USRE13436E - By gertrude s - Google Patents

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USRE13436E
USRE13436E US RE13436 E USRE13436 E US RE13436E
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US
United States
Prior art keywords
water
glue
carbohydrate
starch
base
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Application number
Inventor
Frank G. Perkins
Original Assignee
Glue And Method Of Making The Same
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  • rnnnrns arm's one menus, or sou'm m n a com-cannon or rnmrs'gmwm hs To all whom it may concern:
  • a gw are to: f-makm the mg a'non un'rnonor unknowns-sh m; q
  • the agitation preferably produce b thorough stirring is continued for from our to six hours after the acid has been added and then the acid may be neutralized by the addition of a small amount of caustic soda or similar alkali.
  • the acid actsupon-the starch or carbohydrate to decrease its water absorptive properties. As the acid appears to remain-unchanged in the batch, until neutral ized, I believe it acts catal ically to change the molecular condition 0 without rendering it substantially soluble in the'water. However great care must be exercised not to have the heat suliicient or the acid in such quantity as to carbohydrate in solution. the action of the acid 'and heat is carried too far the starch will be changed into dextrimand will go into solution, and as such it would be 0st to my process, as'I utilize onl the susended material.
  • troymg states of aggres gation or polymerization, which are detrimental t'o'the use of the carbohydrate as a glue base. .
  • the amount of alkali used is only enough to neutralize the acid. After this has been added, the batch is then-cooled, drained and dried" and kept in dry "form until read for use.
  • cassava flour has many advantages over other starches and starchy products and prefer its use, but such other starches or starchy products may be used with more or less success.
  • Other starchy products from the cassava be moreor less adaptable and even other starchy products may be used with some little success but they do not produce glues so tenacious and are otherwise more or less undesirable. affected by impurities.
  • the dri base obtained as above, is mixed with about three parts or less by weight (of dried base) of water. according to the strength of the joint and eoonom desired.
  • the dried base does not materia ly go into solution in the water unless heat is applied, but a liquid suspension is thereby formed which is agiand treated with a solvent of cellulose, as, for example, an aqueous solution of caustic soda orpotash alkaline to phenolcold from siit to ten per cent. of the weight of the dry base, of canstic soda or its equivalent of caustic potash.
  • the alkali acts chemically to unite with one or more starch the water to form a colloidal compound.
  • the alkali is' best added in the form of .a solution of from 33% to '50% strength.
  • Sodium and potassium hydrates are' the most availablemnd among the most'power- To take a specific tity, say 100. lbs. of thedned amylaoeous base was mixed with from of water (preferably 2251bs. or less) After the mixture was thoroughly agitated, 10 lba ofcaustic soda was a ded in a concentrated solution of approximately one part alkali in one to two parts water. This was added with extreme slowness, r to 20 minutes for the 30 lbs.
  • a Perkins viscosimeter was used, which may be constructed of brass tubin 1.295 inches outside diameter, 0.012 inc thick, and 3 inches long, and having a flat brass bottom 0.080 inch thick soldered into the end having a round center hole 0.070 inch in diameter .'the total weight being 39.63 grams, and all edges being made smooth removing practically no weight, thehole being polished until the cup placed quickly at its floating level in water at 60 F. floats upright and fills up-to the point of sudden sinking by top overflow in 16 seconds. If the material directly from the treatment tankof the first step is to be tested, a small quantity is taken, neutralized and diluted with, cold water toei Be. 3150 c. c. of this thoroughly mixed batch are then taken in avessel and the steam similarly ad.- mitted to the bottom of the batch, but this is found to indicate about 6% secondslower;
  • the carbohydrate glue base in the pre ferred form retains substantiall unchanged the size and general form 0 viewed under the microsco e when treated with cold water, and pro uces opalescent cloudy solutions with water at 200 F.
  • the carbohydrate glue'base may be formed into glue by using .only from one to three parts of water, the more water used the Preferably less than 41 ⁇ parts of water should be used in making the glue from the carboh drate base.
  • Inc is tr arent and free from odor, an is very stab c after mixing for use, it is instantly adhesive to-clean surfaces, its cohesioxi is very great but not suflicient to overcome its adhesion and its viscosity is la andlow enough to permit ready a-p-- plication, but so pro ortioned toitscohesion 1 ohinery like hide glue, but still very 10 that it is capable 0 being applied by meh fibers are produced if'freshly- 'oine owing to the reakage of these filaments 1'2";
  • a glue'base characterized .by the facts that-it is prepared from starchy material retains substantially unchanged t e size an general form of particle when treated with cold water, and produces opale'scent cloudy solutions with water at 200 F. 1
  • makin glue which consists 'in treating starch be ow the bursting temperature of the starch, with a digesting agent such as caustic; and water until the material assumes'a viscous semi-fluid consistency adapted to be applied by machinery.
  • the processor making a'glue, which consists in treatin a starch carbohydrate with caustic alkali, and we r, to dissolve the carbohydrate, the total amount of water used being about 3 parts or less by weight off the carbohydrate, the amount of caustic alkaliiused, ca culated as NaQHbeinE about 10% orless by weightof the carbo drate so that a wood glue is formed, as i'stinguished from mucilages, sizes and paste.
  • roperties without rendering the carbohyrate materially soluble in cold water and then putting the product thus produced into a solution containing about t ree parts or less by weight of water to produce a. glue which' for application.
  • he process otmaking glue consists in agitatin a starchy carbohydrate with water and a gesting agent to reduce. the water absorptive properties of the carbohydrate without renderin it materially then mixing the carbohydrate with water and caustic alkali, the amount of water used being about three parts or less by weight of dry carbohydrate, the amount of caustic usedbeing about 1 0% or less b w ht of dry carbohydrate, to dissolve as distinguished. from mucilages, sizes and paste.
  • a glue comprising1 draterendered semi-flui havm substantially the proper ies of mal g ue.
  • a glue comprising chiefly starch dissolved by a digesting agent alkaline. to phenolphthalein and in. about 8' parts'oi' less by weight of water.
  • 32. Aglueas distinguished from mu'cllages, sizes and pastes containing a starchy carbohydrate base substantially insoluble in water and dissolved by caustic and containing free caustic.
  • V 33 A glue consistingof a vegetable can bohydrate base substantially insoluble in water and dissolved by water and caustic soda alkali, the amount of water being about three pnrts'or-less by weight of dry carbohydrate and the amount of caustic present dry carbohydrate.
  • a glue consistlng of a vegetable carbohydrate base substantially insoluble 1n water and dissolved by caustic alkali, the
  • a being about 10% or less by weightof the.
  • a lue composed of a starch carbohydrate ass and a solvent-of cellu ose and having such a character that-itwill be substantiall' unafl'ected by the natural humid- 46 ity and aving substantially as good adhering qualities as the best animal glue.
  • V V c Perkins, deceased; m5 of sou h Bend, Ind.; Gertrude S. Perku a, executrix. Gnvn'azm M'n'rno'n or Mani! 'rrm' mm dated July 2, 191 Disclaimer filed February e, 1919, by the mime,
  • a glue comprising chiefly starch dissolved by a digesting agent alkaline. to phenolphthalein and in. about 8' parts'oi' less by weight of water.
  • 32. Aglueas distinguished from mu'cllages, sizes and pastes containing a starchy carbohydrate base substantially insoluble in water and dissolved by caustic and containing free caustic.
  • V 33 A glue consistingof a vegetable can bohydrate base substantially insoluble in water and dissolved by water and caustic soda alkali, the amount of water being about three pnrts'or-less by weight of dry carbohydrate and the amount of caustic present dry carbohydrate.
  • a glue consistlng of a vegetable carbohydrate base substantially insoluble 1n water and dissolved by caustic alkali, the
  • a being about 10% or less by weightof the.
  • a lue composed of a starch carbohydrate ass and a solvent-of cellu ose and having such a character that-itwill be substantiall' unafl'ected by the natural humid- 46 ity and aving substantially as good adhering qualities as the best animal glue.
  • V V c Perkins, deceased; m5 of sou h Bend, Ind.; Gertrude S. Perku a, executrix. Gnvn'azm M'n'rno'n or Mani! 'rrm' mm dated July 2, 191 Disclaimer filed February e, 1919, by the mime,

Description

no nnwin ori in-.1 I01 1,'oao,uu, dated r ms s, 1812 ,-8 erla1- o. 0,797;
- am n; 11,11 lum nescence;
ods of Making the Same,
UNlTED- I smirk-o. 'bnonAsnnf-mrnof scum nnnn, 'mnxann, Ii -i: pam");
inning; rnnnrns arm's one menus, or sou'm m n a com-cannon or rnmrs'gmwm hs To all whom it may concern:
' Be it knownthat I, FRANK G.- Pnnxms, a citizen of the United States, anda resident of South Bend,' county of St.-v Joseph, and State of Indiana, have invented certain new and useful Improvements inGl-ue and Methlowing is a specification-1' a My invention relates to improvements in glue and the method 'of'making'the same, and more particularly. to the manufacture of glue from carbohydrates'containing amylo cellulose or its equivalent. In the well known method of making a starch paste the solid is mixed with water enough, to make, after tumefying, a paste of such viscosity or density that it can ,be easily applied This mixture is then subjected to heat .to rupture or burst the cellulose walls and this cooln'ng to a considerable degree supposedly reduces the cellulose to soluble starch; particularly ence of soluble starch alrea in solution. To increase the bod or viscosity small amounts of ammonia ave been added prior to or after heating. Such pastes have not the necessary relative tack, viscocity, co-
. here properly when up I e produce. a glue provide 'a- {glue and a method to spread and adlied aswood glues. 0 become extremely hesiveness and tenacity Such pastes 111 cooling a thick and jelly-like and are ractically un-' satisfactory for woodwork w on originally made with water, becausewaterwarpsjthe wood and delays dryingl and the pastes .do not set hard enoug when dry. Iim'ore water is added in an attempt to make it more fluid,- the', aste becomes so weak and diluted that it as practically no power andwould be wholly unfit for most classes of work; especially wood joints.
Various objects of my invention same fromcarbohydrates, whichw: not
have the disadvantages just pointed out, butbe exceptionally tenacious: and
powerful-hut still ainplyfiiudfor easy b, can; be" economical y which will plication, and wlnc and easil produced I of which the folin the presor diluted after cooking,
and-are not dense and elastic enough produced with; a gw are to: f-makm the mg a'non un'rnonor unknowns-sh m; q
",best an'imalx-glue; and possess; certain great advantages of permanency 1 to 9f animal-g} conditions ave never b en met by an. prior A "further -'iniportant ohject -of m .tionis to produce anfadhe'sive which-may and which may then'be -mixing up with or .Snch improvements are of and industrial -advantage andand' have been much "sought;
first take. dourbohydrate of the practical "edyantage"thatiit may beYprac-f I v ."t1cally=usedtor the same purposes as th temperature variations-far .s'uperior to those us; As far as I am aware, such- I I water abs'o tiye-progirsties in 'thesense th'L-it' to render'. uid the tivel the al' glue will not-"thereby ously diluted.- The reagent I starch c'onve lieved it'exercises, lyzing" or. oxidizing similar to that of converting agents: many and 'd'extrin. iflI ms is preferabl much but only Ito eflect" its when put into solution. or
that it decreasesfthecviscosity be mix aj witjs with a'- solvent m ts in fur er objecto'f my: inventlon'is to a which-fwillhaveithe. great a y. use any 'soitable converting agenthut'jth'eaction It produces.
less complete sinceg-it is not my ob ect to convert'tlie' starch wholly hed glue,-t'. m are-'1 little water will have 'to be added and become serif" use I-callva rting agent because at least inpart-g a-hydroi or converting action the well known starch of which have been. used to. convert starclif'into solublephysical properties dissolved to form glue.- The e flect, .-o-this -treatment also i of the glue-.: Y
. By my for application without fcrmcntative chan e. iprocess in its preferred forin tic glue is rec from the complications which attend the use of an adhesive which must be cooked or warmed before use, or kept warm .d uring use, and is more powerful an that which results from the treatment of starch in other-ways. My improved glue when made in its best form and properly applied will not only tear away the wood at some point in the wood joint produced by the use of this glue, but will tour owe. the wood at many points whether wit or against the grain.
Further objects,
will more clearly ap ear from the detailed description given be ow.
' That a large part,
constituents or do In carrying out one embodiment of m inventicn I to e the cassava carbohydrac or flourin dry form and add at least an equal weight of water. The batch is then agitated and heated to about 130 R, which is below the bursting tem erature of the starch..
Then I slowly a d from 2% to 3% by weight (of the raw carbohydrate) of strong sul uric acid. This may be considerably diluted if desired beforeit is'added. The
same is kept in continual a 'tation. The agitation preferably produce b thorough stirring is continued for from our to six hours after the acid has been added and then the acid may be neutralized by the addition of a small amount of caustic soda or similar alkali. The acid actsupon-the starch or carbohydrate to decrease its water absorptive properties. As the acid appears to remain-unchanged in the batch, until neutral ized, I believe it acts catal ically to change the molecular condition 0 without rendering it substantially soluble in the'water. However great care must be exercised not to have the heat suliicient or the acid in such quantity as to carbohydrate in solution. the action of the acid 'and heat is carried too far the starch will be changed into dextrimand will go into solution, and as such it would be 0st to my process, as'I utilize onl the susended material.
ave-.Fthe desired properties if the action were ca'rried too far.
if not all, of the starch improved process, go into solution, is shown by its settling upon stopping the agitation and by the weight and ana ysis of the product yielded. The batch therefore has not been converted into dextrin. Sulfuric and other other starch converting a cuts are stated to have a catalytic action a ecting themolecular state of amylose or its state of hydration. This I believe. to be promoted and equalized by rolon d 'tation both together with t e actfiin does not, in my heat, removing advantages and features plant are found to -used, but .if
the carbohydrate.
. tated ut the starch or- 'phthalein, using f Even this woul cease to --ful of the known solvents cellulose and are well adapted for most puracids as well as.
troymg states of aggres gation or polymerization, which are detrimental t'o'the use of the carbohydrate as a glue base. .The amount of alkali used is only enough to neutralize the acid. After this has been added, the batch is then-cooled, drained and dried" and kept in dry "form until read for use.
I find hat the carbohydralxssecreted by the cassava. plant and mown as cassava flour has many advantages over other starches and starchy products and prefer its use, but such other starches or starchy products may be used with more or less success. Other starchy products from the cassava be moreor less adaptable and even other starchy products may be used with some little success but they do not produce glues so tenacious and are otherwise more or less undesirable. affected by impurities.
The above forms the first part of my improired process and the various steps therein nniy all be carried out at the factory.
11 commercial use I preferably ship the dry material, obtained as above to the consumer who carries out the second part of'the process at the place .where the glue is to be esired the first and second parts of my improved process may be carried out together.
In carrying. out the remaining steps in the repar tion of myimproved glue, the dri base, obtained as above, is mixed with about three parts or less by weight (of dried base) of water. according to the strength of the joint and eoonom desired. The dried base does not materia ly go into solution in the water unless heat is applied, but a liquid suspension is thereby formed which is agiand treated with a solvent of cellulose, as, for example, an aqueous solution of caustic soda orpotash alkaline to phenolcold from siit to ten per cent. of the weight of the dry base, of canstic soda or its equivalent of caustic potash. The alkali, I believe, acts chemically to unite with one or more starch the water to form a colloidal compound. The alkaliis' best added in the form of .a solution of from 33% to '50% strength. Sodium and potassium hydrates are' the most availablemnd among the most'power- To take a specific tity, say 100. lbs. of thedned amylaoeous base was mixed with from of water (preferably 2251bs. or less) After the mixture was thoroughly agitated, 10 lba ofcaustic soda was a ded in a concentrated solution of approximately one part alkali in one to two parts water. This was added with extreme slowness, r to 20 minutes for the 30 lbs. so ution reuinn'g 15 k Some are molecules and with of thestarch I v were usedthe result has not i with less than -6 parts of NaQHper. 100' quit-ed. [Darin this time constant stirring 'w s 'mnintaine in order to ualize'and distribut'e'the action of the caustic sodaas fully as possible.
parts of amylaceous base The result-con sists-in what is calledthe' passing over or 7 coming across of the mixture .andjmay be above example, little difierence the apearance of the mass was apparent Soon, iowever, it became-cream and thenmore nsty and difiicultto stir. hen about mlf the caustic. soda harbeen added,there was faintly observable a minute. mottled face of the mass being so Of'CflUStlC had been added, t e-entire mass passed over or came across being converted from a mixture of suspended starch and water containingcaustic -to .a' homotie and water.. A-little excess of caustic was preferably added to prevent decomposition of the com ounds 'by the carbonic acid or moisture o the air. As much as fourteen per cent. NaOH, or. the equivalent of other caustic may be used, leaving some free caustic in theprepared compound is here. used in the" more modern. chemicalsense of matter connected within. the limits ofsometguantitative relation to produce" afdefin-i ,recognizahle product having; certain-- de- 'tephysical ity;
of starch. Itass sse When normal; temperatures.
been obtained described, as ;follows:. During the earlier stages of the addition of-the caustic in the stirrers and finally {when the proper, amount geneous colloidal compound ofstarch, caus-' glue. -The' word characteristics, is d flmt. PF
the.
workable. improved films-base and method of mixing the same, -t Ei'eatl reduced and can be re ulu-ted, .al-
oug the mixing isdone wit the same proportions of alkali -and carbohydrate or else the same temperature, which have hitherto weakly a hesive pastes or mucilages. And by the use of cassava starch in particular, results can be secured entirely difierent from those hitherto produced, as stated by I find, however, thatusing 'my is water absorbing power can be roduced unworkable jellies or others, preferably with corn. Thus, by
roper adjustment of conditions of mixing.
- am able to produce this glue even with certain grades'ofunt-reated cassava. carbohydrate and with other .starches and .conversion roducts (starchy carbohydrates). The p iminary treatment, however, sub- 'stantially reduces the absorption of water, by the starch and prevents it from becom ing jelly-like and tough when afterward treated either with the water as above indi-.
cated or with the alkali, or both.
In the. second part of my improved process less than about three parts of water by Wight to one part of the dry'material are u and after adding the solvent it is found that even with such a small amount of water, the batchwi'll assume a semi-fluid consistency by the'use of water alone andwill not become jelly-like and tough as in former processes. e alkali added acts, .I believe, to dissolve more or less of the cellulose and carbohydrate, uniting with the same and .with the water and forming a glue of very The dry carbohydrate. is, mixed with the water with a much superior to'that ordinarily obtained Exgeriments indicate-that after the car-. bohy rate base has been treated in accordance with the first ste of my process, the grgportion of amyloulose' in the carboate granule has been increased. a I beortion of the 'ani'lo-ce Eohydrate allows o the same to be changed into a 'good .when-tli'e action'of the solder j 1 its equivalent,-'and==the agitation, have hem i I crried ough in-the first step, is-asfol- .whichnj ustijlw y "th dry live steam at 100; lbs;
-glue with very much ,less water- ,than would otherwise be required; One .way
has been found quite satisfactory determining res,- v
for lso this increase in the percentage or prolulose in the carviscosity while hot, it showed a viscosity between that of cold water and three times that of cold water. In specific examples tried, the carbohydrate base, subjected to the above test, has shown viscosities between that of cold water and three times that of cold water but a product showin about two times the viacosity of water is preferred. In measurin this viscosity 350 grams of base were mix with 3150 c. c. .of cold water and 450 rams of the steam condensed therein and tea ed at 195 F. A Perkins viscosimeter was used, which may be constructed of brass tubin 1.295 inches outside diameter, 0.012 inc thick, and 3 inches long, and having a flat brass bottom 0.080 inch thick soldered into the end having a round center hole 0.070 inch in diameter .'the total weight being 39.63 grams, and all edges being made smooth removing practically no weight, thehole being polished until the cup placed quickly at its floating level in water at 60 F. floats upright and fills up-to the point of sudden sinking by top overflow in 16 seconds. If the material directly from the treatment tankof the first step is to be tested, a small quantity is taken, neutralized and diluted with, cold water toei Be. 3150 c. c. of this thoroughly mixed batch are then taken in avessel and the steam similarly ad.- mitted to the bottom of the batch, but this is found to indicate about 6% secondslower;
The carbohydrate glue base in the pre ferred form retains substantiall unchanged the size and general form 0 viewed under the microsco e when treated with cold water, and pro uces opalescent cloudy solutions with water at 200 F.
When treated in accordance with my process, I find that the carbohydrate glue'base may be formed into glue by using .only from one to three parts of water, the more water used the Preferably less than 41} parts of water should be used in making the glue from the carboh drate base.
I be ieve that thecause of the ,tmacious pro erties whencarbohydrates are treated witd waterand a strong solution of an alkali may be traced to the propezproportionin of viscosity, cohesion and. hesion, toge her with e peculiar chemical action which caustic loosely combined or free in the glue as applied, exerts on the cellulose 4 which it in turn combines with in making the joint to formalkali metal carbonate, bicarbonate and acetate. I believe this propefproportioning'is due to the partial no change of the integlmient and the proper proportioning of the amyl'o-cellulose and the granulose (or the'pro 1' mean polymerization) when united m the caustic and water. Consequently, I believe that to obtain 05 the best results it is necessary to abstain particle as -1utzions now employed industrially, in regreater the delay in drying.
although ot-her materials be mixed with the I to ear aces are so arated. I have foun that,
.quick se V crackle from reducin the cellulose toy true soluble starch, and t at sufiicien-t cellulose must be left to make the glue amply tenacious. Therefore, the action of the-acid and-alkali should not be carried so far nor the temperature-be so high as to destroy all the cellulose and. impair its strength by changing it into soluble starch and the starch into sugar or dextrin. Also, in actual practice I have found that a good glue is produced by treating the base with the chemicals to reduce the water absorbing power to a point where the base if mixedwlth from2 to 3 parts of water and, subjected to'heat of 170 would result in a syrupy condition instead of a thick jelly-like mass I find that by such suitable treatment under my process it is possible to produce from the base long filaments having a strength similarto threads of animal glue. Practically all the watermust be later removed that 4 as into 'the glue solution andis applied to t e joints,
hence an increase of water in the glue solution involves changes in drying methods, or
in drying time, or in risks of injury to the.
material due to warping by the extra water,
all of very serious consequence. -The di--' luted or adulterated pasteshitherto made from the natural carbohydrates inthe manner explained before are unfit for many classes of work and especially wood joint work, since the contain so much water or adulterants at it takes the joints verv long to dryor when they do become dry there 15 so little'binding material left that only a very weak bond 15 obtained. Thus it is of-the. greatest importance and value to roduce a concentrate gluesolution ready or application, which parallels the animal glue solot spect to water contents and physical properties in application, and is equal or .511- perior as to strength and permanency.
Certain advent. of my improved process may be obtained to some extent even am laceous material to form the as base.
a the preferred form'described my improved. Inc is tr arent and free from odor, an is very stab c after mixing for use, it is instantly adhesive to-clean surfaces, its cohesioxi is very great but not suflicient to overcome its adhesion and its viscosity is la andlow enough to permit ready a-p-- plication, but so pro ortioned toitscohesion 1 ohinery like hide glue, but still very 10 that it is capable 0 being applied by meh fibers are produced if'freshly- 'oine owing to the reakage of these filaments 1'2";
ration of such surfaces produces-a eel ectric sparks.
4 My glue. will produce joints which are practicall unaffectedby natural humidity d .whic are unaffected by prolonged dry 13 heat. In the referred form, it forms a joint with woo or other cellulosic material, which joint is distinguished from ordinary mucilagcs, sizes andpastes by the faet'thatit consists of the followin layers in the order named, unaltered cellu osic material, cellulosic.material altered b caustic, tough amylaceous material alters by caustic cellulosic material altered by caustic an unalteredcellulose. This joint can probably be distin ished wherever found, by the shading o the 'above layers intoone another when stained with-iodm and examined under the microscope and 'by other tests,
Glued up panels have been placed behind a radiator for 18 months without cracking or separating of the glue jointu Thesefeatures make In glue especially advantageous for purposes 'm which other vegetable glues are ractically useless.
- though I have described my improvementsin great detail and with much per ticularity' and have mentioned articular compounds which I preferto' use, desire it to be understood that I do not limit myself to such details and compounds, except as clearly specified in the; appended claims, as manymodifications and substitutes may .be found, but,
Having fully and clearly described my invention with respect to one particular embodiment thereof, what I claim and desire to secure by Letters Patent, is:
tpill cable by machinery and then dissol 1. The process of making a glue base which consists in agitating cassava-carbohydrate with water and a starch converting agent whereby the polymerization of the carboh drate is altered to a point such that when 'ssolved it will form a viscous semifluid unjellified product adapted to heappliedby machinery.
2. The process of making wood glue which consists in taking, suitable carbohydrate material and properly groportron: ing the viscosity, cohesiveness an adhesiveness oi the carbohydrate -material resulting'when it, is dissolved to formglue ape carbohydrate material with a solvent 0% cellulose to pit it into solution jto form glue. ,3. The rocess ofm a lue ase ,which consists-in agitating a sta y carbosolved to form' glue properly for the "cat-ion of the glue by m hydrate with water and a. starch converting agent to decrease the water absorptive prop- .ertiesof the carbohydrate to properlyproortion the viscosity, adhesiveness and co-. hesiveness'resulting when the base is disachin'ery.
4. The rocess of making .a which consists in agitating a stare lue base hydrate with water: and suitable c emicals below the bursting-temperature pithe starch to proportion the and -weight of water,
PP icarbocohesiveness resultiiig when the base is dissolved to form glue applicable by machinery. 5 In the making of adhesives, treatin cassava flour with substantially an. equa heating the same to about 13!? -F. and adding about 2% or 8% by weight of strong acid slowly and with agitation, without rendering the flour mate-- rially soluble in water,
acid with an alkali after from 4 to 6 hours agitation.
6. Inthe making. of a glue base, treating amylaceous material with a reagent to de-;
then neutralizing the a crease-its water absorptive properties, leaving a material portion of amylaceous material in the product insoluble in water.
T. In the makingof adhesives, treating a suitable carbohydrate with water and a di-- esting agent without rendering the carbohydrate materially soluble in water, to decrease thewater absorptive properties of the carbohydrate.
8. A glue'base characterized .by the facts that-it is prepared from starchy material retains substantially unchanged t e size an general form of particle when treated with cold water, and produces opale'scent cloudy solutions with water at 200 F. 1
9. The process of makin glue which consists 'in treating starch be ow the bursting temperature of the starch, with a digesting agent such as caustic; and water until the material assumes'a viscous semi-fluid consistency adapted to be applied by machinery.
10.The process of making glue. which consists in dissolving cassava carbohydrate in caustic alkali until a glue is formed as distinguished from mucil-ages, sizes and pastes. l
11. The processor making a'glue, which consists in treatin a starch carbohydrate with caustic alkali, and we r, to dissolve the carbohydrate, the total amount of water used being about 3 parts or less by weight off the carbohydrate, the amount of caustic alkaliiused, ca culated as NaQHbeinE about 10% orless by weightof the carbo drate so that a wood glue is formed, as i'stinguished from mucilages, sizes and paste.
12. Theprocess of making a glue, which consists in'mixin' starch with water and caustic alkali todis the amount of water used bei .a ut 3.
parts-or less by of dry car h drate so that 'a wood glue )8 formed, as istinguished from mucllages, sizes and paste.
' 13. The recess of m a wood glue which consists in treating a suitable starchy product a material :portion of which is substant'iall insoluble "in water with a. solvent of cell ose and about-3 parts or less by weight of water, to produce aglue having dhesive, powerssubstantiallj as great as thoset of good animal glue.
118 solve the carboh drate,
the caustic extrin, and then 1%. In the making of glue treating a suitable starchy product with a )out three parts or less by weight of water andadding a solution of caustic soda or other equiva ent alkali using about 10% or less by weight of soda or its equivalent of other alkali to dissolve the product.
15.-In the process of making wood glue, the combination of the following steps,'ag1- tating a starch carbohydrate with a digesting agent to ecrease its water absorptive )roperties without converting the batch into substantially dixolving the product thus produced with about three parts or less of water unt-il the resulting product has a consistency such'thet it is applicable to glue up veneers.
- for application,
16. In the process of making wood glue, agitating astarchv carbohydrate with a. digesting agent unt-i a sample of the material taken from the batch and dissolved will show a viscosity, adhesiveness and cohesiveness substantially-equal to animal glue.
17, The process of making wood glue which consists in agitating starch with a. diesting agent to decrease its water absorptive properties without rendering the carbohydrate materially soluble in col water and then combining the product thus produced with a solvent of cellulose toiproduce aglue thus proportiomng the viscosity, adhesiveness and cohesiveness of the final glue.
18. The process of making wood lue which consists in agitating a starchy car 0- hydrate with a digesting agent to decrease its water absorptive properties and then combinin the product thus produced with alkali an water to produce a lue' for ap lication having free caustic al ali therein.
19. In the process of making the combination of the following steps, agitating a. cassava carbohydrate with a digesting agent todccrease its water absorptive.
roperties without rendering the carbohyrate materially soluble in cold water and then putting the product thus produced into a solution containing about t ree parts or less by weight of water to produce a. glue which' for application. 20. he process otmaking glue consists in agitatin a starchy carbohydrate with water and a gesting agent to reduce. the water absorptive properties of the carbohydrate without renderin it materially then mixing the carbohydrate with water and caustic alkali, the amount of water used being about three parts or less by weight of dry carbohydrate, the amount of caustic usedbeing about 1 0% or less b w ht of dry carbohydrate, to dissolve as distinguished. from mucilages, sizes and paste.
21. The improved glue process which con:
from 2% to 3% composed wood glue,
- which w on boile sists in treating cassava carbohydrate with Substantially an equal weight of water, heating the same to about 180 F.,.add1ng by weight of an acid, slowly, and durin a -'tation, neutralizing the batch with an allrafi after from 4 to 6 hours agitation, then cooling and drying then adding from 1 to 3 parts by weight of the batch,v
water, andthen while being agitated treat:
ing the same with a solution of a caustic al ali usi n about 10% or less by weight of the dry el ali and applying the resulting product to surfaces with which the caustic is adapted to combine and forming a joint be tween said surfaces. I
22. In the making-of adhesives, treating ,a suitable starchy carbohydrate insoluble in water with water with a reagent to decrease its water absorptive propcrtiesbut without rendering the carbohydrate materially soluble in 'water,'then allowing the batch to dry, then treating the same with water and a solvent of cellulose such as caustid alkali to form glue. i
23. In the making of adhesives, treating a suitable starchy carbohydrate with an agent having an acid reaction without rendering the carbohydrate materially soluble in water, to decrease the water absorptive properties of the carbohydrate and then treating the carbohydrate with a solventof cellulose,-thus proportioning the viscosity, atllhesiveness and cohesiveness of the final g ue. v -24. A carbohydrate base for making glue of suitable carbohydrate which when mixed with about 3 parts or less by weight of water and a. solvent of cellulose will form a'semifl uid mass having substantially the adhesive pro erties of animal glue.
25. A.ba.se for fna ing glue ,as distinguished ains substentiallinsoluble in water on the outer socalle am lo-cellulose coat'm of which insoluble grains has been partie y but not entirel -converted. I
26. base for making gluetcomposed of a starch carbohi'drste or its equivalent for 10 minutes with dry but steam at 100 oundspressure with nine parts of water on tested for viscosity while at will show a viscosit between that of coldv water and three times that of cold water;
' 27 A base for glue as distinguished from muoileges, pastes and sizes, comprising treet ed cassava amy'laceous grains 'm which the proportion of so-called cellulose is ater than in the natural material from'which the base is derived. e car hydrate to form'the glue 28. A glue comprising1 draterendered semi-flui havm substantially the proper ies of mal g ue.
from mucilaga 'zesJmd pastes ,embracmg trested amyliiciious cassava carbohyby-di estion am muse 29. A glue comprising chiefly starch dissolved by a digesting agent alkaline. to phenolphthalein and in. about 8' parts'oi' less by weight of water.
30. A wood and fiber glue formed of a starchy carbohydrate .or' its equivalent by union therewith of about 3 parts or less b3; weight of water and alkali metal hydroxi V 31. A wood .and fiber glue containing 10 wit i'out acid in about three parts of water or less, and being viscous, sem -fluid and unjellified. 32. Aglueas distinguished from mu'cllages, sizes and pastes containing a starchy carbohydrate base substantially insoluble in water and dissolved by caustic and containing free caustic. V 33; A glue consistingof a vegetable can bohydrate base substantially insoluble in water and dissolved by water and caustic soda alkali, the amount of water being about three pnrts'or-less by weight of dry carbohydrate and the amount of caustic present dry carbohydrate. V.
'34. A glue consistlng of a vegetable carbohydrate base substantially insoluble 1n water and dissolved by caustic alkali, the
13,436. (Reissue.)Fmak Perkins Glue Company.
disclaimer in Letters Patent Reissue No. 13,436.
am laceous material as a base dissolved in]?! viscosity to flow through pipes and-the:- a
a being about 10% or less by weightof the.
37. A lue composed of a starch carbohydrate ass and a solvent-of cellu ose and having such a character that-itwill be substantiall' unafl'ected by the natural humid- 46 ity and aving substantially as good adhering qualities as the best animal glue.
38. The process of making a wood lue which conslsts'in suspending a glue containing amylaceous matter insoluble in water in about three parts or less by weight of water and treating the, base with an alkali properly proportioned substantially as described to produce a glue having a last esiveness of animal lue.
In testimony whereo I have signed 'my name to this specification, in the presence of V FRANK G. PERKiNs two subscribing witnesses; V By GERTRUDE s.. PERKINs,
of the last will and testament of F rank '6. Perkins; Witnesses:
S. D. TAYLOR;
-L.- MOMILLEN. V
GERTRUDE S. PERKINS, Ewec'utfigv of the. last will and testament of Frank G. Perkins.
'30 amount of water being about three parts or Wit s V less by weight of dry carbohydrate. S D TAYLOR, 35; {)1 glue colntalmgng a slstarcthyf ca1l-1oo1hy- L MoMlL-mm -drate use disso ve y a so ven 0 cc u ose and water, theampunt of water in the glue E K E ngfigaz 35 bemgabout-Vthree parts or less by weight of y JULIUS B. B STRYKERV V V V dry carbohydrate. V Vice President 36. A glus as distinguished :trom muci- V V A I lages, sizes and pastes, consisting chiefly of, Witnesses:
a starchy carbohydrate base-substantia'll in-. AM A; DELP, 40 soluble 1n water and dissolved by a so vent B. SMITH.
of cellulose.
Discus IMIBJR.
V V c. Perkins, deceased; m5 of sou h Bend, Ind.; Gertrude S. Perku a, executrix. Gnvn'azm M'n'rno'n or Mani! 'rrm' mm dated July 2, 191 Disclaimer filed February e, 1919, by the mime,
Sana:
Eaters m disclaimer ofclaima 1, 3, 4, 6,7, 8, 1e, 24, 25, 2a, and 27 thereof (to wit the claims'for glue base per se and for the process. of making the glue base pea-u) and further it hereby disclaims from claims 9, 10,1-1,.1 2, 18, 14, and
of'sard reissued Letters Patent, N 0. 13,436 anyprooess of making glue, exoepturg where the starch or starchy product or carbohydrate subjected to the procesa is degenerated to the extent described in the said reissued Letters Patent No.
13,436, whereby the process results in'the good as animal lue described inlaid reissued Letters PatentNo. 13,436. V g Y 4 muse 29. A glue comprising chiefly starch dissolved by a digesting agent alkaline. to phenolphthalein and in. about 8' parts'oi' less by weight of water.
30. A wood and fiber glue formed of a starchy carbohydrate .or' its equivalent by union therewith of about 3 parts or less b3; weight of water and alkali metal hydroxi V 31. A wood .and fiber glue containing 10 wit i'out acid in about three parts of water or less, and being viscous, sem -fluid and unjellified. 32. Aglueas distinguished from mu'cllages, sizes and pastes containing a starchy carbohydrate base substantially insoluble in water and dissolved by caustic and containing free caustic. V 33; A glue consistingof a vegetable can bohydrate base substantially insoluble in water and dissolved by water and caustic soda alkali, the amount of water being about three pnrts'or-less by weight of dry carbohydrate and the amount of caustic present dry carbohydrate. V.
'34. A glue consistlng of a vegetable carbohydrate base substantially insoluble 1n water and dissolved by caustic alkali, the
13,436. (Reissue.)Fmak Perkins Glue Company.
disclaimer in Letters Patent Reissue No. 13,436.
am laceous material as a base dissolved in]?! viscosity to flow through pipes and-the:- a
a being about 10% or less by weightof the.
37. A lue composed of a starch carbohydrate ass and a solvent-of cellu ose and having such a character that-itwill be substantiall' unafl'ected by the natural humid- 46 ity and aving substantially as good adhering qualities as the best animal glue.
38. The process of making a wood lue which conslsts'in suspending a glue containing amylaceous matter insoluble in water in about three parts or less by weight of water and treating the, base with an alkali properly proportioned substantially as described to produce a glue having a last esiveness of animal lue.
In testimony whereo I have signed 'my name to this specification, in the presence of V FRANK G. PERKiNs two subscribing witnesses; V By GERTRUDE s.. PERKINs,
of the last will and testament of F rank '6. Perkins; Witnesses:
S. D. TAYLOR;
-L.- MOMILLEN. V
GERTRUDE S. PERKINS, Ewec'utfigv of the. last will and testament of Frank G. Perkins.
'30 amount of water being about three parts or Wit s V less by weight of dry carbohydrate. S D TAYLOR, 35; {)1 glue colntalmgng a slstarcthyf ca1l-1oo1hy- L MoMlL-mm -drate use disso ve y a so ven 0 cc u ose and water, theampunt of water in the glue E K E ngfigaz 35 bemgabout-Vthree parts or less by weight of y JULIUS B. B STRYKERV V V V dry carbohydrate. V Vice President 36. A glus as distinguished :trom muci- V V A I lages, sizes and pastes, consisting chiefly of, Witnesses:
a starchy carbohydrate base-substantia'll in-. AM A; DELP, 40 soluble 1n water and dissolved by a so vent B. SMITH.
of cellulose.
Discus IMIBJR.
V V c. Perkins, deceased; m5 of sou h Bend, Ind.; Gertrude S. Perku a, executrix. Gnvn'azm M'n'rno'n or Mani! 'rrm' mm dated July 2, 191 Disclaimer filed February e, 1919, by the mime,
Sana:
Eaters m disclaimer ofclaima 1, 3, 4, 6,7, 8, 1e, 24, 25, 2a, and 27 thereof (to wit the claims'for glue base per se and for the process. of making the glue base pea-u) and further it hereby disclaims from claims 9, 10,1-1,.1 2, 18, 14, and
of'sard reissued Letters Patent, N 0. 13,436 anyprooess of making glue, exoepturg where the starch or starchy product or carbohydrate subjected to the procesa is degenerated to the extent described in the said reissued Letters Patent No.
13,436, whereby the process results in'the good as animal lue described inlaid reissued Letters PatentNo. 13,436. V g Y 4

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