US20090044921A1 - Bentonite for binding impurities during paper production - Google Patents

Bentonite for binding impurities during paper production Download PDF

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US20090044921A1
US20090044921A1 US11/721,229 US72122905A US2009044921A1 US 20090044921 A1 US20090044921 A1 US 20090044921A1 US 72122905 A US72122905 A US 72122905A US 2009044921 A1 US2009044921 A1 US 2009044921A1
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bentonite
cec
paper
impurities
pulp
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Ulrich Sohling
Hubertus Besting
Genovefa Wendrich
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Sued Chemie AG
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Sued Chemie AG
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/02—Agents for preventing deposition on the paper mill equipment, e.g. pitch or slime control
    • 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
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays

Definitions

  • the present invention relates to the use of special bentonites having a high cation exchange capacity in the binding or removal of impurities in paper production.
  • humic acids for example, humic acids, tree resin colloids, lignin derivatives, ligninsulfonates, which are introduced from the fibers into the paper circulation.
  • anionic impurities which are introduced into the paper machine by recycling of broke. This broke is typically re-dispersed and introduced into the paper machine. As a result, the ingredients and auxiliaries present therein are completely recycled into the circulation. For example, carboxymethylcelluloses, polyacrylates, polyphosphonates and silicates are additionally introduced thereby.
  • Further anionic charged impurities are the latices which are used in the paper coat, which are typically hydrophobic but also carry anionic charges. These have a strong tendency to agglomeration, the agglomerates being deposited as tacky, white residues on the paper machine (so-called white pitch).
  • montmorillonites such as bentonite
  • bentonite for controlling impurities in the paper pulp
  • the alkali treatment of bentonites is also discussed as a possibility.
  • U.S. Pat. No. 4,964,955 likewise describes a process for reducing the impurities in paper production.
  • a particulate composition containing (a) a water-soluble cationic polymer which is applied to (b) a substantially water-insoluble particulate substrate is used for binding impurities.
  • the polymer should be sufficiently electropositive so that the particulate composition has a zeta potential of at least about +30 mV.
  • the polymer is preferably a poly(dialkyldiallylammonium halide).
  • the substrate is, for example, a phyllosilicate mineral.
  • EP 0 760 406 A2 relates to a combination of a poly(dadmac/acrylamide) and a bentonite for binding impurities.
  • GB 2 297 334 A in turn discloses the use of a smectic clay for controlling impurities, the smectic clay being modified as follows: monovalent exchangeable cations are present in an equivalent ionic fraction in the range of from 0.20 to 0.60; a first type of bivalent exchangeable cations is present in an equivalent ionic fraction in the range of from 0.40 to 0.80; and a second type of bivalent exchangeable cations is present in an equivalent ionic fraction in the range of from 0.00 to 0.20, the first type of bivalent exchangeable cations comprising calcium and the second type of bivalent exchangeable cations comprising magnesium.
  • compositions used in the prior art for binding impurities are very expensive and not optimally suitable for certain impurity compositions. There is therefore a constant need for compositions for binding impurities in paper production.
  • An object of the present invention was therefore to provide an improved process for binding impurities in paper production, in which a composition which is easy and economical to prepare can be used and which permits a high degree of binding of impurities, including hydrophobic fractions.
  • this object is achieved by the method as claimed in claim 1 .
  • a bentonite which has a proportion of the monovalent cations, based on the cation exchange capacity (referred to herein as CEC), of at least about 0.7 (i.e. 70%), and a CEC (total) of at least 85 meq/100 g.
  • impurities are understood as meaning both tacky substances, referred to in the literature as stickies, and so-called pitch, i.e. primarily tree resin components. Reference may be made here to the statements made in the introduction to the description with regard to the impurities. A detailed list of the pitch and stickies constituents is to be found, for example, in Wo01/71092 on pages 1 and 2, and the disclosure there is hereby expressly incorporated by reference into the present description.
  • the impurities are thus primarily anionic (negatively charged) or hydrophobic.
  • the highly activated bentonites used according to the invention and having a high CEC can very readily bind both anionic and hydrophobic impurity fractions and can neutralize them in their harmful effects.
  • the bentonites used according to the invention themselves have a relatively high negative layer charge and subsequently make this high (negative) surface charge available in delaminated form to the paper pulp. Thus, good binding of impurities would not be expected for anionic or hydrophobic impurities.
  • a calcium bentonite binds such impurities better because a major part of the charges of the bentonites is saturated by the calcium ions and these could immobilize impurities, for example, via soap formation and fatty acids in the tree resin.
  • the stickies such as tree resin particles, contain many rather nonpolar (hydrophobic) components, e.g. triglycerides. These should bind particularly well to nonpolar surfaces, such as, for example, those of talc. Talc has no surface charges and is therefore also described in the prior art as being optimum for the binding of (hydrophobic) impurities.
  • paper pulp and fiber suspension are intended generally to include all impurity-containing compositions or streams which are used in paper production. Otherwise, the expressions “pulp” and “fiber suspension” are familiar to the person skilled in the art and need not be explained in detail here.
  • the pulp or the fiber suspension is a (fine) groundwood-containing suspension.
  • Groundwood is in general finely digested (finely beaten wood, generally without further chemical or thermal treatment).
  • the groundwood suspension is either used directly after comminution or is subjected to a peroxide bleach, in which case so-called peroxide-bleached groundwood forms.
  • peroxide bleach in which case so-called peroxide-bleached groundwood forms.
  • the bentonite used according to the invention gives particularly good results in the case of paper types containing groundwood or peroxide-bleached groundwood.
  • the method according to the invention can also be advantageously used in the case of other paper types.
  • the pulp or fiber suspension may also contain highly purified fiber fractions, as is the case, for example, in so-called newsprint paper.
  • the invention furthermore gives very good results in the case of so-called “deinked pulp” (DIP).
  • DIP deinked pulp
  • This is a paper stock which is produced from wastepaper.
  • hydrophobic stickies occur there, from the stickies of magazines and newspapers.
  • paper stocks in which the bentonite according to the invention can be advantageously used comprise TMP (thermomechanical pulp) sulfate pulp, sulfite pulp and mixtures of different chemical pulps. Depending on the paper type and localization of the paper mill, such chemical pulps are mixed in different ratios and adapted to the material requirements of the end product.
  • the preferred groundwood fraction in the paper pulp or fiber suspension is at least 10% by weight, in particular at least 30% by weight, based in each case on the dry weight of the total pulp or suspension.
  • the bentonite in the method according to the invention probably acts without the invention being limited to the correctness of this assumption, in that it binds the impurities or interacts with them and thus, counteracts the aggregation and deposition on the parts of the paper machine, such as, for example, the rolls.
  • the bentonite used has a cation exchange capacity (CEC) of at least 85 meq/100 g, preferably at least 90 meq/100 g, in particular at least 95 meq/100 g.
  • CEC cation exchange capacity
  • CEC Core exchange capacity
  • the cation exchange capacity thus comprises, for example, the sum of all exchangeable divalent and monovalent cations, such as calcium, magnesium, sodium, lithium and potassium ions.
  • the bentonite is treated with an ammonium chloride solution. Owing to the high affinity of the ammonium ions for the bentonite, virtually all exchangeable cations are exchanged for ammonium ions. After separation and washing, the nitrogen content of the bentonite is determined and the content of ammonium ions is calculated therefrom.
  • contact can be established in any desired manner familiar to the person skilled in the art, for example by preparing a solids mixture, a suspension with the phyllosilicate and the sodium carbonate or treatment or spraying of the phyllosilicate with a solution of the sodium carbonate.
  • a calcium-containing crude bentonite having a water content of from about 25 to 40% by weight is kneaded with solid sodium carbonate, dried and milled.
  • the crude bentonite is broken beforehand into pieces of less than 3 cm diameter. If the crude bentonite does not have the stated water content, this is established by spraying with water.
  • the activation can also be effected, for example, as follows: 350 g of crude bentonite having a water content of from about 30 to 35% by weight are introduced into a mixing apparatus (for example a Werner & Pfleiderer mixer (kneader)) and kneaded for 1 minute. The amount of sodium carbonate (soda) which corresponds to the difference between CEC and sodium content of the bentonite is then added while the mixing apparatus continues to run and further kneading is effected for 10 min. Here, the added amounts are based on the anhydrous bentonite. If required a little more distilled water is added so that the kneaded material “shears” thoroughly.
  • a mixing apparatus for example a Werner & Pfleiderer mixer (kneader)
  • the kneaded material is then comminuted in to small pieces and dried to a water content of 10 ⁇ 2% in a forced-circulation drying oven at about 75° C. for from 2 to 4 hours.
  • the dry material is then milled in a rotor beater mill (e.g. in a Retsch mill) over a 0.12 mm sieve.
  • the CEC and the fraction thereof of sodium ions were determined as described further below.
  • the stated fraction of monovalent cations is based on the fraction of sodium, potassium and lithium ions, in particular of sodium ions.
  • the bentonite used has a swellability of at least 25 ml/2 9, in particular of at least 30 ml/2 g, more preferably at least 35 ml/2 g.
  • the swelling volume is determined as follows: a calibrated 100 ml measuring cylinder is filled with 100 ml of distilled water. 2.0 g of the substance to be measured are introduced slowly in portions of from 0.1 to 0.2 g onto the water surface. After the material has sunk, the next portion is added. After the end of the addition, a waiting time of 1 hour is allowed and the volume of the swollen substance is then read in ml/2 g.
  • the proportion of iron ions, based on the CEC, should preferably be less than about 0.005 (0.5%). It has been found that such bentonites give better results with regard to the whiteness of the paper pulp.
  • the proportion of the monovalent cations, based on the CEC of the bentonite is more than 0.7, in particular more than 0.8, preferably more than 0.81, more preferably more than 0.85. It is furthermore preferable if the proportion of calcium and/or magnesium ions, based on the CEC of the bentonite, is less than 0.2, in particular less than 0.18, preferably less than 0.15.
  • the BET surface area (determined according to DIN 66131) of the bentonites used is less than 100 m 2 /g, in particular less than 90 m 2 /g. It is surprising that bentonites having a relatively low specific BET surface area exhibit particularly advantageous binding of impurities in comparison with bentonites which can provide a higher specific surface area for adsorption of impurities.
  • the demand for cationic charges in the headbox decreases while the method according to the invention is being carried out. This is demonstrated by the binding of the negatively charged impurities by charge interactions.
  • the concentration of the impurities in paper production is typically determined in the white water by the three customary processes of cation demand (cationic charge demand), stability measurement and chemical oxygen demand.
  • cation demand it is assumed that the impurities are all negatively charged and the white water filters in short-chain cationic polyelectrolytes.
  • the consumption is converted into the so-called cation demand.
  • turbidity measurement it is assumed that the impurities are partly present in colloidal form and their concentration can be determined via the extinction caused by the turbidity.
  • the proportion of organic compounds present is tested by means of an oxidizing agent.
  • the addition of the bentonite used according to the invention to the pulp or fiber suspension can be effected at any desired point in the paper production which is suitable for the person skilled in the art.
  • the addition directly in the pulper is also advisable because a long contact time with the paper stock is possible there and there is the probability of a high degree of binding of impurities.
  • Further addition points are in the entire so-called high-consistency stock region. Addition for dissolved air-floatation for water purification is also conceivable.
  • an already present addition point for additives for example in the form of a metering apparatus or metering pump, will also be present in the apparatuses used in each case for paper production, which apparatus or pump can be used for the addition of the bentonite used according to the invention.
  • the bentonite can be used both in powder form and in the form of a suspension or slurry.
  • the suspension or slurry will in many cases permit better meterability and is more easily automatable in industrial, continuous processes.
  • the effect of the bentonite used according to the invention is particularly positive if a certain particle size is maintained.
  • the particle size of the bentonite is chosen so that in the wet sieve residue less than 2% by weight, preferably less than 1% by weight, in particular less than 0.5% by weight, is 45 ⁇ m.
  • the determination of the wet sieve residue is explained in more detail before the examples.
  • the preferred particle size can also be determined by the light scattering method (Malvern).
  • the median particle size (D50) (based on the sample volume) is from 0.5 to 10 ⁇ m, in particular from 2 to 6 ⁇ m, particularly preferably from 3 to 5 ⁇ m.
  • the use of the bentonite used according to the invention leads to particularly good binding of impurities if talc is not used in the method.
  • the use of cationic polymers, such as, for example, poly(dadmac) or polyacrylamide, according to the prior art can also be reduced or even completely omitted with the aid of the bentonite used according to the invention.
  • the amounts of bentonite used in the method according to the invention can be determined by the person skilled in the art in a routine manner using empirical experiments. In most cases, it is advantageous to use amounts of from 0.5 to 12 kg/t of paper pulp or fiber suspension, preferably from 1 to 8 kg/t, and in particular from 1.5 to 7 kg/t, based in each case on the anhydrous pulp/suspension (dry weight).
  • the method according to the invention permits not only very good binding of anionic impurity fractions, such as fatty acids, but also outstanding binding or elimination of hydrophobic impurity fractions, such as sterols, steryl esters and triglycerides.
  • anionic impurity fractions such as fatty acids
  • hydrophobic impurity fractions such as sterols, steryl esters and triglycerides.
  • a further aspect of the present invention relates to the use of a bentonite as described herein for binding impurities in paper production.
  • the bentonite is preferably used in a paper pulp or fiber suspension which contains groundwood fractions.
  • all paper types or pulps are covered by the use according to the invention.
  • the paper types mentioned further above such as paper types containing groundwood or peroxide-treated groundwood, those which (in addition to the groundwood) also contain highly purified fiber fractions, as is the case, for example, in so-called newsprint paper, so-called deinked pulp (DIP), TMP (thermomechanical pulp), sulfate pulp, sulfite pulp and mixtures of different chemical pulps are particularly preferred.
  • DIP deinked pulp
  • TMP thermomechanical pulp
  • sulfate pulp sulfite pulp and mixtures of different chemical pulps are particularly preferred.
  • Apparatuses Sieve, 63 ⁇ m; conical flask with ground glass joint, 300 ml; analytical balance; membrane suction filter, 400 ml; cellulose nitrate filter, 0.15 ⁇ m (from Sartorius); drying oven; reflux condenser; hotplate; distillation unit, VAPODEST-5 (from Gerhardt, No. 6550); graduated flask, 250 ml; flame AAS.
  • the NH 4 + -bentonite is filtered off over a membrane suction filter and washed with demineralized water (about 800 ml) until substantially free of ions.
  • the testing of the wash water for freedom from ions is carried out for NH 4 + ions with Nessler's reagent which is sensitive to them.
  • the washing time can vary from 30 minutes to 3 days, depending on the type of clay.
  • the washed-out NH 4 + -bentonite is removed from the filter, dried at 110° C. for 2 h, milled, sieved (63 ⁇ m sieve) and dried again at 110° C. for 2 h. Thereafter, the NH 4 + content of the bentonite is determined according to Kjeldahl.
  • the CEC of the clay is the NH 4 + content of the NH 4 + bentonite, determined by means of Kjeldahl (for CEC of some clay minerals, cf. appendix). The data are given in meq/100 g of clay.
  • the cations liberated by the exchange are present in the wash water (filtrate).
  • the proportion and the type of the monovalent cations (“exchanged cations”) are determined spectroscopically in the filtrate according to DIN 38406, part 22.
  • the wash water (filtrate) is concentrated, transferred to a 250 ml graduated flask and made up to the mark with demineralized water. Suitable measuring conditions for FAAS are shown in the following tables.
  • overactivated bentonites i.e. those which were activated with an amount of, for example, sodium carbonate which is greater than the stoichiometric amount
  • the sum of the amounts of monovalent cations determined may be greater than the CEC determined as stated above.
  • the total content of monovalent cations (Li, K, Na) is regarded as 100% of the CEC.
  • the material to be investigated contains coarse fractions which differ in their particle size from the normal particles and how much of said coarse fractions said material contains. These fractions are determined by sieving an aqueous suspension with water as wash liquid. The wet sieve residue is considered to be the residue determined under specified conditions.
  • Apparatuses analytical balance, plastic beaker, Pendraulik LD 50; sieve: 200 mm diameter, mesh size 0.025 (25 ⁇ m), 0.045 mm (45 ⁇ m), 0.053 mm (53 ⁇ m) or 0.063 mm (63 ⁇ m); ultrasonic bath.
  • a 5% strength suspension of the bentonite (oven dry, i.e. after drying at 110° C.) in 2000 g of water was prepared.
  • the bentonite is stirred in at 930 rpm in about 5 min.
  • the suspension is poured into the cleaned and dried sieve (mesh size 45 ⁇ m) and washed with flowing tap water while tapping until the wash water runs out clear.
  • the sieve is placed for 5 min in an ultrasonic bath in order to sieve off the remaining fine fractions. When using the sieve in the ultrasonic bath, it should be ensured that no air remains between water surface and sieve bottom.
  • the chosen paper stock (e.g. 45% of chemical pulp and 55% of peroxide-bleached groundwood) can either be obtained directly from the paper mill or stored in a refrigerator before use.
  • the paper stock was then thoroughly shaken at 20 g absolutely dry and diluted to 2% with warm demineralized water in a 2000 ml beaker. While being stirred at 400 rpm, the paper stock batch warmed up to 40° C. with the aid of a hotplate. When the temperature is reached, the amount of adsorbent to be tested is added to the paper stock batch with the aid of a Pasteur pipette. Thereafter, the adsorption time in the stock batch is fixed at 30 min at 40° C. and the mixture is stirred for this time at 400 rpm. Thereafter, the paper stock batch of the adsorbent is diluted to 1% solids content with the aid of demineralized water (40° C.).
  • FIG. 1 shows a graph of the dependence of the concentration of the impurity particles in the white water (filtrate water) on the type and amount of the adsorbent used (bentonite or talc).
  • the wet sieve residue (45 ⁇ m) was less than 0.5% by weight.
  • Bentonite 2 was obtained from bentonite 1 by kneading bentonite 1 with 5% by weight of sodium carbonate, based on the anhydrous bentonite, according to the above method, drying to a water content of 10% by weight and milling to a particle size corresponding to that of bentonite 1 (comparison: table 2).
  • the mineralogical data of the bentonite are not changed, so that the montmorillonite content and the content of impurity minerals remain unchanged.
  • the BET surface area was 85 ⁇ 2 m 2 /g.
  • the content of fatty acids, lignins, sterols, steryl esters and triglycerides was determined for the above samples by means of the gas chromatographic analysis (cf. method section).
  • the bentonites 1 and 2 were used in each case in an amount of 6 kg/t of paper (dry weight); the cationized talc was used in an amount of 11.25 kg/t of paper, since 6 kg/t gives poor results.
  • the values obtained are shown in table 4.
  • the sample treated with the bentonite 2 according to the invention shows substantially better binding/removal of fatty acids, lignins, styrenes, styryl esters and triglycerides both compared with the sample treated with cationized talc and with the sample treated with the calcium bentonite (bentonite 1) not according to the invention.
  • the bentonite according to the invention was compared with conventional bentonites which have a proportion of monovalent cations, based on the CEC, of at least 0.7 (70%) but a CEC of less than 85 meq/100 g.

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US11/721,229 2004-12-16 2005-11-30 Bentonite for binding impurities during paper production Abandoned US20090044921A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102004060587.4 2004-12-16
DE102004060587A DE102004060587A1 (de) 2004-12-16 2004-12-16 Bentonite zur Störstoffbindung in der Papierherstellung
PCT/EP2005/012775 WO2006063682A2 (de) 2004-12-16 2005-11-30 Bentonite zur störstoffbindung in der papierherstellung

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US (1) US20090044921A1 (ko)
EP (1) EP1825056B1 (ko)
JP (1) JP2008524451A (ko)
KR (1) KR20070089805A (ko)
BR (1) BRPI0515785A (ko)
DE (1) DE102004060587A1 (ko)
ES (1) ES2531071T3 (ko)
MX (1) MX2007006952A (ko)
PL (1) PL1825056T3 (ko)
PT (1) PT1825056E (ko)
WO (1) WO2006063682A2 (ko)

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US20100094035A1 (en) * 2006-11-07 2010-04-15 Süd-Chemie AG Amorphous adsorbent, method of obtaining the same and its use in the bleaching of fats and/or oils
US20100129454A1 (en) * 2006-11-13 2010-05-27 Süd-Chemie AG Absorbent composition for surface treatment
US20100132251A1 (en) * 2006-11-07 2010-06-03 Ulrich Sohling Method for purification of biodiesel

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JP4868282B2 (ja) * 2006-09-15 2012-02-01 星光Ｐｍｃ株式会社 汚れ防止方法
WO2010070682A1 (en) * 2008-12-15 2010-06-24 Imi Fabi S.P.A. Talc- and/or chlorite-based compositions and use thereof in controlling pollutants in papermaking industry processes
EP3128073A1 (de) 2015-08-06 2017-02-08 Clariant International Ltd Kompositmaterial für die störstoffbekämpfung bei der papierherstellung
SI3260597T1 (sl) 2016-06-22 2019-10-30 Buchmann Ges Mit Beschraenkter Haftung Večplastni izdelek iz vlaken z zavrto hitrostjo migracije aromatskih ali nasičenih ogljikovodikov in postopek za njegovo izdelavo
CN115109451B (zh) * 2022-06-17 2023-08-18 阳原县仁恒精细粘土有限责任公司 一种包含高膨胀性膨润土的水性乳胶漆

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US20100094035A1 (en) * 2006-11-07 2010-04-15 Süd-Chemie AG Amorphous adsorbent, method of obtaining the same and its use in the bleaching of fats and/or oils
US20100132251A1 (en) * 2006-11-07 2010-06-03 Ulrich Sohling Method for purification of biodiesel
US8394975B2 (en) 2006-11-07 2013-03-12 Sud-Chemie Ag Amorphous adsorbent, method of obtaining the same and its use in the bleaching of fats and/or oils
US20100129454A1 (en) * 2006-11-13 2010-05-27 Süd-Chemie AG Absorbent composition for surface treatment
US8956630B2 (en) 2006-11-13 2015-02-17 Sued-Chemie Ip Gmbh & Co. Kg Absorbent composition for surface treatment

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EP1825056B1 (de) 2015-01-14
ES2531071T3 (es) 2015-03-10
KR20070089805A (ko) 2007-09-03
MX2007006952A (es) 2007-06-25
DE102004060587A1 (de) 2006-07-06
EP1825056A2 (de) 2007-08-29
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BRPI0515785A (pt) 2008-08-05
WO2006063682A2 (de) 2006-06-22

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