US2263903A - Apparatus for the extraction of cellulosic fibers from vegetable material - Google Patents

Apparatus for the extraction of cellulosic fibers from vegetable material Download PDF

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Publication number
US2263903A
US2263903A US153993A US15399337A US2263903A US 2263903 A US2263903 A US 2263903A US 153993 A US153993 A US 153993A US 15399337 A US15399337 A US 15399337A US 2263903 A US2263903 A US 2263903A
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Prior art keywords
alkali
tower
chlorine
treatment
extraction
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US153993A
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English (en)
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Pomilio Umberto
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POMILIO Corp Ltd
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POMILIO CORP Ltd
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Application filed by POMILIO CORP Ltd filed Critical POMILIO CORP Ltd
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    • 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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/18—Pulping cellulose-containing materials with halogens or halogen-generating compounds

Definitions

  • the invention is for improvements in or relating to apparatus for the extraction of cellulosic fibers from vegetable material and particularly from vegetable material such as the stalks of the velocity at which the reactions take place and the rate at which the heat evolved is dissipated through the mass of the material and through the walls of the reaction vessels.
  • grasses such as esparto, tow-residues and
  • a feature of the invention consists in emp yresidues from the manufacture of textile matein e a i in q ah eS only j s fll t t rials.
  • One of the objects of the invention is to react with and/or dissolve the encrustmg subproduce cellulosic fibers suitable for the manustances referrvlelii to abo there s ot be facture of high-grade and other forms of paper an xcess of a a and cardboard and the like
  • the c ll l io A further feature of the invention consists in fibers which are present in the materials set out employing a alkali lu 6 a Caustic soda above are for the most patrtdembtelllided in ligneous i gilg 213111 1237 8?
  • the reacting substances are selected to be one eral compounds (e. g. silica compounds).
  • the a all removes a su s an ia part of the encrusting b t while t solution, the extent of the mitial dlsmtegratlon chlorine reacts with the ligneous of woody matof t material a i th r tu y va y t-er.
  • the concentration of the alkali solution 25 fIOm usually t been g i is 21SZ Zxfiifiitii is iiffiit 3552352??? amounting 0 107 or hig er, and sim ar y, where chlorine has been used, it has been em- 3 3 21 9 5 l g ig fi g i ployed in an undiluted state.
  • Paper manufac- 6 1g 6 m 9 6 5a 6 me tured from the resulting fibers has tended to be 30 g g a e g y ge harsh and crackly. 0
  • a proce'ss for the consists in effecting the chlorination treatment of the vegetable material bycausing chlorine gas extraction of cellulosrc fibers fromvegetable madiluted with air to be conducted through the te
  • the proportion of air used with the Vessel 1m1 ned1ate 1Y upon compktlfm of the chlorine is dependent on the nature of the vegetion and lmmelfismg the matePal m a colfi Water table material being treated and it may vary bath, transferrlhg the matfina1 t a Sald h from .5 to 1. part by volume of air to one part to another vessel and treating it with an alkali by volume of chlorine, while the moisture solution for dissolving the previously reacted subt t of the chlorine may be up to its Saturation Y stances. Since the react1ons are exothermi e point and the moisture content of the mass may tempe aturation s built p are d p nt t a n be two to five times the dry weight of the mass itself.
  • the rate at which the chlorine-air mixture is passed through the vegetable material also varies with the nature of the material being treated,
  • wheat straw may be treated up to a temperature of 55 C. while hemp straw may be treated up to 65 C.
  • the rate at which chlorine may be passed through the material per pound of the material per hour varies from of a pound to V of a pound.
  • the length of the chlorination treatment may vary from half an hour to three hours.
  • volves reactions which are controlled as to concentration of solutions, maximum temperature rise and time of treatment, which reactions are carried out successively in separate reaction chambers. in reducing to a minimum the time when the fibres are in contact with the hydrochloric acid resulting from the chlorination, for example, the mass is immersed in cold water as soon as the chlorination is complete.
  • a further aspect of the invention consists in that the vegetable material is subjected to a further treatment with alkali after the chlorination treatment.
  • the first alkali treatment is carried out under conditions which remove a substantial part of the encrusting substances and do not attack the: capitaous matter.
  • first reaction is a partial reaction.
  • the chlorine treatment reacts with the ligneous matter-and forms chloro-ligriine compounds. These compounds may not be entirely removed by the immersion in water and the function of the second alkali treatment is to dissolve out these chloro-lignine compounds.
  • the strength of the alkali solution employed for this latter treatment may be as low as .l%.
  • the quantity of solution employed is from 5 to 20 parts by weight of solution to 1 part by weight of vegetable material.
  • the quantity of alkali required in the last alkali treatment is less than half that employed in the first treatment.
  • the temperature at which the reaction takes place may be up to 100 C., and the length of time of the treatment may be as low as a few minutes.
  • the plant employed may embody an apparatus for mixing solid divided material, such as the aforesaid chopped vegetable material, with a reacting liquor, such as the alkali, which appa ratus comprises a hopper or thelike arranged above an elongated mixing chamber having a bottom wall sloping in the direction of the length of the chamber. a conveyor in said chamber arranged to traverse the material from the deep end to an outlet at the shallow end, means for introducing the reacting liquor at a controlled rate to said chamber. By these means the material can be-arranged to pick upor absorb the desired quantity of liquor during its passage through the mixing chamber.
  • the mixing chamber may be.
  • a feature of the invention consists.
  • the plant may also embody an apparatus for extracting compacted masses of interlaced fibers from the bottom of treating towers or the like, which apparatus comprises a number of parallel or horizontal shafts spaced apart and having radially extending arms and means for driving adjacent shafts in. opposite directions. Means may be provided for varying the distance apart of said shafts.
  • means are provided for converting the material to a fioccular state after the removal of the liquor in the alkali treatment and a blower connected with a suitable conduit is provided for conveying by cold air the floccular material in a divided state to the top of the chlorine tower.
  • a receiving chamber may be arranged over the top of the chlorine tower which is provided with a deflecting wall on to which the floccular material is directed by said conduit and is thereby caused to fall into said tower.
  • FIGS. 1a and lb taken together represent a side elevation of the plant showing diagrammatically the general arrangement.
  • Figure'2 is a vertica'lsection on the line 22 of Figure la showing the alkali towers'in elevation.
  • Figure 3 is a section through a tower on the line 3-4 of Figure 1.
  • Figure 4 is an enlarged view of one of the mixing devices of Figure 2.'
  • FIG. 5 is an enlarged view ofthe mechanism for tilting the hopper nozzle as shown in Figure 4.
  • Figure 6 is a side elevation of the device shown in Figure 5. 4
  • Figure 7 is a plan view of the extractor for the reaction towers.
  • Figure 8 is an elevation of the arrangement shown in Figure '7.
  • Figure 9 is a cross section on the line 8-9 of Figure 8.
  • each hopper is arranged to deliver the material to an apparatus II which mixes the stalks with an alkali solution in, the required proportions and delivers the" mixture to the upper ends of a pair of vertically-arranged reaction towers l2.
  • Each mixing apparatus thus serves two towers, and comprises a long horizontally-disposed chamber "open at the top, the lower wall ll of which is inclined downwardly from each end to the centre to form a V.
  • a screweconveyor .15 is horizontally-disposed along-the length of the chamber and has two sets of helical blades arranged end to end, which blades vare oppositely pitched to one another, and are driven by a motor 22. Disposed above the chamber and at the centre of the screwconveyor is a V-shaped deflector I6.
  • the hopper is arranged to deliver the material on to the deflector through a flexible nozzle I! which may be swung from one side to the other of the V-shaped aaeaoos deflector thereby adiusting the relative quantitles of the material being fed to the two towers.
  • the movement of the nozzle may be effected by a hand wheel ll to a worm shaft I!
  • the reaction towers may be about 34 feet high and in cross-section are flattened oval-shaped (as will be seen from Figure 3), the smaller dimension being about inches and the larger dimension 8 feet.
  • the conveyor I 3 is so arranged as to eflect a mixture of straw and solution in proportions of one of straw to four of the solution.
  • Steam is introduced through the walls of the tower by a number of pipes 24 in a zone substantially above the horizontal centre line, e. g. onequarter of the length from the top.
  • the steam generating plant 25 and main delivery pipe 2 are shown to the left of Figure l.
  • the mass of material gradually descends under gravity and becomes compacted as it descends, and at the bottom forms a seal which prevents too rapid an escape-of the liquid.
  • the time of descent may vary from one to four hours according to the nature of the material and the strength of the caustic solution. During this time the alkali is almost completely used up'to form spent liquor of a dark colour.
  • the tower is provided with inspection windows 9 and sockets 8 for thermometers at different heights.
  • the speed of extraction beingadjustable; thus, the time of treatment may be varied.
  • These towers may also be about 30 feet in height although those shown in thedrawings are shorter.'-' They are of a flattened oval shape in cross-section, the general dimensions being the same as those of the alkali towers. Chlorine is introduced into the fibrous mass at a zone about 10 feet from the top of each tower. As already indicated the top of each tower is open but the 10 foot column of fibrous material above the zone is sufllcient'completeiy to absorb the chlorine Aswillbeseenfrom Figure7to9theextractor'- comprises'two parallel shafts 2! each of which can-is a ,number of star-shaped members II.
  • the two shafts are rotated through gearing 80 in opposite directions so that the arms of the stars draw the material downward and flrst move towards one another and then away from one another.
  • the mounting for shafts 28 and the ing device is formed in two parts 33, 34 arranged. end to end along the length of its conveyor and the part at the outlet end 34 receives a supply of wash water through a pipe 38 which wash liquor is delivered by an outlet pipe I to a tank 31.
  • washed and partly-treated fibers are delivered by the conveyor through an outlet conduit ll to a screw-press 39 where the remainder of the spent liquor is squeezed out of them and delivered to a tank 4
  • the consolidated mass is then passed through a conduit and prevent leakage, and the sealing action is enhanced'by the fact that the material is descending".
  • the "chlorine is' introduced into the zone by pipes 48 which extend from a header pipe II through the walls of the tower and'stop flush with the inside face, and also by means of a set of pipes il which extend downwardly from a header pipe. From practical considerations the width between the side walls of the tower cannot be made much less than I! inches and since chlorine cannot readily penetrate the librous material to that extent, the additional vertical delivery pipes are provided.
  • Chlorine with the required degree of moisture may-be prepared in an electrolytic plant 53 from which it passes through a delivery conduit 54 to a blower l5 driven by a motor 56.
  • the inlet or suction side of the blower communicates with the atmosphere through a valve 51 and alrpipe ll. 13y adjusting the valve 5! a desired vquantity of air may be mixed with the chlorine.
  • thermometers 9 and sockets for thermometers are provided.
  • the material is then delivered by the extractor into a tank I having rotating stirrers ll therein through which tank cold water is circulated.
  • the material passes thence along a trough 62 to a rotating conical sieve 82, the axis of which is horizontal and the angle of inclination of the walls of which is such as to feed the material from the smaller end of the'sleve to the larger end.
  • the diluted hydrochloric acid percolates out through the sieve walls into a'tank 64 and the fibrous material thus partially freed of acid is passed through screw-presses 65 where it is consolidated.
  • the fibrous material is then passed through a mixing vat I containing a weak solution of caustic soda, e. g. a soda solution of 2% concentration or less.
  • the material is treated in this vat for a fraction of an hour and this results in the removal of the chloro-lignine compounds and/or other non-cellulose soluble matter. Also, any remaining hydrochloric acid or chlorine combines with the caustic soda. Thereafter the fibers are passed through the usual washing and sorting apparatus where knots are removed.
  • the towers both for the alkali and chlorine treatments are provided with thermometers so that the predetermined temperatures of the reactions may be maintained, for example, by controlling the rate of extraction of the material from the bottom of the towers. Furthermore, means are provided for periodically testing the air and moisture content of the chlorine mixture.
  • the starting material may be considered to contain roughly 50% cellulose constituent and 50% non-cellulose constituent.
  • the stalks of plants contain about 8% ligninby weight of the material and about 42% of waxes, resins, pectic, mucic and albuminous matter, etc.
  • the amount of alkali required for reaction with these latter substances is about half their weight.
  • the chlorine gas reacts with all the lignin and with certain other non-cellulosic materials. It is important that the first alkali treatment should remove only about 30% of the non-cellulosic encrustants, since their presence in the material duringthe chlorination treatment insures the formation of chloro-lignins which are readily removed by the final alkali treatment.
  • the weight of alkali required is about 7 by weight of the raw material or roughly the weight of the raw material.
  • chloro-lignin and certain other chlor-organic compounds there remains in the material after the chlorination treatment chloro-lignin and certain other chlor-organic compounds, together with some remaining encrustants.
  • the chloro-compounds require very little alkali for their dissolution and the total amount of alkali required in the last step is less than half that of the first alkali treatment.
  • An apparatus for extraction of cellulosic fibers from vegetable material comprising a mixing chamber having a bottom wall sloping in the direction of the length of the chamber, means for introducing the vegetable material into said chamber, a conveyor in said chamber arranged to traverse the material from the deep end to an outlet at the shallow end, means for introducing an alkali solution at a controlled rate to said chamber, means for directing the mixture from said outlet to the top of a vertical reaction tower open at the top, means for introducing steam into the upper part of the tower, means for extracting at a controlled rate the treated material from the bottom of the tower, means for removing the liquor from the treated material, a second vertical reaction tower open at the top, means for introducing the treated material into the top of the second tower, means for introducing at a controlled rate chlorine diluted with air into the upper part of the second tower, means for extracting the chlorinated material at a controlled rate from the bottom of said tower and for introducing it into a cold water bath, a vessel containing a weak alkali solution,
  • a conveyor in said chamber arranged to traverse material from the centre outwards to an outlet opening at each end of the chamber, means for introducing an alkali solution at a controlled rate to said chamber and means for directing the mixture from each outlet to a separate vertical reaction tower open at the top, means for introducing steam into the upper part of each tower, means for extracting at a controlled rate the treated material from the bottom of each tower, means for removing the liquor from the treated material, another vertical reaction tower open at the top, means for introducing the material to the top of the later tower, means for introducing at a controlled ,rate chlorine diluted with air into the upper part of said latter tower, means for extracting the chlorinated material at a controlled rate from the bottom of said tower and for introducing it into a cold water bath, a vessel containing a weak alkali solution, and means for transferring material from the water plant to said vessel.
  • An apparatus for the extraction of cellulosic fibers from vegetable material comprising a vertical reaction tower open' at the top, means for introducing into the top of the tower the vegetable material mixed with alkali solu-" tion; means for introducing steam into the upper part of the tower, means for extracting at a controlled rate thetreated material from the bottom of the tower, means for removing the liquor from the treated material, a second vertical reaction tower open at the top, means for introducing the treated material into the top of the second tower, means for introducing at a controlled rate chlorine diluted with air into the upper part of the second tower, means for extracting the chlorinated material at a controlled

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US153993A 1936-08-15 1937-07-16 Apparatus for the extraction of cellulosic fibers from vegetable material Expired - Lifetime US2263903A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB22529/36A GB480170A (en) 1936-08-15 1936-08-15 Improvements in or relating to processes and apparatus for the extraction of cellulosic fibres from vegetable material
GB2061/37A GB489302A (en) 1936-08-15 1937-01-23 Improvements in or relating to processes and apparatus for the extraction of cellulosic fibres from vegetable material

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US153993A Expired - Lifetime US2263903A (en) 1936-08-15 1937-07-16 Apparatus for the extraction of cellulosic fibers from vegetable material
US153995A Expired - Lifetime US2178266A (en) 1936-08-15 1937-07-16 Continuous process for the manufacture of semipulp

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US153995A Expired - Lifetime US2178266A (en) 1936-08-15 1937-07-16 Continuous process for the manufacture of semipulp

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BE (1) BE423106A (enrdf_load_html_response)
FR (1) FR825509A (enrdf_load_html_response)
GB (3) GB480252A (enrdf_load_html_response)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2607680A (en) * 1947-02-17 1952-08-19 Buckeye Cotton Oil Company Apparatus and method for processing vegetable fibers
US2668110A (en) * 1948-06-18 1954-02-02 Spencer Method for fiber liberation in cotton stalks and the pulp
US2675311A (en) * 1948-08-09 1954-04-13 John W Natwick Paper pulp process and apparatus
US2996421A (en) * 1957-12-18 1961-08-15 Sprout Waldron & Co Inc Pulp manufacture
US3016088A (en) * 1954-09-07 1962-01-09 Bauer Bros Co Rapid cycle digester

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1132120A (fr) * 1954-10-04 1957-03-05 Mo Och Domsjoe Ab Perfectionnements apportés au blanchiment de matières fibreuses contenant de la cellulose
US5172867A (en) * 1991-09-09 1992-12-22 Kamyr, Inc. Utilization of a paper pulp digester as a structural support

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2607680A (en) * 1947-02-17 1952-08-19 Buckeye Cotton Oil Company Apparatus and method for processing vegetable fibers
US2668110A (en) * 1948-06-18 1954-02-02 Spencer Method for fiber liberation in cotton stalks and the pulp
US2675311A (en) * 1948-08-09 1954-04-13 John W Natwick Paper pulp process and apparatus
US3016088A (en) * 1954-09-07 1962-01-09 Bauer Bros Co Rapid cycle digester
US2996421A (en) * 1957-12-18 1961-08-15 Sprout Waldron & Co Inc Pulp manufacture

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BE423106A (enrdf_load_html_response) 1937-09-30
GB480252A (en) 1938-02-15
US2178266A (en) 1939-10-31
FR825509A (fr) 1938-03-04
GB489302A (en) 1938-07-25
GB480170A (en) 1938-02-15

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