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EP0249891B1 - Procédé de préparation de papier et carton - Google Patents

Procédé de préparation de papier et carton Download PDF

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Publication number
EP0249891B1
EP0249891B1 EP87108446A EP87108446A EP0249891B1 EP 0249891 B1 EP0249891 B1 EP 0249891B1 EP 87108446 A EP87108446 A EP 87108446A EP 87108446 A EP87108446 A EP 87108446A EP 0249891 B1 EP0249891 B1 EP 0249891B1
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EP
European Patent Office
Prior art keywords
phenol
pulp
polymers
vinylformamide
drainage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP87108446A
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German (de)
English (en)
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EP0249891A1 (fr
Inventor
Friedrich Dr. Linhart
Hans-Juergen Dr. Degen
Werner Auhorn
Michael Dr. Kroener
Heinrich Dr. Hartmann
Wilfried Dr. Heide
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BASF SE
Original Assignee
BASF SE
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Publication date
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Priority to AT87108446T priority Critical patent/ATE55789T1/de
Publication of EP0249891A1 publication Critical patent/EP0249891A1/fr
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Publication of EP0249891B1 publication Critical patent/EP0249891B1/fr
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates

Definitions

  • crosslinked polyamidoamines grafted with ethyleneimine as dewatering and retention agents in the production of paper.
  • Suitable crosslinking agents are a, m-dichlorohydrin ethers of polyalkylene oxides with 8 to 100 alkylene oxide units. The crosslinking is carried out so far that the resulting products are still water-soluble.
  • Anionic polyacrylamides are used to some extent in practice as retention and drainage agents in the manufacture of paper. However, it is necessary to use a cationic additive which fixes the anionic polymer to the negatively charged surfaces of the particles.
  • Suitable cationic additives that are used in practice for this purpose are, for example, aluminum salts or cationic starches.
  • nonionic water-soluble polymers such as high molecular weight polyacrylamides
  • nonionic products can only be adsorbed onto the negatively charged particles of the pulp by means of comparatively weak hydrogen bonds.
  • the effectiveness of the nonionic products is therefore low, but is by no means reduced to the extent of dissolved or colloidally distributed anionic compounds in the paper stock, as is the case when using cationic polymers.
  • the anionic compounds present in the paper stock accumulate in the returned water due to the increasingly restricted water cycles of the paper mills in recent years and interfere with the effectiveness of cationic polymeric auxiliaries in dewatering the paper stock and with retention.
  • the invention has for its object to provide a drainage, retention aid and flocculant for the papermaking process, which is more effective than known nonionic auxiliaries and whose effectiveness is not adversely affected by anionic contaminants.
  • the dewatering of the paper stock is additionally carried out in the presence of 0.02 to 1.0% by weight, based on dry paper stock, of a synthetic phenolic resin or natural oligomers and / or polymers containing phenolic groups.
  • a paper stock is dewatered, for the production of which all fiber qualities come into consideration, either alone or as a mixture with one another.
  • water is used for the production of the paper stock, which is at least partially or completely returned from the paper machine. These are either clarified or unclarified white water and mixtures of such water qualities.
  • the returned water contains more or less large amounts of so-called contaminants, which are known to severely impair the effectiveness of cationic drainage and retention aids.
  • the content of such contaminants in the paper stock is usually characterized by the sum parameter chemical oxygen demand (COD value). With this sum parameter also phenolic compounds are er that do not necessarily interfere per se, but as degradation products of lignin always occur as accompanying substances for interfering substances.
  • the COD values are 300 to 30,000, preferably 1,000 to 20,000 mg oxygen / kg of the aqueous phase of the paper stock.
  • wood pulp includes wood pulp, thermomechanical material (TMP), chemo-thermomechanical material (CTMP), pressure grinding, semi-pulp, high-yield pulp and refiner mechanical pulp (RMP).
  • TMP thermomechanical material
  • CMP chemo-thermomechanical material
  • RMP refiner mechanical pulp
  • suitable pulps are sulfate, sulfite and sodium pulps.
  • unbleached pulps which are also referred to as unbleached kraft pulp, are preferably used.
  • Suitable 1-year plants for the production of paper materials are, for example, rice, wheat, sugar cane and kenaf.
  • a paper stock containing interfering substances can advantageously be dewatered with high molecular weight, water-soluble polymers of N-vinylamides and increased retention and flocculation of fibers and fillers can be achieved.
  • the homopolymers or copolymers of N-vinylformamide, N-vinyl acetamide, N-methyl-N-vinyl formamide, N-methyl-N-vinyl acetamide, N-ethyl-N-vinyl formamide, N-ethyl-N-vinyl acetamide and N are suitable -Vinyl propionamide.
  • Suitable comonomers are acrylamide, methacrylamide, acrylonitrile, methacrylonitrile, acrylic acid esters of monohydric Ci to G 18 alcohols, methacrylic acid esters of monohydric C 1 to C 18 alcohols, vinyl acetate, vinyl propionate, vinyl butyrate, vinyl methyl ether, vinyl ethyl ether, vinyl n-butyl ether and vinyl isobutyl ether.
  • the copolymers of compounds of the formula I contain at least 50, preferably 80 to 99% by weight of a compound of the formula I copolymerized.
  • the homopolymers and copolymers are in non-hydrolyzed form and therefore do not contain any amino groups.
  • K value of at least 130 (determined according to H. Fikentscher in 5% by weight saline solution at 25 ° C and a polymer concentration of 0.1% by weight).
  • the K value of the homopolymers and copolymers is preferably in the range from 160 to 250.
  • the compounds of the formula II are homopolymers or copolymers of N-vinylpyrrolidone, N-vinylpiperidone, N-vinylcaprolactam, N-vinyl-3-methylpyrrolidone, N-vinyl-5-methylpyrrolidone, N-vinyl-5-phenylpyrrolidone , N-vinyl-3-benzylpyrrolidone, N-vinyl-4-methylpiperidone, N-vinyl-2-oxazolidone, N-vinyl-5-methyl-2-oxazolidone, N-vinyl-5-ethyl-2-oxazolidone , N-vinyl-5-phenyl-2-oxazolidone, N-vinyl-4-methyl-2-oxazolidone, N-vinyl-3-oxazid-2-one and N-vinylmorpholinone.
  • the polymers have a K value of at least 130 (determined according to H. Fikentscher in 5% sodium chloride solution at 25 ° C. and a polymer concentration of 0.1% by weight).
  • the K value of these polymers is preferably in the range from 160 to 250.
  • suitable comonomers for the preparation of the copolymers are acrylamide, methacrylamide, acrylonitrile, methacrylonitrile, acrylic acid esters of monohydric C1 to C 18 alcohols and the corresponding methacrylic acid esters .
  • Copolymers can also be prepared which contain two or more comonomers in copolymerized form.
  • the copolymers contain at least 50% by weight of compounds of the formula II in copolymerized form, preferably 80 to 99% by weight.
  • Copolymers of compounds of the formula I and the formula 11 are of particular importance.
  • These comonomers can be copolymerized with one another in any ratio and used in the process according to the invention.
  • the copolymers of N-vinylformamide and N-vinylpyrrolidone and copolymers of N-vinylformamide and N-vinylcaprolactam are examples of the copolymers of N-vinylformamide and N-vinylpyrrolidone and copolymers of N-vinylformamide and N-vinylcaprolactam.
  • the homopolymers and copolymers which act as drainage, retention and flocculants are used in an amount of 0.002 to 0.1, preferably 0.005 to 0.05,% by weight.
  • the polymers are added to the paper stock in a very dilute solution, as is customary when using other high molecular weight water-soluble polymers.
  • the concentration in the aqueous solution is generally between 0.001 to 0.1% by weight.
  • the high molecular weight compounds containing N-vinylamides polymerized develop their effectiveness as drainage, retention and flocculants in the presence of interfering substances which, as accompanying substances, contain phenolic groups-containing oligomers and / or polymers from the constituents of the wood which are used in paper production in restricted or closed form Water cycles are always present. If the paper stock to be dewatered does not contain any oligomers or polymers containing phenolic groups, such compounds can be added to the paper stock before dewatering without this having an adverse effect on the effectiveness of the polymers to be used according to the invention.
  • polymers of N-vinylamides and phenolic group-containing oligomers or polymers result in a synergistic effect in dewatering, retention and flocculation.
  • the compounds containing phenolic groups are either synthetic phenolic resins or natural oligomers and / or polymers containing phenolic groups. Mixtures of natural and synthetic products can also be used. Examples of synthetic products are phenolic resins, which can be obtained by condensation from phenol and aldehydes, such as formaldehyde, acetaldehyde, propionaldehyde, n-butyraldehyde and isobutyraldehyde.
  • phenolic resins come into consideration which result from the condensation of phenol and formaldehyde.
  • Resol or novolak type resins are suitable.
  • Resol-type resins are known to mean phenol-formaldehyde resins which are formed by the condensation of phenol with formaldehyde in an alkaline medium.
  • Non-curable phenolic resins or Novoiak type resins are produced by the condensation of phenol with formaldehyde in the presence of acids.
  • Resol or novolak type resins are preferably used in the form of alkaline aqueous solutions. The pH of the solutions is 9 to 14.
  • Phenolic resins of the novolak or resol type are described, for example, in Ullmanns Encyklopadie der Technischen Chemie, 4th edition, Verlag Chemie, Weinheim 1979, volume 18, pages 245-257.
  • the phenolic resins in question are preferably water-soluble or water-dispersible. Based on dry paper stock, the phenolic resins are added in an amount of 0.02 to 1, preferably 0.05 to 0.4% by weight.
  • Natural oligomers or polymers containing phenol groups are the known wood extracts, lignin degradation products from sulfate pulp production, the so-called kraft lignin, and humic acids or their salts.
  • the wood extracts contain lignin degradation products, i.e. phenolic oligomers.
  • the exact composition of the natural products is not known and strongly depends on the working conditions when extracting them.
  • phenolic groups on their surface, which are more numerous the less bleached.
  • the presence of phenolic compounds in the paper stock promotes the drainage-accelerating properties of the poly-N-vinylamides.
  • a major advantage of the process according to the invention is the insensitivity to the presence of contaminants. In the production of wood-free white papers, the whiteness of the paper is hardly affected by the drainage and retention agents compared to the corresponding cationic products.
  • the parts given in the examples are parts by weight. The percentages relate to the weight of the fabrics.
  • Determining the dewatering time 1 l of the pulp slurry to be tested is dewatered in a Schopper-Riegler test device. The time that is determined for different outlet volumes is evaluated as a criterion for the drainage rate of the substance suspension examined in each case. The drainage times were determined after a run of 500 or 600 ml of water.
  • Optical permeability of the white water it was determined with the aid of a photometer and is a measure of the retention of fine and fillers. It is given in percent. The higher the value for the optical permeability, the better the retention.
  • the charge density was determined according to D. Horn, Polyethyleneimine - Physico Chemical Properties and Application, (IUPAC) Polymeric Amins and Ammoniumsalts, Pergamon Press Oxford and New York, 1980, pages 333-355.
  • a pulp with a consistency of 2 g / l is made from unprinted newsprint of Central European origin and 0.2 g / l of kaolin is added to the pulp.
  • the paper stock has a pH of 7.3.
  • the drainage rate for the substance so produced is determined (see (a) in Table 1).
  • (b) is added to part of the pulp 0.1%, based on dry pulp, phenol I and again the dewatering rate and the optical permeability of the white water are determined.
  • Another sample of the material thus produced is then mixed with 0.02% polymer VII in accordance with (c) and the dewatering effect and the optical permeability of the white water are assessed.
  • Another substance sample (d) is first mixed with 0.1% phenol 1 and then with 0.02% polymer VII and tested for dewatering rate in a Schopper-Riegler device. The specified additional quantities always refer to dry paper stock. The following results are determined:
  • a paper stock is made from 80 parts of bleached sulfite pulp and 20 parts of kaolin and the consistency is adjusted to a value of 2 g / l.
  • the pH of the substance is 7.5, the COD 440 mg 0 2 / kg.
  • sheets are formed with the help of the Rapid-Köthen device and their basis weight and filler content are determined. The higher these two values, the better the retention.
  • 2 test series are carried out, (a) 0 - 0.04%, based on dry fiber, of polymer VII is added to the paper stock mentioned above and (b) in which the paper stock is first treated with phenol I in an amount of 0.1% and then the amounts of polymer VII given in the table.
  • a paper stock in demineralized water from ground wood with a consistency of 2 g / l is produced using 200 ml spruce wood extract / 1 paper stock.
  • the paper stock has a pH value of 5.
  • the spruce wood extract is obtained by boiling 3 kg of spruce wood chips in 30 l of demineralized water for 2 hours and has a COD value of 3,400 mg 0 2 / kg.
  • the tests given in Table 4 are then carried out, (a) firstly in the absence of additional phenol-containing compounds and then (b) after the addition of 0.1% of phenol II to the pulp, the dewatering and permeability of the white water are determined.
  • poly-N-vinylformamide is a more effective drainage agent than a commercially available very effective cationic polyacrylamide.
  • the effectiveness of poly-N-vinylformamide is particularly evident after the addition of phenolic resin to the paper stock.
  • Test (g) is an example according to the invention and shows that poly-N-vinylformamide is an effective drainage and retention agent after the addition of a phenolic compound.
  • a substance is first prepared from 75 parts of ground wood, 25 parts of bleached sulfate pulp, 20 parts of kaolin, 0.5% aluminum sulfate and the consistency is adjusted to 2 g / l.
  • the pH of the substance is 6.
  • the dewatering time and optical permeability of the white water for this substance and the polymers specified in tables (b) to (d) are investigated, and then a further series of experiments is carried out, in which the first step is to Substance described above 0.1% phenol and then the amounts of polymers given in the table under (b) to (d).
  • a paper stock from unprinted newsprint of Central European origin with a pH of 6 and 0.5% aluminum sulfate and a consistency of 2 g / l is dewatered under the conditions (a) to (d) given in Table 8.
  • Test (d) is an example according to the invention and shows that natural phenol group-containing compounds with poly-N-vinylformamide also have a synergistic effect in dewatering and retention during papermaking.
  • the drainage time and optical permeability of the white water are checked on a paper stock that consists of 100% semi-pulp and is adjusted to a stock density of 2 g / l.
  • the pH of the substance is 8.2.
  • This material model is a pulp that contains a lot of contaminants and whose aqueous phase has a COD of 1 100 mg 0 2 / kg.
  • a highly cationic polymer that is highly effective under other conditions is practically no longer effective under these conditions (values from test series (b) are comparative examples), while poly-N-vinylformamide according to test series (a) is a dewatering and retention agent which is effective under these conditions.
  • the tests (a) to (e) are carried out on a paper stock which consists of 30 parts of bleached sulfate pulp, 70 parts of bleached beech sulfite pulp and 30 parts of kaolin.
  • the consistency is adjusted to 2 g / l, the pH of the pulp is 7.2, the freeness is 45 Schopper-Riegler, and the COD of the aqueous phase is 420 mg 0 2 / kg.
  • the fabric is dewatered in each case under the conditions given in Table 13 in a Rapid-Köthen device, leaves with a basis weight of 60 g / m 2 being obtained.
  • the filler content of the paper sheets is a measure of the retention.
  • the whiteness of the paper sheets was measured using an Elrepho device.
  • a wastewater is produced as a model substance which contains 1.25 g / l of a highly ground thermomechanical wood pulp (TMP) and has a pH of 6.
  • TMP thermomechanical wood pulp
  • the test series (b) is an example according to the invention.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)
  • Machines For Manufacturing Corrugated Board In Mechanical Paper-Making Processes (AREA)
  • Making Paper Articles (AREA)
  • Cartons (AREA)
  • Containers And Packaging Bodies Having A Special Means To Remove Contents (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
  • Diaphragms For Electromechanical Transducers (AREA)
  • Ultra Sonic Daignosis Equipment (AREA)

Claims (7)

1. Procédé de fabrication de papier, de carte et de carton par déshydratation d'une pâte à papier en présence d'agents de déshydratation, de rétention et de floculation, avec formation de la feuille, caractérisé en ce que l'on utilise, à titre d'agents de déshydratation, de rétention et de floculation, des polymères de N-vinylamides, de poids moléculaires élevés, solubles dans l'eau, de la formule (I)
Figure imgb0021
dans laquelle RI, R2 représentent des atomes d'hydrogène, des radicaux CH3 et CH2
et en ce qu'on réalise la déshydratation de la pâte en la présence complémentaire de 0,02 à 1,0% en poids, par rapport à la pâte sèche, d'une résine phénolique synthétique ou de polymères et/ou d'oligomè- res naturels contenant des radicaux phénol.
2. Procédé suivant la revendication 1, caractérisé en ce qu'à titre d'agent de déshydratation, de rétention et de floculation, on utilise des homopolymères ou copolymères du N-vinyl-formamide, du N-vinylacétamide, du N-méthyl-N-vinyl-formamide, du N-méthyl-N-vinylacétamide, du N-éthyl-N-vinylformamide, du N-éthyl-N-vinylacétamide, et du N-vinylpropionamide, où les polymères sont exempts de radicaux aminoalkyle et possèdent une valeur K d'au moins 130 (telle que déterminée selon H. Fikentscher en solution à 5% en poids de sel de cuisine à 25°C et à une concentration en polymère de 0,1% en poids.
3. Procédé suivant la revendication 1 ou 2, caractérisé en ce que l'on utilise des copolymères du N-vinylformamide et de la N-vinylpyrrolidone, ou du N-vinylformamide et du N-vinylcaprolactame.
4. Procédé suivant la revendication 1 ou 2, caractérisé en ce qu'à titre de résines phénoliques synthétiques, on utilise des produits de condensation du phénol et du formaldéhyde du type résol ou novolaque.
5. Procédé suivant la revendication 1, caractérisé en ce qu'à titre de polymères et/ou d'oligomères contenant des radicaux phénol, on utilise des composés du type acide lignique ou acide humique.
6. Procédé suivant la revendication 1, caractérisé en ce qu'à titre de polymères et/ou d'oligomères naturels contenant des radicaux phénol, on utilise un extrait de bois.
7. Procédé suivant l'une quelconque des revendications 1 à 6, caractérisé en ce qu'à titre de pâte à papier, on utilise la pâte de bois, la pâte mi-chimique et/ou la pâte au sulfate, non blanchie.
EP87108446A 1986-06-14 1987-06-11 Procédé de préparation de papier et carton Expired - Lifetime EP0249891B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87108446T ATE55789T1 (de) 1986-06-14 1987-06-11 Verfahren zur herstellung von papier, pappe und karton.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3620065 1986-06-14
DE19863620065 DE3620065A1 (de) 1986-06-14 1986-06-14 Verfahren zur herstellung von papier, pappe und karton

Publications (2)

Publication Number Publication Date
EP0249891A1 EP0249891A1 (fr) 1987-12-23
EP0249891B1 true EP0249891B1 (fr) 1990-08-22

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EP87108446A Expired - Lifetime EP0249891B1 (fr) 1986-06-14 1987-06-11 Procédé de préparation de papier et carton

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Country Link
US (1) US4772359A (fr)
EP (1) EP0249891B1 (fr)
JP (1) JP2605043B2 (fr)
AT (1) ATE55789T1 (fr)
AU (1) AU586781B2 (fr)
CA (1) CA1287453C (fr)
DE (2) DE3620065A1 (fr)
FI (1) FI88062C (fr)
NO (1) NO166735C (fr)
NZ (1) NZ220553A (fr)
ZA (1) ZA874222B (fr)

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JP6325813B2 (ja) * 2012-12-27 2018-05-16 栗田工業株式会社 ピッチ抑制剤、ピッチ抑制方法、及び脱墨パルプの製造方法
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EP0017353B2 (fr) * 1979-03-28 1992-04-29 Ciba Specialty Chemicals Water Treatments Limited Production de papier et de carton
US4444662A (en) * 1979-10-22 1984-04-24 Applied Membrane Technology, Inc. Microporous laminate
DE3213873A1 (de) * 1982-04-15 1983-10-27 Basf Ag, 6700 Ludwigshafen Flockungsmittel fuer schlaemme
DE3128478A1 (de) * 1981-07-18 1983-02-03 Basf Ag, 6700 Ludwigshafen Verfahren zur herstellung von linearen, basischen polymerisaten
FI70230C (fi) * 1981-07-18 1986-09-15 Basf Ag Rakkedjiga basiska polymerisat foerfarande foer deras framstaellning och deras anvaendning
US4644020A (en) * 1983-01-28 1987-02-17 Phillips Petroleum Company Production of high molecular weight vinyl lactam polymers and copolymers

Also Published As

Publication number Publication date
US4772359A (en) 1988-09-20
DE3620065A1 (de) 1987-12-17
AU586781B2 (en) 1989-07-20
FI872610L (fi) 1987-12-15
EP0249891A1 (fr) 1987-12-23
ZA874222B (en) 1989-02-22
DE3764407D1 (de) 1990-09-27
NO166735C (no) 1991-08-28
NZ220553A (en) 1989-01-06
FI88062C (fi) 1993-03-25
ATE55789T1 (de) 1990-09-15
FI872610A0 (fi) 1987-06-11
NO166735B (no) 1991-05-21
NO872454L (no) 1987-12-15
CA1287453C (fr) 1991-08-13
AU7418387A (en) 1987-12-17
JP2605043B2 (ja) 1997-04-30
FI88062B (fi) 1992-12-15
JPS62299600A (ja) 1987-12-26
NO872454D0 (no) 1987-06-12

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