1478 707 10 15 30 35 40 45 PATENT SPECIFICATION (22) Filed 25 Sept, 1974 (21) Application No. 41760/74 G1) Convention Application No. 172.101 (33) New Zealand (NZ) (44) Complete Specification published 6 July (1) INT. CL? 423 3/00 (52) Index at acceptance CSC 4.5A3 SBS 9B5 9B9A 904 9EX G2) Filed 27 Sept. 1973 in ay 1478 707 1977 (4) IMPROVEMENTS IN OR RELATING TO MILKFAT CONTAINING PRODUCTS AND PROCESSES THEREFOR, Ql) We, New Zracaxo Day Re- seancu Issritute, a Body Corporate under the Charitable Trust Act 1957, of Dairy Farm Road, Fitzherbert, Palmerston North, New Zealand, do hereby declare the inven’ tion, for which we pray that a patent may be granted to us, anid the method by which it is to be performed, to be particularly described in and by the following: state- ment:— ‘This invention relates to milk fat con- ‘taining products and processes therefor and has been devised particularly though not solely for producing a soft dairy spread. Tt is desired that dairy:spread should bbe available which will be spreadable at domestic refrigerator temperatures say 5°C and ‘which will have little change im its spreading characteristics as between that temperature -and a warm ambient tem- perature; say 22°C. Tis threlore an objec of the present in- vention to provide @ milkfat containing pro- duct and/or processes therefore which pro- duct “may be easily spread over a wide range of temperatures: The most important property of high fat content spreads whic determines their spreadabiliy is the sold fat content of the fat phase. ‘The solid fat content of a giyceride mixture is defined as the proportion of solid giycerides present at a given temperature, The solid fat con- ‘ent is conveniently measured by wide fine nuclear magnetic resonance spectroscopy. Related measurements such as the so called solid fat_index (American Oil Chemists Society Offical Method) or the integral curve obiained by differential scanning calorimetry (Norris and Munro, 1974) are 2lso commonly used. Variation in the solid fat content accounts for more than’ 50% of the variation in butter hardness. Because the solid fat content of butter-ike products ig the principal factor in determining their theological properties, a further object of this invention is to provide a milkfat con- taining product and/or processes therefor Which shows litle change in the sold fat content of its fat phase over a wie range of temperatures, ‘Accordingly in one aspect the invention consists in process for producing the fat component ofa soft dairy spread the pros cess. comprising the steps of fractionating a milkfat or a milkfat containing substance 55 {nto three fractions 1A fraction’ in which substantially ol the mika old at 20°C making increasingly at higher temperatures 2, A TrciSh fe Rk SamTereS® a 0. the milkfat is solid at O°C and Lguid ar 20°C 3. A fraction in which substantially all the milkfat ig melted at 0°C and blending fractions T'ang 3 in propor- tions such that the ratio of fiquid fat con- tent 0 sofid fat content of 2 soft dairy Spread including such fat content remains substantially constant over. a temperature Finge of $°C to 22°C. na farther aspect in a preferred form the invention consists in a process for pro- ducing sat diy spread’ comprising the steps of taking a Tat component. prepared according to the preceding paragraph, and in which the weight ratio of Traction one to fraction threo is about 1:3, adding water, sale and solids—not fat and mixing t0 pro’ duce a soft dairy spread, "As used heroin, the expression “solds- 80 not fat” is intended to relate to such sub. stances mot including fat which are found in milk solids, Tha Sill fore aspect the invention consists in a soft dairy spread ‘comprising faction of milkfat which is substantially Solid at 20°C melting increasingly at higher temperatures blended vith a further frac. tion of milkfat which is substantially liquid af O°C 9 that the ratio of liquid fat oom- 90 50 65. 10 15 as1478707 2 ‘ponent to solid fat component remains sub- antially constant over a temperature range of 3°C fo 22°C and mixed with water, salt and solid — not fat 5 One preferred form of the invention and ‘modifications thereof will now be described. ‘a the present invention milkfats or a milkfat containing substance is fractionated into the following fractions: 1. A fraction melting below 0°C 2. A fraction melting between 0°C and 20°C 3, A fraction or fractions melting above 20°C, 45 Fraction I is then blended with one of the fractions 3 in suitable proportions and with @ desired proportion of water, salt_and Solids — not fat preferably obtained from milk: or milk products resulting in a dairy spread or butter having substantially similar spreading, characteristic between temperatures of 5°C and 22°C ic, having fiwle change in spreading characteristics ‘within this range. ‘Tr may be desirable in some cases to pro- duce more than one fraction melting above 20°C so that the final melting point of the said dairy’ spread is ator below mouth temperature. 1 preferred form of fractionation com- prises solvent fractionation of anhydrous ilk fat, Solvent. fractionation processes may be of several typ 1, Liquid extraction, by which the melted fat to be fractionated is contacted with solvent, ¢.g. propane or furfural in which only some of the triglyeerides are soluble. 2 Leaching by which higher melting slyceride fractions ‘are first crystallised from the melt and organic solvent is added to the slurry and the slurry filtered. ‘The slurry may also be filtered first and the. solvent used to wash the higher melting fat tal aggregates free of lower_meltin as SIAL aggregates free of dower, melting 10 35 40. 3. Solvent crystallisation, by which a slurry of higher melting fat’ crystal agare- gate in solvent/fat solution is first produced, either by mixing hot fat and cold solvent so that the mixture attains the desired cxystallisation temperature or by producing ‘an entirely liquid solution of fat in solvent and cooling the solution until the desired crystallisation temperature is reached. The crystal aggregates are then separated from the solution by, for example, decantation, filtration or centrifuging. Washing of the crystal aggregates with, fresh or other solvent during or after separation by-any of the above methods may be carried out if desired. After further crystallisations on either the filtrate or precipitate at the same or other temperatures are cartied out if desired, the solvent may be removed © from the fractions by, for example, evapora- 50. tion and stripping using steam or other 55 gr vapour. If a scheme for a solvent fractionation involves recrystallisation these farther recrystallisations can usually be carried out in any order adding or remov- ing solvent as desired between crystallisa- tions, Substantially pure organic solvents, mixtures of organic solvents, organic solvent plus water, and mixtures of organic solvents plus water may be used, In the present 75 Invention. the preferred form of solvent fractionation is solvent crystallisation. The solvent, used ig an organic solvent or mix- ‘ure of solvents selected from for example propan-2-ol(isopropanol), acetone, ethyl Acelate, hexane and petroleum derivatives Preferably acetone or propan-2-0l is used fas solvent using preferably four parts by ‘weight of solvent to one part by weight of 80 fat. ‘The following are examples of the pro- cesses according to the invention through- {ue whieh the pars and percentages are ‘weight, Brample f i0'6 of anhydrous mila obtained in the, spring (oftening point (Dolby, = 32.0, Iodine value = 36.9) was dissolved in 160 g Analar (Registered Trade Mark) acetone in a 500 mi flat bottomed flask. ‘The solution was heated to 26.5°C then placed in a water bath at 22°C for 2 hours ‘without. stirring. “The. slurry was then filtered in a jacketed sintered glass funnel. The precipitate was washed on the filter with 8g of acetone at 22°C and the wash liquor combined with the Strate, The bulk of the solvent was removed from the pre- Cipitate in a rotary vacuum evaporator and the, last traces removed by stripping with nitrogen gas. The fat recovered from the precipitate amounted to 0.54 g (fraction 1). ‘The combined filtrate and washings were heated to 22°C, cooled to 120°C in 40 mins, and held at that temperature for 25 hours, The slurry was filtered and washed with 16 g acetone at 12°C and the wash Hquor combined with the filtrate. The pre- cipitate contained 3.15 g fat (fraction TH). rhe combined filtrate and washings from ‘the 12°C crystallisation were. then heated to 20°C and cooled to —14°C in 5 hours and held for 1 hour. After filtration and ‘washing with 80 g acetone at —15°C the cipitate contained 17.5 g of fat (fraétion. THD nd the Ala plus wash liquor con. tained 16.6g (fraction 1V). Selected fractions ‘were then ,recombined in selected, propor- tions and éccordingly one part of fat from fraction II was combined with three parts’ of fat from fraction IV and the thermal properties of the mixture analysed using a Differential Scanning Calorimeter (Norris ‘and Munro, 1974). The results. showed that the fat blend contained approximately so 95 100 110 1s 1203 1.478707 46% of solid fat at 5°C and 38% at 22° indicating only a small change in (coi sistency) solid fat content over this tempera- ture range. ‘The temperatures given in this example may of course be varied to vary the melting points of the fractions, The holding steps may be omitted if desired but are provided to give time for aggregations of crystals ‘to build up. Example 2 1.5 kg of anhydrous milkfat obtained in the summer was dissoived in 6.4 kg an- hhydrous acetone and placed in a jacketed Stainless steel vessel. “This vessel ‘consists of an upper and lower chamber. The upper chamber is fitted with a “near wall” paddle and the lower chamber contains a filter ‘medium as its floor. Refrigerant can be circulated through the jacket from a con ‘trolled temperature bath, ‘Throughout the solution was heated to 33°C and cooled at 24°C.ir* to 22°C and held for 70 minutes before being dropped to the lower chamber where the slurry was filtered. The crystals were washed on the filter with 0.4 kg of acetone at 20°C, The precipitate (fraction 1) was removed from the vessel by heating the jacket to 30°C and dissolving the fat in 4 kg of acetone at 50°C, After removal of solvent from the precipitate 0084 kg of fat remained, The filtrate plus wash liquor was returned to the top chamber, heated at 30°C, cooled at 17°C.h* to 11.5*C and held for'1 hour before filtration, 0.8 kg of wash liquor at 10°C was-used. 0.136 kg of precipitate (Frac- tion Tl) was produced. ‘The filtrate from the 12°C crystallisation was retumed to the vessel, heated to 22°C, cooled at 162°C: to 15°C, held for 110 minutes ‘and filtered. After washing with 3.2 kg acetone at ~i7°C, the pre- cipitaie was found to contain 0.534 ke (frac tion TI) and the filtrate plus washings 0.49 kg (fraction IV), ‘Fractions TL and IV were combined in the ratio of 1:3 by weight, and used to make a butter containing 15.6% moisture, 50 1.3% salt and 83.19% fat. The butter had a hardness value of 135 by sectility at 5°C (faylor ef af 1971) and a “stand up” value of 1.3 at 22°C. On the scale used, a spread should have a “stand up” value of less than 5 units at 22°C to be considered satis- factory, The butter was spreadable on bread at 5°C’and appeared to have substantially the same consistency at 22°C. Example 3 1.6 kg of Anhydrous Milkfat obtained in the summer was dissolved in 64 kg anhydrous propan-2-ol and placed in the vessel described i example 2. The solution Was heated £0 36°C, cooled at 6°C.h~ to @ 20°C and held for’ 1 hour before being 10 15 25 30 35 45 58 o dropped to the lower chamber where the slurry Was filtered. The crystals were washed ‘on the filter with 1 kg propan-2-ol at 18°C. ‘The precipitate: (raction 1) was removed from ‘the vessel by heating the jacket to 70 50°C and dissolving the fat in 4 kg of ropan-201 at 50°C. After removal of solvent from the precipitate 0.296 ky of fat remained, The filtrate plus wash liquor was returned 75 to the top chamber, heated to 33°C, cooled at 20°C.b to 14°C, held for 15 minutes, cooled at 1°C.h to 11°C then cooled at 6°C.hr* to —5°C at which temperature the slurry produced was held for 1 hour. Slow 80 cooling of not greater than 1°C:h-* between the temperatures of 14°C and 11°C was found essential in order to produce good crystals when propan-2-ol was used as solvent for this crystallisation step. After filtration 85 and washing with 2 kg propan-2-ol at ~7°C the precipitate was found to contain 0.726 kg of fat Graction ID. The filtrate plus washings were found to contain 0.537 kg of fat (fraction TI) fraction 1 was found 90 to melt entirely above 20°C, fraction II between 0° and 20°C, and friction TIT en- tirely below 0°C, Fractions I and ill were combined in the ratio 1:3 by weight, and used to make a but- ter with a hardness value of 180 and a “stand up” value of 2.0. 95 WHAT WE CLAIM IS: 1.. A process for producing the fat com- ponent of a soft dairy. spread the process comprising the steps of fractionating @ milk- fat or a milkfat containing substance into three fractions : 1A fraction in which substantially all the milla is solid at 20°C. melting. in- creasingly at higher temperatures 2. A fraction in which substantially all the milkfat is solid at 0°C and liquid at 20°C uo 3. A fraction in which substantially all the ‘ilkfat is melted at 0°C and blending fractions 1 and 3 in propor- tions such that the ratio of liquid fat content to solid fat content of a soft dairy spread including such fat content remains substan- dally constant over temperature range of S°C to 22°C. i 2, A process as claimed in Claim 1 wherein said steps of fractionation are effec- ted by the use of a solvent. : 3. A. process as claimed in Claim 2 wherein said steps of fractionation are effec- ted by the techniques of solvent crysiallisa- tion. 4. A process as claimed in Claim 2 ot Glaim 3 which includes the step of decanta~ tion, filtration or centrifuging to separate crystals from the solution. 5. A process as claimed in any one of 130 100 105 us 120 1251478707 Claims 2 to 4 wherein said solvent is an organic solvent or mixture of solvents selec ted from propan-2-o}, acetone, ethyl acetate, hexane and petroleum derivatives. 5 6. A process as claimed in Claim 1 which includes ‘the steps of adding solvent to anhydrous milkfat, heating the mixture to a first temperature ‘sufficient. to dissolve the milkfat, cooling the solution to a second 10 lower iemperature over a period of time, filtering the solution and removing the sol. vent from the precipitate so that the precipi- tate forms said first fraction, if necessary heating the filtrate to about said second tem- 15 perature and cooling the filtrate to a third fomperature lower than said second tempera- ture over a petiod of time, fitering the solu- tion at about said third temperature and re- moving the solvent from the precipitats so 20 that the precipitate forms suid second frac- tion and removing the solvent from the fil trate to form said third fraction. 7. A. process as claimed in Claim 6 wherein. said solvent comprises acetone, 25 propan-2-0), ethyl acetate, hexane or troleum derivatives Pg. A process as described in Claim 7 wherein. anhydrous acetone is used as sol- vent, mixed with milkfat in the ratio of four 30 parts by weight of solvent to one part by Weight of milkfat, and the said first, second and third temperatures are respectively about 27°C, 22°C and 12°C. 9.” A process as claimed in any one of 135 Claims 610 8 which includes the steps of holding the solution for periods of time, at one or more of said temperatures, 10. A process as claimed in any one of Claims 6 fo 9 wherein said precipitates are 40 washed with solvent and the wash liquor Added to the filtrate before any next step is carried out thereon. LL. A process for produicing the fat com- ponent of a soft dairy spread according to ny one of the preceding’claims wan ele. 45 ted subseantaly ag herein described 12 prowis for produsing & sft dairy spread comprising the steps of taking a fat hmponent prepated according to ay" one St ho precelgg claims in whieh the weight 50 ratio of fraction one to fraction three is about 1:3, adding water, salt and solids—not isO and ning produce aft day PTB. A. process as claimed in Claim 12 55 wherein sal solide “not ft are denved from TRE ore mile product, 1M.” A proces for producing a sot dairy spread acdonling to Claim 12 ot Chim 1S when ced Subst" ag herein de 6) 5. A soft dairy spread comprising a fract of milkfat which is substantially solid at 20°C melting increasingly at highet ‘Smpeatares ened wits furor fraction 65 or peta yeh fe substantially bid at 0°C so that the ratio of liquid fat component to solid fat component remains substantially ceastnt wer ¢ tempers range of 3° {206 and mixed with ‘water, sal and 70 solids—not fat. Te. A soft dairy spread when produced by a process as claimed in any one of Claims iets nA soft, dary spread according: to Cian 13 or Casi 16 ten proauced sob Sanat sb ets deseo. NEW ZEALAND DAIRY RESEARCH INSTITUTE, 6 per: BOULT, WADE & TENNANT 34 Cursitor Street London EC4A 1PO Chartered Patent Agents Printed for Her Majesty's Stationery Office by The ‘Tweoddsle Press Tid., Berwick-upon-Tweed, 1977. Foblsed att “alent ‘fee, 23” Southampton "Being, London, WC2A TAY, ‘om which’ copies ‘may be obtain