EP0232015B1 - Hilfsmittel zur Harzkontrolle - Google Patents

Hilfsmittel zur Harzkontrolle Download PDF

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Publication number
EP0232015B1
EP0232015B1 EP87300212A EP87300212A EP0232015B1 EP 0232015 B1 EP0232015 B1 EP 0232015B1 EP 87300212 A EP87300212 A EP 87300212A EP 87300212 A EP87300212 A EP 87300212A EP 0232015 B1 EP0232015 B1 EP 0232015B1
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EP
European Patent Office
Prior art keywords
polymer
amine
component
pulp
added
Prior art date
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Expired - Lifetime
Application number
EP87300212A
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English (en)
French (fr)
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EP0232015A1 (de
Inventor
Thord Gustav Gunnar Hassler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Veolia WTS USA Inc
Original Assignee
WR Grace AB
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Priority to AT87300212T priority Critical patent/ATE59068T1/de
Publication of EP0232015A1 publication Critical patent/EP0232015A1/de
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Publication of EP0232015B1 publication Critical patent/EP0232015B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/08—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching
    • D21C9/086—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching with organic compounds or compositions comprising organic compounds
    • 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

Definitions

  • This invention relates to the control of pitch in the manufacture of pulp and paper.
  • pitch can accumulate in paper making and also in the manufacture of pulp, causing significant problems.
  • “Pitch” is the term used to describe the sticky materials which appear in paper making; these originate from the wood from which the paper is made.
  • "pitch” is now used as a general term for all material soluble in organic solvents but not soluble in water, for example the ink or adhesive present in recycled paper.
  • the pitch can accumulate at various points in the system. For example, it can block the felt and thus hinder drainage of the paper web. In addition, it can adhere to the wires or drying cylinders causing it to pick holes in the paper. Deposits may also build up at any earlier stage in the papermaking process. When these deposits break loose they may form a defect in the paper such as a spot or a hole. Such defects may even create a weakness in the paper sufficient to induce a breakage in the paper during the production resulting in unappreciated production down-time.
  • the present invention provides a method for the control of pitch in an aqueous system used during pulp or paper making which comprises adding to the system or to the pulp making or paper making machinery, a water soluble poly-quaternary branched polymer derived from (a) an epihalohydrin, a diepoxide or a precursor of an epihalohydrin or diepoxide, (b) an alkyl amine having a functionality with respect to an epihalohydrin of two, and (c) ammonia or an amine which has a functionality with respect to an epihalohydrin greater than two and which does not possess any carbonyl groups, with one or more of the following conditions:
  • the polymer is added to the pulp making or paper making machinery, (ii) the pulp is of recycled paper containing adhesive, and (iii) components (a) and (b) are reacted to form a coupling agent which is then reacted with component (c).
  • a special feature of the products used in the present invention is that they may combine with dissolved anionic material originating from the wood from which the pulp and paper is produced, providing a method of removing these anionic materials thereby lowering the concentration of such materials in the process water.
  • Water soluble anionic materials are released from the wood during pulp manufacture. These components interfere with paper production negatively in several ways: they decrease the efficiency of many products used in the papermaking process to alter the character of the paper. Examples of such additives include sizes, wet and dry strength agents and dyes.
  • Anionic dissolved materials also reduce the efficiency of retention agents. They limit the extent to which the water system can be closed and they may also lower the quality of the paper such as its strength. Reference is made to TAPPI papermakers Conference 1979 p49-66 which further discusses, the significance of anionic dissolved materials.
  • Component (a) is preferably an epihalohydrin, especially epichlorohydrin or epibromohydrin, but dihalohydrins, preferably dichlorohydrins or dibromohydrins, having three to twenty, especially three to ten, carbon atoms per molecule may also be used.
  • dihalohydrins which may be used include the following:
  • the alkyl amine may be a compound possessing two tertiary amino groups such as N,N,N',N'-tetramethyleneethylenediamine. Details of the preparation of products derived from such component (b) and component (a) can be found in UK-A-1 486 396.
  • component (b) is preferably a dialkylamine in which the alkyl groups individually contain one to three atoms. Dimethylamine is especially preferred.
  • component (c) is ammonia or an amine which possesses a functionality greater than two with respect to epihalohydrin and which does not possess any carbonyl groups; it can therefore act as a branching agent. It has been found that the use of a branched polymer is an important feature in the performance of the polymer to prevent deposition of pitch, as the comparative experiments below show.
  • a primary amino group is capable of reacting with three molecules of epihalohydrin so that a simple primary amine possesses a functionality of three.
  • a simple secondary amine will possess a functionality of two and a simple tertiary amine a functionality of one.
  • component (c) is typically ammonia, a primary amine, a primary alkylene polyamine having four to twenty-five, preferably four to twelve, carbon atoms and at least one, preferably one to six, primary amino groups per molecule including polyglycolamines as well as aromatic and heteroaromatic diamines but not polyamidoamines because they possess carbonyl groups.
  • Preferred materials include ammonia, diethylaminobutylamine, dimethylaminopropylamine and ethylenediamine, the latter two being especially preferred.
  • the polymer may also be derived from a further component which generally has the ability to act as a "end-capping" agent.
  • these materials will also be amines or other material having reactivity towards epichlorohydrin and which possess a functionality less than two and which also possess some other functional group or a fatty chain of, say, at least 12 carbon atoms, such as a simple tertiary amine such as a trialkylamine, especially trimethylamine or a hydroxyalkylamine, typically triethanolamine, or a fatty amine such as octadecylamine.
  • the polymers used in the present invention may be prepared by first reacting components (a) and (b) to obtain a "coupling agent" and then reacting this with component (c) and, if desired, the fourth component.
  • Preferred polymers for use in the present invention include those in which the coupling agent is derived from epichlorohydrin and dimethylamine, which is subsequently reacted with ethylenediamine and, if desired, also with trimethylamine, triethanolamine or octadecylamine.
  • the polymers may also be prepared by reacting a mixture of components (b) and (c) with component (a).
  • component (a) The preferred raw materials for such a process are the same as those given above.
  • the reaction is carried out in an aqueous medium, typically maintaining the reaction temperature at 5 to 125 ° C, preferably 30 to 95 ° C
  • the equivalent ratio of component (b) to component (c) is suitably 1:0.009 to 1.0 and preferably 1:0.02 to 0.5 while the equivalent ratio of component (a) to components (b) and (c) may vary widely depending on the amount and nature of component (b).
  • the ratio of component (c) to component (a) and component (b), together should be selected so that the viscosity of the aqueous polymer solution is at least 20 mPa - (Cps) at 50% dry content.
  • the ratio is from 1:0.22 to 2.5 and preferably 1:0.25 to 1.3.
  • reaction can be continued until the desired viscosity, and therefore molecular weight, has been achieved although acid can be used to reduce the pH and thereby terminate the reaction.
  • the upper viscosity limit is not critical provided it is consistent with having a workable solution; the upper limit is normally about 2000 mPa . (Cps).
  • a particularly preferred polymer for use in the present invention is formed by reacting ethylenediamine with a precondensate of dimethylamine and epichlorohydrin, and reacting the product with triethanolamine to form a water-soluble reaction product.
  • Another preferred product is formed by reacting a mixture of dimethylamine and ethylenediamine or dimethylaminopropylamine with epichlorohydrin to form a water-soluble reaction product.
  • the polymer is generally added to the aqueous system with the furnish containing the paper pulp but it is possible to add it at different points in the system depending on the precise nature of the problem.
  • the amount of polymer required will, of course, depend to some extent on the nature of the wood or other material used to prepare the paper pulp. Also, some polymer once added will tend to recirculate in the system thus requiring a lower addition rate. In general, however, from 0.1 to 20 ppm of polymer by weight based on the aqueous medium is suitable. Preferably, the amount is I to 10 ppm. This corresponds in the normal case to an addition of 10 to 2,000 grams, preferably 100 to 1,000 grams, polymer per tonne fibre.
  • the reaction product used in this invention onto a particular part of the pulp- or paper-making machinery such as the wire or press felts.
  • the polymer is preferably pre-diluted with water, generally to a concentration below 10% by weight and preferably I to 5% by weight.
  • biocide examples include those in the following classes:
  • the polymer is generally compatible with the usual pulp and paper making additives including starch, for example potato or corn starch, titanium dioxide, a defoamer such as a fatty acid alcohol, a size, for example a rosin size based on abietic acid, a neutral size based on alkyl ketene dimer or a succinic acid anhydride based size and a wet strength resin such as, if neutral, an epichlorohydrin polyamide or, if acid, a melamine- or urea-formaldehyde resin.
  • starch for example potato or corn starch
  • titanium dioxide titanium dioxide
  • a defoamer such as a fatty acid alcohol
  • a size for example a rosin size based on abietic acid, a neutral size based on alkyl ketene dimer or a succinic acid anhydride based size
  • a wet strength resin such as, if neutral, an epichlorohydrin polyamide or,
  • compositions used in the present invention are commercially available, typically as aqueous solutions containing a concentration of 40 to 50% per cent.
  • compositions used in the present invention will possess from I to 70%, especially 10 to 30%, by weight of the polymer.
  • the temperature was then kept at 60 ° C for one hour.
  • the reaction mixture was heated to 90 ° C and 32.48 g of 30% trimethylamine was added during ten minutes; 90 ° C was then maintained for two hours and the reaction mixture cooled to room temperature. This reaction mixture had a total solids content of 40.7%.
  • Example II Using the equipment described in Example I, 25.35 g of 36% hydrochloric acid was added to a mixture of 68.81 g of 32.7% dimethylamine solution and 121.4 g water. The temperature was kept below 35°C by cooling. 83.25 g epichlorohydrin was added at such a rate that temperature was maintained at 40 ° C. This temperature was then kept for one hour. The reaction mixture was heated to 60 ° C and 7.5 g ethylene diamine was added over 15 minutes while maintaining the temperature at 60 ° C. This temperature was kept for another 30 minutes. The reaction mixture was heated to 90 ° C and 37.25 g triethanolamine was added dropwise over 30 minutes. This temperature was maintained for a further two hours to complete the reaction. The total solids content was 44.6%.
  • the mixture was boiled for 15 minutes and then cooled rapidly to 55 ° C. 42 g of methanol was added to etherify free methylol groups and the mixture was agitated for 2.5 hours and then cooled to 25 ° C.
  • the resulting reaction product was a water soluble dicyandiamide-formaldehyde condensate in the form of a clear water soluble syrup containing 40% by weight solids.
  • Example 4 The product of Example 4 was evaluated using the method described in Example 3, but a different synthetic pitch was used. This time a pitch solution was made by adding a mixture of 2.0 g tall oil and 20.0 g glycerol ester of rosin to 10.5 g 5% potassium hydroxide to form an emulsion. This was then diluted with 187.5 g isopropanol and 110 g acetone to form a clear pitch solution. 15 ml of this solution was added to one litre water at 20 ° C and a hardness of 200 ppm expressed as calcium carbonate. The pH was adjusted to 3.0 using concentrated hydrochloric acid and the test was carried out over three minutes.
  • Poly DADMAC Polydiallyl dimethyl ammonium chloride
  • the preferred type of quaternary compound for control of pitch deposition in US-A-3 619 351 is a meth- yltriethanolamine. This material was synthesized from triethanolamine and dimethyl sulphate to form quaternary ammonium methyl triethanolamine monomethyl sulphate. This material was evaluated using the procedure in Example 3 with the following results:
  • a resin was prepared only from dimethylamine and epichlorohydrin following essentially the procedure of Example I of US reissue 28,807.
  • 92.5 grams (1.0 mole) epichlorohydrin was added to the flask.
  • 112.5 grams of 40% aqueous dimethylamine 45 grams real, 1.0 mole was added with vigorous stirring over one hour keeping the temperature below 50 ° C. Heating was applied for another two hours at 50 ° C whereafter 70g water was added.
  • the viscosity of this resin was determined to be 72 mPa- s (cps) and dry content was found to be 47 percent.
  • Comparative Example 5 The equipment of Comparative Example 5 was used. A resin was prepared in the following way: 112.5 grams 40% dimethylamine was added to the reaction flask together with 10.2 grams dimethylaminopropylamine. These two amines were mixed and 102 grams of epichlorohydrin was added over 30 minutes with vigorous stirring maintaining a temperature of 30-40°C. Temperature was then increased to 60 ° C which was maintained for 5 hours. During this period of time, 300ml of deionised water was added in small portions. This resin had a viscosity of 20 mPa s (cps) and a dry content of 33%.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Farming Of Fish And Shellfish (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Liquid Crystal Substances (AREA)
  • Valve Device For Special Equipments (AREA)
  • Epoxy Resins (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Claims (19)

1. Verfahren zur Kontrolle von Harzablagerungen in einem wäßrigen System, das bei der Zellstoff-oder Papierherstellung verwendet wird, bei dem dem System oder der Zellstoffherstellungs- oder Papierherstellungsanlage ein wasserlösliches poly-quaternäres verzweigtes Polymer zugesetzt wird, das sich von (a) einem Epihalohydrin, einem Diepoxid oder einem Vorläufer eines Epihalohydrins oder Diepoxids, (b) einem Alkylamin mit einer Funktionalität bezüglich eines Epihalohydrins von 2 und (c) Ammoniak oder einem Amin, das eine Funkionalität bezüglich eines Epihalohydrins von mehr als 2 aufweist und keine Carbonylgruppen besitzt, bei einer oder mehreren der folgenden Bedingungen ableitet:
(i) das Polymer wird der Zellstoffherstellungs- oder Papierherstellungsanlage zugesetzt,
(ii) der Zellstoff ist aus zurückgeführtem, Klebstoff enthaltendem Papier und
(iii) die Komponenten (a) und (b) werden zur Bildung eines Kupplungsmittels miteinander umgesetzt, welches dann mit Komponente (C) umgesetzt wird.
2. Verfahren nach Anspruch 1, bei dem Komponente (a) Epichlorhydrin oder Epibromhydrin ist.
3. Verfahren nach Anspruch 1 oder 2, bei dem Komponente (b) ein Dialkylamin ist, bei dem die Alkylgruppen individuell 1 bis 3 Kohlenstoffatome enthalten.
4. Verfahren nach Anspruch 3, bei dem Komponente (b) Dimethylamin ist.
5. Verfahren nach einem der vorangehenden Ansprüche, bei dem Komponente (c) ein primäres Amin oder ein primäres Alkylenpolyamin ist.
6. Verfahren nach Anspruch 5, bei dem Komponente (c) Diethylaminobutylamin, DimethylaminoPropylamin oder Ethylendiamin ist.
7. Verfahren nach einem der vorangehenden Ansprüche, bei dem das Polymer sich außerdem von einem tertiären Amin oder einem Hydroxyalkylamin ableitet.
8. Verfahren nach Anspruch 7, bei dem das Polymer sich außerdem von Trimethylamin oder Triethanolamin ableitet.
9. Verfahren nach einem der vorangehenden Ansprüche, bei das Polymer ein solches ist, das durch Umsetzung von Ethylendiamin mit einem Vorkondensat aus Dimethylamin und Epichlorhydrin und Umsetzung des Produkts mit Triethanolamin zur Bildung eines wasserlöslichen Reaktionsprodukts gebildet ist.
10. Verfahren nach einem der Ansprüche 1 bis 8, bei dem das Polymer ein solches ist, das durch Umsetzung einer Mischung von Dimethylamin und Ethylendiamin oder Dimethylaminopropylamin mit Epichlorhydrin zur Bildung eines wasserlöslichen Reaktionsprodukts gebildet ist.
11. Verfahren nach einem der vorangehenden Ansprüche, bei dem das Equivalentverhältnis von Komponente (c) zu Komponenten (a) und (b) zusammen 1:0,22 bis 2,5 beträgt.
12. Verfahren nach einem der vorangehenden Ansprüche, bei dem das Polymer dem wäßrigen System mit der die Papierpulpe enthaltenden Stoffzusammensetzung zugesetzt wird.
13. Verfahren nach einem der vorangehenden Ansprüche, bei dem das Polymer in einer Menge von 1000 bis 50 000 g je Tonne Fasern zugesetzt wird.
14. Verfahren nach einem der Ansprüche 1 bis 11, bei dem das Polymer bei der Papierherstellung zumindest auf einen Teil der Papierherstellungsanlage gesprüht wird.
15. Verfahren nach Anspruch 14, bei dem das Polymer auf das Papierherstellungssieb gesprüht wird.
16. Verfahren nach Anspruch 14 oder 15, bei dem das Polymer als wäßrige Lösung mit einer Polymerkonzentration unterhalb 10 Gew.% angewendet wird.
17. Verfahren nach Anspruch 16, bei dem die Polymerkonzentration 1 bis 5 Gew.% beträgt.
18. Verfahren nach einem der vorangehenden Ansprüche, bei dem das Papierherstellungsverfahren zurückgeführtes, Klebstoff enthaltendes Papier verwendet.
19. Verfahren nach einem der vorangehenden Ansprüche, bei dem außerdem ein Biozid zugesetzt wird.
EP87300212A 1986-01-09 1987-01-09 Hilfsmittel zur Harzkontrolle Expired - Lifetime EP0232015B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87300212T ATE59068T1 (de) 1986-01-09 1987-01-09 Hilfsmittel zur harzkontrolle.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB8600506A GB2186895B (en) 1986-01-09 1986-01-09 Pitch control aid
GB8600506 1986-01-09

Publications (2)

Publication Number Publication Date
EP0232015A1 EP0232015A1 (de) 1987-08-12
EP0232015B1 true EP0232015B1 (de) 1990-12-12

Family

ID=10591145

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87300212A Expired - Lifetime EP0232015B1 (de) 1986-01-09 1987-01-09 Hilfsmittel zur Harzkontrolle

Country Status (8)

Country Link
EP (1) EP0232015B1 (de)
JP (1) JPH07113200B2 (de)
AT (1) ATE59068T1 (de)
CA (1) CA1306570C (de)
DE (1) DE3766623D1 (de)
ES (1) ES2019376B3 (de)
FI (1) FI88814C (de)
GB (1) GB2186895B (de)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE467667B (sv) * 1988-08-11 1992-08-24 Grace W R & Co Foerfarande foer reglering av produktionsstoerande mikrobiologiska avsaettningar paa papperstillverkningsutrustning
JP2618496B2 (ja) * 1988-09-16 1997-06-11 グレイス・ディアーボーソ・インコーポレーテッド 製紙機フエルト等への析出防止法
US4995944A (en) * 1988-09-16 1991-02-26 Dearborn Chemical Company Ltd. Controlling deposits on paper machine felts using cationic polymer and cationic surfactant mixture
US4997523A (en) * 1990-06-20 1991-03-05 Betz Panerchem, Inc. Method for effectively breaking up latex-coated paper during pulping to decrease the potential for white pitch deposition
GB2251868B (en) * 1990-12-24 1994-07-27 Grace W R & Co Pitch control
TW202043331A (zh) * 2018-11-30 2020-12-01 美商Ｂｌ科技公司 焦化加熱器之積垢減量

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3248353A (en) * 1963-05-17 1966-04-26 American Cyanamid Co Alkylene polyamine resin
USRE28808E (en) * 1972-02-04 1976-05-11 American Cyanamid Company Polyquaternary flocculants
US3855299A (en) * 1973-06-11 1974-12-17 Grace W R & Co Water soluble reaction product of epihalohydrin and alkylamines
US4093605A (en) * 1975-01-24 1978-06-06 Wolff Walsrode Aktiengesellschaft Auxiliary agent for improving retention, drainage and treatment
US4250269A (en) * 1979-11-26 1981-02-10 Buckman Laboratories, Inc. Water-soluble mixtures of quaternary ammonium polymers, nonionic and/or cationic vinyl-addition polymers, and nonionic and/or cationic surfactants
CA1150914A (en) * 1980-11-28 1983-08-02 Margaret J. Molnar Amine-epichlorohydrin polymers for pitch control

Also Published As

Publication number Publication date
JPS62223394A (ja) 1987-10-01
FI88814C (fi) 1993-07-12
JPH07113200B2 (ja) 1995-12-06
GB8600506D0 (en) 1986-02-12
GB2186895A (en) 1987-08-26
CA1306570C (en) 1992-08-18
FI870072A0 (fi) 1987-01-08
ES2019376B3 (es) 1991-06-16
FI88814B (fi) 1993-03-31
ATE59068T1 (de) 1990-12-15
DE3766623D1 (de) 1991-01-24
FI870072L (fi) 1987-07-10
EP0232015A1 (de) 1987-08-12
GB2186895B (en) 1989-11-01

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