EP2875114B1 - Procédé de préparation de composition de savon dans un mélangeur de soc - Google Patents

Procédé de préparation de composition de savon dans un mélangeur de soc Download PDF

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Publication number
EP2875114B1
EP2875114B1 EP13729376.7A EP13729376A EP2875114B1 EP 2875114 B1 EP2875114 B1 EP 2875114B1 EP 13729376 A EP13729376 A EP 13729376A EP 2875114 B1 EP2875114 B1 EP 2875114B1
Authority
EP
European Patent Office
Prior art keywords
soap
bars
moisture
added
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
Application number
EP13729376.7A
Other languages
German (de)
English (en)
Other versions
EP2875114A1 (fr
Inventor
Anal PUSHKARNA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Priority to EP13729376.7A priority Critical patent/EP2875114B1/fr
Publication of EP2875114A1 publication Critical patent/EP2875114A1/fr
Application granted granted Critical
Publication of EP2875114B1 publication Critical patent/EP2875114B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00Making of soap or soap solutions in general; Apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047Detergents in the form of bars or tablets
    • C11D17/006Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar

Definitions

  • the present invention relates to the field of making soap bars, particularly to a process for making high-moisture soap bars using ploughshare mixers.
  • Conventional toilet soaps generally include predominantly soap (e.g., >70 % TFM, Total Fatty Matter), 10 to 13 % water and the usual additives (e.g., soda, salt, dyes and perfumes). These bars are typically produced by mixing soap and/or other synthetic surfactants with useful additives, followed by milling, plodding and stamping. Soap bars are produced on a commercial scale by two well known processes; a comparatively newer ploughshare mixer (PSM) process and a relatively older crutcher/Mazzonni/ Spray drier process.
  • PSM ploughshare mixer
  • Drying on a commercial basis is achieved by several different methods.
  • One procedure employs a water-chilled roll in combination with a second feed roll to spread molten, neutralized soap into a thin, uniform layer.
  • the cooled soap is then scraped from the roll to form chips and dried to a specific moisture level in a tunnel dryer.
  • Soap chips already having a low moisture level are further dried by repeatedly conducting the chips through close-set water cooled steel rolls (i.e., three-roll mill) in the procedure known as milling, which has been already described.
  • a modern technique for the drying of soap is known as spray drying. This process directs molten soap to the top of a tower via spray nozzles.
  • Process related problems include production of soft soap mass which is difficult to mill, plod and stamp. For these reasons, the soap bars sold in some countries generally contain only 12 to 13 % moisture.
  • CN1182789A discloses a process for producing a high moisture laundry bar having improved firmness.
  • the process comprises preparing a premix of 75 to 90% neat soap, 3 to 20% added water, 1 to 10% electrolyte salt and forming the mixture into a shaped bar.
  • the premix that is prepared in accordance with this disclosure contains pre-saponified soap which is mixed with water to further make bars.
  • the ploughshare mixer is very commonly used in processes requiring granulation of detergent powders and to produce powders by dry neutralisation. Typically, the ploughshare mixer does the following tasks in the powder mixing process; mixing of ingredients, agglomeration and de-agglomeration of particles, unification of the mean particles sizes and layering of material. Until recently, such mixers were not used for making soap bars.
  • a typical plough share mixer is primarily designed for powder mixing but is also an efficient mixer for soap saponification at moisture content of 15 % to 20 %.
  • EDTA ethylene di-amine-tetra acetic acid
  • EHDP 1-diphosphonate
  • Viscosity of saponified mass is generally 80,000 to 100,000 cP (at 25°C). This viscosity is necessary for downstream processing. However, when an attempt was made to increase the moisture content of the mass by addition of water, the viscosity of the saponified mass reduced. For example, in order to get soap noodles having 24 % moisture, when necessary amount of added water was added to the mixer, the resultant mix was found to have a viscosity of about 4000 to 10,000 cP.
  • added water is used to distinguish this water from the water of neutralisation which is generated in-situ when distilled fatty acids are saponified with an alkali.
  • Some ingredients such as caustic soda also contain water.
  • a holding tank can be fitted between the plough share mixer and the chilled rolls.
  • the tank helps in ensuring a steady supply of saponified mass to the chilled drum in a controlled manner.
  • installation of such holding tanks is not possible in all manufacturing set-ups because in some factories, there is not much space between the mixer (PSM) and the chilled rolls. Installation of holding tanks also involves capital expenditure.
  • a further problem with holding tanks is that it is difficult to synchronise the speed at which the holding tank is emptied with a typical PSM batch cycle time which is 20 to 30 minutes. Many times it may so happen that the holding tank has only partially emptied but the next batch of saponified mass is ready for further processing.
  • the PSM process is generally not considered suitable for making soap bars with higher moisture content (generally 20 % or more).
  • saponified mass having about 30 % moisture is dried down to about 14 to 17 % moisture.
  • This is achieved by raising the temperature of neat soap from 90 to 95°C to 140 to 145°C by passing through a heat exchanger/heat exchangers followed by spray-drying under vacuum (approximately 100 mm Hg pressure).
  • This process is generally not recommended for making soap bars with more than 20 % moisture. The reasons have been explained earlier.
  • At least 80 % of added water is added before 80% saponification. Most preferably all of the added water is added before 80% saponification.
  • Preferred electrolytes include sodium halides especially sodium chloride, potassium halides especially potassium chloride and lithium halides, especially lithium chloride.
  • Other less preferred electrolytes include nitrates, nitrites, sulphate, sulphites, chlorates, carbonates, bicarbonates and acetates of sodium, potassium or lithium. It was observed that direct addition of sodium sulphate to the mixer as a solid (solid dosing) had a limitation. Addition of excess sodium sulphate in this form lead to products (soap bars) which showed crystal growth on storage. Such a phenomenon is not desirable.
  • the soap composition has at least 20 % moisture. More preferably, moisture content of the soap composition is 20 % to 32 %, preferably 22 to 30 % and most preferably 24 % to 26 %. Moisture content can be determined by any means, such as by drying at 105°C. It is preferred that free alkali content of the noodles is 0.01 % to 0.1 %. It is preferred that Iodine value of the soap composition is 30 to 60 g l 2 /100 g, more preferably 35 to 50 g l 2 /100 g and most preferably 40 to 45 g l 2 /100 g.
  • the soap composition so formed is generally further processed.
  • the soap base is in the form of a viscous liquid which is dried and plodded into homogenized noodles or chips.
  • the soap noodles/chips are then processed into finished products such as bars/tablets.
  • the process disclosed herein is used for making soap composition.
  • a particularly preferred form of the soap composition is bars.
  • Another preferred form is noodles or chips.
  • the process disclosed herein is for making milled and plodded soap compostion in the form of bars or noodles, or the like. This process is unsuited for making framed bars, or freezer bars or melt-cast soap bars.
  • Milling is meant the homogenization of the soap in the sense of eliminating granules of abnormal size and hardness contained in soap paste, thus making it uniform and of a very fine grain by touch.
  • Soap milling can be effected either by making the material pass through mesh nets by successive extrusions (a relatively modem process) or by making it pass through successive rolling cylinders having different peripheral speeds (a traditional process). Milling involves feeding pressurized soap continuously from a chamber and under pressure into a nip of adjustable dimensions.
  • the nip is formed between a pair of rolls counter-rotating at different peripheral speeds and detaching milled soap from the rolls.
  • the aim of this experiment was to find out the effect of addition of timing of added water at different stages (2 stages).
  • an identical formulation was processed in two ways. In the first case, all of the added water was added to saponified mass (i.e. after 100 % saponification step was over) and in the second case, equal quantity of water was added simultaneously with the addition of fatty acids and caustic soda, i.e. before saponification. In the second case, all of sodium chloride was added along with the water. The fat charge of non-lauric to lauric soaps was fixed at 85/15, the Iodine value was in the range of 38 to 43 g/100 g.
  • the Total Fatty Matter of resultant soap composition in noodle form was 50 wt%.
  • Table 1 Ingredient Wt % Sodium soap 54.0 Sodium chloride 0.6 Primary alkyl sulphate 4.2 Talc 10.0 Perfume 1.0 Glycerin 6.0 Sodium sulphate (100%) 1.5 Moisture 21.4 Total including minors to 100
  • Table 2 a formulation sheet is shown for a batch size of 1650 kg, which (after processing) gives the soap noodles with the composition of Table 1.
  • Table 2 Ingredient/raw material kg Sodium chloride 12 Distilled fatty acids blend 1000 Caustic soda (48 % strength) 330 Glycerin 120 Sodium Sulphate (25 % solution) 120 Water added 55 Other minors 10
  • the sodium chloride was added into an empty PSM mixer. Then the chopper and the plough were started. The fatty acids and caustic soda were added together next, followed by glycerine, water and sodium sulphate. This step of addition of the fatty acids to the sodium sulphate lasted for 12 minutes. Thereafter, the minor ingredients were added in about 1 minute. The contents were mixed for 10 minutes.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Claims (7)

  1. Procédé de fabrication d'une composition de savon broyée et extrudée présentant au moins 20 % en masse d'humidité, ledit procédé comprenant une étape de saponification d'huile ou d'acides gras en présence d'eau ajoutée, dans lequel au moins 60 % d'eau ajoutée sont ajoutés avant ou simultanément avec ladite saponification.
  2. Procédé selon la revendication 1, dans lequel au moins 80 % d'eau ajoutée sont ajoutés avant une saponification à 80 %.
  3. Procédé selon la revendication 2, dans lequel la totalité de l'eau ajoutée est ajoutée avant une saponification à 80 %.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel ladite saponification est réalisée en présence d'un électrolyte présentant un ion commun avec le savon qui est formé.
  5. Procédé selon l'une quelconque des revendications précédentes, dans lequel ladite saponification est réalisée dans un mélangeur à soc.
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel ladite composition est dans la forme de barres.
  7. Procédé selon l'une quelconque des revendications 1 à 5 précédentes, dans lequel la composition est dans la forme de nouilles ou de chips.
EP13729376.7A 2012-07-23 2013-06-18 Procédé de préparation de composition de savon dans un mélangeur de soc Not-in-force EP2875114B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13729376.7A EP2875114B1 (fr) 2012-07-23 2013-06-18 Procédé de préparation de composition de savon dans un mélangeur de soc

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
IN2105MU2012 2012-07-23
EP12184952 2012-09-19
PCT/EP2013/062599 WO2014016055A1 (fr) 2012-07-23 2013-06-18 Procédé de préparation d'une composition de savon dans un outil de malaxage ploughshare®
EP13729376.7A EP2875114B1 (fr) 2012-07-23 2013-06-18 Procédé de préparation de composition de savon dans un mélangeur de soc

Publications (2)

Publication Number Publication Date
EP2875114A1 EP2875114A1 (fr) 2015-05-27
EP2875114B1 true EP2875114B1 (fr) 2016-03-02

Family

ID=48628710

Family Applications (1)

Application Number Title Priority Date Filing Date
EP13729376.7A Not-in-force EP2875114B1 (fr) 2012-07-23 2013-06-18 Procédé de préparation de composition de savon dans un mélangeur de soc

Country Status (5)

Country Link
EP (1) EP2875114B1 (fr)
BR (1) BR112015000666A2 (fr)
ES (1) ES2574602T3 (fr)
IN (1) IN2015MN00099A (fr)
WO (1) WO2014016055A1 (fr)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
HU215484B (hu) 1990-11-26 1999-01-28 Procter And Gamble Co. Semlegesített karbonsavak háromdimenziós, összefonódó hálózatából álló rideg, formázott, szilárd tisztító formatest, és eljárás előállítására
AU5605396A (en) 1996-06-20 1998-01-08 Procter & Gamble Company, The Process for manufacture of high moisture soap-based laundry bars
US6440908B2 (en) 1999-11-30 2002-08-27 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. High moisture retaining bars compositions comprising borax as water structurant
WO2002046341A2 (fr) 2000-12-05 2002-06-13 Unilever N.V. Composition detergente solide non granulaire et son procede de fabrication

Also Published As

Publication number Publication date
WO2014016055A1 (fr) 2014-01-30
ES2574602T3 (es) 2016-06-21
IN2015MN00099A (fr) 2015-10-16
BR112015000666A2 (pt) 2017-08-08
EP2875114A1 (fr) 2015-05-27

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