EP1277880A1 - Procedé de préparation de papier de p-Aramide, papier de p-Aramide, pulpe de p-Aramide et l'utilisation du papier et de la pulpe - Google Patents

Procedé de préparation de papier de p-Aramide, papier de p-Aramide, pulpe de p-Aramide et l'utilisation du papier et de la pulpe Download PDF

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Publication number
EP1277880A1
EP1277880A1 EP01117805A EP01117805A EP1277880A1 EP 1277880 A1 EP1277880 A1 EP 1277880A1 EP 01117805 A EP01117805 A EP 01117805A EP 01117805 A EP01117805 A EP 01117805A EP 1277880 A1 EP1277880 A1 EP 1277880A1
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EP
European Patent Office
Prior art keywords
aramid
pulp
paper
solution
aramid paper
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.)
Withdrawn
Application number
EP01117805A
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German (de)
English (en)
Inventor
Helga Werlich
Wolfgang Zwilling
Ulrich Dr. Wecker
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.)
Teijin Aramid GmbH
Original Assignee
Teijin Twaron GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Teijin Twaron GmbH filed Critical Teijin Twaron GmbH
Priority to EP01117805A priority Critical patent/EP1277880A1/fr
Publication of EP1277880A1 publication Critical patent/EP1277880A1/fr
Withdrawn legal-status Critical Current

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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
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/10—Organic non-cellulose fibres
    • D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/26—Polyamides; Polyimides

Definitions

  • the present invention relates to a process for producing p-aramid paper, p-aramid paper, p-aramid pulp and the use of paper and pulp.
  • Papers based on p-aramid pulp include in seals, as calenders or Filter paper and used as friction lining paper for gearboxes. This will be multiple Ever increasing demands are placed on the tensile strength of p-aramid papers.
  • WO 98/46827 describes a method for improving the dispersion behavior aqueous aramid fiber dispersions by adjusting the pH of the aramid fiber dispersions to a value> 10.
  • a prepared from such dispersions Paper is characterized by increased uniformity. About the tensile strength nothing is said of the paper.
  • the object of the present invention is to provide a method with which the tensile strength of p-aramid paper is increased.
  • the present invention has the object of a p-aramid paper with increased To provide tensile strength.
  • the object of the present invention is to provide a p-aramid pulp To provide, with the help of a p-aramid paper produced increased tensile strength can be.
  • p-aramid is a fully aromatic polyamide, one would have expected that treatment with a base in an aqueous or alcoholic Solution in the above Temperature range - due to the hydrolytic degradation of the Polyamide bonds in the polymer chain - the strength of the pulp fibers and the The tensile strength of papers made with this pulp is reduced.
  • the process according to the invention leads to a p-aramid Paper with significantly higher tensile strength, which is up to four times higher than the tensile strength a p-aramid paper, the same pulp is used for its production and processed into p-aramid paper in the same way as in step b), but the pulp before step b) is not treated according to step a) of the invention Was subjected to the procedure.
  • the treatment is preferably carried out in step a) of the method according to the invention in a temperature range from> 50 ° C to the boiling point of the solution and especially preferably in a temperature range from> 80 ° C to the boiling point of the solution instead, because - under otherwise identical conditions - in these temperature ranges a treated pulp results, its further processing to a p-aramid Paper with particularly high tensile strength leads.
  • the treatment is preferred over a period of> 5 minutes to 10 hours and particularly preferably in a period of 1 hour to 7 hours.
  • an amine such as ammonia
  • (earth) alkali hydroxides such as Lithium, sodium, potassium, magnesium, calcium or barium hydroxide
  • alkaline earth oxides such as e.g. Calcium oxide
  • inorganic carbonates such as. Sodium carbonate, sodium hydrogen carbonate or potassium carbonate
  • alcoholates of (earth) alkali metals such as Sodium alcoholate, potassium alcoholate or Magnesium alcoholate and alkylates of (earth) alkali metals such as e.g. Lithium or Magnesium alkylate
  • alkylates of (earth) alkali metals such as e.g. Lithium or Magnesium alkylate
  • step a) of the method according to the invention a 0.5 to 2 molar aqueous or alcoholic solution of the base used.
  • the concentration of the pure p-aramid pulp used in step a) in the solution the base is preferably 0.5 to 5% by weight, based on the weight of the solution the base.
  • step a) Remove the finish of the p-aramid pulp, for example by extracting the pulp in a Soxhlet sleeve with an aliphatic alcohol.
  • the processing of the treated pulp to p-aramid paper in step b) of the invention can be done in a manner known per se, for example by suspending and dispersing those treated according to the invention Pulp in water, sheet form and dry. Alternatively, you can after Sheet form the sheet hot press.
  • the method according to the invention performs to a p-aramid paper, the tensile strength of which is significantly higher than the tensile strength a p-aramid paper, the same pulp is used for its production and processed into p-aramid paper in the same way as in step b), but the pulp is not mixed with an aqueous or alcoholic solution of a base treated in a temperature range> 25 ° C to the boiling point of the solution has been.
  • a p-aramid Paper can be made from a with an aqueous or alcoholic solution Base treated in a temperature range> 25 ° C to the boiling point of the solution p-aramid pulp.
  • the object on which the invention is based is finally achieved by a p-aramid Pulp with a Schopper-Riegler value in the range of 60 to 85, preferably with a Schopper-Riegler value in the range of 75 to 82.
  • p-Aramid Pulpe has - due to the hydrolysis of polyamide bonds - an increased Number of amino end groups and thus an increased reactivity towards reagents for surface modification of the pulp fibers. Therefore, this can p-aramid pulp advantageous for the chemical modification of its fiber surface with Epoxides, ketenes, acid chlorides, isocyanates, diisocyanates, alkyl halides, Use benzyl halides or esters, which creates a p-aramid pulp with chemical surface-modified fibers results.
  • the p-aramid pulp with chemically surface-modified fibers is because of the functional groups inserted for a variety by chemical modification other connections suitable. Therefore, the p-aramid pulp can be chemically mixed with Surface-modified fibers are advantageous for binding dye molecules use, resulting in a colored p-aramid pulp.
  • this colored p-aramid pulp is used for paper production, the result is dyed p-aramid paper with increased tensile strength. Therefore, this colored one p-aramid pulp advantageous for the production of a colored p-aramid paper use.
  • the tensile strength is measured based on DIN 53112. To do this, the to be examined p-aramid sheet 8 strips cut, the width of one non-compacted sheet is 30 mm and 15 mm for a cold / hot compacted sheet. The strips are air-conditioned for 48 hours at 23 ° C and 50% relative humidity. Subsequently we measure the thickness of the strips according to DIN 53105 part 1 with a thickness gauge from the company Frank (load masses No. 1 and 2, measuring probe with 16 mm Diameter). The strips are then placed on the top and bottom of the universal testing machine from Zwick with pneumatic sample jaws, inductive Position transducer and a load cell for the range 0 - 2 kN clamped.
  • the Clamping pressure is 4 bar, clamping length 100 mm.
  • the withdrawal speed is set so that the break occurs within 20 ⁇ 5 seconds.
  • width and the thickness of the strips are entered, the force / strain curve via the program "Tensile” recorded and with this program the tensile strength as an average the 8 strips calculated in MPa.
  • the Schopper-Riegler value of the p-aramid pupa is determined according to the "operating instructions for grinding degree tester Schopper-Riegler SR 1 "from Karl Schröder KG, Weinheim measured.
  • the moisture content of the pulp is measured on an LP 16 IR balance from Mettler certainly. For this purpose, 3 g of moist pulp are dried at 160 ° C to constant weight, the weight is measured at 30 second intervals.
  • the mixture with the treated pulp is placed in 2.5 l of water suspended and in accordance with an impact device from Lorentzen and Wettre the requirements of the leaflet of the Association of Pulp and Paper Chemists and Engineers, No. V / 4/61, French paper standard TAPPI 205, at a stroke rate stirred from 6000 for two minutes.
  • the suspension thus obtained is in a Sheet forming column from Ernst Haage, Mühlheim an der Ruhr, according to the system Rapid-Köthen (constructed based on the leaflet of the Zellstoffund Association Paper chemists and engineers, No. V / 8/76 and DIN 54358) and that Volume of the suspension increased to 6 l by adding additional water.
  • the sheet former column Before filling, the sheet former column was covered with a polypropylene sieve (Mesh size 105 ⁇ m). The sheet former column is opened for 5 seconds “Swirl” and then set to "suction” and wait until the column completely drained above the sieve. The emptying time required for this is 35 seconds.
  • the sheet formed together with the polypropylene fabric from the sheet former column removed, covered with tissue and sucked off with a felt roller. Then the leaf with bottom and top fabric in a contact dryer for 15 minutes dried at 90 ° C and negative pressure. After qualitative assessment under the light bank the sheet thickness and tensile strength are measured. The tensile strength of the paper is 2.31 MPa.
  • Example 1 The procedure is as in Example 1, with the difference that the 9.3 g of p-aramid Pulp not treated with aqueous sodium hydroxide solution as in the first paragraph of Example 1 but suspended directly in 2.5 l of water and then as in Example 1 to p-aramid Paper is processed.
  • the draining time of the sheet formation is 17 seconds, the tensile strength of the p-aramid paper is 0.76 MPa.
  • Example 1 The procedure is as in Example 1, with the difference that that with aqueous Sodium hydroxide solution-treated pulp is first suctioned off on a suction filter and on the Nutsche is washed with water until the washing water runs off neutral, and only then suspended in 2.5 l of water and as in Example 1 to p-aramid Paper is processed.
  • the emptying time for sheet formation is 19 seconds
  • Example 1 The procedure is as in Example 1, with the difference that the 9.3 g of p-aramid pulp is heated to reflux instead of with aqueous sodium hydroxide solution with 250 ml of 1% by weight aqueous sulfuric acid for a treatment time t of 6, 18 and 30 hours , The pulp treated with the sulfuric acid solution is then suspended in 2.5 l of water and processed to p-aramid paper as in Example 1. This results in the following emptying times for sheet formation and tensile strengths of the p-aramid paper. t (hours) Emptying time (seconds) Tensile strength (MPa) 6 16 0.73 18 17 0.68 30 18 0.75
  • Example 1 The procedure is as in Example 1, with the difference that the treatment times in the aqueous sodium hydroxide solution are 2.5, 4.5 and 9 hours.
  • the p-aramid pulp is then suspended in 2.5 l of water and processed to p-aramid paper as in Example 1. This results in the following emptying times for sheet formation and tensile strengths of the p-aramid paper.
  • t hours
  • Emptying time seconds
  • Example 2 The procedure is as in Example 2, with the difference that the treatment times in the aqueous sodium hydroxide solution are 2.5, 4.5 and 9 hours.
  • the p-aramid pulp is then suspended in 2.5 l of water and processed to p-aramid paper as in Example 1. This results in the following emptying times for sheet formation and tensile strengths of the p-aramid paper.
  • t hours
  • Emptying time seconds
  • Example 1 The procedure is as in Example 1, with the difference that the duration of treatment in the aqueous sodium hydroxide solution is 2.5 hours. Then, as in Example 1 p-aramid sheet formed, with an emptying time of 20 seconds being measured. The p-aramid sheet is heated with a Fontijne hot press for 2 minutes at one temperature of 180 ° C and a pressure of 200 bar. The compressed paper has a tensile strength of 3.48 MPa.
  • a p-aramid sheet is formed with an emptying time of 18 seconds is measured.
  • the p-aramid sheet is made with a Fontijne hot press For 2 minutes at a temperature of 180 ° C and a pressure of 200 bar pressed.
  • the compressed paper has a tensile strength of 3.00 MPa.
  • Example 11 The procedure is as in Example 11, with the difference that a highly fraying Mixing set is used. The result is a p-aramid fleece with a Moisture of 74.7% by weight, a pH of 10 and a Schopper-Riegler value of 80. As in Comparative Example 1, 11.85 g of the nonwoven thus obtained is used p-aramid paper. The draining time of the sheet formation is 38 seconds, the tensile strength of the p-aramid paper is 1.50 MPa.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)
EP01117805A 2001-07-21 2001-07-21 Procedé de préparation de papier de p-Aramide, papier de p-Aramide, pulpe de p-Aramide et l'utilisation du papier et de la pulpe Withdrawn EP1277880A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP01117805A EP1277880A1 (fr) 2001-07-21 2001-07-21 Procedé de préparation de papier de p-Aramide, papier de p-Aramide, pulpe de p-Aramide et l'utilisation du papier et de la pulpe

Applications Claiming Priority (1)

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EP01117805A EP1277880A1 (fr) 2001-07-21 2001-07-21 Procedé de préparation de papier de p-Aramide, papier de p-Aramide, pulpe de p-Aramide et l'utilisation du papier et de la pulpe

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EP1277880A1 true EP1277880A1 (fr) 2003-01-22

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3880710A (en) * 1973-01-12 1975-04-29 Hooker Chemicals Plastics Corp Process for fiber treatment
JPS62225539A (ja) * 1986-03-27 1987-10-03 Asahi Chem Ind Co Ltd 変性アラミド材料の製造法
JPH03217429A (ja) * 1990-01-22 1991-09-25 Asahi Chem Ind Co Ltd 着色シートの製造法
US5202184A (en) * 1989-06-05 1993-04-13 E. I. Du Pont De Nemours And Company Method and apparatus for producing para-aramid pulp and pulp produced thereby
EP0572002A2 (fr) * 1992-05-28 1993-12-01 Sumitomo Chemical Company, Limited Solution à filer de para-aramide à bas degré de polymérisation, fibre de para-aramide et demi-produit de fibres de para-aramide fabriqué à partir de celle-ci et procédés de production de ceux-ci
WO1994005854A1 (fr) * 1992-09-02 1994-03-17 Akzo Nobel N.V. Pate de polyamide aromatique contenant de l'eau et procede de production
US5644003A (en) * 1994-07-19 1997-07-01 Sumitomo Chemical Company, Ltd. Epoxy resin composition, process for producing the same and resin-sealed semiconductor device
US5833807A (en) * 1997-04-17 1998-11-10 E. I. Du Pont De Nemours And Company Aramid dispersions and aramid sheets of increased uniformity
US6045897A (en) * 1996-05-15 2000-04-04 Matsushita Electric Industrial Co., Ltd. Nonwoven fabric cloth substrate for printed wiring boards, and prepreg using the same

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3880710A (en) * 1973-01-12 1975-04-29 Hooker Chemicals Plastics Corp Process for fiber treatment
JPS62225539A (ja) * 1986-03-27 1987-10-03 Asahi Chem Ind Co Ltd 変性アラミド材料の製造法
US5202184A (en) * 1989-06-05 1993-04-13 E. I. Du Pont De Nemours And Company Method and apparatus for producing para-aramid pulp and pulp produced thereby
JPH03217429A (ja) * 1990-01-22 1991-09-25 Asahi Chem Ind Co Ltd 着色シートの製造法
EP0572002A2 (fr) * 1992-05-28 1993-12-01 Sumitomo Chemical Company, Limited Solution à filer de para-aramide à bas degré de polymérisation, fibre de para-aramide et demi-produit de fibres de para-aramide fabriqué à partir de celle-ci et procédés de production de ceux-ci
WO1994005854A1 (fr) * 1992-09-02 1994-03-17 Akzo Nobel N.V. Pate de polyamide aromatique contenant de l'eau et procede de production
US5644003A (en) * 1994-07-19 1997-07-01 Sumitomo Chemical Company, Ltd. Epoxy resin composition, process for producing the same and resin-sealed semiconductor device
US6045897A (en) * 1996-05-15 2000-04-04 Matsushita Electric Industrial Co., Ltd. Nonwoven fabric cloth substrate for printed wiring boards, and prepreg using the same
US5833807A (en) * 1997-04-17 1998-11-10 E. I. Du Pont De Nemours And Company Aramid dispersions and aramid sheets of increased uniformity

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 012, no. 092 (C - 483) 25 March 1988 (1988-03-25) *
PATENT ABSTRACTS OF JAPAN vol. 015, no. 496 (C - 0894) 16 December 1991 (1991-12-16) *

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