CN115821635B - Fibrous flexible filler high-filling paper and preparation method thereof - Google Patents
Fibrous flexible filler high-filling paper and preparation method thereof Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses fibrous flexible filler high-filling paper and a preparation method thereof, and belongs to the technical field of papermaking fillers. The composite structure is formed between the precipitated calcium carbonate and the cellulose nanofibrils through a simple mechanical force co-grinding method, so that the combination capability of the filler and the combination capability between the filler and the fibers are improved, meanwhile, the filler is endowed with flexibility through an injection molding method and is subjected to shape design, and the retention rate of the filler and the tensile strength of the high-filling paper in the wet papermaking process of the filling paper are improved; meanwhile, the method can finish production under the existing factory conditions through simple operation, so that the filler content and the paper strength of the high-filling paper are obviously improved, the consumption of plant fiber resources is reduced, and the method has important significance for reducing the cost and sustainable development of the paper industry.
Description
Technical Field
The invention belongs to the technical field of papermaking fillers, and particularly relates to fibrous flexible filler high-filling paper and a preparation method thereof.
Background
Papermaking fillers, which are understood to mean some solid particles which are substantially insoluble in water and are added to the pulp, are mostly mineral fillers. Fillers commonly used in the paper industry are mainly light calcium carbonate (PCC), heavy calcium carbonate (GCC), kaolin clay and talc. Compared with plant fibers, the mineral filler has the characteristics of small particle size, high whiteness, high refractive index and low water absorption, and after being added into paper, the mineral filler can effectively improve the opacity, brightness, smoothness, printing adaptability (such as improving the absorbability and the ink absorbability), softness, uniformity and dimensional stability of the paper, replaces the plant fibers with higher cost with the filler with lower cost, and improves the filler content in the paper, so that the mineral filler has become one of research hot spots and development trends of the paper industry at home and abroad.
The price of calcium carbonate is 3-4 times lower than that of chemical pulp on the market, and cultural paper usually contains 20-35% GCC or PCC (by weight), by increasing the amount of GCC or PCC in the paper without losing the basic properties, it means at the same time that it will consume lower drying energy, lower wood fiber consumption and lower production costs. The benefits of increasing the filler content of paper are self-evident, since 1970 to 2000, the filler content of cultural paper has nearly doubled, which is sufficient to demonstrate that increasing filler levels have become one of the goals pursued by enterprises. With the increased filler content of paper, there is also a series of non-negligible problems, such as: 1) An increase in the filler particle content affects the bonding of hydrogen bonds between fibers, resulting in a decrease in the strength of the paper; 2) Serious hair and powder falling can occur on the surface of the paper; 3) Since the particles of the filler are much smaller than the fibers and are negatively charged as the fibers, the filler can be lost with white water to reduce the retention rate of the filler; 4) The water treatment becomes difficult due to the increased filler content in the white water.
In order to solve the series of problems, the prior reported filler pre-flocculation technology uses ionic polymers to flocculate mineral fillers, and the agglomerated filler flocculation is flattened and formed through the procedures of water filtering, squeezing and the like, so that the deformable and compressible characteristics bring high retention rate, and the technology is widely put into use in the paper industry. However, although the size of the flexible filler can be controlled by changing the concentration of the ionic polymer, the shape is irregular, the shape of the filler cannot be designed artificially, and the improvement of the strength performance of paper is limited. The in-situ synthetic filler technology takes fine fibers or nano fibers as carriers, and the filler prepared by in-situ mineralization is characterized in that the fiber is a linear core, so that the whole filler can be regarded as a fibrous filler, and the purposes of improving the retention rate of the filler and the strength of paper can be achieved by the technology, however, the effect of improving the strength performance of the paper is limited, the operation is complex, and the large-scale production is difficult to realize. And filler modification technology, such as in-situ sol-gel method for preparing silica modified precipitated calcium carbonate, starch coated modified filler, carboxymethyl cellulose/alum composite coated modified precipitated calcium carbonate and the like. These methods, while effective in improving the strength properties of paper when compared to unmodified fillers, are either more complex or more costly to filler modify. Therefore, how to prepare a filler which can reduce the amount of plant fiber in paper while ensuring the strength performance and retention of the paper by a simple and effective method becomes a key problem.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide fibrous flexible filler high-filling paper and a preparation method thereof, which are used for solving the technical problems of poor paper strength, low retention and complex technology of papermaking fillers manufactured in the prior art.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a preparation method of fibrous flexible filler high-filling paper, which comprises the following steps:
s1: performing co-pulping on a mixture consisting of precipitated calcium carbonate and cellulose nano fibers to obtain a composite filler; the composite filler is gelled to obtain the composite flexible filler; injecting the composite flexible filler into the hydraulic vortex to obtain a fibrous flexible filler;
s2: fluffing the plant fiber pulp board and pulping together to obtain mixed pulp; adding fibrous flexible filler into the mixed slurry, then adding cationic polyacrylamide, stirring, screening to form, and then squeezing and drying to obtain fibrous flexible filler high-filling paper.
Further, in S1, the mass ratio of the precipitated calcium carbonate to the cellulose nanofiber is 10:1.
further, in S1, the pulp separation of the common pulp is 0.15mm, and the pulp grinding revolution is 10000r; the precipitated calcium carbonate has a triangle structure, and the average grain diameter is 4.530 mu m; the cellulose nanofiber is prepared by a TEMPO oxidation method, and has a cellulose I-type crystal structure; the cellulose nanofiber has the diameter of 5-20 nm, the length of 1-3 mu m, the carboxyl content of 2.0mmol/g and the mass concentration of 1.2%.
Further, in S1, the gelation time is 12-24 hours; the hydraulic vortex is formed by stirring the stirrer in water; the rotation speed of the hydraulic vortex is 400rpm; injecting the composite flexible filler into the hydraulic vortex by adopting an injection needle cylinder; the syringe is a 10mL syringe, and is provided with an injection needle with an inner diameter of 0.11-0.45 mm.
Further, in S2, the freeness of the mixed slurry is 40 ° SR; the plant fiber pulp board is a hardwood pulp board and a softwood pulp board; the mass ratio of the hardwood pulp plate to the softwood pulp plate is 3:1.
further, in S2, the mass of the fibrous flexible filler is 40% -60% of the mass of the mixed slurry.
Further, in S2, the cationic polyacrylamide is prepared into an aqueous solution with the mass concentration of 0.03% before use; the dosage of the cationic polyacrylamide is 2mL.
Further, in S2, the stirring time is 10-20S; the mass concentration of the net surfing during net surfing forming is 0.025%; the squeezing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature was 105℃and the time was 6min.
The invention also discloses the fibrous flexible filler high-filling paper prepared by the preparation method.
Further, the basis weight of the fibrous flexible filler high-filled paper is 63g/m 2 。
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of fibrous flexible filler high-filling paper, which adopts mechanical force to jointly grind pulp, so that physical crosslinking is formed between precipitated calcium carbonate and cellulose nanofibrils, and a complex is formed by designing cellulose nanofibres and the precipitated calcium carbonate under the action of mechanical force, so that the coating effect of the cellulose nanofibres on the precipitated calcium carbonate is realized; during wet forming, the cellulose nanofiber/precipitated calcium carbonate complex can be well combined to form a scale effect, so that the retention rate of the filler is improved, and meanwhile, as the cellulose nanofiber has a nanoscale, a larger specific surface area, more active groups and active sites and forms a good complex structure with the precipitated calcium carbonate, the interface between the fiber and the complex and between the complex and the pore diameter can be enhanced, more uniform and compact high-filler paper is formed, the thickness of the high-filler paper is reduced, and the mechanical property of the high-filler is enhanced; in addition, the flexibility of the filler is fully utilized to carry out morphology design on the filler, so that more combinations are formed between the filler and the plant fiber in microcosmic, interweaving force is generated on the whole, and the problems of low filler retention rate, no bonding strength between the fillers and the fiber in the existing high filler paper filling process are solved. The reasons for its improved tensile strength are: 1) The cellulose nanofibrils are coated on the surface of the precipitated calcium carbonate to form a composite structure through co-pulping, so that good hydrogen bonding is formed between the flexible fillers and the plant fibers; 2) Through morphology design, a new structure is given to the flexible filler, and surface interweaving force exists between the new structure and the plant fiber; 3) The composite filler has certain flexibility, and can be compressed and deformed in the paper filtering and water pressing process, so that the flexible filler and the plant fiber are better combined, and the retention rate and the tensile strength of the filler of the high-filling paper are obviously improved; the preparation method disclosed by the invention is simple to operate, easy to realize industrial production and has a wide application prospect.
The invention also discloses the fibrous flexible filler high-filling paper prepared by the preparation method, which is more uniform and compact, has low filler retention rate and high mechanical property.
Drawings
FIG. 1 is a schematic illustration of a process flow for preparing a fibrous flexible filler of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the fibrous flexible filler highly filled paper prepared in example 2 of the present invention;
wherein: a-d are flexible filler microcosmic shapes with different diameters; e and f are partial enlarged views of the composite flexible filler.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The invention provides a preparation method of fibrous flexible filler high-filling paper, which is characterized in that cellulose nanofibers and precipitated calcium carbonate are designed to form a complex under the action of mechanical force, so that the coating effect of the cellulose nanofibers on the precipitated calcium carbonate is realized, the cellulose nanofibers/precipitated calcium carbonate complex can be well combined to form a scale effect during wet forming, the retention rate of filler is improved, and meanwhile, as the nanoscale of the cellulose nanofibers, the larger specific surface area, more active groups and active sites and the precipitated calcium carbonate form a good composite structure, the interface combination between the fibers and the complex and the gap and pore diameter between the complex can be enhanced, more uniform and compact high-filling paper is formed, the thickness of the high-filling paper is reduced, and the mechanical property of the high-filling material is enhanced. In addition, the flexibility of the filler is fully utilized to carry out morphology design on the filler, so that more combinations are formed between the filler and the plant fiber in microcosmic, interweaving force is generated on the whole, and the problems of low filler retention rate, no bonding strength between the fillers and the fiber in the existing high filler paper filling process are solved.
The method specifically comprises the following steps:
1) Precipitating calcium carbonate and cellulose nano fiber by using a filler for papermaking according to a proportion of 10:1, mixing and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is 1.2-3.0 mmol/g in carboxyl content, and the mass concentration is 1.2%.
2) Adding the mixture uniformly mixed in the step 1) into a PFI pulping machine, and uniformly smearing the mixture on the periphery of the millstone wall; co-refining under the condition that the refining gap is 0.15mm and the refining revolution is 10000r;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is batch type equipment, and the single pulping capacity is about 300mL.
3) Transferring the composite filler subjected to the common pulping in the step 2) into a beaker, and gelling after about 24 hours to form the composite flexible filler;
4) Sucking the composite flexible filler in the step 3) by a needle cylinder, and adding a needle head, so as to inject the composite flexible filler into a hydraulic vortex with the rotating speed of 400rpm, thereby forming fibrous flexible filler;
wherein the syringe is a 10mL syringe, and the inner diameter of the syringe needle is 0.11-0.45 mm; the hydraulic vortex forming method comprises the following steps: adding 800mL of deionized water into a 1000mL beaker, and placing a digital display stirrer with a propeller at a position 10mm away from the bottom of the beaker to stir to generate the deionized water;
5) Taking broadleaf wood with plant fiber content: the needle wood=3:1 pulp board is subjected to fluffing and PFI pulping treatment after mixing to obtain mixed pulp, the beating degree of the mixed pulp is 38-40 DEG SR, 40-60% of the fibrous flexible filler prepared in the step 4) is added into the mixed pulp, after mechanical stirring and mixing are uniform, 2mL of 0.03% CPAM is added, after stirring for 10s, the mixed pulp is subjected to net surfing forming, and the fibrous flexible filler high-filling paper is obtained after squeezing and drying;
wherein the mass concentration of the internet is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; the basis weight of the paper is 60-65 g/m 2 。
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
A preparation method of fibrous flexible filler high-filling paper comprises the following steps:
s1: precipitated calcium carbonate and cellulose nanofibers as fillers for paper making were mixed in an amount of 10:1, mixing and uniformly stirring to obtain a mixture, adding the mixture into a PFI pulping machine, uniformly smearing the mixture on the periphery of the wall of a grinding disc, and performing common pulping under the condition that the pulping gap is 0.15mm and the pulping revolution is 10000r to obtain a composite filler; transferring the composite filler into a beaker, and after about 24 hours, gelatinizing to obtain the composite flexible filler; sucking the composite flexible filler by a needle cylinder, adding a needle head, and injecting the composite flexible filler into a hydraulic vortex with the rotating speed of 400rpm to obtain a fibrous flexible filler;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is intermittent equipment, and the single pulping capacity is about 300mL;
wherein the syringe is a 10mL syringe, and the inner diameter of the syringe needle is 0.45mm; the hydraulic vortex forming method comprises the following steps: adding 800mL of deionized water into a 1000mL beaker, and placing a digital display stirrer with a propeller at a position 10mm away from the bottom of the beaker to stir to generate the deionized water;
s2: taking broadleaf wood with plant fiber content: the mass ratio of the conifer wood is 3:1, mixing, fluffing, performing PFI pulping treatment, and obtaining mixed slurry, wherein the beating degree is 40 DEG SR; adding fibrous flexible filler into the mixed slurry according to the filling amount of 40% of the mass of the mixed slurry, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10s, performing net forming, and squeezing and drying to obtain fibrous flexible filler high-filling paper;
wherein, the mass concentration of the internet is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Example 2
A preparation method of fibrous flexible filler high-filling paper comprises the following steps:
s1: precipitated calcium carbonate and cellulose nanofibers as fillers for paper making were mixed in an amount of 10:1, mixing and uniformly stirring to obtain a mixture, adding the mixture into a PFI pulping machine, uniformly smearing the mixture on the periphery of the wall of a grinding disc, and performing common pulping under the condition that the pulping gap is 0.15mm and the pulping revolution is 10000r to obtain a composite filler; transferring the composite filler into a beaker, and after about 24 hours, gelatinizing to obtain the composite flexible filler; sucking the composite flexible filler by a needle cylinder, adding a needle head, and injecting the composite flexible filler into a hydraulic vortex with the rotating speed of 400rpm to obtain a fibrous flexible filler;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is intermittent equipment, and the single pulping capacity is about 300mL;
wherein the syringe is a 10mL syringe, and the inner diameter of the syringe needle is 0.45mm; the hydraulic vortex forming method comprises the following steps: adding 800mL of deionized water into a 1000mL beaker, and placing a digital display stirrer with a propeller at a position 10mm away from the bottom of the beaker to stir to generate the deionized water;
s2: taking broadleaf wood with plant fiber content: the mass ratio of the conifer wood is 3:1, mixing, fluffing, performing PFI pulping treatment, and obtaining mixed slurry, wherein the beating degree is 40 DEG SR; adding fibrous flexible filler into the mixed slurry according to the filling amount of 50% of the mass of the mixed slurry, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10s, performing net forming, and squeezing and drying to obtain fibrous flexible filler high-filling paper;
wherein, the mass concentration of the internet is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Example 3
Unlike example 1, in this example, the fibrous flexible filler was added to the mixed slurry in a filling amount of 60% by mass of the mixed slurry, and the remaining preparation process and experimental parameters were the same as those of example 1, to obtain a fibrous flexible filler highly filled paper.
Example 4
Unlike example 1, the injection needle in this example had an inner diameter of 0.21mm, and the rest of the preparation process and experimental parameters were the same as those of example 1, to obtain a fibrous flexible filler highly filled paper.
Example 5
Unlike example 1, the injection needle in this example had an inner diameter of 0.11mm, and the rest of the preparation process and experimental parameters were the same as those of example 1, to obtain a fibrous flexible filler highly filled paper.
Comparative example 1
The preparation method of the flexible filler high-filling paper comprises the following steps:
s1: the filler precipitated calcium carbonate for papermaking is selected, deionized water is added to prepare the filler liquid with the mass concentration of 10 percent, and the filler liquid is prepared by fully and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m;
s2: taking broadleaf wood with plant fiber content: conifer = 3:1, mixing, fluffing, performing PFI pulping treatment, obtaining mixed pulp, adding filling liquid into the mixed pulp according to 40% filling amount, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, forming on a net, and squeezing and drying to obtain flexible filler high-filling paper;
wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 2
The preparation method of the flexible filler high-filling paper comprises the following steps:
s1: the filler precipitated calcium carbonate for papermaking is selected, deionized water is added to prepare the filler liquid with the mass concentration of 10 percent, and the filler liquid is prepared by fully and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m;
s2: taking broadleaf wood with plant fiber content: conifer = 3:1, mixing, fluffing, performing PFI pulping treatment, obtaining mixed pulp, adding 50% of filling liquid into the mixed pulp, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, forming on a net, and squeezing and drying to obtain flexible filler high-filling paper;
wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 3
The preparation method of the flexible filler high-filling paper comprises the following steps:
s1: the filler precipitated calcium carbonate for papermaking is selected, deionized water is added to prepare the filler liquid with the mass concentration of 10 percent, and the filler liquid is prepared by fully and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m;
s2: taking broadleaf wood with plant fiber content: conifer = 3:1, mixing, fluffing, performing PFI pulping treatment, wherein the beating degree is 40 DEG SR, obtaining mixed pulp, adding the filling liquid into the mixed pulp according to the filling amount of 60%, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, forming on a net, and squeezing and drying to obtain the flexible filler high-filling paper;
wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 4
The preparation method of the flexible filler high-filling paper comprises the following steps:
s1: the filler for papermaking is selected to precipitate calcium carbonate and cellulose nano fiber according to the proportion of 10:1, adding deionized water to prepare a filler solution with the mass concentration of 10%, and fully and uniformly stirring to prepare the filler solution;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is 1.2-3.0 mmol/g in carboxyl content, and the mass concentration is 1.2%.
S2: taking broadleaf wood with plant fiber content: and (3) carrying out fluffing and PFI pulping treatment on a pulp board with a needle wood=3:1 after mixing, obtaining mixed pulp with a pulping degree of 40 DEG SR, adding filling liquid into the mixed pulp with a filling amount of 40%, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, carrying out net surfing forming, and carrying out squeezing and drying to obtain the flexible filler high-filling paper.
Wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 5
The preparation method of the flexible filler high-filling paper comprises the following steps:
s1: the filler for papermaking is selected to precipitate calcium carbonate and cellulose nano fiber according to the proportion of 10:1, adding deionized water to prepare a filler solution with the mass concentration of 10%, and fully and uniformly stirring to prepare the filler solution;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%.
S2: taking broadleaf wood with plant fiber content: conifer = 3:1, carrying out fluffing and PFI pulping treatment after mixing, obtaining mixed pulp, adding the filling liquid into the mixed pulp according to the filling amount of 50%, adding 2mL of 0.03% CPAM after mechanical stirring and mixing uniformly, carrying out net surfing forming after stirring for 10 seconds, and obtaining the flexible filler high-filling paper after squeezing and drying.
Wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 6
S1: the filler for papermaking is selected to precipitate calcium carbonate and cellulose nano fiber according to the proportion of 10:1, adding deionized water to prepare a filler solution with the mass concentration of 10%, and fully and uniformly stirring to prepare the filler solution;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%.
S2: taking broadleaf wood with plant fiber content: conifer = 3:1, carrying out fluffing and PFI pulping treatment after mixing, obtaining mixed pulp, adding the filling liquid into the mixed pulp according to the filling amount of 60%, adding 2mL of 0.03% CPAM after mechanical stirring and mixing uniformly, carrying out net surfing forming after stirring for 10 seconds, and obtaining the flexible filler high-filling paper after squeezing and drying.
Wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 7
S1: the filler for papermaking is selected to precipitate calcium carbonate and cellulose nano fiber according to the proportion of 10:1, mixing and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%.
S2: adding the blend uniformly mixed in the step S1 into a PFI pulping machine, uniformly smearing the blend on the periphery of the wall of a grinding disc, and performing common pulping under the condition that the pulping gap is 0.15mm and the pulping revolution is 15000 r;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is batch type equipment, and the single pulping capacity is about 300mL.
S3: transferring the composite filler subjected to the common pulping in the step S2 into a beaker, and gelling to form the composite flexible filler after about 24 hours;
s4: adding water into the composite flexible filler in the step S3 to prepare a suspension with the mass concentration of 10%, and fully stirring in 400rpm hydraulic vortex to prepare a filler liquid;
the hydraulic vortex forming method comprises the following steps: 800mL of deionized water was added to a 1000mL beaker, and the digital display stirrer with propeller was placed at a distance of 10mm from the bottom of the beaker and stirred to produce the product.
S5: taking broadleaf wood with plant fiber content: conifer = 3:1, carrying out fluffing and PFI pulping treatment after mixing, obtaining mixed pulp, adding filling liquid into the mixed pulp according to 40% filling amount, adding 2mL of 0.03% CPAM after mechanical stirring and mixing uniformly, carrying out net surfing forming after stirring for 10s, and obtaining the flexible filler high filling paper after squeezing and drying.
Wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 8
S1: the filler for papermaking is selected to precipitate calcium carbonate and cellulose nano fiber according to the proportion of 10:1, mixing and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%.
S2: and (3) adding the blend uniformly mixed in the step S1 into a PFI pulping machine, and uniformly smearing the blend on the periphery of the millstone wall. Co-refining under the condition that the refining gap is 0.15mm and the refining revolution is 15000 r;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is intermittent equipment, and the single pulping capacity is about 300mL;
s3: transferring the composite filler subjected to the common pulping in the step S2 into a beaker, and gelling after about 24 hours to form the composite flexible filler;
s4: adding water into the composite flexible filler in the step S3 to prepare a suspension with the mass concentration of 10%, and fully stirring in 400rpm hydraulic vortex to prepare a filler liquid;
the hydraulic vortex forming method comprises the following steps: 800mL of deionized water was added to a 1000mL beaker, and the digital display stirrer with propeller was placed at a distance of 10mm from the bottom of the beaker and stirred to produce the product.
(5) Taking broadleaf wood with plant fiber content: conifer = 3:1, mixing, fluffing, performing PFI pulping treatment, obtaining mixed pulp, adding 50% of filling liquid into the mixed pulp, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, forming on a net, and squeezing and drying to obtain flexible filler high-filling paper;
wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
Comparative example 9
S1: precipitating calcium carbonate and cellulose nanofibers with papermaking fillers at 10:1, mixing and uniformly stirring;
wherein the precipitated calcium carbonate has a triangle structure and an average particle diameter of 4.530 mu m; the cellulose nanofiber is gel-like cellulose nanofiber prepared by a TEMPO oxidation method, the diameter is 5-20 nm, the length is 1-3 mu m, the cellulose I-type crystal structure is formed, the carboxyl content is 2.0mmol/g, and the mass concentration is 1.2%;
s2: the blend obtained by uniformly mixing the S1 is added into a PFI pulping machine, and is uniformly smeared on the periphery of the millstone wall. Co-refining under the condition that the refining gap is 0.15mm and the refining revolution is 15000 r;
the rotating speed of the PFI pulping machine is 1200rpm, the PFI pulping machine is intermittent equipment, and the single pulping capacity is about 300mL;
s3: transferring the composite filler subjected to the common pulping in the step S2 into a beaker, and gelling after about 24 hours to form the composite flexible filler;
s4: adding water into the composite flexible filler in the step S3 to prepare a suspension with the mass concentration of 10%, and fully stirring in 400rpm hydraulic vortex to prepare a filler liquid;
the hydraulic vortex forming method comprises the following steps: adding 800mL of deionized water into a 1000mL beaker, and placing a digital display stirrer with a propeller at a position 10mm away from the bottom of the beaker to stir to generate the deionized water;
s5: taking broadleaf wood with plant fiber content: conifer = 3:1, mixing, fluffing, performing PFI pulping treatment, obtaining mixed pulp, adding the filling liquid into the mixed pulp according to the filling amount of 60%, mechanically stirring and uniformly mixing, adding 2mL of 0.03% CPAM, stirring for 10 seconds, forming on a net, and squeezing and drying to obtain the flexible filler high-filling paper;
wherein the mass concentration of the net surfing is 0.025%; the pressing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature is 105 ℃ and the time is 6min; basis weight of paper was 63g/m 2 。
The fibrous flexible filler high-filled papers prepared in examples 1 to 5 were examined using a tensile strength tester to measure the paper strength and a muffle furnace to measure the filler ash to calculate the retention, and the examination results are shown in table 1.
Table 1 comparative properties of examples 1 to 3 for the preparation of flexible filler highly filled papers
The filler ash content was measured using a tensile strength tester and a muffle furnace to calculate the filler retention, and the flexible filler high-filled papers prepared in comparative examples 1 to 9 were examined. The detection results are shown in Table 2.
Table 2 comparative examples 1 to 9 comparative properties of the highly filled papers
As can be seen from tables 1 and 2, the mechanical strength of the high-filled paper is obviously reduced along with the increase of the filler content, and compared with the paper forming performance of the conventional calcium carbonate filled paper and the fibrous flexible filler filled paper in the case that the plant fiber content is the same in comparative example 1 and examples 3, the mechanical strength of the flexible filler filled paper prepared by the method is obviously improved compared with that of the conventional preparation method. Meanwhile, compared with the simple blending and filling of the precipitated calcium carbonate/cellulose nanofiber, the fibrous composite flexible filler prepared by the invention has obviously improved paper strength performance and filler retention rate under the same filling amount as compared with the fibrous composite flexible filler prepared by the invention in examples 1-3, because an obvious composite structure is formed between the cellulose nanofiber and the precipitated calcium carbonate under the strong mechanical co-grinding effect, the interface combination of the filler and the fiber and the filler is obviously enhanced, the gaps and pore diameters between the fiber and the filler are reduced, the formed paper is more compact, the thickness is reduced, and the strength is obviously improved. Comparative example 3 it can be seen that the fibrous flexible filler has higher paper strength properties and filler retention than examples 1-3. This is because the fibrous fillers are entangled with the fibers and the fine fibers produced by beating in the sheet, and the physical entanglement is provided in addition to the chemical bonding of the surfaces, further improving the strength properties of the sheet. Further, as compared with examples 1, 4 and 5, it was found that as the fibrous filler diameter was reduced, more fiber-entangled structures could be formed, and the effect of improving the paper strength properties was more remarkable.
FIG. 1 is a flow chart of a process for preparing a fibrous flexible filler, wherein precipitated calcium carbonate and TEMPO oxidized cellulose nanofibrils are mixed and then put into a PFI pulping machine for co-grinding, and the materials are subjected to mechanical forces such as shearing force, friction force, impact force and the like in disc grinding, so that mechanochemical effects are generated to crosslink between the calcium carbonate and the nanocellulose, and the flexible filler is obtained after gelation. Based on the flexibility, a fibrous flexible filler with a certain length-diameter ratio is prepared by adopting an injection molding mode.
From fig. 2a to 2d, which show the microscopic morphology of the prepared flexible filler with different diameters, fig. 2e shows that the flexible composite filler can be clearly recognized on the surface of the highly filled paper of the flexible filler, the flexible composite filler still maintains a certain shape in the handsheet, and the wood fibers with smaller size are interweaved and attached on the surface of the linear flexible composite filler or penetrate into the interior of the flexible filler, and the interweaving and attaching nature is generated by the interaction of hydrogen bonds and interweaving force based on the shape of the self. The series of dewatering and pressing processes of handsheet formation makes this connection stronger by external force, and another reason for enhancing this effect is that fine fibers brought about by mashing and fibrillation are rooted in the composite filler; fig. 2f is a partial enlarged view of a composite flexible filler, from which it can be found that the surface of precipitated calcium carbonate of the spindle body is tightly covered with a network of cellulose nanofibrils, thereby forming a compact composite structure, and the groups carried by nanofibrils covered on the surface of precipitated calcium carbonate enable a good combination of inert fillers on the surface and fibers, and between fillers and fillers, thereby significantly improving the strength properties of the high-filled paper.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. The preparation method of the fibrous flexible filler high-filling paper is characterized by comprising the following steps of:
s1: performing co-pulping on a mixture consisting of precipitated calcium carbonate and cellulose nano fibers to obtain a composite filler; the composite filler is gelled to obtain the composite flexible filler; injecting the composite flexible filler into the hydraulic vortex to obtain a fibrous flexible filler;
s2: fluffing the plant fiber pulp board and pulping together to obtain mixed pulp; adding fibrous flexible filler into the mixed slurry, then adding cationic polyacrylamide, stirring, screening to form, and squeezing and drying to obtain fibrous flexible filler high-filling paper;
s1, a pulping gap of the common pulping is 0.15mm, and the pulping revolution is 10000r; the precipitated calcium carbonate has a triangle structure, and the average grain diameter is 4.530 mu m; the cellulose nanofiber is prepared by a TEMPO oxidation method, and has a cellulose I-type crystal structure; the diameter of the cellulose nanofiber is 5-20 nm, the length of the cellulose nanofiber is 1-3 mu m, the carboxyl content of the cellulose nanofiber is 2.0mmol/g, and the mass concentration of the cellulose nanofiber is 1.2%;
in the S1, the gelation time is 12-24 hours; the hydraulic vortex is formed by stirring the stirrer in water; the rotation speed of the hydraulic vortex is 400rpm; injecting the composite flexible filler into the hydraulic vortex by adopting an injection needle cylinder; the syringe is a 10mL syringe, and is provided with an injection needle with an inner diameter of 0.11-0.45 mm.
2. The method for preparing fibrous flexible filler highly filled paper according to claim 1, wherein in S1, the mass ratio of the precipitated calcium carbonate to the cellulose nanofiber is 10:1.
3. the method for producing a fibrous flexible filler highly filled paper according to claim 1, wherein in S2, the freeness of the mixed slurry is 40 ° SR; the plant fiber pulp board is a hardwood pulp board and a softwood pulp board; the mass ratio of the hardwood pulp plate to the softwood pulp plate is 3:1.
4. the method for preparing the fibrous flexible filler high-filling paper according to claim 1, wherein in the step S2, the mass of the fibrous flexible filler is 40% -60% of the mass of the mixed slurry.
5. The method for preparing fibrous flexible filler highly filled paper according to claim 1, wherein in S2, the cationic polyacrylamide is prepared into an aqueous solution with a mass concentration of 0.03% before use; the dosage of the cationic polyacrylamide is 2mL.
6. The method for preparing fibrous flexible filler high-filled paper according to claim 1, wherein in the step S2, the stirring time is 10-20S; the mass concentration of the net surfing during net surfing forming is 0.025%; the squeezing conditions are as follows: the pressure is 0.4MPa, and the time is 4min; the drying conditions are as follows: the temperature was 105℃and the time was 6min.
7. The fibrous flexible filler high-filling paper is characterized by being prepared by the preparation method of the fibrous flexible filler high-filling paper according to any one of claims 1-6.
8. A fibrous flexible filled high filler paper according to claim 7, characterized in that the basis weight of the fibrous flexible filled high filler paper is 63g/m 2 。
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| CN103938488A (en) * | 2014-04-29 | 2014-07-23 | 陕西科技大学 | Method for preparing porous calcium silicate/ fiber co-milled filled paper |
| CN103966896A (en) * | 2013-02-05 | 2014-08-06 | 金东纸业（江苏）股份有限公司 | Modified filler and preparation method thereof, pulp stock applying modified filler and paper |
| CN104863008A (en) * | 2015-04-23 | 2015-08-26 | 中国制浆造纸研究院 | Method using microfibrillated cellulose modified filling material for improving paper nontransparency |
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| EP2236545A1 (en) * | 2009-03-30 | 2010-10-06 | Omya Development AG | Process for the production of nano-fibrillar cellulose gels |
| TW201142107A (en) * | 2010-04-27 | 2011-12-01 | Omya Development Ag | Process for the manufacture of structured materials using nano-fibrillar cellulose gels |
| CN103966896A (en) * | 2013-02-05 | 2014-08-06 | 金东纸业（江苏）股份有限公司 | Modified filler and preparation method thereof, pulp stock applying modified filler and paper |
| CN103938488A (en) * | 2014-04-29 | 2014-07-23 | 陕西科技大学 | Method for preparing porous calcium silicate/ fiber co-milled filled paper |
| CN104863008A (en) * | 2015-04-23 | 2015-08-26 | 中国制浆造纸研究院 | Method using microfibrillated cellulose modified filling material for improving paper nontransparency |
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