Cellulose and paper of higher brightness

FIELD: textile, paper.

SUBSTANCE: full bleaching/extraction of craft cellulose fibres is carried out with a chorine agent. Afterwards fibres are washed and exposed to contact in solution with at least one optical bleach (OB) upstream the mixing box and the discharge box of the machine. Fibres in solution have consistency from 7 to 15%, pH of solution in process of contact of fibres with OB makes from 3.5 to 5.5, temperature of contact makes from 60 to 80°C, and time of contact is from 0.5 to 6 hours. Additional contact of OB with fibres is carried out in the device for coating application or in the gluing press. Contact may be carried out at the stage of storage, both at high density and low density of the craft-cellulose fibres, and also at the stage of refinement.

EFFECT: improved whiteness and brightness of fibres when using lower quantity of OB.

19 cl, 11 dwg, 12 tbl, 6 ex

 

This application claims the benefit of provisional application U.S. serial number 60/654,712, filed February 19, 2005, and claims the priority application U.S. serial number 11/358,543, filed February 21, 2006, entitled "Pulp and paper increased brightness", which are fully incorporated herein by reference.

The technical field

The present invention relates to a method of increasing the brightness of the pulp, the pulp produced by such methods, and methods of use of such cellulose.

The level of technology

Bleaching is a traditional method of increasing the whiteness of the pulp. Industry practice improve the appearance of loose cellulose lies in its bleaching to a higher brightness levels (Technical Association of the pulp and paper industry (TAPPI) or the international organization for standardization (ISO)). However, bleaching is an expensive process, harms the environment and is often the cause of performance degradation. The pervasive preference of consumers to a brighter and more white pulp is forcing manufacturers to use more aggressive methods of blanching. Although after an intense bleaching cellulose whiter, it still has a yellowish-white color. Yellowish-white product undesirable. Numerous studies the Oia show consumers clearly prefer bluish-white yellowish-white color. The first is perceived as more white, meaning "fresh", "new" and "clean", and the latter is considered "old", "faint" and "dirty".

Although bleaching right increases the brightness, it only indirectly increases the whiteness. Due to the recent bleaching is not always the most effective way to increase the whiteness of the product. For example, even after an intense bleaching whiteness of the product you can always improve by reasonable add dye.

The practice of coloring pulp for making paper is not generally and is not usually desirable. In relation to the first aspect, the intentional change of the optical properties often leads to poor performance of the product, such as brightness TAPPI, which is undesirable. Regarding the latter aspect, there is a risk that the dyes can fail in unpredictable production environment subsequent processes. This may occur because of pre-added dye may experience adverse chemical or physical effects during subsequent processing operations, which will lead to unexpected or undesirable color change or a complete loss. In addition, some dyes may deteriorate or be in Economics is suspended in the course of subsequent processing operations, that would violate the integrity and reliability of the method. Therefore, any improvement of the optical properties is usually achieved by adding priming dyes, fillers and/or fluorescent dye at the stage of making paper. The way to increase the whiteness, brightness and color described in U.S. patent No. 5,482,514. The method applies to adding photoactivation, in particular water-soluble phthalocyanines into fibers for making paper to enhance its optical properties by bleaching in the presence of a catalyst of the photosensitizer. The resulting fiber for making paper can be successfully introduced into paper sheets.

For loose cellulose, as well as for most types of pulp and paper products TAPPI brightness actually serves as a standard instead of specific industries specifications "white", such as white CIE (international Committee on chromatics). Because of this, the brightness performs two key roles. First, the brightness is a manufacturing option. Secondly, the brightness is a technical feature for the classification of varieties of the final product. Indirect, but controversial assumption is that the brightness is equivalent to white. The usual practice of making paper consists in adding blue tinting dye or tinting pigment the s and/or in addition bluish-violet fluorescent dyes to improve the properties of whiteness. Semi-permanent dyes are or colored pigments high degree of grinding, suspended in the dispersant, or synthetic direct dyes. Semi-permanent dyes have some affinity to cellulose, while toning pigments practically do not have it.

Fluorescent brighteners (FD) or optical brighteners (PA)used in the pulp and paper industry may be classified into three types, such as compounds of di-, Tetra - or hexachlorophene stilbene. These chemicals require ultraviolet (UV) irradiation to activate fluorescence. Although in daylight contains a large amount of ultraviolet light, even the light bulb normal office produce enough UV radiation to some activation. In the manufacture of paper PA add on the wet stage of the paper manufacturing process, including, for example, the machine reservoir and/or pump fan, where the solution of the fibers has a low concentration of approximately 3% solids. In these traditional points add most of the NGO goes to waste, because OO is not necessarily has a strong affinity with the fibers in the solution. Accordingly, the NGO must be added at high concentrations (in pounds per ton of fiber or pulp) in order to obtain high quality fibers having you will fetter the brightness and significant improvement in brightness.

Accordingly, there is a need to cellulose with high whiteness and brightness. There is also a need in the method of manufacturing a whiter and brighter pulp for any application, especially pulp for making paper and loose pulp, while using a smaller amount of PA in order to obtain such levels of whiteness and brightness at lower cost. The present invention is directed to the fulfillment of these needs and has a number of associated benefits.

Brief description of the invention

In one aspect the present invention relates to a method of bleaching cellulose fibers containing contact a certain number of fibers with at least one optical Brightener at any time after the last stage bleaching/extraction chlorine bleach and before processing the fibers chemicals for paper manufacturing. In another aspect the present invention relates to clarified the cellulose fibers obtained by the method of the present invention and preferably has a CIE whiteness of not less than 130, the ISO brightness not less than 90 or CIE whiteness is not less than 130 and the ISO brightness not less than 90. In another aspect the present invention relates to a paper or paperboard base containing cellulose fibers of the present invention.

Brief description of drawings

Figure 1: Graph of the brightness ISO against GS in leaves of manual casting, manufactured from pulp processed OO, a complete set of data.

Figure 2: Graphs of brightness ISO against GS in leaves of manual casting manufactured from pulp processed OO, the set of data on the dose.

Figure 3: Graphs of brightness ISO against GS in leaves of manual casting manufactured from pulp processed OO, the influence of the dose of PA in the presence of 10 and 20% filler.

Figure 4: Graphs of brightness ISO against GS in leaves of manual casting manufactured from pulp processed OO, the influence of the dose of PA in the presence of 10 and 20% filler, added to the regression line.

Figure 5: Raman spectra only PA and cellulose with different levels of PA during the sequential addition.

6: Raman spectra of cellulose with different levels of PA added according to one aspect of the present invention.

7: Raman spectra of cellulose with different levels of PA added sequentially and according to one aspect of the present invention.

Fig: Graph of the maximum ratio (1604/900 cm-1in Raman spectra of cellulose with different levels of PA added sequentially and according to one aspect of the present invention (hardwood and softwood pulp), as shown in table 10.

Figure 9: Optical density of the aqueous extract in the UV/optical spectrum of the radiation at a wavelength of 350 nm PR is against the actual number of PA on the fibers, in pounds per ton.

Figure 10: peak height-OO versus quantity PA (pounds per ton), added in the traditional way and added according to one aspect of the present invention (hardwood pulp and softwood pulp).

11: peak height-OO versus quantity PA (pounds per ton), added in the traditional way and added according to one aspect of the present invention (hardwood pulp and softwood pulp).

Detailed description of the invention

The author of the present invention has found a non-obvious way to effectively increase the brightness and whiteness of pulp and paper using fewer OO, this offering is a much more effective way of getting complex fiber-OO, containing in the whole, increased interaction "fiber-OO"than the traditional ways of creating complex fiber-OO". This complex fiber-PA", manufactured by the method according to the present invention, provides a greater increase in the brightness and whiteness than just fiber in comparison with traditional methods, as discussed below.

The present invention partially relates to a method of manufacturing cellulose. Cellulose may be loose or be used for making paper. This method can be used both separately and together with any conventional method of manufacturing a ry the Loy pulp or pulp for making paper. Cellulose can be used for any traditional use, including any traditional way of making paper and/or cardboard base. Such traditional methods of making pulp and making paper can be found, for example, in the "Handbook technologist pulp and paper industry" (Handbook For Pulp & Paper Technologies), 2nd edition, J. Asmuch (G.A.Smook), publisher Angus Wilde Publications (1992) and referred to in the sources, which are incorporated herein in full by reference.

A typical method of manufacturing pulp/paper may include without limitation the following steps:

A. Stage of cooking, in which wood chips are cooked to free the cellulose fibers from lignin;

B. Stage leaching of sulphate pulp, which is washed pulp after boiling;

C. Stages of bleaching/extraction, in which the pulp is extracted and bleach using various chemical substances, such as oxygen during oxygen delignification, chlorine dioxide, elemental chlorine, peroxide, ozone and the like, followed by one or more rinsing steps;

D. the storage at high density, which is bleached and washed pulp is maintained at a relatively high density, such as preferably more than 7%, more preferably from 7.5 to 15% and most preferably about the 10%to 12%;

E. Stage of storage at low density, where the bleached and washed pulp is maintained at a relatively low density, as, for example, preferably less than 7%, more preferably from 3% to 7% and most preferably from 10%to 12%;

F. Stage refining of cellulose in which the cellulose ennoble if preferred consistency from 4 to 5%;

G. Steps mailbox mixing/headbox of the machine, on which the pulp with the preferred consistency of from 3 to 4% is mixed with chemicals used in the wet stage of the manufacture of paper, such as fillers, means of restraint, dyes, optical brighteners, etc. These traditional methods may include repetitions of any one or more of the above steps. In addition, the present invention can be combined with traditional methods of adding OO to the fibers in the traditional points add to the wet stage, as well as in the sizing press, and the points add coatings in the manufacture of paper and/or cardboard.

The present invention partially relates to a method for adding OO to the fibers at any point after the last stage bleaching/extraction using bleach, chlorine-based, such as elemental chlorine and chlorine dioxide, and before processing, pulp chemicals used is in the manufacture of paper, add in the box mixing/discharge box of the machine. For example, cellulose fibers can be treated at any stage of the bleaching/extraction without the use of chlorine during bleaching with chlorine, if any. Examples of such stages without the use of chlorine are those in which the pulp is treated with oxygen, ozone, peroxides, peroxynitrate, acid derivatives of hydrogen peroxide (such as peroxymonosulfate acid and peroxidasa acid), dimethyldioxirane, hydrosulfite sodium, sodium bisulfite, hydrosulfite zinc and any other bleach that does not contain chlorine, such as specified in the publication "the Bleaching of pulp, The Bleaching of Pulp) 3rd edition. Rping (R.P.Singh), Publisher TAPPI PRESS, Atlanta, GA, 1979. As further examples of the cellulose can be processed PA during storage at high density, which is bleached and washed pulp is maintained at a relatively high density; during storage at low density, where the bleached and washed pulp is maintained at a relatively low density; at the stage of refining pulp, which pulp refining in the preferred consistency from 4 to 5%; or any combination of these steps.

Source of fibers can be any fiber the East plant. Examples of such fibrous plants are trees, including deciduous and coniferous or mixtures thereof. In some embodiments, the implementation of at least part of the cellulose fibers can be obtained from non-woody herbaceous plants, including, without limitation, kenaf, hemp, jute, flax, sisal or abaku, although legal restrictions and other considerations may make the use of cannabis and other sources of fibers impractical or impossible. In the method of the present invention it is possible to use fibers of bleached or unbleached pulp. Fiber can be secondary, and free from paint and/or primary, but preferably are the primary fibers.

Cellulose of the present invention may contain from 1 to 99 wt.%, preferably from 5 to 95 wt.%, cellulose fibers derived from hardwood and/or softwood, from the total amount of cellulose fibers. This range includes 1, 2, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95 and 100 wt.%, including any and all ranges and subranges within these limits, the total amount of cellulose fibers.

If the pulp contains hardwood and softwood fibers, it is preferable that the relationship between hardwood fibers and softwood fibers ranged from 0.001 to 1000. This range may include 0,001, 0,002, 0,005, 0,01, 0,02, 0,05, 0,1, 0,2, 0,5, 1, 2, 5, 10, 15, 20, 25, 30, 35,40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 200, 300, 400, 500, 600, 700, 800, 900 and 1000, including any and all ranges and subranges within these limits, as well as any and all ranges and subranges within these limits with the inverse relationship.

Optical brighteners (PA)used in the practical implementation of the method of the present invention, may vary within wide limits, and any NGO that is used for bleaching mechanical pulp or Kraft pulp can be used in the process of the present invention. Optical brighteners are similar to dyes, fluorescent compounds, which absorb short-wave ultraviolet radiation, not visible to the human eye and is emitted as blue light of longer wavelengths, with the result that the human eye perceives white high degree, and the degree of whiteness is thus increased. This provides additional brightness and can compensate for the natural shade of yellow in a paper basis. Optical brighteners used in the present invention, may vary within wide limits, and you can use any suitable optical Brightener. The review of these bleaches can be found, for example, in the publication "encyclopedia of Ullmann industrial chemistry" (Ullmann''s Encyclopedia of Industrial Chemistry), Sixth edition, 2000, e is t he launch, "OPTICAL BRIGHTENERS - Chemicals technical products", which is incorporated herein in full by reference. Other suitable optical brighteners are quoted in U.S. patents№5,902,454; 6,723,846; 6,890,454; 5,482,514; 6,893,473; 6,723,846; 6,890,454; 6,426,382; 4,169,810 and 5,902,454 and the indicated sources, which are all incorporated herein by reference. Other suitable optical brighteners are listed in the published patent applications US # US 2004/014910 and US 2003/0013628; in patent application WO 96/00221 and the indicated sources, which are all incorporated herein by reference. Examples of suitable optical brighteners are 4,4'-bis-(creatininemia)-stilbene-2,2'-disulfonate, 4,4'-bis(triazole-2-yl)stilbene-2,2'-disulfonate, 4,4'-dibenzofuran-biphenyl, 4,4'-(diphenyl)-stilbene, 4,4-DISTEARYL-biphenyls, 4-phenyl-4'-benzoxazolyl-stilbene, stilbene-naturezone, 4-styryl-stilbene, bis-(benzoxazol-2-yl)derivatives, bis(benzimidazole-2-yl)derivatives, coumarins, pyrazoline, naphthalimide, triazinyl-layer, 2-styryl-benzoxazol or naftoxate, benzimidazole-benzofuran or oxanilide.

Most commercially available optical brighteners made on the basis of stilbene, coumarin and pyrazoline, and they are preferred for practical implementation of the present invention. More preferably the mi optical brighteners for the practical implementation of the present invention are optical brighteners, usually used in the manufacture of paper and made on the basis of stilbene, such as 1,3,5-triazinyl-derivatives of 4,4'-diaminostilbene-2,2'-disulphonate and its salts, which may have additional sulfopropyl, for example at positions 2, 4 and/or 6. Most preferred are the commercially available derivatives of stilbene, for example, offered by the company Ciba Geigy under the trade name "Tinopal", by the company Clariant under the trade name "Leucophor"company Lanxess under the brand name "Blankophor" and the company 3V under the brand name "Optiblanc", such as optical brighteners based disulfonate, tetrasulfonated and hexadentate stilbene. Of these the most preferred commercially available optical brighteners more preferred are optical brighteners based disulfonate and tetrasulfonated stilbene, and most preferred are optical brighteners based disulfonated stilbene. Although in the present invention, the preferred methods and systems of the fiber-PA using the above-mentioned NGO, the present invention is in no way limited to such implementation options, and you can use any of the PA.

The present invention is due in part to the complex fiber-PA", whose affinity of PA added to the fiber according infusion is he to the invention, preferably more than OO, traditionally added to the fiber. If PA is added to the fiber according to the method of the present invention, the required amount of PA is reduced by 30-60% compared with the traditional methods and points added. The decrease can be 30, 31, 32, 33, 34, 35, 40, 45, 50, 55, 56, 57, 58, 59 and 60% compared with the number required by traditional methods and points are added, including any and all ranges and subranges within these limits.

The increased affinity of PA with the fiber can be measured by the methods of extracting any solvent, preferably water, at any temperature. Because PA has a high affinity for the fiber in the pulp and made of them a paper the basics according to the present invention, more time will be needed for the extraction OO of complex cellulose-OO" of the present invention (cellulose and/or paper) at some given period of time and temperature for any given solvent.

In addition, the present invention preferably relates to a method of enhancing penetration of the PA in the cell walls of the fibers. Preferably, after treatment of the fibers in accordance with the present invention a larger number of PA penetrates the cell walls than the fibers treated with traditional methods. More preferably, the amount is creation OO, present in the wall of the fiber cells increases by at least 1% compared with the number of NGOs present in the wall of the fiber cells treated with traditional methods. However, more preferably, the number of NGOs present in the wall of the fiber cells, was increased by at least 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 100, 200, 300, 500 and 1000% in comparison with the number of NGOs present in the cell wall of the fiber, processed by conventional methods, including any and all ranges and subranges within these limits.

More preferably, the NGO does not penetrate less than 1% of the cell's wall. However, more preferably, OO penetrated at least in 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85 or 90% of the cell's wall, including any and all ranges and subranges within these limits.

The number of NGOs present in the wall of the fiber cells, can be measured, for example, microscopy, and more specifically by fluorescence microscopy.

Although fiber can be added to any number of the PA, if it is added at any point after the last stage bleaching/extraction and before the steps of mixing box/headbox of the machine, preferably the addition of the PA in the amount of from 1 to 60 pounds OO per ton of fiber, more preferably not more than 30 pounds per ton, Naib is more preferably not more than 15 pounds of PA per ton of fiber. This range includes 60, 55, 50, 45, 40, 30, 35, 30, 25, 20, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5,4, 3, 2 and 1 pound of PA per ton of fiber, including any and all ranges and subranges within these limits.

In addition, the fiber may be in solution or suspension, or may be added in solution or suspension simultaneously with the NGO. Preferably, the fiber is in solution or suspension prior to contact with the NGO. In one embodiment of the present invention, the fiber may have any consistency. However, it is preferable that the consistency of the solids was equal to or greater than 4%, more preferably not less than about 5%, most preferably not less than approximately 10%. In addition, it is preferable that the fiber had the consistency of solids, which does not exceed about 35%, more preferably not more than 20%, most preferably no more than about 15%. These ranges include 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 and 20% solids as the consistency of the fibers at the time of addition of the NGO, including any and all ranges and subranges within these limits.

At the time of adding OO to the fibers, the pH value can be anything. Preferably, the pH value may be in the range from 2.5 to 8.0, more preferably from 3.5 to 5.5. This range includes values 2,5, 3,0, 3,5, 4,0, 4,5, 5,0, 5,5, 6,0, 6,5, 7,, 7,5 and 8,0, including any and all ranges and subranges within these limits.

At the time of adding OO to the fiber temperature may be any. However, it is preferable to use a means such as heating, to create a temperature from 35 to 95°C, preferably from 50 to 90°C, more preferably from 60 to 80°C. This range includes 35, 40, 45, 50, 55, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 85, 90 and 95°C, including any and all ranges and subranges within these limits.

The contact time of the PA with the fibers can be any. Preferably, the NGO and the fibers may be in contact from 30 minutes to 12 hours, more preferably from 45 minutes to 8 hours, most preferably from 1 hour to 6 hours. This range includes 0,5, 0,75, 1, 1,25, 1,5, 1,75, 2, 2,25, 2,5, 2,75, 3, 3,25, 3,5, 3,75, 4, 4,25, 4,5, 4,75, 5, 5,25, 5,5, 5,75, 6, 6,5, 7, 7,5, 8, 8,5, 9, 9,5, 10, 11 and 12 hours, including any and all ranges and subranges within these limits.

At the moment of contact of the NGO with the fibers can be optionally added or already present means of restraint. Examples of such means of restraint are alum and/or cationic means of restraint. Examples of means of restraint are contained in provisional patent application U.S. No. 60/660703 filed March 11, 2005, and U.S. patent No. 6,379,497, which are incorporated herein in full by reference. However, you can use any cf the rotary retention, usually used in conjunction with the NGO. Although the means of restraint may be present in any amount, or not present at all, preferably the number of present funds hold less than that required in traditional ways and when points are added, used for the implementation of PA contact with the fibers. It is preferable not to use means of restraint. If you are using means of restraint, it is preferable that the reduction in the number of present means of restraint was at least 1% compared with the traditional methods and points added for PA contact with the fibers. The preferred reduction in the number of means of restraint present in the present invention, is at least 2, 3, 4, 5, 10, 15, 20, 25, 30, 35, 40, 50, 60, 75, 100, 200, 300, 500 and 1000% in comparison with the traditional methods and points added for PA contact with the fibers, including any and all ranges and subranges within these limits.

Although fiber can be refined at any time, preferably fiber ennoble after PA contact with the fiber. Therefore, the complex fiber-OO" of the present invention improved. Respectively, may be any conventional refining, including, without limitation, chemical refining, mechanical finishing, thermochim the economic improvement, thermomechanical refining, chemical-thermomechanical beautification, etc. So the resulting pulp may include thermo-mechanical, chemi-thermomechanical, mechanical, bleached chemi-thermomechanical etc.

Cellulose of the present invention and the method of its manufacture can be included in any traditional way of making paper. Pulp and/or paper base may also contain other conventional additives, such as, for example, starch, mineral and polymer fillers, a sizing agent, a means of retaining and reinforcing polymers. As fillers can be used organic and inorganic pigments, such as, for example, minerals such as calcium carbonate, kaolin, talc, and expanded or expandable microspheres. Other conventional additives are, without limitation waterproof resin, the inner adhesives, shopruche resin, alum, fillers, pigments and dyes. Of the dyes are particularly preferred dyes of the type of blue that can improve the whiteness CIE pulp and/or paper base. Preferably, the pulp and paper Foundation of the present invention, manufactured according to the present invention, the methods to achieve whiteness CIE, which is much higher than traditional cellulose and foundations, made traditionally the diversified ways, even when the levels of CIE whiteness, which usually lead to lower levels of ISO brightness. Pulp and/or paper base of the present invention can have any whiteness CIE, but preferably have a CIE whiteness more than 70, more preferably greater than 100, most preferably more than 125 or even 150. The CIE whiteness can be in the range from 125 to 200, preferably from 130 to 200, most preferably from 150 to 200. The range of CIE whiteness may be greater than or equal 70, 80, 90, 100, 110, 120, 125, 130, 135, 140, 145, 150, 155, 160, 65, 170, 175, 180, 185, 190, 195 and 200 points of CIE whiteness, including any and all ranges and subranges within these limits. Examples of measurement of CIE whiteness and the receipt of such whiteness in the fibers and the paper made from them, can be found, for example, in U.S. patent No. 6,893,473, which is incorporated herein in full by reference.

Preferably, the pulp and/or paper base of the present invention have the whiteness CIE, which is more than the traditional pulp and/or paper bases obtained by conventional methods. A preferred improvement of the whiteness CIE is at least 2, 3, 4, 5, 10, 15, 20, 25, 30, 35, 40, 50, 60, 75, 100, 200, 300, 500 and 1000% compared with traditional pulp, paper, made by traditional methods, and points added for PA contact with the fiber, including any and all ranges and podiamos who are within these limits.

Pulp and paper the basis of the present invention can have any brightness ISO, but preferably more than 80, more preferably greater than 90, most preferably more than 95 points ISO brightness. The ISO brightness may be preferably from 80 to 100, more preferably from 90 to 100, most preferably from 95 to 100 points ISO brightness. This range includes values greater than or equal to 80, 85, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99 and 100 points brightness ISO, including any and all ranges and subranges within these limits. Examples of measuring the brightness ISO and obtain a brightness in the fiber for making paper and made of him the paper can be found, for example, in U.S. patent No. 6,893,473, which is incorporated herein in full by reference. Preferably, the pulp and/or paper base of the present invention have an ISO brightness, which is more than the traditional pulp and/or paper basics, made in traditional ways. Preferably, the increase is at least 2, 3, 4, 5, 10, 15, 20, 25, 30, 35, 40, 50, 60, 75, 100, 200, 300, 500 and 1000% increase in brightness ISO compared to traditional pulp, paper, made by traditional methods, and points added for PA contact with the fiber, including any and all ranges and subranges within these limits.

The present invention now is explained in more detail in the following variant example of implementation, which is not intended to be any limitation of the scope of the present invention.

COMPARATIVE EXAMPLE 1

Performed laboratory experiments to simulate the manufacture of commercial paper, in which the T-100, tetrachlorophenyl PA company Clariant, was added to three samples of bleached hardwood Kraft pulp. For mixing the pulp with chemicals used low-speed laboratory stirrer Warring. Before adding an optical Brightener (g) of deionized water was added to 5 grams of sample pulp kiln drying to bring it to the consistency of up to 1%. Soon after adding OO to 5 ml of 5%solution of alum was added to a mixture of cellulose for fixing CV on the fiber. After mixing in the mixer for one minute, the mixture of cellulose obezvozhivani to obtain tablets for measuring the brightness according to the standard procedure of measuring the brightness of the pulp by TAPPI. In these experiments we used three samples of pulp and three doses of T-100. The results of the brightness of individual samples of cellulose before and after fixing the CV to the following:

Table 1.
Deciduous #1Deciduous #2 Deciduous #3
Brightness (GE)IncreaseBrightness (GE)IncreaseBrightness (GE)Increase
080,5084,4086,60
483,12,687,73,390,03,5
884,23,789,75,190,4the 3.8
1684,94,389,45,090,74,1

COMPARATIVE EXAMPLE 2

Performed laboratory experiments to simulate the manufacture of commercial paper, in which the T-100, tetrachlorophenyl PA company Clariant, was added in one about ASEC Kraft pulp from southern hardwood. For mixing the pulp with chemicals used low-speed laboratory stirrer Warring. Before adding an optical Brightener (g) of deionized water was added to 5 grams of sample pulp kiln drying to bring it to the consistency of up to 1%. For experiments in the series I soon after adding OO to 5 ml of 5%solution of alum was added to a mixture of cellulose for fixing CV on the fiber. In the experiments of series II alum is not used. In wall-cases, after mixing in the mixer for one minute, the mixture of cellulose obezvozhivani to obtain tablets for measuring the brightness according to the standard procedure of measuring the brightness of the pulp by TAPPI. In these experiments we used three samples of pulp and three doses of T-100. The results of the brightness of individual samples of cellulose before and after fixing OO below.

Table 3.
Series I - Without alumSeries II - alum
Brightness (GE)IncreaseBrightness (GE)Increase
0084,08
387,43,4
689,05,0
1089,7the 5.7
2085,80,8of 89.15,1
4086,42,386,22,1
6086,72,782,21,8

Table 4.
Water bath at 60°CWater bath at 75°C
Col. T-100 (funtown tonne) Reaction time (hours)Brightness (GE)IncreaseBrightness (GE)Increase
0088,9088,90
2193,04,191,82,9
4193,64,6for 93.44,5
8194,96,094,75,8
0088,9088,90
2592,23,392,03,1
4 593,64,6of 92.7the 3.8
8594,05,193,9a 4.9

EXAMPLE 1.

Samples of fully bleached Kraft pulp of hardwood and softwood were taken at the exit from the installation of commercial bleaching pulp and paper mill in the southern United States for use in experiments on fixing the PA at high consistency. Conditions of the experiments, including the type of NGO and consistency pulp E, were identical to the conditions for Comparative example 1. Coniferous pulp obtained sample had a pH of 5.2, the pH of the sample hardwood pulp was 6.7. All experiments were performed within two hours, when the temperature of the water bath to 65°C. for some experiments with deciduous cellulose to cellulose have also added a dilute solution of hydrochloric acid to reduce its pH to 4.9 in response to PA. The following results are obtained.

EXAMPLE 2

Samples of fully bleached Kraft pulp of hardwood and softwood were taken at the exit from the installation of commercial bleaching pulp and paper mill in Europe to use the tion in experiments on fixing the toe. The pH value of the filtrate of both cellulose samples was 3.0. In this example, used disulfonates OO Leucophor ANO company Clariant. Experiments fixation was performed with a variable number OO, consistency 10%, within two hours at the temperature of the water bath of 65°C. was Observed the following changes in the brightness of the pulp in the fixation of the toe.

Table 6.
Col. OO Leucophor (pounds per ton)DeciduousConiferous
Brightness (GE)IncreaseBrightness (GE)Increase
089,3088,40
593,64,392,84,3
1094,3a 4.9to 92.13,7
15of 92.7 3,490,42,0
2091,92,689,61,1
3089,3086,0a-2.5

EXAMPLE 3

In this example, used samples of pulp and PA in example 3. However, before mixing with the NGO added a dilute solution of NaOH to increase the pH of samples from 3.0 to 5.7 for hardwood pulp and up to 7.0 for softwood pulp. All other conditions were identical to those used in example 4. Observed the following changes in the brightness of the pulp resulting from the pH adjustment and fixation of the toe.

Table 7.
DeciduousConiferous
Col. OO Leucophor (pounds per ton)Brightness (GE)IncreaseBrightness (GE)Increase
089,0087,9 0
4for 93.44,492,54,6
894,95,893,85,9
1295,16,394,06,1
2095,56,594,86,8
3089,36,695,17,2

EXAMPLE 4

The experiments were conducted for fixing T-100 on samples of fully bleached softwood and hardwood Kraft pulp with pulp and paper mill in the North of the USA. Coniferous cellulose had a degree of grinding 690 csf, brightness 90 GE and pH 4.0. A sample of hardwood cellulose had a degree of grinding 570 csf, the brightness of 89.2 and pH 4.0. Variable doses of the T-100 was mixed with the pulp at a consistency of 10% and contained in a separate sealed plastic bags. The bags were placed in a water bath with a temperature of 70°C for 2 hours. Observed the following change is to be placed in the brightness of the samples of cellulose in the fixation of the toe.

Table 8.
ConiferousDeciduous
Col. T-100 (pounds per ton)Brightness (GE)IncreaseBrightness (GE)Increase
090,0089,20
294,44,492,02,8
4for 95.25,2of 92.73,5
695,85,893,34,1
896,36,393,84,6
1096,66,6942 5,0
12to 97.17,194,35,1

EXAMPLE 6

The original samples of softwood and hardwood pulp from Example 5, together with samples, which were recorded using 12 pounds in the British ton T-100 was subjected to high mechanical shear force in a laboratory PFI refiner. The degree of refining pulp controlled so as to reduce the degree of grinding softwood pulp with 690 CSF before finishing up to 450 CSF after finishing. For hardwood pulp reduction of the degree of grinding amounted to 570 CSF to 330 CSF. Changes in the brightness of the original cellulose samples and samples containing PA, were as follows.

Table 9.
ConiferousDeciduous
Before you commitAfter fixationIncreaseBefore you commitAfter fixationIncrease
Before finishing 9096,66,689,2a 94.25,0
After finishing88,494,76,388,494,05,6
Loss1,61,90,80,2

The loss of brightness in the refining of cellulose is well known in the manufacture of paper. In terms of refinement used in Example 6, it was 1.6 points for the original softwood pulp and 0.8 for the original hardwood pulp. Loss of brightness is very similar for the case when the cellulose was recorded with the help of the NGO, which suggests that the relationship between the NGO and the fibers are very strong, and it is not affected by mechanical cutting force refiner. The net increase in brightness resulting from fixation OO, remained almost unchanged, and it is not affected by the process of refining pulp.

EXAMPLE 6: a Study sheets manual casting

Summary

Study sheets manual casting confirmed that the addition of optical Brightener (PA) Clariant Leucophor ANO in terms of processing at high consistency gave increased brightness compared with the addition of PA at low consistency.

For a fixed dose of a new insertion point resulted in increased brightness ISO about 1.9 units.

Based on the results of this study concluded that to achieve the same brightness ISO in the transition to a new way to add a dose of PA can be reduced by £ 3 per tonne.

These estimates are based on data for dose levels of PA in the range from 3.3 to 10 pounds per ton.

The experiment showed that two factors, namely the dose of PA (nominally 3.3 and 10 pounds per ton) and how to add PA (new method against adding to the cellulose of low concentration), were statistically significant in determining the brightness.

Experimental part

Cellulose

This study used a highly plasticised deciduous and coniferous pulp taken from the installation after the last washing stage bleaching.

1. Commit PA

Separately deciduous and coniferous pulp with two levels of PA, 3.3 and 10 pounds per ton. Used OO Leucophor ANO (the company Clariant), which is desulfuromonas PA. Conditions: consistency of 10%, was stirred for 2 hours at 70°C.

2. About agoriani

Before finishing cellulose samples were combined in the ratio of 70:30 deciduous/coniferous. The elevation was performed in a laboratory disc refiner LR1. Used two levels of power: 35 kW and 45 kW. The degree of grinding of the obtained cellulose was ~580 and ~320 csf, respectively.

3. Manufacturing sheets

The sheets were made on a dynamic casting machine in the following order. The pulp was diluted to a consistency of 1% and intensively stirred. First added precipitated calcium carbonate Albacar LO SMI and allowed to mix for one minute. Then added a certain exact number of NGO and was stirred for 15 minutes, then was molded sheet. After molding the sheets were pressed to the solids content of 45% and dried at 230°F in a drum dryer. Had taken special precautions to ensure that the sheets "fixed" PA had a similar number of NGO and was used as sheets with the addition of a standard amount of PA. In addition to the samples pre-treated CV and samples, prepared as above, were also produced several control samples, for which the order of addition of precipitated calcium carbonate and PA changed to the opposite (first toe).

4. Test

The sheets were tested on different optical properties with ISOE what Itanium spectrophotometer DataColor Elrepho.

5. The experiment plan

The plan for this experiment consisted of four main factors:

I) the Consistency of raw materials, to which was added OO (10% vs. 1%)

II) the Elevation (force 35 kW to 45 kW)

III) filler Content (10% versus 20%)

IV) Dose of PA (3,3 against 10 pounds per ton)

Results and conclusions

Comparison of the brightness of the sheets manual casting for the new and traditional methods of fixation.

Adding an optical Brightener (PA) Leucophor ANO company Clariant under the new method of processing at high consistency gave increased brightness of the leaves compared to the addition at low consistency. The results, shown in figure 1-Figure 4 shows data on the brightness against the dose of PA obtained in the course of the study. There are several different classes listed samples are separated according to the method of fixing (at high and low consistency) and the content of the filler (10 and 20 pounds per ton).

The study of cellulose with CV by Raman spectroscopy

Raman spectroscopy was used to study the cellulose with the NGO added according to the traditional and new ways. Figure 5 compares the spectrum of PA (Leucophur ANO) with the spectra of cellulose with and without PA. The most pronounced peak in the spectrum of PA at approximately 1600 cm-1see in the spectrum of cellulose with the addition of PA. N the Fig.6 shows the spectra of cellulose (...range from 300 to 1700 cm -1) with different amounts of added PA. The intensity of the peak at 1600 cm-1increases with the number of PA. When comparing the spectra of cellulose with the NGO added according to the traditional and new ways, was not observed changes in the form of peaks and more peaks (Fig.7). To determine the relative amount of PA remaining on the fibers was calculated by the ratio of the intensity of the peak at 1600 cm-1to the intensity of the peak at 900 cm-1(the peak of cellulose to cellulose with different number of CBOs that are added during the process. The results are presented in the table and Fig.

Table 10.
MethodCol. OO, pounds per tonThe ratio of the peak heights
Traditional00,026
100,469
150,637
200,711
New hardwood pulp00,034
3,30,238
100,648
New softwood pulp00,071
3,30,371
100,685

Measurements using Raman spectroscopy show that when the number of PA 10 pounds per ton of the pulp obtained in a new way, you can get results comparable with the number of PA 15-20 pounds per ton of the pulp obtained in the traditional way.

A study of NGO in cellulose by the method of spectroscopy with inductively coupled plasma (ICP)

Samples of softwood and hardwood pulp with the NGO added according to the traditional and the new method, cooked on a hot plate with hydrogen peroxide and nitric acid. Sample PA, used in the method, dried and cooked under the same conditions. Samples after cooking analyzer the Wali for sulfur content using ICP spectroscopy. The results are presented in the table below. The raw pulp is also analyzed under the same conditions, and certain sulfur concentration subtracted from the concentrations in the treated cellulose in order to set the amount of pas in cellulose, which was reported on dry weight of the toe.

MethodAdded OO, pounds per tonSulfur by ICP-spectroscopy, parts per millionSera from PA on the fiber, parts per millionCV on fiber parts per million (according to the results of S)
Traditional0150
1019040697
202501001744
New hardwood pulp 0140
102501101918
New softwood pulp066
10150841465
OO (kiln drying)57600; 57100

The sulfur concentration in the pulp show that the number of NGOs present in the pulp treated according to the new method, adding 10 pounds of PA per ton of pulp is comparable with the number present in the pulp treated in the traditional way, with added and 20 pounds per ton.

Research extraction

Approximately 1 gram pulp was cut into small pieces and soaked in approximately 150 ml of water for 6 hours at 60°C.

Water extracts were filtered through a 0.45 µm filter, brought up to a volume of approximately 2 ml in the system of evaporation LABCONCO Rapidvap using air as the purge gas. The evaporator worked for 24% of the vortex velocity at 30°C. After evaporation to approximately 2 ml of the sample was brought to 5 ml in a volumetric flask.

Part of this water extract 5 ml were analyzed using high performance liquid chromatography (HPLC).

Part of the aqueous extract of 5 ml was diluted in the ratio 1:10 for analysis in the UV/optical spectrum of the radiation.

For liquid chromatography HPLC used the following equipment: Name of device: separation module (Waters Alliance 2695 with matrix photodiode detector Waters model 996;

Mobile phase: 50% methanol 50% PIC-A buffer solution at 0.7 ml per minute. PIC-And is offered by the company Waters Corporation and serves as a buffer solution for reversed-phase ion-pair chromatography, containing 0,M of tetrabutylammonium, brought to pH 7.5.

Column: Phenomenex Luna 5 μm C-8 (2) 250 mm X 4.6 mm, operating at 35°C.

Detector: photodiode matrix detector Waters 400 for a range of 200800 nm. For analysis was selected peak at 254 nm.

Running time: 60 minutes

Injected volume: 10 ál

Equipment for analysis in the UV/optical spectrum of radiation:

Name of the instrument: Shimadzu model UV-160 operating in the photometric mode.

The wavelength used for the analysis: 350 nm. The results are shown in Figures 9-11.

In light of the above description numerous possible modifications and changes of the present invention. It is therefore understood that within the scope of the attached claims, the invention may be implemented otherwise than specifically described above.

Used in the text descriptions of the ranges is used as a short code for each value that enters into them, including all their sub-bands.

All links and references referred to therein, incorporated by reference in relevant parts of the description relating to the subject matter of the present invention and all variants of its implementation.

1. A method of manufacturing pulp and/or paper base containing the complete bleaching/extraction of a certain amount of fiber Kraft pulp bleach agent, washing the specified number of bleached fiber Kraft pulp after bleaching/extraction and after cleaning the contacts specified number of bleached Kraft fibers-cellulose solution with at least some of the optical bleach (OO) to the mixing box and the headbox of the machine.

2. The method according to claim 1, wherein the fibers in the solution have a consistency more than approximately 4%.

3. The method according to claim 1, wherein the fibers in the solution have a consistency from 7 to 15%.

4. The method according to claim 1, in which contact with the fibers used from 1 to 15 pounds OO per ton.

5. The method according to claim 1, wherein the pH of the solution during contact with OO fibers is from 3.5 to 5.5.

6. The method according to claim 1, in which the temperature upon contact with OO fibers ranges from 60 to 80°C.

7. The method according to claim 1, in which OO in contact with the fibers in the course of from 0.5 to 6 hours

8. The method according to claim 1, wherein the contact is carried out at a point of the manufacturing process of pulp and paper to the stage of refinement.

9. The method according to claim 1, in which the specified contact is carried out in the absence of means of restraint.

10. The method according to claim 1, additionally containing contact for more OO to the fibers in the device for applying the coating.

11. The method according to claim 1, additionally containing contact for more OO to the fibers in the sizing press.

12. The method according to claim 1, wherein the fibers in the solution have a consistency of 10 to 12%.

13. The method according to claim 1, wherein the specified number of bleached Kraft fibers-cellulose in solution have an ISO brightness is not lower than 90 to contact the specified number of bleached Kraft fibers-cellulose solution with at least one OO and brightly the th ISO more than or equal to 90 after contacting the specified number of bleached Kraft fibers-cellulose solution with at least one OO.

14. The method according to claim 1, wherein the specified number of bleached Kraft fibers-cellulose in solution have an ISO brightness is not less than or equal to 90 to contact the specified number of bleached Kraft fibers-cellulose solution with at least one OO and have an ISO brightness of more than or equal to 92 after contacting the specified number of bleached Kraft fibers-cellulose solution with at least one OO.

15. The method according to claim 1, in which the fiber Kraft pulp from hardwood trees.

16. The method according to claim 1, in which the fiber Kraft pulp from coniferous trees.

17. The method according to claim 1, wherein the contacting is carried out on the stage of storage at high density.

18. The method according to claim 1, wherein the contacting is carried out on the stage of refinement.

19. The method according to claim 1, wherein the contacting is carried out on the stage of storage at low density.



 

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