BE628080A - - Google Patents

Description

       

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  The first invention results in a new composition of itifttlfcrua Int4r4 * (irit <* fit. "'\ 4 \ 1 J, ro.1uit' an island form Cnunlea obtained Using this composition, More part1cul16rGt. The invention relates to a pulp or pulp cor. tan ont do la calluloao, as well as to a product produced from excavations obtained from this pto.
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 relates to a new process for the manufacture of glassine paper and high strength paper.
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  In the manufacture of paper and other products produced in the form of excavations from 1-AteS or cellulosic pulpos, it is common practice to package the raw materials (i.e., fibrous and non-fibrous tler3 which are mixed together). in an aqueous solution to ultimately produce a paper having certain characteristics. Deleted by threshing and / or refining, so as to obtain.
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 nish prenièreo materials possessing the desired Canadian freedom for the particular operation envisaged.

   This in-
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 The invention relates to an addition material or particles which,
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 when present damns the pulp or pulp before bu after
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 conditionnemont, contributes to obtaining values of freedom
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 Canadian low. from raw materials weighing 61v6c Canadian freedom thieves. The conditioned raw materials obtained start to obtain paper having very unexpected decirablo3 properties, in particular.
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 when the paper is prepared in the manner indicated
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 in the present # 6o1re.

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  The invention relates to a novel pulp or plte containing culltilogstàe. f: 1 1 still has for objat matters prenièrea- coi- dit.loi-itiL'uo catit uii4à4-t of I.fà cellulose, c,.: 5 'prorirea.: wat dnatt.nca iu flee the cation of paper, '' j. ' The invention also relates to a new paper used in the callulu or a process for its manufacture. The subject matter, as well as other objects of the invention, will confirm the following description and the claims to which it is claimed.



  In the remainder of the present tense, we will make i-dft "reinserted to the 'leasing ci-e: r.naxis', drrria which bzz the figure shows a series of cojrboa, which are. Described more an..lc5tuils dune l' exeiiifilo 1, ces: ouz-bj% indicating the duration of threshing or pounding ui minutes (on the x-axis), p .i- liberty -tar ratio, .Iard (ordotitilia) for different wood troiaots, each di cca totos with and without the addition of 4ti cellulose particles according to the present invention;

   - lea fi, ¯rttra3 II. to IV mor.tr.mt a series of courboa, # .. # ri which have been described in more detail in example 1, the due beating or shelling of the pulp in minutes being indicated on the abscissa, while the resistance to tensile expressed in kilograms per meter of pupictr produced from the pu] pu is indicated an ordinate, each type of pàto being represented with and cana the additive material of etherified cellulose according to the present invention. ### '1: the figure V mmtryma strie di court ,, which are described more in i3tsiladç.r..a lf oxenplr, 1 8 these curves cite.nt obtained by basking the standard cenatiuitriu freedom of una pul- pe or paste on the abscissa and work until breaking, expressed ## i'1. # an kg / cm2, papiar produced from the pulp in Oi'dont.e;

   

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 '. - figure VI showed a series il cousbti6, which adent described more a Jétullt d lioxu, nlile 8, c'je courhua ôtuiit dbtanuJa a "II'-1tt..Ut. have a er.pb1qL.U read llLrrtd cUlihJ1u.liú standard du lu IJulp, jau ēUcrcibeu mi function, I ... vu! Jura Je 'lI'êIOD'1 & 1 ad pua "1'orutlon du, - ncor ;, ton kJcm ..', (an uriu ,, r , u) pap1u "pirtir do cuttu pulp.



  Lob préabiitu lnvùnclon has for objut a coaljJo, 1t1on of motll: r \ :: 8 co-uprerinrit (1) uno, Itu or pulpu of 4elluloa ut "fIfJ about 23 to 5, pi r compared to the poilu doa lIIc..tlnlo bol1 - due to the composition tutblu, from the prc1dp1t púrtlculu6 (,,,, o of a * Cellulose éthûrifi3e hydropliila, inaolublu dam gluau, microe- cd1quÓnt uniforrati, byanting a hard substitution cumprio # fcnt're about 0.1 and 0 , 7 in the chlorine polymer chuînaa pc.rÚullc: smùnt 8ubet 1tu. The composition can be prepared as a pater or pulpu bruta utJLliaaUu couuao rnti: re '' prumi & rH in papermaking, soue forma d ' an aquouâe aula- penafon of a constituent J 'uni2 mut 16ca prbIJ1ru condi-
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 tionned or in the form of a sheet obtained, canvas that a thread of paper.

   Although the nature of cellulose pulp does not
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 Abit pa6 critical, the use of about 5.1 'to u5, by weight, pure refurt at the pair of solids contained in the composition 4ea particles of the cellulo2u etherlti precipitated by "' c't'cfbillol. Of which and identified above , in a well-beaten, well-beaten sulphite paste, having a standard Canadian freedom of about 500 to about 100, prmut the formation of cria-ta4 paper possessing a degree of transparency, an impurmâebillt6 A tasvepeur, a resistance at the graiuso # an etiptrtitic shine, a flat character and a printable character which it is not evoluollerns possible to obtain only with much more often pounded or beaten in the prior art.

   The umplol of about 2 to about 15-, in weight, prirrrap- 'port au weight duc tnatièrur solids contIJnu08 in the coinpqattion, d. particles of etherlCl6a callulosa precipitated by (i5aillg.

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 ment and identified higher, with pulp of the pulp #cr t, gives, when the cup is transformed into a dig) 1 par. application on a perforated surface with relaxation of the still wet sheet, to allow its contraction in direction! transverse from about 36 to about 2G 'avuc ur. 8ue- i quant drying, a paper exe.npt of int tensions.

   rnca, which has 1 strong tensile strength, great mechanical strength,
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 high elongation, and high energy absorption capacity,
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 dc, noting that a toughness, a resistance to bending and a
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 high abrasion resistance ** compared to the properties of a
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 kraft paper from the raôrav poLOa.

   Regardless of the nature of the palpa used, the use of at least about 2 by weight, relative to the total of the solid material present, of the cellulose particles GtllGrifi4ea urlcrito8 percot a 1iJ \ l1ol at1'Ó / I dat.3 loa papermaking processes, this improvement being constituted by 110'1 substantial reduction in the liG rta of the raw material without the, -m-ntation of the duration of threshing or pilor.nage, r: r6ce to the addition of particle dd çyunothylcalluloaô la mEatl'r6 prernH: re, this addi-
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 An alternative to beating was to remove dough. This addition
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 AàJnél1or .. amused the formation I the girl, all one allowing the use ji) tuacttlna5 operating at higher speeds- Vu * 4 at rt,. rn r.t. the use of materials #: .... of u! '. contiatunce greater elbv6c, sana porta da finished product.



  Lda jilrticulma pr & clpito8 by shearing in ellu- lou 4thljtrlé "t which oont use 1liE ± 1blt: o in the process according to the present invention are collo3 described in Belgian patent n * 61) .55 'blan qua cortainua calluloues etherifices are known tactically (MacCragor et al., "J. ::

  jonc., Dyers and Colourleta ", 6, 6? -i, 3i and b" 6 \ 1lttO duo tats-ünia of America n. 2,522,627 dt 1,914.17 *), the i-rivs described in the aforementioned bravât have conaldéré comma .o'jvaaux and as possessing

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 properties which could not be obtained JuLiqtilà pre- are, by a result of a new molecular structure, in addition to their hydrophilic character, their insolubility in water and their microscopic surface laurel, described above, the derivatives referred to in the bruvut bule this characterizing ti'1uoent by an aldv3 dugrô1 of water absorption, when they were dabhyd! Mt. <a, Minai, quu by urf5 molecular structure earisiblument not criamilinu, but well ordered with great mobility in the aut> moultàt, of the chalno. Derived cases that can be obtained by various procedures.

   The cyunothyl3 aat product obtained, the most 4onunolémant, by Addition of acrylonitrile is dd hiaulfura do cm bonu with the churn, during the conventional process of OU> f., Ltlul, 7, xo.ntlrog3netiorJ, an amount tuffioanta of acrylonitrile being added to obtain an amount of alcohol content of between 0.2 to 0.7.! .n n .- .al, then about 0.5 mole to .0 mole. ma aci ylonitrlla per mole illuiiliydroilucotàto.



  The purpose of the cat j ion contributed to aolu2ili: rar the product tnate cuci have not been able to aauanttul for the production of I) ru, iuit. eyuro3tt, yl.Àru.l, da, ulvali cullulo. can be yanoûthylôu by dirocto addition of aoyionitrilu, consmu described in an exan.pla given further. Cutto fotTnu'du rcalita- tion of the product according to the invuntion axises the use.) 'M ... Lolu- tion eLu2 * licua pluma concufttrau for 1 aolubilia.'r, per t.uit dd iibsoiicj do ¯rjupu ; xanthata, :: n plua xantij'hution,, i: t da 1!, 3thrifi4ütion ai, nultfn # dn, on n pci u auaui i o 1; % i has una 'taothoe, 4nation before or after the ettrlfication ut on ot. then holds a more alsûtient tolubla product.



  # '' '# La pfodu.-ion d4u'tiara autan dua lois Utitui-a Lyaj) o- èthyiào ae made by contact of the alkali callulorsd noua forma zo 1 tci cy with laan, dl'cth4riti (-ation, such that an oxy, lu of alkylene or of ethylene cllorr.ylrtn, 1-c, rn, uôn utilim- c-'te tqclinique, a e.ftployajtt da l'oxyda J'alcoylétia colije & Lt4tit

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 di6th4rificationp It is essential that the alkali çellulooo have a caustic content less than about 30, relative to the weight of the cellulose, this content being di r0 ferencej from about 18 to 22; (, while IT is; ralemon -. ē :. r:

  '. such that a sufficient amount of the ethicidal agent is added to provide at least about 30% by weight of alkylenoxide, based on the weight of the cellulose employed in the
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 the reaction, The use of alkali cellulose 4 concentration more
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 High alkali and / or the use of a lesser amount of the etherifying agent generally promotes the production of a water insensitive rayon-type aα-1r.



  Particulars precipitated by 'shear' - 'critea in the aforementioned patent, which are useful for the present invention, are formed by precipitation of the other cellulosic in solution, under conditions of normal shear and speed. coagulation such that one ob-
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 holds a total shear value (R'3), tcllo that de-
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 finished higher. between approximately: 1 and 10,000 and,
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 ference, between about 100 and 1600.
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 The "total shear value" (R'S) is dt "1ni"
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 by the formula:
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 Rfa ...! U ..

   R t.
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 in which Vs and V3 are the viscosities of the precipitating agent and of the re3poctiv% lmoiil cellulose ether solution, in weight these viscosities being measured at temperatures rrs-
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 pectives of the agents in question before combining them, to
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 rormQ the precipitating agent, t being the duration gold. microte-
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 condoa during aquello the precipitate this deformable. When we
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 wishes to use the material COTn.'n1) constituting a pulpa or: Ge, it is preferred that the length of the precipitated particuloa dQ): yJr .. tdoa be cornpz: 01eoc between about 8 mm and u # 5 an, Cuanioit, avoc , an appropriate device, we can treat partlculoo

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 u f; u% 0 v% i up to 20 mm in length.

   Particles less than 0.001 mm in length are generally too fine to be of appreciable practical value. Dosage procedures suitable for the preparation of these particles are described in Example 1.
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  The test and coracterioation methods employed to measure various properties discussed herein are shown in the following Table I. Unless otherwise stated, code numbers indicate standard TAPPI tests.
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  A BL7.AU I
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<tb> <SEP> Esal properties
<tb> Liberty <SEP> Canadian <SEP> standard <SEP> T <SEP> 227-58
<tb>
 
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 Abrasion is A9Tt D-1175-55T (method A) Dielectric strength ASTg-C-149-5'ST (iron. Apec.LP4 6B. Method 4031)
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<tb> Resistance <SEP> to <SEP> tearing <SEP> Ilmendort <SEP> T414M49
<tb>
<tb> Elongation <SEP> T <SEP> 457
<tb>
 
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 Grease resistance Tt; St ,:

  60
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<tb> MIT <SEP> Fold <SEP> T423M50
<tb>
 
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 Mullen burst strength Tt03M53 Opacity - T425M60 Porosity Tt, ôOil9
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<tb> <SEP> perforation test <SEP> <SEP> Thwing <SEP> Albert <SEP> Instrument <SEP> Co.,
<tb>
<tb> Phila., Pa.- <SEP> Directives <SEP> for
<tb>
<tb> <SEP> perforation test <SEP> apparatus <SEP>
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 SPisNC R,
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<tb> Rigidity <SEP> T <SEP> 451M60
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 Surface gloss T 4801451
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<tb> Resistance <SEP> to <SEP> the <SEP> traction <SEP> process <SEP> T404 <SEP> revised <SEP> (process <SEP> Tappi
<tb>
<tb>
<tb>
<tb>
<tb>
<tb>
<tb> proposed <SEP> in <SEP> project <SEP> Tappi <SEP> 769)

  
<tb>
 
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 Vapor transmission T44atdti9 Work until breakage process T404 revised (Tappi process
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<tb> proposed <SEP> in <SEP> project <SEP> Tappi <SEP> 769)
<tb>
 The following examples are given to further illustrate the invention, but it is understood that the latter is not limited thereto.
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  ¯¯SÎB5ÎTLE 1 Preparation of particles of C1 \ QO <5th <* rl.fléo.



  Standard cotton lintor sheets are trem-
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 pa "oa in a caustic elbow solution, after which they are added to hydraulic pressure in a ratio of 3/1 (so11-doo% liquido3j by weight. Alca-M cellulose excavations are

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 then d <chlqu tt4 and 9taintanu '! 9, laying the tr * lt rï5ont cuh.' 'quente in a retrigbr6o encointq, At a tepdratura Inf' # * lrlauro II SOC, IaIe0.lt celluloaa thus obtained at the c: -,;.



  #ulvtnt! c'Hloft priclfl tubl Jl # 2 pourcsnt tn pat 'a hy.! ro <ydw a r1n ao1 iurr 1 $ ,? "## J 5.03 20 pounds of this alkali cellulose are in a 12-gallon bat- tle. We turn the cott6 churned when the clteurfo is used until a ttynp6r & t * ure ir) t '! Ri'uro in 2tC. Cv mi - ment # 'i6i t (2 # 13 litron) of carbon disulphide and read, 0 (2.27 lbs) of acrylonitrile eont adjuutdz on the aapacra asr 10 minutes. Penlant the xarvt !, uf, , 0 and garlic cyanoethylutin, m: Sr; " the tomp4r & tur * of the reactionnulla ataaae have ssin'o, to cr, turns :: 300- '. The reaction proceeds about 30 ninutin and has ended by interrupting the d4,, ati, fesint de ciealr, tr la -mâs3, p r4actlonnollo, Ln xanthato rio cyanothyl cell'109 <! obtained was then said in a solution A 4 '% # d9lydroxydo te coilur. ot
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 rorro1d1 to Î 4C.

   Loa prpr1td 1 la viacoa * do cyano1thy \ c!: Lu- '1080 i co o-ant eont 1rdlqtJAftO (1nt) le t.ahlQal.1 1.



  1r b n
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 Soil index le ViecoaH4 30 to 50 etronden Du Pont at 13'G z Cellulose 1 '5t0 (approx.)% D' <JLc <Min! T4 5.44 total sulphide 1.12% total doa.ots 0.43
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 A Degree of substitution of ether Co4 "I at Kaourb on precipitated particle and rn'e4n4r & e.



  The solution to is primarily prtr c18al11fnt, by linking a collector to a tp4rQtr. 19 15'C rx toue a pressure of about 5 # 6 kg / cta2t a pure prasant 12 holes of a diameter in 0 # 05 cm, in a tube with a diameter of 4 * 0.31 passing through the manifold , an aont of precipitation iquaux eontonant; r on polis of adda sulfurlquo nt 15! by weight of the roof sulfate = being fed into this tube, a trrp4rature of about 35 ° C ot under a pressure of about 5A krJcm2.

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  The byctemo gives a total value of clQG111'ent of about 351. The * particaloa precipitated flbr uiî. a are rcJcuofll106 on a truillia and err1: o helped him with a rouluau, so A forma r dos nappoa 't'un', t5p loo ur da le-17 en. Loa tablecloths Which then malntonuoa At the ambient toap4t'atur} poniant at least 30 minutes to ensure uno rt:, nûratl.n complete cyano-ethyl celluloso. at: ro what elloa 3, rit: s1nsul tanÓant noutra- lie4et and d Sshy1ratâos oemottquemont. par i "M ') ralon in a bath containing 17% by weight of sultato de nolitim and 2% by weight of phO9phht dbod1que mon" hydrogné. adjusted to a pH between 5.0 and 60. After draining to about 1%, by weight of solids, the water is added to about 30% by weight of satiCrtia aoliJoa.

   Loa particles have an enu uptake amount of about 9 g per particle size 8.



  Use of nrtt 1 \ 1 ..,. ,,, {'' '1.1' 1 \., .. éi f1.f) co-1 mplre lii o rl'ro, ': irH riun "l:"' 1 ln.



  Three .5ct, o.otUlonn do 200 g do patec d't toit C ') I # \.' T- cialoa con treated at constant speed, we a load of Valley 5 <4 kdana und pile do laboratory / d 'a capacity of 06d kg atandard TAPPI T2GQa: .S, on nuopenaion aqueuae, with uno ClAt1br03 aollios content of about 1;:, PQnJ8flt of divorsea durations.



  As the traitoraent in the stack progresses the samples
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 samples from which the value of Canadian freedom is
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 determined, Loa obe <rvationa are repeated in figure I, where the curvy G, 0 ot 1 'which relates to reapoctivcsent pltao de scluro di boize de chine and do pin indicate the durdu do bottaqo on minutes (in abocloao), according to the Canadian atanftrd freedom in ordinate. Doo excavations are made From each sample taken, aolon proceeds TAPPI T2O5M50, except that one uttllli8 a sheet of 20.32 x 20.32 cm having a weight of hwrw dm 22.65 (2 x 36-500) from the fulpo do pin ot "0 chfine and a leaf do

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 16.12 kg (21, x 36-500) From ground wood pulp or sawdust.

   The tensile strength, expressed in kg / c #, is indicated for these excavations, on the y-axis, a function of the threshing duruo, we abacisao, In Figure II ("P" pin), at 1 fi; III ("00 a oak) and in figure IV (" ù ". Ground wood), During the same threshing operation, we add?
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 In the samples / do pfita beaten, a sufficient quantity of etherified cellulose particles, prepared as described above, to obtain 10% by weight of solids of these particles, at a consistency of 1% .

   The reduction in threshing time necessary to obtain the same value of freedom emerges clearly from a comparison between the curves Pl (pine paste + particles), O1 (oak paste + particles)
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 and Gl (ground wood pulp + particles) avic of the r.o '...,' l ',,?, 0 and G of Figure I, while the presence of etherified cellulose particles also provides an increase in the re-
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 tensile strength of the leaves forces Ii from the m3- langos, as seen in Figures II, III and IV respectively-
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 (the sheets P1, al and 0, being comparable, with regard to their weight, to the collas described previously for each figure).



   The duration of threshing can also be reduced,
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 by adding the etherified cellulose particles to the raw material, before refining.



     Example 2.
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  Production Znninl: 3 of typn -cri 2ta.



  'A pulp bleached with sulfitefost treated slowly in a Hollandor type pile with a capacity of 136 kg for 3 hours and 50 minutes, until obtaining a standard Canadian freedom value of 331. The pulp thus treated is retained in a first tray on China. A second tray contains I) p6 kg of the deherifido cellulose particles of Example 1, also at a consistency of 1%, 13.6 kg of pulp are

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 transferred to the reservoir containing the etherified cell particles *, so that a mixture of 50% is obtained
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 of particles of th6r'lfido cellulose ot 50; 6 of sulfite.



  A portion of the 100w sulfite parte was processed into a paper weighing 43.6 kg per ream in a 78.7 cm Fourdrinior paper machine, this paper being used as the control paper. In the following test 3.85 kg of sulfitu and
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 3> 85 particles of etherified cellulose are pumped into the 21.29 kg of sulphite pulp contained in the first tank, so that a mixture is obtained containing 13% of particles of etherified cellulose, this mixture being used for
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 the manufacture of a strip of paper several tens of meters long.

   In the final test, a mixture containing 20% by weight of etherified cellulose particles is prepared and produced.
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 a banda of paper of several tens of dqT.otres with this mixture. mixed. The data in Table III show that the addition of the etherified cellulose particles made it possible to obtain sheets of paper of a quality similar to that
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 of glassine paper, from bleached sulphite pulp with a Canadian value of 300. This shows that the particles are able to seal the pores in the sheets. The substantial improvement in grease resistance and
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 Water impermeability should be noted.

   The strong decrease in opacity round the product very desirable for the manufacture of transparent paper. Comparative fine back, the properties of a classic crystal paper, prepared from a material
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 The first having a Danadian freedom value is also shown.



     TABLE III
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 r '! \, 111J n' t) l (lnd111'1 nu tlJ.f.'1t,., (llb. çnnndinno 300)
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 nt, r "l¯e 12 CYRC 20.) CYEQ Ba3o weight 32.5 lb / oar 6, J 11vrre 29 # 6 will deliver Porosity 2O sec. 1800eec. 1800000. me R601and'Il \ C0 at the 30 eoc graicoo . 18003qc. 1680 coo.



  Vipuur trancaiMaicn 455s / m2 / 24 hr. àOJm2 / 24 hra. S5r) m2} 24 hours.



  Opacity> 1> X 3ü% 25e4

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 ; I \ .f} 3 t e'Aiftt {llh.1'lnrjl "o" 'Jr: O} Mrt ILI 2 f! E 0- -1 1!%, L 1 E &, -, (%.
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  Coorr12 12. 0.1, 'r4 Y' - 1 O.J.y.!;, Weight of bac # 33,8 llvroßrtue 29,3 itvrrr'ram, 31, ï ilvc-- '; Poroatt4 '601. oe ... 11 \ 1.; 0 MC :. "Z''tJtJ n'n.



  , .ra n 6 CIl hll. c te. born. A 1 <f \ .. '/ 0 ..- tluo (tG r <iae <io A!, Ait' ,,. 1'L / u 89, Tranmission) GO) / 24 106 -, jmj4 96 / m / 24 do steam hit h'Jur., 1) h ": Jr.,., Opacity. 1% 25:" 20%
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 Pépier crial p-l'n ohMt 11fut, l = fInhtA'i r.:t '7 I n v1 orLa .7 ^: I t..T1 r,
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 PoiJtsd bA4 * in livrae / rwne Foroi 1 t4 --- ----- - # - # - # t4oo'o c, R Soiatanoe 1 la gr laA.; ##: # I'jOO a c, '# .- # .;' ? ranolaoion dē vanur, GOp, / m2 / t4 .hour Opacity 16, j
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 BXM! D1 <paper di41: -iT! '!. una -par'ticles of? cellulose 4th4ririo, pri, -. r.::c 5¯ la maniera described dani 1oxrnplo 1, August m-îlangéfla in divoraea proportfon4'à sulphite bleached p & ta pru'5antant a librt5 value c'annifonnn! n 1 ' .Co prayed threshing or pounded ?, *) do cotts dough;

   Ûoo separate addition of 20, '.0, 60 and 40 on weight, relative to the total d-in matthrec eo114 psiafn.a porticuloe, were made and dne louillas of 2 g eint fa- lighter in a mold 3 fouilla, d It re-described in the exMtpl <1. Uno a'.rie 3a sheet '& (A) is a4ch'e in air temperature arabi.nt; a necon-li 54.-le'do'feuillis, (3) was compriaie at J5 k / Jcn2 during the minutas at mpratur iabiante, tandia that a third series of leafy (C) eet ccaprioe A 35 kg / cm2 for 8 'minutes 4 1C, the dielectric reinstatement of leafy trees is tustde. The results are shown in Table IV.

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  Bzz li3i3tanca diSlActriquo (rupture volta / mlll Itinu do thumb)
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 $ 3rt.l! 11l ..? 1. (t1- .r..r 9 C 100 0:! 9 929 517 00 20 47 tJ. 9) 2 6 <5 J * 0 "" G '> 74 t, 16 40 60 517 1. '.: \' Il 20 ti0 417 U7 iid 0 100) :. 3 j: 0 329
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 : y ;; PG ;, &.



  CD.cit r "\ l111Qo de- 21 ,. Ott rtIP 1 Ait -Cillfily.



  The effect of already particles of ClZuloco tt: 4; ifia on i'opocit3 of deciduous trees obtained from a sulphite block at 4t4 4tti-àà, 4 à divurcoo concuntrationa un prwticulos. Two types of particles. obtained in the manner described in ex. 4- pla 1 and at a constancy of 1: on matibron aoliden on cuapon- son aquouso, are used, without beating and After beating for 1 minute in a laboratoiro melaigouro rotating at full speed. Three grades of sulphite bleached pulp are used, these pdtoa have a standard Canadian freedom of 120o 24S and 75.

   The p & ta particle suspensions are combined on tnalaxunt dOuc4ml4ilt, da r, ', OI1 a tOM4r (lets eue- penoiona contrant 1 ..: de matter 8olir: a Na c'jopenaton and From these outpenuion3 paper excavations pisant 2 granmoa are made in a mold, lying and edch4o3 by operating the raaniro described in 10cxe-iplo 1. The opaci. tea dos various feuill-ja are indicated as a percentage of the incident light removed by the excavation.
 EMI13.4
 indicated in Table V.
 EMI13.5
 



  Taal .-: AL: Opacity dg "at, ui-¯ 11 ^ 5
 EMI13.6
 Dl'rt1 <: ulq /.5 t'u1.D 175 pulp r150 YB9 0 73, 2t 10 66.6 70.8% 65 20 55.6 * 66.8. "61 JC 30 43.0": 60.4 : '8 40 J5.6': 51.1 35.Î 0 33. 30J 60 31.4 '50% 2l ± 100 12,

 <Desc / Clms Page number 14>

 
 EMI14.1
 Examples 2 to 4 given above illustrated the use of etherified cellulose particles as an additive material for crystal paper type papers and
 EMI14.2
 other special papers. Within the scope of the present invention, however, it is also possible to obtain single-faco or non-homogeneous papers which have a high concentration of etherified cellulose particles on one side of the paper. The following example illustrates this impact of the present invention.



  FX '.' PL '; 5.leaves with a very shiny color. "Sheets are prepared with various percentages
 EMI14.3
 of sulphite bleached pulp and hydrated cellulose particles of Example 1. Two embodiments of the! a311as, designated "B" and "L" are employed. In the "br 'type, 103 ingredients are mixed before the suspension is v3r3c in the mold (technique of Example 1), while in the" L "type, the sulphite paste is laid as the substrate and particles are laid down. deposited, in the form of a surface layer,
 EMI14.4
 on the substrate. The tests were repeated with a paste showing two different values of the standard Canadian freedom: 110 and 205.

   Each dig is compressed to approximately 4 # 2 kg / cra2 after air drying at room temperature.



  The excavations obtained are tested, with a view to determining their resistance to tearing and their opacity. The results obtained are shown in Table VI. Further, the surface gloss of the sheets is also assessed in a subjective manner. Finally, the leaves are metallic
 EMI14.5
 in the usual way with the aid of a 16por rovt3mont evaporated aluminum deposited on the surface in otherified colluloso.

 <Desc / Clms Page number 15>

 
 EMI15.1
 2A7Ga:

  IN VI
 EMI15.2
 
<tb>% <SEP> parti- <SEP> Freedom <SEP> Structure <SEP> Resistance <SEP> Opacity
<tb>
<tb> cules <SEP> from <SEP> aul- <SEP> from <SEP> to <SEP> tear-
<tb>
 
 EMI15.3
 rite excavation3 ment lmen- dorf ¯¯¯ ¯¯¯¯¯¯ (E / g / a2) ¯¯¯¯¯¯¯¯¯¯
 EMI15.4
 
<tb> 25 <SEP> 110 <SEP> B <SEP> 0.24 <SEP> 38
<tb>
<tb> 25 <SEP> 110 <SEP> L <SEP> 0.46 <SEP> 49
<tb>
<tb> 25 <SEP> 205 <SEP> B <SEP> 0.29 <SEP> 47
<tb>
<tb> 25 <SEP> 205 <SEP> L <SEP> 0.42 <SEP> 55
<tb>
<tb> 50 <SEP> 110 <SEP> B <SEP> 0.33 <SEP> 24
<tb>
<tb> 50 <SEP> 110 <SEP> L <SEP> 0.43 <SEP> 37
<tb>
<tb> 50 <SEP> 205 <SEP> B <SEP> 0.38 <SEP> 26
<tb>
<tb> 50 <SEP> 205 <SEP> L <SEP> 0.46 <SEP> 42
<tb>
 
 EMI15.5
 In each case, the multi-layered paper has a greater tear resistance than the mixed paper, while its opacity is orally greater.

   The surface gloss of multi-layered sheets is very high and is even higher than glue: mixed sheets. Metallized foils have a very high reflectance and multi-layer pits are significantly brighter than aluminum foil. Papers of the type in question can also be prepared using conventional multi-tank machines, in the same way.
 EMI15.6
 whereby a high concentration of etherified cellulose particles is deposited on a surface of materials forming heavy papers.

   In the product obtained, which is a heavy cardboard or paper, a high surface gloss was observed, as well as a good capacity or printability as well as a good permeability to water vapor and a good resistance to grease, which are due to particles of
 EMI15.7
 cyanothylcellul03e found on one side of the product, while the structural resistance of co-product is not otherwise
 EMI15.8
 no affnetdeo to causa of the presence of the other constituents in the other layers.



   Diaper papiora '! multiples of the typa described in
 EMI15.9
 the example given above possesses other unexpected qualities, in addition to those of conventional materials. Thus, the presence of thermo-cellulose particles in the layer

 <Desc / Clms Page number 16>

 
 EMI16.1
 superficial non-flow gives better superficial shine, greater resistance to grease and better resistance to water vapor, milking ello p ') 1: \' lt attani more sticking and more use " <5c n (, 71.r. \ '. Glue, lora do lu making bolées.

   In addition, the net rartotl far superior to materials C: ": t .. '1Iu!' 1mlJnt u'.l liedea for the manufacture of said boots, we co which concerns con
 EMI16.2
 printability.
 EMI16.3
 pXDlQ
 EMI16.4
 Atjdltlon..J2 Dl1n1, uh do cft11 \ iloc 6thirlC11) &. 4? the nftr, *; Krft.



  1
 EMI16.5
 435 kg of kraft pine payroll is pounded in a Hollander ponant 130 minutes pile, to a value of the standard Canadian li- berj3 d4 5O ce. The material obtained 4 a
 EMI16.6
 
 EMI16.7
 fold of 9.0 ejunq conzietanre of 3.55 ;. The matllrn is tr-'nr.f'r. 'in uri4etirvôire and then in a Fonrdrinter paper muctvin, in dilu6o lac4uullorezt until a conttetanec of 0.28. An "A" paper having a basis weight of 20.33 K (24 x 36-500) was obtained under conventional conditions, a Vit433o of 45 cm / 30C. da ra; on for a 100 cm excavation.

   A second charge of "3" pila is handled by maniro
 EMI16.8
 similar. unless a commercial variant of the
 EMI16.9
 conventional process ("C lu pa c" treatment of the tats-'Jrsis!
 EMI16.10
 
 EMI16.11
 of America No. 2,624,245) to give an allonzeiiont of at least about 10 in the direction of the machine. 1. * proc <î <1 <î lm;> H-! that a compression during the aûc = ae, to give an extenaiblo paplor, The unit "Clupah" oat diapoc: o utter the second c4-- choir and the third aécholr. Speed at the end. 3rd echo have 47.5 cm / sec. And 43 c-n / sec. after the "Clupak" treatment, a pressure of about 1.4 kz / c2 Ctcnt applied to the product. Those sweet eaaaia nervunt of control.



  A troiae pays (498e3 kg) of pine "C" this treated in 150 minutes up to a value of 600 of Canadian liberty! na standard. 8 $ do etherified cellulose particles do

 <Desc / Clms Page number 17>

 
 EMI17.1
 Example 1 are added to the particle thus treated, the addition of coe particles lowers the value of freedom to 410, The material Qat then brought into a machine is paper and diluted until uno Cvn1I3tMe do 3î, t76 ot a fold from 7.1. The stalk is treated under current humiliating conditions. Sn controlling the t!: 1., ": R: .t \ U'c. Les Jc: iQ1r (tly.r '-: t1té îlfltieiârui'e! 2? OC and final end at 83 * C) and operate in a loose way, using Eeutl '(j8 lAcho :: s), we obtain uno relaxa-
 EMI17.2
 tion ot a contraction in transverse direction, the final sheet having in fact 96.52 cm.

   Half the material of
 EMI17.3
 do offset is * rait6o in this way. The remainder, namely the material "D" is treated in the unit "Clupuk" resides so as to give an extension of about 10 in the direction.
 EMI17.4
 of the machine. The four papers obtained above are tested, in
 EMI17.5
 d4turminur view of their physical properties. The obArv8tlon: s
 EMI17.6
 are shown in Table VII.
 EMI17.7
 



  TABLE VII
 EMI17.8
 JL JL Il -EL Boa weight. (lbslr & me) (24 x 36-500) 46.0 47.0 45.6 43.5 Tensile strength 464 238 603 (kg / a) * MD 464 23Ô 603 455! CD 255 187 455 318 Elongation (#) MD 2.7 16.2 4.4 18.8 CD 5.8 6.6 11.1 11.0 Working Until breaking (pouco-Uvrwa / nouca MD O, 4 ? 1,26 0,90 2,5 squares4) CD z6 0, '. A 1,8 1,4 Rdciatancc nu d4ciiiremunt 14D 107 122 82 97 I.1mondort (t) CD 117 12, 95 101 Maiettnce to the burst - mont Mulleu (kg / cm2) 1.75 2.0) 3p43 3.64 Spencer perforation z 3.2 3.9 6.5
 EMI17.9
 
<tb> base:

   <SEP> 2couchea)
<tb>
 
 EMI17.10
 ipouce-livrenipouco carré) R6e1otanco au folding MIT MD 370 560 1660 1140 CD 1d0 70 3110 2940 Abrasion C3I MD 4 2 25 104 (cycles) CD 9 20 130 12
 EMI17.11
 t properties of the machine direction - ---- * property of the transverse direction

 <Desc / Clms Page number 18>

 The comparison of the two commercial products A and
 EMI18.1
 B shows that paper B sacrificed tensile strength in favor of increased elongation in the direction of the mucl: "mu". In addition, the work to breakage in increased d1rctl rJ: 'D cat is in the transverse direction "CD" the work to break is substantially constant. The tear resistance is slight and increased, both in the longitudinal direction and in the transverse direction.

   As for the crushing resistance, and the puncture resistance (non-directional properties), they are higher. The resistance to bending will improve in the longitudinal direction, but it is much
 EMI18.2
 poorer in the transverse direction, while the abrasion r, 5qistcra in the longitudinal direction is decreased by T.ltio.



   The comparison between products A and C, namely the control product and the simplest form of the product according to the present invention allows the following observations:
 EMI18.3
 almost every physical property of sheet C Qat improved over cello of sheet A. Tensile strength is increased in gentle directions. A11onemontt increased by 50% in the longitudinal direction and by 80 in the transverse direction. The work to break is doubled in the longitudinal direction and tripled in the transverse direction. The increases in folding and abrasion resistance are / * to 15X. It is clear that product C is ideally suited for the manufacture of bags.



   When we compare product C to product B, which is an oommorcialo quality product, we see that the pro-
 EMI18.4
 result 0 is greater than one, which concurs most properties.



   Finally, when comparing products B and D, which both underwent the treatment. extensible kraft *, we can clearly see
 EMI18.5
 #qn product D is a <* riflijr, co which makes it pt1'.1lièrf "ptQ to be used as material for the manufacture of bags.

 <Desc / Clms Page number 19>

 



    All properties except tear resistance are superior to those of product 8.



   Products C and D all provide soft, tough, high tensile strength and high energy absorbing backing papers which contain ideally for bag making and many other uses.



     EXAMPLE 7. Preparation of papers suitable for the preparation of bags.



   The procedures of Example 6 can be applied on a large scale, for the manufacture of control papers and experimental papers suitable for the tabbing of multi-wall bags. Six separate tests are performed with the same paper machine. Five tests relate to the manufacture of paper having a basis weight of about 22.65 kg per ream, while the sixth test relates to the manufacture of paper having a basis weight of 45, 2 kg / year. In the first test, "A", a control nutural peta kraft is used.

   In the second test "B". the same kraft pulp is used which has been treated by the commercial "Clupak" process,
In order to obtain extensibility. / Tests C, D, E and F, in each of which the "Clupak" process is applied, a mixture of kraft pulp and particles of cyanoethylated cellulose of the type prepared in Example 1 are used, Escai "C" using a mixture containing 8% by weight of particles, while the other tests use a pulp containing 6% cyancethylated cellulose particle. The papers obtained are tested and their physical properties are shown in Table VIII below.

   These physical properties were determined in an atmosphere of 50% relative humidity and a temperature of about 3 ° C.

 <Desc / Clms Page number 20>

 
 EMI20.1
 



  TABLE VIII
 EMI20.2
 
 EMI20.3
 A pcp 1 p Freedom mix kraft 650 6W 650 650 650 715 Cabinet weight (liTrea / rMte-24x36.500) 9.6 50.6 52.1 4.9.7 9 *, 9 LB, 3 Resistance to t.rt 'et1oc Pu 424.63 209se4 574.77 "' O, t9 1.165.6 426.4 (* / # CD le", 07 1 * 422 1c, 35 J78.A.2 717.57 340.93 111 = 84.- Bent M) 1.5 11.9 12.8 10.5 10.0 9, e I: 'J CD 3.1 3.8 6:

  6 6.1 6.9 5.0 8aiataics MD strain 0.23 0 63 2.06 1.55 3.60 1.31 (inch-pounds / square inch) CD 0.22 0.26 1.05 o, eg 1093 0.65 Tear resistance Rla niorf l'.a a8 09 100 <. 'At 191 101) CD 91 127 116 107 273 122 Spencer perforation 1.17 1.96 6.20 4.82 12.0 3, tus
 EMI20.4
 
<tb> (inch-pound / inch <SEP> square)
<tb>
 
 EMI20.5
 Burst strength mulleu 1.59 1.45 3.95 i, 43 7, Sb 2,9, (kg / cB2) Bending strength KIT XD 80 130 3.050 1.R80 2.640 1.970 (cycles) CD 225 30 z , 0 840 1.270 630 Porosity -), 0.9 91.6 27.3 59.0 13, (bag / 1o0 cc) CSI abrasion

   KD 8.0 8.3 134 108 730 6j (cycles) CD 3.5 5.8 163 132 580 65 Stiffness Clark XD 1.720 18.1 2.6 0.2 10 <) 1.-1.7 CD 62.6 z ?, 5 ol, 457.4 zg J3 3 0

 <Desc / Clms Page number 21>

 
 EMI21.1
 De * * osais de chut * have 4t4 * ffectuès with sacks made with the help of papers obtained in dares C, D, E and V. These tests have revealed that the bags are remarkably superior to the usual bags with regard to their resistance to
 EMI21.2
 rupture, tear, tearing, etc.

   C9Drplon 2y2c a known stack additive,
 EMI21.3
 An unbleached pine kraft is pounded to a consistency of 1% in a 0.68 kg laboratory pile to obtain a series of samples exhibiting freedom. Canadian Standard of 715, 597, 4) 6, 305 and 170. Fractions of each of these materials were used to make dao Jchntl11ono dt paper, as a series of control samples (curve "1" of figures
 EMI21.4
 V and VI), from a second series containing 5, e. by weight of the comuarial addition material called ^ Cato n. 8 "vend1.8 by National Starch Co.

   (curve "2" of Figures V and VI), and a third series containing 5% by weight, by ratio to the total weight of the solids in the presence, of cellulose particles
 EMI21.5
 6t5rifiéa of Example 1 (curve "3" of figure V ot VI).



  The particles of Example 1 are added * as a 1% slurry (Cato No. 8) * and stretched with water to a consistency of 3%. then the mixture is heated to 195 ° C, dissolved and kept at this temperature for 15 minutes, after which it is diluted to a solids content of 1% and used at this concentration.

   Among the 15 different types of papers thus obtained, some are dried
 EMI21.6
 under tenoion on a heated plate (curves in plain lines of Figures V and VI), while others were displayed at the relaxed state (curves were treated interrupted in Figures V and VI) .After drying, all the leaves are tested for determi.
 EMI21.7
 to determine their working properties J, '4that rupture and resistance

 <Desc / Clms Page number 22>

 to the Spencer perforation. these values are shown on the ordinate, according to the standard Canadian freedom values
 EMI22.1
 which are indicated on the abscissa in Figures V and VI.

   The 8p6r1o-. rite of excavations according to the present invention is obvious. when considering these curves.
 EMI22.2
 



  Example 9 Effect of 18 particles of collulose thrown by DeDier pine kraft obtained by o11qunt conventional treatments and 19 trfite'ntnt relaxation.



   Papers are made using kraft pine pulp. A portion of the paper is made by the current commercial process, while the second portion is released wet overnight during processing, after
 EMI22.3
 where it is, various percentages of etherified dp-cp.lulose particles of Example 1 are employed. Sample A refers to a control sheet without additive material, while sample B refers to a material containing
 EMI22.4
 1.9b of additive material and that sample C refers to a material containing 9% additive material, these samples B and C being used in the current process as compared to the modified process.

   The properties of the various sheets are shown in Tables IX ot X.
 EMI22.5
 



  TA9LrAU X Current processing
 EMI22.6
 . -1- JL Tensile strength (kg / m) MD 511.63 647.95? 63.6l
 EMI22.7
 
<tb> CD <SEP> 253.47 <SEP> 265.58 <SEP> 431.97
<tb>
<tb> Elongation <SEP> (%) <SEP> MD <SEP> 3.6 <SEP> 3.1 <SEP> 3.6
<tb>
<tb> CD <SEP> 6.6 <SEP> 7.0 <SEP> 11.6
<tb>
<tb> Resistance <SEP> to <SEP> 1 <SEP> bursting <SEP>
<tb>
<tb> (kg / cm2) <SEP> 41.6 <SEP> 55.3 <SEP> 79.0
<tb>
 
 EMI22.8
 Folding resistance MD 895 1525 5250 (cyclea) CD 270 1650 3490 Rb! Stance au d4chire- un l '18 1.07 1 OJ llZÂfoït Z) CD 59 1.11 1.10 Ramo (PC? 1 \\ a (lhrlO ) has x> 6-5O0 51 47 52
 EMI22.9
 
<tb> Work <SEP> Until <SEP> break <SEP> MD <SEP> 0.47 <SEP> 0.72 <SEP> 0.90
<tb>
<tb>
<tb>
<tb>
<tb>
<tb> CD <SEP> 0.47 <SEP> 0.90 <SEP> 1.91
<tb>
 

 <Desc / Clms Page number 23>

 
 EMI23.1
 In addition, donation oooaie on hardwood and on paper machinn,

   using about 56 particles of oxapTe 1 also resulted in substantial reductions in physical properties.
 EMI23.2
 



  TA9LAU- Machine-ached papers after wet relaxation period.
 EMI23.3
 
<tb>



  A <SEP> B <SEP> C
<tb>
 
 EMI23.4
 Tensile strength (kg / m) MD 465.88 696.15 806.82 CD 248.11 333.79 385: 56
 EMI23.5
 
<tb> Elongation, <SEP> (%) <SEP> MD <SEP> 5.0 <SEP> 6.0 <SEP> 7.1
<tb>
<tb>
<tb> CD <SEP> 8.3 <SEP> 12.1 <SEP> 15.0
<tb>
<tb>
<tb> Resistance <SEP> to <SEP> bursting
<tb>
 
 EMI23.6
 (kg / cm2) 3.40 5.23 damn
 EMI23.7
 
<tb> Resistance <SEP> to <SEP> bending <SEP> MIT) <SEP> MD <SEP> 715 <SEP> 4120 <SEP> 7580
<tb>
<tb>
<tb> (cycles) <SEP> CD <SEP> 710 <SEP> 1525 <SEP> 2790
<tb>
<tb>
<tb> Resistance <SEP> to <SEP> tearing <SEP> MD <SEP> 1.26 <SEP> 1.03 <SEP> 0.90
<tb>
 
 EMI23.8
 Elmondort (g / g / m2) CD 1.57 1.25 1.00
 EMI23.9
 
<tb> Perforation <SEP> Spence-
<tb>
<tb>
<tb>
<tb> (inch-lb / inch <SEP> square) <SEP> 1.8 <SEP> 2.3 <SEP> 3.0
<tb>
<tb>
<tb>
<tb> Abrasion <SEP> (cycles)

   <SEP> 49 <SEP> 51 <SEP> 54
<tb>
<tb>
<tb>
<tb>
<tb>
<tb> Ream <SEP> weight <SEP> pounds <SEP> MD <SEP> 0.84 <SEP> 1.42 <SEP> 1.90
<tb>
<tb>
<tb>
<tb> 24 <SEP> x <SEP> 36 <SEP> - <SEP> 500 <SEP> CD <SEP> 0.79 <SEP> 1.57 <SEP> 2.34
<tb>
 
 EMI23.10
 In claosi paper making techniques. Quoa, it is common practice to tone the sheet on the felt to prevent it from wrinkling or wrinkling. The present invention, however, provides a wet dig, capable of undergoing relaxation as it exits the wet press section, a sheet which rolaxes in this manner, and a wet dig.
 EMI23.11
 which, after relaxation, shows substantial improvements, in particular with regard to its toughness and isotopic resistance.

   In the large-scale practice of the present invention, the wet sheet which exits the hutrid section of the press with a water content of about 65% by weight is drawn over the felt with a minimum of tension in the direction. of the machine, so as to allow maximum relaxation
 EMI23.12
 male in the transverse direction and z allows some relaxation in the longitudinal direction. A minimum of 32 contraction or contraction in the direction of trunaversole

 <Desc / Clms Page number 24>

 
 EMI24.1
  and recommended "this narrowing being preferably of
 EMI24.2
 
 EMI24.3
 4 11 69. By operating with hand searches, contractions! going up to 20 ', C in Chrlquo direction have been obtained, col which. a parsnip to get dda results bt1n.t1quo8.



  When using uno machlno a papier non raoliti ::, we operate do pr6ronco with a loose rust, under zero tension. When using aechor machines of the tunnol or cotton type we can achieve a relaxation -In 10% therefore the dlrec-! longitudinal tion. This p raot to obtain a final feulllo exhibiting maximum tenacity.



  Although the plaintiff does not wish to li-41ter A
 EMI24.4
 any theory, she believes that relaxation is about
 EMI24.5
 pore 'cellulosic fibers de ce rs-alitçner following a configuration plun <J4sor1onnée. However, the 1S. Orderly character of the fibers alone could not explain the graininess of the products.

   Kraft paw digs, in loaquhlloo the fibers are necessary stretched completely at random,
 EMI24.6
 do not exhibit this tenacity It seems that it is happening,
 EMI24.7
 thanks to the present invention, an a / nori. and uno combina, oon
 EMI24.8
 beneficial effects, although the mechanism of this combination
 EMI24.9
 or of this aynnrgy not fully known.
 EMI24.10
 Example 10 is given below to allow a
 EMI24.11
 comparison between the duration3 of threshing or pounding of the cora- position according to the appraising invention and of a pite known as t, t1 ('.- nique earlier.



  W ->? L ", 1 rt
 EMI24.12
 Trojan threshing tests were carried out using
 EMI24.13
 a Valley do O pile, bf3 kg, to obtain a pAr, o having a value of 100 of the freedom c: .nudioso standard * A control sample of pgto bleached with 1OCiX sulfite receives or bublt a m4xl threshing. :, sn using a weight of 5.57 k.
 EMI24.14
 



  B9 {d i, while a / - controls this performed by not using
 EMI24.15
 p & 4 do poido. The first test test 18 minutes

 <Desc / Clms Page number 25>

 to reach the desired freedom value, while the second test takes 18 hours. The third test is carried out with an addition of 5% of the etherified cellulose particles of Example 1, using the maximum speed, Dana
 EMI25.1
 At this cad, a period of threshing at 7 minutes is necessary to obtain a value of 100 of the Canadian 1 freedom.

   This pulp had treated sulphite laying a minimum of the temple to the pile gives a
 EMI25.2
 paper whose tensile strength is t, b, 6 g / ca / g / m2 ', As for the pulp which has undergone a stack treatment, for a period of
 EMI25.3
 maximum duration, it gives a paper having a tensile strength of 1.33g / cra / gia2 ;. The pulp according to the present invention gave a paper having a tensile strength of 47el C / c-.a / g / m2 X ':; J.PL !. 11 We prepare papers From suspensions
 EMI25.4
 containing 15 by weight of solidos derived from etherified cellulose particles produced in (a) at (b) below, each with 85% by weight of a sulfite paste having a standard Canadian freedom of 300, the technique of The paper making of Example 1 being used.



  A flask and a graduated vertical tube connected to this flask by a tap are evacuated to about 5 mm of mercury, after loading the flask with 150 g of alkali cellulose.
 EMI25.5
 and 1. 17.9 g tube of 4thylne condensa oxyde,
 EMI25.6
 a4paroLnt the tube A oxyclo dtdtyyltno from the flask aat tem4 ot 1 ory-
 EMI25.7
 of frozen doithylene is melted by means of an ice-water bath. The gaseous ethylene oxide is then allowed to distill in the flask containing the cellulose alkali at a rate such that the reaction temperature does not exceed 45 ° C. The total reaction time is 5 to 5 hours.
 EMI25.8
 161 "3 E of alkali cellulose hydroxy 6thyade groin! Obtained are dissolved in 660 ml of a 4% aqueous solution of

 <Desc / Clms Page number 26>

 NaOH.

   The solid matter content is 6.7%. The solution is used to form shear precipitated particles, according to the procedure of Example 1, the total shear value of the system being about 300.



   249 g of carbon disulphide are added to 454 g of crumbled alkali cellulose in a flask. The alkali cellulose aat stirred in the flask for 80 m at a temperature of
27 * C. To the crumbled cellulose xanthate obtained, one then adds
51.5 g of acrylonitrile and stirred for a further 80 minutes. As soon as the acrylonitrile is added, the color of the xanthute crumbs turns from orange to yellow. The xonthe and cyanoethylated product (277 g) is then dissolved in hard 978 g of a 3.7% NaOH solution, over the course of 2.5 hours, A 3 C.



   80 g of this viscose solution was precipitated by shear in 300 ml of a bath of 5% HZSO4 and 15% NaCH4 in a Waring mixer at maximum tension. The washed particles have a water absorption capacity of 10.0 g per gram and a nitrogen content of 3.80, which corresponds to a degree of substitution of 0.51. Example12
A cotton rag paste is processed in a Valley pile of 0.68 kg capacity until a value of approximately 180 ° Canadian standard freedom is obtained.

   A sheet obtained from this paste, applying the technique of Example 1 and forming a structure having a basis weight of 40.5 g / m2, has a tensile strength of 34.98 g / cm. / g / m2, an opacity of 73% and a resistance to pliago do 12 cycloe in one direction and 21 in the other. When a paper of the same weight is obtained with the aid of a material containing 15% of cellulose whey particles of the type obtained in Example 1, a sheet is obtained with a tensile strength of 80%. 5g / cm / g / m2, which opacity is 56% at which the folding resistance is
10,344 cycles in one direction and 13,500 in the other.

   The paper is particularly suitable for making calico paper as well as fine filtration paper.

 <Desc / Clms Page number 27>

 



   The alkali cellulose can be prepared to be drawn from any suitable source of cellulose, for example from cotton linters, chemical pulp, crushed pulp, waste and used newspapers or printed matter. The current commercial reaction conditions are satisfactory. The alkali content should be between 15 and 30%, the preferred content being 18%. The alkali cellulose can be subjected to aging or curing for or less 1 hour and for up to 24 hours at room temperature.

   Aging at temperatures above 40 ° C is undesirable. Cellulose can be held for longer times even up to 200 hours, provided that when the time exceeds 24 hours the temperature is below 15 ° C but above -50C. Freezing is not desirable.



   The etherification takes place by reacting the etherifying agent with the alkali cellulose in the solid state. The etherification reaction takes place at a temperature between about 5 and 45 ° C and, preferably, at a temperature between 15 and 30 ° C. Preferably the concentration of the etherifying agent should not exceed about 20% (based on the weight of alkali cellulose) at any time during the reaction. The reaction time is between 10 minutes and 10 hours, depending on the reactivity of the etherifying agent.



   If desired, the cellulose ether obtained by etherification can be made more suitable for processing (suitable subsequent, by forming a readily soluble cellulose ether ester, such as a cellulose ether xanthnte. such products can be formed, for example, by reaction of CS2 on cellulosic material in the solid state. Xanthnge can take place at the same time as rerefication

 <Desc / Clms Page number 28>

 
 EMI28.1
 or can be done before or after it. The two reacts
 EMI28.2
 tions have. preferably, read substantially in 8. t aps.
 EMI28.3
 wl1l.Jn 4 The conditions of JtAnth "t, 8 co \ement. used in 1.1n {.lu-
 EMI28.4
 sort of rayon, for the most part of viscose, cunt profbrbea.

   The xAnthllg41 must, by preference, take place until an xsrnthnte group is present in two nuclei of other
 EMI28.5
 hydroglucose.
 EMI28.6
 



  After the etherification and the x "r, t.h" f; optional, 1A substituted cellulosic material * may be subjected to vatting & 6x * nt, before reprecipitation, for 1 A $ 0 heurtov J
 EMI28.7
 
 EMI28.8
 At a temperature above about 0 * C, but interior ..



  Cellulose ethers, which can be used in accordance with the present invention, have defrHs in the range of between about 0.02 and 0.7 and preferably between about 0.1. and 0.6. These cellulosic ethers JH) '. J.,:' \ T contain more than one type of 4ther group.

   The most interesting products are con3ibl4mofit lt & 3ulubles in a crJMt1 ".6 water nllnt Up to 30 times the own wall weight, although n9 commercial preparations, in quantity nllint Up to 25% by weight of soluble derivative3 may be present as impurities. # P 'nni the appropriate derivatives, one can quote' the nleoilic ethers, such as ethyl cellulose, ethers cArboxy "lc: oyl1qun t, ele that 1k cArboxy .'th ,, 1.c., l. Luloae and Boxyethylellulose, hydroxyalkyl ethers, such as hydroxyylcellulose, trylalkyl ethers, such as benxylcelluloso and substituted alkylcellulose, such as cyano4thyl cellulose. The preferred compound of this class is cynnoethyl cellulose.



  Mixed ethers can also be employed.



  Aini, some of the nitrile groups of cyano ethyl cellulose

 <Desc / Clms Page number 29>

 can be hydrolyzed; some of these groups may terminate at the nmide stage, while the remainder is converted to carboxyl groups. So. three types of ether groups may be present. Mixed ester ethers can also be used, for example an ether eater containing a mixture of acetate and ether moieties.



   A large number of shaped products falling within the scope of the present invention can be obtained by extruding from a solution of the ether described above in a coagulation bath or by precipitation of the cellulosic ethers in solution, thus. range of the aforementioned total shine values, so as to force fibrous particles. The extruded filaments are obtained by the usual techniques. The main factors affecting the nature of the product precipitated by shear are the viscosity of the solution, the degree of shear applied during coagulation and the nature of the precipitation bath. Among these factors, the last is the most important.



   The overall efficiency of the coagulation system, i.e. the speed of coupling, the applied shear force, etc., constitutes the main factor regulating the process and the nature of the precipitated products. regulation has the greatest effect on the nature of the product obtained. Another very important variable factor is the degree of shear applied to the precipitate while it is deformable.

   Thus, the shear is varied together with the rate of coagulation, to obtain a fiber product having the desired properties. If a faster coagulating agent or medium is used and a similar product is desired, it may be necessary to increase the rate of shearing to a corresponding extent. bath, namely its viscosity

 <Desc / Clms Page number 30>

 and its temperature, for example, have less effect on said product properties than the nature of the coagulation medium.



   The overall effectiveness of the bath, as an agent of; coagulation, can be determined by the index or salt index method which is common in the rayon industry. Although this method has been limited to viscose solutions, it can be very easily extended to alkaline solutions of cellulose ethers which are relatively insoluble in water. For convenience, a description of this method, suitable for cellulose ethers, is given below. !
The main condition in the course of coagulation is that the shear must be adequate in order for the precipitate to take the form of a fibrous or ribbons-like product.

   Within permissible limits, the shear can be varied to an appreciable extent while still obtaining products having comparable properties. The shearing action during coagulation depends to some extent on the type of agitator employed and the vessel in which precipitation takes place. A suitable shearing action for preparing the products according to the present invention can be obtained by using a stirrer the blade or blade of which is at an angle with the plane of rotation.



  The modela of the agitator blade or blade used in a Waring mixer has proved particularly satisfactory. Turbulence can be increased by introducing suitable deflectors into 1. 1 mixer. Fibers were obtained whose morphology is particularly desirable. When the precipitation takes place in a shear zone which is also turbulent, the combination of the action of the agitator and the design of the vessel, generally used in the practice of the present invention, allows to achieve precipitation conditions that combine turbulence with

 <Desc / Clms Page number 31>

 adequate shear.



   Other types of apparatus may also be used, provided that they impart sufficient turbulence and shear. Thus, certain solutions of cellulose ether can be projected into appropriate coagulation media, so as to obtain satisfactory absorbent products. Some of the examples illustrate the preparation of these products by injection of the solution of the cellulose derivative into a stream of the precipitating agent. Other variants can be imagined by specialists.



   The formula given for R's above is derived from the degree of shear R, which is proportional to the shear stress S. By introducing the viscosity V, as a constant of proportionality, the equation becomes:
S = VR Using the index s for the solution and the index p for the precipitation or coagulation medium, the shear force in the precipitation medium and in the solution is given by the following equations: Sp - VpRp (1)
Ss = VsRs (2) It is reasonable to assume that the shear stress .et transmitted, without decrease, from the precipitation medium to the solution, resulting in:

     Sp - Sa (3) equations (1) and (2) being able to be made equal, which gives
 EMI31.1
 Ra. Go p Rp (4!
The type of fibrous products formed depends on t, that is, on the time interval during which the precipitate is deformable. The Rat product will be designated by R's (shear

 <Desc / Clms Page number 32>

 
 EMI32.1
 total) .Nf4 and terminated by 1. relation 8u1.YI \ nt.e,
 EMI32.2
 R1 w Rpt (5) V.
 EMI32.3
 



  Certain generalizations can be made and which concern the conditions of the process, anna rIiC6r-1lOc., '\ Specific experimental results. Thus, if the> r¯ #ticles obtained by precipitation of cellulosic tn.r in a given series of conditions are too fine, 11 e-5t need * to reduce the shear forces (we d1: nlr.u "nt . the Yltt8a..dtftg1ta1on or by increasing the viscosity) and / or increasing the rate of coagulation. This last effect is not obtained by increasing the degree of polym4rlutlon, q 1n Cellulose, the concentration of cellulose, etc, oj ru tuff "lying the soil content of the bath, or even in heating 1
 EMI32.4
 bath, where again by choosing a stronger coupling agent. Conversely, if the particles are too ro51ro. reverse changes can be made.



   The cellulosic ether solution or the cockling bath or both may contain adjuvants to modify the nature of the products obtained. Thus, the solution or precipitating agent may contain short syathetic and / or natural fibers, such as nylon fibers, nylon fibers.
 EMI32.5
 poly (ethylene terephthalate) or crylonyl pulp, discontinuous or short cellulose fibers, glass fibers, amine fibers, cellulose pulps, etc.

   In addition, the precipitating solution or agent may contain the
 EMI32.6
 fibrids described in U.S. Patent Applications No. 635t
 EMI32.7
 635,876 of January 23, 1957; ne z35.721 of January 23, 1957; no 635,731 of January 23, 1957; tu * 675.038 of) July 0, 157 and ne 675.0 of July 30, 1957.

   These products may contain dyes, intestinal agents, tenalo-actives, charges, such as garlic or titanium oxide, pigments, anti-oxidants, braaifs,

 <Desc / Clms Page number 33>

 lubricants, flame retardants, natural or synthetic, dispersed or emulsified polymer or resinous materials, adhesives, gums, natural or synthetic fibers and inorganic materials.

   Addi- tional materials which have been found to be useful either titanium dioxide, dispersa dyes, silica, wood flour, quaternary ammonium salts, emery powder, graphite, resinous polytetrafluoroethylene or powder, antimony salts, phosphates, synthetic elastomeric acrylic resins, casein type adhesives, polyamide resin type granules, glass fibers, polyamide fibers, fibrids, asbestos, talc, cermetes, metallic powders and magnetic iron oxide powder.



   In particular, pigments and fillers, such as titanium dioxide, can be added before precipitation, to give fibrous materials containing 20-70% TiO2 based on the weight of total solids In particulate form. As constituents of sheets, these compositions provide a remarkable means of adding high concentrations of pigment to sheet products without substantial loss of pigment in water.

   For other end-use applications it is often more desirable to add fibrous materials to the precipitation or coagulation bath, because of the greater difficulty experienced in dispersing these materials in viscous solutions. cellulose ether,
The cellulosic ether solution may also contain polymer / dispersion particles, especially polytetrafluoroethylene or polyacrylonitrile particles, these modified solutions have been converted to fibrous precipitates, cellulosic ether can be removed, by heating ** or by chemical action,

     so as to form fies

 <Desc / Clms Page number 34>

 fibrils of the synthetic polymer that has been added.



   The additive materials described above may
 EMI34.1
 also to be incorporated as pulp constituents in the compositions according to the present invention, from 11 to forming sheet products in which these ingredients. addition are mechanically retained by the intermixing of the particles forming the sheet, rather than as a constituent of etherified cellulose particles.



  Since the products according to the present invention exhibit high confidence in the presence of water, "T" f precautions must be taken! taken during their preparation to prevent their swelling. Or, these products must be submitted there. subsequent processing, to bring them bzz z 1 f;) r "'" not swollen. As indicated previously, a {.:; .3 by heat alone generally results in the production of a horny and hard material poorly suited for use as an absorbent, although, as shown in the examples, heat can be employed to remove moisture, condition that a surfactant is present on the surface of the swollen particles.

   Another method of dehydration or deflation which can be used is to displace water in the shaped structure, for example by means of acetone. Although this system is very interesting and gives excellent results in the laboratory, the problems of solvent recovery make it attractive on a large scale. A more practical deflation method is osmotic dehydration, in which the objects or shaped articles are deflated by the action of relatively concentrated solutions of inorganic salts, such as sodium sulfate.

   The deflated particles can advantageously be decompressed in the wet state or centrifuged to obtain compositions containing 30% by weight or more of solids.

 <Desc / Clms Page number 35>

 sodium sulphate in the form of a 17% solution is a preferred salt, but other salts with high ionic resistance] can also be used, in particular sulphates, phosphates, bortes of magnesium or ammonium and other materials known in the viscose industry.



   Since the precipitated etherified cellulose is expensive to transport in the swollen state, it is preferred to avoid the washing or other operational steps which have the purpose or the effect of bringing the freshly regenerated material into contact with water, This can be done by a process in which the excess acid present in the freshly precipitated articles is neutralized by means of a buffer, such as disodium monohydrogen sulfate, in the presence of a salt, such as sodium sulfate.

   An aqueous neutralizing solution containing about 10 to 20% by weight of sodium sulfate and about 0.1 to 2% by weight of monohydrogen disodium phosphate, having a pH of 5 to 6 obtained by adding sulfuric acid. - ric and caustic soda, has been shown to be of interest for the large scale production of particles. The freshly coagulated products can be left for 30 minutes or more and then introduced, with vigorous stirring, into a reservoir of a neutralization solution, in which a concentration of about 2% by weight of cellulose ether is maintained.

   The suspension can be drained from the lower part of the tank by means of a soup hose. so as to be brought into a settling tank equipped with a settling bag and a filtrate recycling pump. the 2% suspension from the reservoir is allowed to drip off until it has a content of about 10% by weight of cellulosic ether, after which it is returned to a centrifuge, for further removal and removal. recycling

 <Desc / Clms Page number 36>

 neutralization solution.

   Contrifugation gives a material containing 30 to 50% solid, more than one titer of which may be sodium sulfate. Filtration in a multi-stage filter press 4. gives similar results. Drying with superheated steam results in a higher solids content.

   The wet compressed gatenu can usai be dried, by passing it in the form of a sheet on the roller of a dryer, so as to obtain a soft sheet. It has been found, not without surprise, that the residual sodium sulfate, which may be present in a concentration between 5 and 50% by bag weight, contributes to the smoothness and extrudability of the dried product * The salt appears to crystallize in the particles carriers, in such a way that it there is no visual evidence of its presence, for example in the form of encrustation which is normally encountered when salt solutions are dried, in the fibrous product. A solid mass containing about 30% cellulosic ether and 1% sodium sulfate is preferred.



   Such a mass, which does not contain more than about 70% by weight of water, can be transported in conventional containers without special handling. Despite its high water content, it is dry to the touch and can be
 EMI36.1
 stored or stored for prolonged periods, without decomposition or loss of food. The product little *. be easily treated by let ,. classic sheet forming, applying niques of papermaking.

   The reseating of particles is carried out in a pestle or a neck machine contained in the mass can be 411m1n4 as desired, without the need for narrow diatir.cta stages; Or, if desired, the dispersed material has a high concentration, eg most of the salt will be retained in the sheet product.

 <Desc / Clms Page number 37>

 
 EMI37.1
 



  The compositions of collulone and colulone particles precipitated according to the prior invention can be used to give a coherent product, by current techniques for the manufacture of paper or of aoula, Lou pro. The obtained t5 exhibited remarkable self-bonding properties, compared to those of conventional products formed from cellulose pulps.
 EMI37.2
 It is often desirable to treat the precipitated particles in the usual piloa, in the presence of the cellulose pulp or pulse or in the absence of calla therein, before formation.
 EMI37.3
 of the sheet.

   The th6rt16o cellulose particles, which have thus been treated in a pila or which have not been treated in this way, are mixed with cellulose pulps or pulps.
 EMI37.4
 e1qU & è and, mid 04e dÓ8ir, in addition, such as staple fibers or artificial fibrids, before preparation of the sheet products. The compositions following the pre-
 EMI37.5
 The present invention can also be made directly from aquousea suspensions, in which the particles of 4thdrified cellulose are formica, without intermediate isolation or coating.



   The nature of the pulp or cellulose pulp is not criticized. Any type of pulp suitable for use in a conventional papermaking machine can be used. Rag, wood, sulphate or sulphite pulp or pulps are satisfactory. The pulp can be combined with etherified cellulose. before or after treatment in the stack. As mentioned above, it is preferred to add the etherified cellulose, which forms precipitated particles by shear, after treatment of the pulp in the stack, to the desired degree of freedom, taking into account the decrease in the value of freedom which results from the addition of the adjuvant.

   In general, we will prefer
 EMI37.6
 avoid violent agitation during the mixing, moderate mixing during ur) ke "! pa Gufr1ant furnace ensure a uniform distribution of the calluloao 6thrlflé in the puipt being a-sule-

 <Desc / Clms Page number 38>

 
 EMI38.1
 muggy. Apr '. Having mixed the cellulose pulp in the precipitated etherified cellulose composition, the mGlan $ was processed in the usual manner at any commercial dock. The application of the "Clupa." presents an i. ' particular lift, for the production of products in -. 'Lai: .. from the compositions according to the prdsante invention. This process is described in US Pat. No. 2,624,245.

   In accordance with this process, the paper is subjected, by removing a sufficient quantity of water to obtain a coherent structure, but before this, to a treatment which introduces a dietorsioryàos long fibers, by contraction of the area in which they are located ot thus by raCCO \ 1r "f.:..,!- rise of the leaf, without decrease in the actual length of the fibrea elle5-mmos, while at the same time maintaining lac: : J! "':"' \ Of the sheet of paper flat and parallel and preventing this sheet from thickening.

   During this treatment, strong pressure is maintained on the surfaces of the sheet of paper, so as to prevent the latter from creping and also in order to drive out the fibers deformed in the voids existing in the sheet of paper, in such a way that the fibers are brought as intimately as possible into contact with each other as well as with the fibrids mixed or intermixed so as to ensure good adhesion and good bonds in the sheet.



    Upon subsequent drying, the altered orientation of fibers and fibriiea is retained in the dry state and the sheet acquires its final strength and firmness, which are due to the mutual adhesion of the finely interwoven fibrids and other small structures,
It is obvious that the invention is not limited to the details described above and that many modifications can be made to these details, outside the scope of the invention, as defined in the caivan-test claims.


    

Claims (1)

EMI39.1 ; L.: VOICATIO!: 3. 1.- A composition of matter comprising (1) a cellulose pulp or pulp and (2) about 2 to 95%. based on the weight of solids contained in the total composition, of particles precipitated by shear of an ethereal cellulose EMI39.2 hydrophilic, water insoluble, uni- form lcro3coplquocnt bond having a degree of substitution of about 0.1 at C, 7, on the partially substituted cellulose polymer chains *, 2. A composition according to claim 1, characterized - Sec in that the etherified cellulose is cyano-ethylated cellulose. 3. A composition according to claim 2, characterized in that the pulp or cellulose pulp is a sulphite pulp. 4. - Raw material for papermaking, not stacked, containing a composition according to claim 3. 5. - Conditioned raw material consisting of water and a composition according to claim 3. 6. A solid, substantially dry shaped structure comprising the composition of claim 3. 7. A sheet of glassine paper comprising a composition according to claim 3. 8 '. Composition according to Claim 2, characterized in that the pulp or pulp of cellulose is a sulphate pulp, 9. - Raw material for the manufacture of paper, not stackable, comprising a composition according to Claim 8. 10. A conditioned raw material comprising water and a composition according to claim 8. 11. A solid and substantially dry shaped structure comprising the composition of claim 8. <Desc / Clms Page number 40> 12. A kraft paper search comprising the composition of claim 11. EMI40.1 13.- Sheet of icotropic paper and wet relaxed of the composition of the rovn11catlon 11. 14.- Process for conditioning a material pro1re from cellulose pulp to achieve a conadiorv value of freedom. predetermined standard, characterized in that one adds to the cna- Position at least about 2 'weight of ciill, .jloto etherifia hydrophilo, mlcr08copluo}! Tlont uniform, having a d-re do aub3ti- tution of about 0.1 to 0.7 on partially aubatitrl cellu- loco polymer chains; roa. * 9f '151- Process according to the ravondication 14, characterisa on that the colluloso th \) r1flo ost added to the pA, t or pulp of cullulosn before treating in the stack. 16. A process according to claim 14, because co that the colluloao 6thlr16o is added we f Bzz particles precipitated by shearing. EMI40.2 17.- Process according to the rtvondication 16. characterized in that the particles of etherified cellulose precipitated by ci- aailloment aont added to the pulpo or pàto, apr''t! partial conditioning of collo-ci, by bettage or pilo treatment. 18.- The method of claim 17, character on EMI40.3 what ether cellulose does to cyano-ethyl cellulose. 19. A process for preparing a product is excavated, characterized in that an aqueous suspension of a composition according to claim 1 is deposited on a perforated surface, maintained. EMI40.4 the slick forced to the state r;! 14ch & during the flow from the water to the púnJél..1t ur, amp3 sufficient to ensure a contraction of at least about 3% in the transverse direction. 20.- The method of claim 19, characterized in EMI40.5 that cellulose pulp or pulp is sulfate pulp. <Desc / Clms Page number 41> 21. A method according to claim 20, characterized in that the etherified cellulose is cyanoethylated cellulose. 22.- Method according to claim 21, characterized in that the web is subjected to a subsequent treatment, which ..consists in moving this web in the longitudinal direction and to remove slowly, while the web is in the physical state qu when it leaves the wet end of a paper machine, only a part of the moisture collects there, after which the fibers of the partially dried web are uniformly pushed and clamped against each other in the space between the faces of the web as it was laid, applying continuous pressure in the web and making ac; ir forces in a direction parallel to the faces of the web in a direction opposite to the direction of movement, while preventing the web from creping, during compression, under the back effect pressures acting in response to the faces of the sheet.