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Publication numberUS3607394 A
Publication typeGrant
Publication dateSep 21, 1971
Filing dateMay 29, 1969
Priority dateMay 29, 1969
Publication numberUS 3607394 A, US 3607394A, US-A-3607394, US3607394 A, US3607394A
InventorsGermino Felix Joseph, Miller Gerald Donald, Moskaluk Jerry Adam
Original AssigneeGermino Felix Joseph, Miller Gerald Donald, Moskaluk Jerry Adam
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Novel pregelatinized starches and process for preparing same
US 3607394 A
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Description  (OCR text may contain errors)

United States Patent [72] Inventors Felix Joseph Germino 12414 83 rd Ave., Palos Park, 111. 60464; Gerald Donald Miller, 3621 Douglas Road, Downers Grove, Ill. 60515; Jerry Adam Moskaluk, 14500 Sawyer Ave., Midlothian,

in. 60445 Appl. No. 829,083 Filed May 29, 1969 Patented Sept. 21, 1971 NOVEL PREGELATINIZED STARCHES AND PROCESS FOR PREPARING SAME 5 Claims, No Drawings [1.8. CI 127/32, 75/2, 127/69 Int. Cl C131 1/08 Field of Search 127/28, 32, 69, 70, 71

OTHER REFERENCES Ward Pigman, ed., The Carbohydrates," 676, Academic Press, New York, 1957.

Primary ExaminerMorris O. Wolk Assistant Examiner-Sidney Marantz Attorneys Frank E. Robbins, Janet E. Price, Robert D.

Weist, Martha A. Michaels and Dorothy R. Thumler ABSTRACT: Pregelatinized starches are prepared by pasting an aqueous slurry of a starch which contains at least 50 percent amylopectin at a temperature of at least 300 F, and then rapidly, preferably instantaneously, removing the water therefrom as by roll or spray drying. The resultant products rapidly disperse in water to form smooth pastes which are characterized by low initial viscosity and minimal setback.

NOVEL PREGELATINIZED STARCHES AND PROCESS FOR PREPARING SAME This invention relates to cold water dispersible starch products and to a method for preparing same.

So-called pregelatinized starches, i.e. starches which have been gelatinized and dried and which will disperse when added to cold water to form pastes, have long been known to the art. They are generally prepared either by first gelatinizing an aqueous slurry of starch, as by heating it to its gelatinization temperature, and then instantaneously removing the moisture, as by means of a roll or spray drier, or, alternatively, by passing an aqueous slurry of granular (i.e. ungelatinized) starch through a suitable apparatus, e.g. a roll or spray drier, wherein the starch is simultaneously gelatinized and dried.

When an ordinary (i.e. unmodified and underivatized) starch is subjected to a conventional pregelatinizing treatment the product will, upon addition to cold (i.e. room temperature) water, form a smooth, relatively viscous paste. For certain applications, pregelatinized starches which will form pastes of low viscosity are desirable; such products are customarily prepared by hydrolyzing the starch, as with acid or enzyme, prior to or simultaneously with the pregelatinizing treatment. Hydrolysis causes molecular degradation of the starch, that is to say, it breaks down the starch molecules; because of this the resultant pastes are not only low in viscosity but low in molecular weight as well.

Another feature of pastes prepared from ordinary pregelatinized starch is their tendency to increase in viscosity upon standing; this characteristic is generally referred to as setback." conventionally, setback is minimized by derivatizing the starch, i.e. adding substituent groups to the molecule.

We have discovered a simple, rapid, and inexpensive method for preparing pregelatinized starches having the ability to disperse rapidly in cold water to form exceptionally smooth pastes, which pastes are characterized by low initial viscosity and exceptionally good viscosity stability (i.e. minimal setback). Furthermore, unlike conventional pregelatinized starches which have been subjected to hydrolysis to lower their paste viscosity, the starches of our invention are characterized by substantially no, or at most very slight, molecular degradation.

It is an object of the present invention to prepare cold water dispersible starches which will reconstitute to form pastes having low initial viscosity and minimal setback.

Another object is to prepare pregelatinized starches which will rapidly disperse in cold or warm water to form exceptionally smooth pastes of low viscosity.

An additional object is to treat starch in such a way that the molecules of same will be substantially undegraded, but pastes of the starch will nevertheless exhibit low viscosity and exceptionally good viscosity stability.

Other objects and advantages will be apparent from the specification and the appended claims.

Briefly, the process is as follows. A granular starch which contains at least 50 percent amylopectin is slurried in water and pasted at a temperature of at least about 300 F., after which the water is instantaneously removed.

The starch can be any starch provided it contains at least about 50 percent amylopectin. Cereal starches, such as those derived from corn, wheat, barley, etc.; tuber starches, such as those obtained from potatoes, tapioca, or the like; and the waxy starches," e.g. waxy maize, waxy rice, and waxy sorghum, which consist entirely or substantially entirely of amylopectin, and are all suitable for the practice of the invention. The high amylose" starches, i.e. those which contain 60 percent amylose or more, as well as amylose itself, are not suitable, in that these starches produce products which form gels upon reconstitution with water, and gel formation is an undesirable characteristic in the applications for which the products of the invention find their greatest utility. The starches can be modified and/or derivatized prior to the pasting treatment. The only critical requirements for starches to be treated in accordance with the invention are (1) they must be granular, i.e. ungelatinized, (2) they must be capable of being gelatinized in water (for example, a starch which is so highly cross-linked that it will not undergo gelatinization could not be used), and (3) they must contain at least 50 percent amylopectin.

The instantaneous removal of the water after the high temperature pasting can be performed in any suitable apparatus, e.g. a drum drier, a spray drier, a belt drier, a foam mat drier, or the like, the only requirement being that the apparatus be capable of drying the starch paste very rapidly.

The original slurry can contain up to about 35 percent starch solids (by weight, based on the weight of the total slurry). As stated before, the starch must be pasted at a temperature of at least about 300 F. The only upper temperature limit is that at which substantial molecular degradation of the starch will take place, e.g. over about 450 F. Temperatures of from about 315 F. to about 360 F. are preferred.

It is very important that the paste not be permitted to cool to a point at which the starch begins to retrograde or becomes aggregated prior to removal of the water. The temperature at which retrogradation or aggregation begins depends upon the solids content of the paste. For example, a 35 percent solids paste will begin to retrograde at about 190 F., while one of 12 percent solids will begin to retrograde at about -l50 F. Also, it is preferred that the paste be fed to the drier very quickly after the completion of the pasting step, because the longer it is held at a high temperature the greater is the likelihood of molecular degradation an-d/or crystallization.

The products, because of their ability to reconstitute in cold water to form smooth pastes of relatively low viscosity, high molecular weight and minimal setback, are extremely useful as adhesives and as coatings and sizings for paper and textiles. It has also been observed that the reconstituted pastes have excellent film-forming properties, i.e., they will readily form films which exhibit excellent oil holdout and water holdout properties. The products are also excellent iron oxide depressants in the calcium soap flotation process for concentrating iron ores.

Structurally, the products of the invention are characterized by complete granular fragmentation, as contrasted with the conventional pregelatinized starches which contain a certain amount, usually about 10-15 percent, of intact granules.

The following examples will illustrate the practice of the invention. They are intended for illustrative purposes only, and should not be construed as limiting the scope of the invention in any way.

EXAMPLE I A series of runs was made in which aqueous slurries, at 25 percent solids concentration by weight, of regular, unmodified corn starch were heated in a steam injection cooker to temperatures of from 212 F. to 355 F. until they were completely pasted. Immediately after pasting the products were passed over a 24 inch roll drier, operated at 2.6 rpm. and 100 lbs.

steam, the skin temperature of the rolls being 284 F. The

TABLE 1 Brooktield vis- Concentration Brookfield viscosity of reconol reconstituted cosity of reconstitutod pastes Pasting temp., pastes, weight stituted pastes after 24 hours at F. percent atF., cps. 150 F., cps.

Approximately.

As can be seen from Table l, pastes of starches prepared in accordance with the invention (cooked at temperatures of 300 F. and 355 F.) were substantially lower than those cooked at 212 F. and 250 F.

Blender at 4,000 r.p.m. prior to addition to the pulp. ln run 5 the alkaline starch dispersion was cooked at 100 C. for minutes prior to addition to the pulp.

Table ll sets forth the amounts of starch used in each run As can also be seen from the table, pastes of starches 5 (calculated on the basis of pounds of starch per ton of ore), prepared in accordance with the invention which were held and the analyses of the froth and concentrate portions of each for 24 hours increased only slightly in viscosity. r

IABLE 11 Percent Lb. starch Percent Percent Fe re- Run No. Corn starch used per ton ore Product weight Fe covery 1 Prepared according to lnvention- 3 Froth 25. 94 33. 65 15.93 Concentrate 74. ()6 62. 21 84. U7

2 Regular. 3 Frotli 51. 00 47. 75 44. 21 Concentrate. 4U. 00 62.71 55. 79

3 Regular 4 Froth 23. 90 30. 40 13. 23 Concentrate. 76. 10 62. 64 86. 77

4 Homogenlzed regular 3 Froth 21. 7O 28. 19 11. 24 Concentrate. 78. 30 6'2. 31 88. 76

5 Cooked regular 3 Froth 48. 72 46.73 41. 39 Concentrate- 51. 28 62. 88 58. 61

EXAMPLE II An aqueous slurry at 25 percent solids of white milo starch 25 was pasted at 3350 F in a Steam injection cooker and from the percent iron recovery in the concentrates, ll. 18 mediately roll dried as in Example 1. The product was added to f P at 3 SFarch per ton of ore the starch of the at a of 26 percent sohds; the starfzh re.adlly dlspflsed to form a smooth 30 $112! has been subjected to extensive shearing in a blender or as paste The Brookfield vlscosny (at 20 'h 7200 regular starch used at the increased rate of 4 lbs. per ton. Ad-

EXAMPLE I" vantages in the use of starch prepared in accordance with the invention are that less of it needs to be used as a depressant A 16 percent aqueous slurry of regular unmodified corn and that its dispersions do not need to be sheared extensively starch was pasted at 360 F. in a Votator indirect heat to be obtained in a useful form. exchanger. Immediately after pasting the product was dried in While the invention has been described in connection with a spray drier. A 25 percent solids paste was prepared in water specific embodiments thereof, it will be understood that it is at 110 F. The Brookfield viscosity of the paste was l26,000 capable of further modification, and this application is inc.p.s. tended to cover any variations, uses, or adaptations of the in- Th example was repeated using wheat h, waxy i 40 vention following, in general, the principles of the invention starch and potato starch with comparable results. In all cases and ing such departures from the present disclosure as the products rapidly dispersed in water to form smooth pastes come within known customal'y Practice in the to which which were characterized by low initial viscosity and minimal the invention pertains and as y be pp the essemial Setback features hereinbefore set forth, and as fall within the scope of the invention. EXAMPLE lV What is claimed is: This example illustrates the use of starch prepared in ac- Process for preparmga-prefgelanmzed Cvold water dlsper' slble starch product comprising. cordance with the invention in the concentration of lron ores. L heating an aqueous slurry f a granular r h, said granu- S tandard procedure for ore flotanon a lar starch containing at least 50 percent amylopectin, at a descnpilon ofwhlch was emPloyed temperature of at least about 300 F. for a time sufficient A 500-gram sample of iron ore lS pulped to 30 percent to paste completely Said Starchand solids in a batch laboratory conditioner. To this ls added a 2 thereafter rapidly removing substantially all of the percent starch dispersion prepared by stirring the starch in 0.5 moisture from the pasted starch N sodium hydroxide solution for 30 mlnutesat room tempera- 2. process of claim {wherein the moisture is removed by ture. The pH of the pulp and starch mixture is ad usted to 1 1.8 roll-drying the pasted starch. and the pulp is conditioned for 2 minutes. This is followed by process f claim 1 wherein the moisture is removed by 1-minute conditioning with calcium chloride (2 lbs. per ton Spray drying the pasted starch.

Ore) h 2 minutes Conditioning with Actihol FAQ 4. Process of claim 1 wherein said starch slurry is heated at a P The Conditioned P p is transferred to Fager- 6o temperaturewithin the range of between about 315 F. and gren laboratory flotation machine, diluted to 20 percent about 360 F solids, and floated for 5 minutes. The froth and the concen- 5, A l i i d Starch product hi h ill idl Irate are Weighed and yz fOrifOn Content disperse in water to form a smooth paste having low initial Five runs were made, employing different starches as folviscosity and excellent viscosity stability, said starch being lows. Run 01 used a corn starch treated in accordance with further characterized by complete granular fragmentation and Example I, pasted at 340 F. Runs 2 and 3 employed regular, substantially no molecular degradation, said starch having unmodified corn starch in two different amounts. ln run 4 been prepared in accordance with the process of claim 1. regular unmodified corn starch was used, and the alkaline starch dispersion was homogenized for 5 minutes in a Waring

Patent Citations
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US2314459 *Apr 15, 1939Mar 23, 1943Dryfood LtdDry starch product
US2900335 *Jun 13, 1956Aug 18, 1959American Maize Prod CoOil well drilling mud
US3137592 *Apr 3, 1961Jun 16, 1964Staley Mfg Co A EGelatinized starch products
US3434880 *May 27, 1966Mar 25, 1969Ind Et L Agriculture Soc D EtStarch pastes of improved fluidity
Non-Patent Citations
Reference
1 *Ward Pigman, ed., The Carbohydrates, 676, Academic Press, New York, 1957.
Referenced by
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US4667654 *Jul 10, 1985May 26, 1987National Starch And Chemical CorporationPulse combustion process for the preparation of pregelatinized starches
US4853114 *Mar 3, 1989Aug 1, 1989American Cyanamid CopanyMethod for the depressing of hydrous, layered silicates
US5131953 *Sep 12, 1988Jul 21, 1992National Starch And Chemical Investment Holding CorporationContinuous coupled jet-cooking/spray-drying process and novel pregelatinized high amylose starches prepared thereby
US5188674 *May 8, 1991Feb 23, 1993National Starch And Chemical Investment Holding CorporationSlurrying polymer with water, cooking with steam to disperse or solubilize, conveying to nozzle of spray dryer, atomizing, drying, recovering powder
US5307938 *Mar 16, 1992May 3, 1994Glenn LillmarsTreatment of iron ore to increase recovery through the use of low molecular weight polyacrylate dispersants
US5318635 *Jul 27, 1992Jun 7, 1994National Starch And Chemical Investment Holding CorporationContinuous coupled jet-cooking/spray-drying process and novel pregelatinized high amylose starches prepared thereby
US5435851 *May 9, 1994Jul 25, 1995National Starch And Chemical Investment Holding CorporationContinuous coupled jet-cooking/spray-drying process and novel pregelatinized high amylose starches and gums prepared thereby
US5571552 *Apr 6, 1995Nov 5, 1996National Starch And Chemical Investment Holding CorporationContinuous coupled jet-cooking/spray-drying process and novel pregelatinized high amylose starches and gums prepared thereby
US5641349 *Jan 31, 1996Jun 24, 1997National Starch And Chemical Investment Holding CorporationWater-based adhesives containing thermally-inhibited starches
US5718770 *Jan 17, 1996Feb 17, 1998National Starch And Chemical Investment Holding CorporationDehydrating a starch to anhydrous; heat treatment
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Classifications
U.S. Classification127/32, 127/69
International ClassificationC08B30/14, C08B30/00
Cooperative ClassificationC08B30/14
European ClassificationC08B30/14