium sulfate or titanium dioxide and zinc oxide. A combination of titanium dioxide, barium sulfate, and zinc oxide is also possible.

[0060] The particle size of the white pigment used in the impregnating resin is between 1 and 10 pm, preferably between 2 and 8 pm, particularly preferably between 3 and 5 pm.

[0061] In a further embodiment of the present process, the impregnating resin contains between 1.0 and 10.0 wt.% (based on the total amount of impregnating resin) of titanium dioxide as a white pigment, preferably between 2.0 and 8.0 wt.% titanium dioxide, particularly preferably between 3.0 and 5.0 wt.% titanium dioxide. For this purpose, between 2 and 20 wt.%, preferably between 4 and 16 wt.%, particularly preferably between 6 and 10 wt.% of a titanium dioxide dispersion with a titanium dioxide solids content of 50 wt.% is added to the impregnating resin. Preferred amounts are 5, 10, or 15 wt.% of an approximately 50 wt.% titanium dioxide dispersion.

[0062] In another embodiment, the impregnating resin contains between 5 and 10 wt% barium sulfate and / or zinc oxide as a white pigment, alone or in combination with titanium dioxide. Accordingly, preferably 10 or 20 wt% of a dispersion with a solids content of barium sulfate and / or zinc oxide of approximately 50 wt% is added to the impregnating resin.

[0063] In a further embodiment, the at least one impregnating resin containing the white pigment for the core or pre-impregnation of the paper layer is a formaldehyde resin, in particular a urea-formaldehyde resin, a melamine-formaldehyde resin or a mixture thereof, particularly preferably a urea-formaldehyde resin.

[0064] If a mixture of melamine-formaldehyde resin and urea-formaldehyde resin is used for the core or pre-impregnation, the quantitative ratio of melamine-formaldehyde resin and urea-formaldehyde resin in the resin mixture used can be between 90 wt% : 10 wt% and 10 wt% : 90 wt%, preferably between 75 wt% : 25 wt% and 25 wt% : 75 wt%, particularly preferably between 55 wt% : 45 wt% and 45 wt% : 55 wt%.

[0065] The resin application for the core or pre-impregnation of the paper layer is 80 to 100 wt%, preferably 85 to 95 wt%, particularly preferably 90 wt%.

[0066] In a further preferred embodiment, the pre-impregnated or core-impregnated paper layer is surface-impregnated with at least one additional impregnating resin. The impregnating resin used for surface impregnation can also contain a white pigment. However, it is preferred if the impregnating resin for surface impregnation does not contain a white pigment.

[0067] The impregnating resin used for surface impregnation is also a formaldehyde resin, in particular a melamine-formaldehyde resin. The resin application for surface impregnation of the paper layer is 30 to 50 wt%, preferably 35 to 45 wt%, particularly preferably 40 wt%.

[0068] The total resin application for core impregnation and surface impregnation is thus 110 to 150 wt%, preferably 120 to 140 wt%, particularly preferably 130 wt%.

[0069] In a further embodiment, the paper layer to be measured and / or impregnated has a paper weight between 50 and 100 g / m 2 , preferably between 60 and 80 g / m 2 , especially between 65 and 75 g / m 2 on.

[0070] In a particularly preferred embodiment, the paper layer to be impregnated consists of raw paper. The term "raw paper" refers to paper that is not (yet) impregnated; that is, a paper layer that is not impregnated with an impregnating resin, in particular a formaldehyde resin such as melamine, urea, and / or phenol-formaldehyde resin, or other resins such as melamine ether resins, acrylic resins, or epoxy resins, and thus consists solely of bonded cellulose fibers and, if appropriate, additives.

[0071] As already indicated above, impregnation with a white pigment-containing impregnating resin increases the whiteness of standard white papers. Accordingly, in one embodiment, a base paper that already has a (basic) titanium dioxide content can be used for the impregnation. Typically, the amounts of titanium dioxide in such a white base paper are between 25 and 35 wt% (based on the total paper weight).

[0072] The present method for determining the amount of white pigment in a (raw) paper layer and / or impregnated paper layer can be carried out continuously and online in a production line, in particular in an impregnation plant.

[0073] The determination of the amount of white pigment in a (raw) paper layer is advantageously carried out upstream of an impregnation plant, e.g. at the unwinding of the paper layer before the impregnation plant or during the incoming goods inspection in the laboratory.

[0074] A system for impregnating at least one paper layer passing through the system comprises

[0075] - optional paper unwinding and changing device - a first impregnation station for pre-impregnation (core impregnation) of at least one paper layer with an impregnating resin containing a white pigment;

[0076] - a second impregnation station for surface impregnation of at least one pre-impregnated paper layer,

[0077] - wherein after the second impregnation station at least one NIR measuring head, in particular at least one NIR multi-measuring head, is provided for recording at least one NIR spectrum of the paper layer impregnated with the white pigment, and

[0078] - optional clipper and storage table.

[0079] The NIR measuring head is preferably positioned so that the top side of the impregnated paper layer is irradiated. However, it is generally also possible to install additional NIR measuring heads in the impregnation system to measure the top and bottom sides of the impregnated paper layer.

[0080] The NIR sensor head can be located after core impregnation, before or after the first dryer. Another option would be after the second dryer, before the clipper.

[0081] It is particularly preferred if the at least one NIR measuring head traverses the width of the paper layer and analyzes specific problem areas (e.g., in the edge or center area of ​​the boards, etc.). Accordingly, the at least one NIR measuring head moves transversely to the direction of travel of the (pre)impregnated paper layer. Furthermore, the measured values ​​are immediately available and allow immediate intervention in the process. This is not readily possible with other methods.

[0082] In one embodiment of the present impregnation system, a first drying station is provided after the first impregnation station, wherein the at least one NIR measuring head is arranged after the first drying station.

[0083] In a more specific embodiment, the impregnation system comprises impregnation tanks or impregnation immersion baths (as impregnation stations), if necessary a breathing section, a doctor blade system / squeeze roller pair for removing excess resin, at least one dryer (e.g. a floating dryer), optionally a screen unit and an optional second dryer, at least one cooling device (e.g. a cooling roller system).

[0084] Thus, a method is provided in which, by using an NIR measuring head, the amount of white pigment in a (pre)impregnated paper layer can be determined from an NIR spectrum using a non-contact measurement. In an advantageous embodiment of the invention, the data acquired with the measuring head(s) are used directly for system control or regulation.

[0085] Furthermore, in a further advantageous embodiment of the invention, storing the data enables improved quality control. The stored data can also advantageously contribute to the evaluation of system tests, e.g., commissioning of a system during a new installation or after maintenance or repair, or for in-situ testing of new production or measurement processes. The immediate availability of the measured values ​​and the high measurement frequency enable very close monitoring, control, or regulation of the systems.

[0086] This method enables the provision of measured values ​​in a short time (online, preferably without disruptive time delays) compared to conventional (known) measurement methods. The measured data can be used for quality assurance, research and development, process control, process regulation, process control, etc. The measurement process does not reduce production speed, etc. Fundamentally, it improves production monitoring. Furthermore, downtimes due to quality control and system adjustments are reduced.

[0087] The advantages of this method are manifold: non-contact multi-parameter determination ("real-time" measurement) with significantly reduced time delay in the evaluation of the measured parameter values; improved plant control and regulation, reduction of waste, improvement in the quality of the products manufactured on the plant, and improvement in plant availability.

[0088] The control system of the impregnation plant comprises at least one computer-assisted evaluation unit (or processor unit) and a database. The evaluation unit compares or compares the NIR spectrum measured for the product (i.e., pressed porous coating material) with the calibration models created for the individual parameters. The parameter data thus determined is stored in the database.

[0089] The data determined using this spectroscopic method can be used to control the impregnation system. The non-contact measured parameter values ​​of the NIR multi-sensor head ("actual values") can, as previously described, be used directly and in real time for the control or regulation of the respective system. For example, by storing the measured actual values ​​in a database, e.g., a relational database, and comparing them with the target values ​​of these parameters available there. The resulting differences are then used to control or regulate the production line.

[0090] For the calibration and control of the impregnation system, a computer-implemented method and a computer program comprising instructions that, when executed by a computer, cause the computer to execute the computer-implemented method are provided. The computer program is stored in a memory unit of the control system of the impregnation system.

[0091] The invention is explained in more detail below using exemplary embodiments with reference to the figures. They show:

[0092] Figure 1 NIR spectra of raw paper sheets containing titanium dioxide, of paper sheets impregnated with titanium dioxide and reference samples,

[0093] Figure 2 NIR spectra of titanium dioxide impregnated paper sheets and reference samples, and

[0094] Figure 3 NIR spectra of paper sheets impregnated with titanium dioxide and zinc oxide / barium sulfate and reference samples.

[0095] Example 1:

[0096] A white (raw) decorative paper (paper weight: 65 g / m 2 ), which had a titanium dioxide content of approximately 25 wt%, were first impregnated with a urea resin (core impregnation) and then with a melamine resin (surface impregnation) (total resin application: 130 wt%, urea resin: 90 wt%, melamine resin: 40 wt%), dried in between and pressed onto a chipboard in a laboratory press (standard 65 g / m 2 ).

[0097] In addition, an overlay without white pigment (paper weight: 35 g / m 2 ) impregnated with the same resins. The resin application was 400 wt%. The resin distribution was similar to that of the white papers. The pigment-free overlay served as a reference sample or blank sample (OV without TiO2). It was pressed onto a particle board under the same conditions.

[0098] With the decorative paper with a basis weight of 65 g / m 2Two additional samples were subsequently produced. 5 and 15 wt% of a titanium dioxide dispersion (titanium dioxide content: approximately 50 wt%) were added to the urea resin used for core impregnation. The melamine resin used for surface impregnation did not contain any titanium dioxide dispersion. The impregnation was carried out analogously to the first impregnation. The total resin application was also approximately 130 wt%. These two impregnated materials were also pressed onto a particle board in a laboratory press under identical conditions (Fentak 17-5%-TiO2, Fentak 17-15%-TiO2).

[0099] NIR spectra of the reference sample and the three sample samples were then recorded (see NIR spectrum in Figure 1). The different titanium dioxide contents are clearly visible in the spectrum.

[0100] Example 2:

[0101] A white decorative paper (paper weight: 65 g / m 2), which had a titanium dioxide content of approximately 25%, were first impregnated with a urea resin (core impregnation) and then with a melamine resin (surface impregnation) (total resin application: 130 wt%, urea resin: 90 wt%, melamine resin: 40 wt%), dried in between, and pressed onto a particle board in a laboratory press. These served as reference samples or blank samples (standard 65g / m 2 ).

[0102] With the decorative paper with a basis weight of 65 g / m 2Two further samples were then produced. 5 and 15 wt% of a titanium dioxide dispersion (titanium dioxide content: approx. 50 wt%) were added to the urea resin used for core impregnation. The melamine resin for surface impregnation did not contain any titanium dioxide dispersion. Impregnation was carried out analogously to the first impregnation. The total resin application was also approx. 130 wt%. These two impregnated materials were also pressed onto a particle board in the laboratory press under identical conditions (Fentak 17-5% TiO2, Fentak 17-15% TiO2). NIR spectra of the reference sample and the two sample samples were then recorded (see NIR spectrum in Figure 2). The different titanium dioxide contents are clearly visible in the spectrum.

[0103] Example 3:

[0104] A white decorative paper (paper weight: 65 g / m 2), which had a titanium dioxide content of approximately 25 wt%, were first impregnated with a urea resin (core impregnation) and then with a melamine resin (surface impregnation) (total resin application: 130 wt%, urea resin: 90 wt%, melamine resin: 40 wt%, moisture: approximately 6 wt%). 10% of a titanium dioxide dispersion was added to the urea resin used for core impregnation.

[0105] (Titanium dioxide content: approx. 50 wt.%) was added. It was then dried and pressed onto a particle board in a laboratory press (zero sample, Fen-19-10%-TO2).

[0106] With the decorative paper with a basis weight of 65 g / m 2Further samples were subsequently produced. The melamine resin for surface impregnation again did not contain any titanium dioxide dispersion. The impregnation was carried out analogously to the first impregnation. The resin application was also approximately 130 wt% and the moisture content was approximately 6 wt%. The proportion of urea and melamine resin also remained the same. Furthermore, titanium dioxide dispersions with 10 and 20 wt% zinc oxide and barium sulfate, respectively, were prepared and used analogously to the first impregnation. These four impregnated materials were also pressed onto a particle board in the laboratory press under identical conditions (Fen-19-10%-Ba10%, Fen-19-10%-Ba20%, Fen-19-10%-Zn10%, Fen-19-10%-Zn20%).

[0107] NIR spectra of one reference sample and the four sample samples were then recorded (see NIR spectrum in Figure 3). The different contents of zinc oxide and barium sulfate are clearly visible in the spectrum.

Claims

Patent claims 1. A method for determining white pigment in a paper layer, in particular the amount and type of a white pigment in a paper layer, comprising the steps - Providing several layers of paper, each with different quantitatively defined amounts of white pigment, as reference samples; - recording at least one NIR spectrum of each of the reference samples using at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; - Allocation of the different quantitatively defined amounts of white pigment in the reference samples to the recorded NIR spectra of the reference samples; and - Creation of a calibration model for the relationship between the spectral data of the NIR spectra and the corresponding quantitatively defined amounts of white pigment in the reference samples using a multivariate data analysis; - Providing at least one sample of a paper layer containing a white pigment to be measured; - Recording at least one NIR spectrum of the impregnated paper layer using the at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; and - Determination of the quantitative amount of white pigment introduced into the impregnated paper layer in the sample to be measured by comparing the NIR spectrum recorded for the sample to be measured with the calibration model created from the reference samples.

2. Method according to claim 1, characterized in that the amount of white pigment in a paper layer is determined, wherein the white pigment to be determined is introduced into the paper layer during an impregnation of the paper layer with an impregnating resin, comprising the steps - Impregnating several layers of paper with an impregnating resin, each containing different quantitatively defined amounts of the white pigment as reference samples; - recording at least one NIR spectrum of each of the reference samples using at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; - Allocation of the different quantitatively defined amounts of white pigment in the reference samples to the recorded NIR spectra of the reference samples; and - Creation of a calibration model for the relationship between the spectral data of the NIR spectra and the corresponding quantitatively defined amounts of white pigment in the reference samples using a multivariate data analysis; - Providing at least one sample of an impregnated paper layer to be measured by impregnating at least one paper layer with an impregnating resin containing white pigment, - Recording at least one NIR spectrum of the impregnated paper layer using the at least one NIR measuring head in a wavelength range between 1350 nm and 1650 nm, preferably between 1400 nm and 1600 nm, particularly preferably between 1450 nm and 1550 nm; and - Determination of the quantitative amount of white pigment introduced into the impregnated paper layer in the sample to be measured by comparing the NIR spectrum recorded for the sample to be measured with the calibration model created from the reference samples.

3. Method according to one of the preceding claims, characterized in that the white pigment to be determined comprises titanium dioxide, barium sulfate, calcium sulfate and / or zinc oxide, or a mixture thereof, in particular titanium dioxide.

4. Method according to claim 2-3, characterized in that the white pigment to be determined is introduced into the paper layer during a core impregnation (or pre-impregnation) of the paper layer.

5. Process according to one of claims 2-4, characterized in that the impregnating resin contains between 1.0 and 10.0 wt% (based on the total amount of impregnating resin) of titanium dioxide as white pigment, preferably between 2.0 and 8.0 wt% titanium dioxide, particularly preferably between 3.0 and 5.0 wt% titanium dioxide.

6. Process according to one of claims 2-5, characterized in that the impregnating resin contains between 5 and 10 wt% barium sulfate and / or zinc oxide as white pigment.

7. The method according to any one of claims 2-6, characterized in that the at least one impregnating resin containing the white pigment is a formaldehyde resin, in particular a urea-formaldehyde resin, a melamine-formaldehyde resin or a mixture thereof, particularly preferably a urea-formaldehyde resin.

8. Method according to one of claims 2-7, characterized in that the pre-impregnated / core-impregnated paper layer is surface-impregnated with at least one further impregnating resin.

9. The method according to claim 8, characterized in that the impregnating resin for surface impregnation does not contain any white pigment.

10. The method according to claim 8 or 9, characterized in that the impregnating resin used for the surface impregnation is a formaldehyde resin, in particular a melamine-formaldehyde resin. 11 . Method according to one of the preceding claims, characterized in that the paper layer has a paper weight between 50 and 100 g / m 2 , preferably between 60 and 80 g / m 2 , especially between 65 and 75 g / m 2 has.

12. Method according to one of the preceding claims, characterized in that the paper layer consists of raw paper.

13. Method according to one of the preceding claims, characterized in that the determination of the amount of white pigment in the paper layer is carried out continuously and online.

14. Method according to one of the preceding claims, characterized in that spectral data from the entire recorded spectral range are used to create the calibration model.

15. Method according to one of the preceding claims, characterized in that spectral data from the NIR spectral range between 1400 nm and 1600 nm, preferably between 1450 and 1550 nm and / or between 1150 and 1300 nm are used to create the calibration model, which data are pretreated by means of suitable mathematical methods and are then fed to the multivariate data analysis.

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