DE1617214A1 - Detergent and process for its preparation - Google Patents

Description

^ Patent attorneys

; Ing.A. van dor Werth

? S3 ^ 16172U

Dr. F. Lederor December 6, 1966

8Munich & lucUe-Grahn-Str. 22 _B>

UUILEVBR Ii ₉ V.
Rotterdam / Holland, Museum Park 1

Detergent and process for its preparation.

Priority: British patent application

IFr. 52153/65 of December 8, 1965.

The invention relates to improved finely divided soap-based and syndet-based detergents' with reduced tendency to slouch and improved Wettability, and methods of making them.

Soap products in finely divided form, for example spray-dried soap, spray-cooled soap, powdered or ground tires and soap granules, have a tendency to clump when water at temperatures above about 40 ^° C. is too hot. This probably occurs because the external parts, which are in direct contact with the hot water, melt and flow together, thereby enclosing dry particles and forming a gel-like mass that dissolves relatively slowly.This problem occurs very clearly with combinations, which have 4-0-60 <f » total fatty acid content, derived from mixtures of tallow and nut oils, eg coconut oil, palm kernel oil or peanut oil, or from their fatty acids, in the ratio of clay 75 to 100% * falg χ 25-0 * nut oil. Xn practice Zui _a maenkluaptn occurs on most, if powder is added to ehmaeehine dormant "Vftsser in a container or Wa *, and especially when laundering iat already in the water. The lumps often cling to the laundry after washing. Thus the lump does not only reduce the size of the lump

10 9 §01 / U 4

Cleaning and foaming power, but they also affect the appearance of the washed laundry. On the other hand, detergents based on syndets with a low content of soaps, especially those made from long-chain (fatty acids with ^ trsr ^/ Tf carbon atoms, show the disadvantage of insufficient wetting when added to water.

So far, attempts have been made in various ways to remedy this problem. For example, it has been proposed to increase the coconut oil content beyond the amount of the above-mentioned 25%. This is easily accomplished by incorporating more coconut oil or coconut oil fatty acids into the fat base before saponification or by mixing a soap made from a little coconut oil, ie one made from a fat base with less than 25% nut oil, with a soap rich in coconut oil. However, coconut oil soap is considerably more expensive than tallow soap and is also inferior at machine wash temperature. Other suggestions for reducing clumping have been to incorporate an alkali metal sulfonate into a silicate or carbonate-containing, spray-dried, granular soap product, or to coat the surfaces of the particles with glue, starch, or wetting agents. Another suggestion has been to use a saturated fatty acid with 8-H carbon atoms in the molecule in the flow state on silicate-containing soap particles in order to cause a reaction on the surface of the particles. Other proposals deal with changing the physical form of the product by forming the particles in special shapes, reducing the content of fine "in de" comminuted product or increasing the water content.

However, these earlier proposals have found no technical application

You invention now overcomes the shortcomings mentioned. BATH ORIGINAL

109808/1941

Dae erfindungsgemäfle powdery "saponaceous Detergena, the soap content is at most about 25J & Mtisölseife from Ko» _t iat characterized by cry additional content of at least 2 j C in saturated fatty acids with 5-11 carbon atoms in the molecule or the water-soluble salts "

In one embodiment, the invention the wettability of syndet-based detergents Improved with low soap contents from fatty acids with predominantly at least * 16 carbon atoms.

In another embodiment, the invention reduces the tendency to form lumps of finely divided Soap products.

In both cases this is done by homogeneously dispersing a saturated aliphatic carboxylic acid with a total of 5-11 carbon atoms in the molecule, or one of its alkali salts, through the entirety of the particles

The problem is in particular that soap powders are not enough with contents of less than 25Jl coconut oil soap or * the syndet powders mentioned · In such cases, a valuable reduction in lumps or · improvement of wettability through the dispersion of 2-10 wt. jfc (based on the total agent) from the acid or the salts are preserved

The invention can be applied to soap bases from 75-1OOj ( Sebum and 25-Oji Nuas Oil can be applied. she is suitable for soap bases rich in sebum, e.g. from 95 * tallow and 5 * coconut, palm kernel or peanut oil Dissolving, cleaning and foaming power of the oil is not adversely affected by the dispersion. The same goes for the addition to the syndet powders mentioned.

BATH ORIGINAL

10910 * 7194

Ί6Ί7Ζ1Λ

The soap products can be a non-soap detergent contain, e.g. an anionic, such as alkali alkylarylsulfonate, or a nonionic, e.g. a fatty acid alkali amide. All products can also contain the usual ingredients have, e.g. sodium tripolyphosphate, sodium silicate, Sodium carbonate, sodium sulfate, perfume, water, in the usual quantities *

Corresponding additives can also be present in the case of non-soap-based detergents; preferably such on a syndet basis with a very low content of soaps from long-chain fatty acids, i.e. fatty acids with over 18 carbon atoms. These powders show special the lack of poor wettability when added to warm water and this disadvantage is made by adding at least 2 # of fatty acids with 5-11 carbon atoms, or their water-soluble salts fixed

The fatty acids which can be used according to the invention are valeric, caproic, heptylic, caprylic, pelargonic, capric and undecylenic acids or mixtures thereof, or mixtures which predominantly consist thereof. Caprylic and pelargonic acids are particularly valuable. A suitable technical material is Emfac 1202 (Unilever Emery NV) which is a mixture of fatty acids, predominantly pelargonic acid, with the typical composition of 91% pelargonic acid, 5% caprylic acid, 4 % capric acid. This acid can, for example, be used individually or as an alkali salt, or in combination with other acids and their alkali salts.

Although coconut oil has already been suggested as a clumping reducing agent for soaps, show dl · named acids, which · constituents of coconut oil are surprisingly effective in comparison with the remaining acids in coconut oil to reduce the tendency to decrease lump

BATHROOM ORIGSMAL ■

109808/1948

The carboxylic acid or its salts can be added to the fat preparation before saponification or in the mixer in the usual process for the production of finely divided products.This process comprises saponifying the fat preparation, separating the resulting soap from the lower liquor, cleaning the precipitated soap and mixing it in Mixer with the other ingredients of the desired agent, e.g. sodium tripolyphosphate, alkaline sodium sulfate, syndet, etc. »The mixer mixture is thoroughly mixed, heated and then spray-cooled or spray-dried by spraying the molten mixture in a tower through which hot or cold air is passed. Perfume and other minor ingredients are added to the powder obtained, sieved and packaged. In the process according to the invention, it is undesirable to include the shorter-chain fatty acids in the fatty acids, because washing the soap can cause losses of these water-soluble acids Powders are preferred to maintain the powder alkalinity to a relatively high level This can be done by adding enough caustic soda to the mixer (at the same time as the acid is added) to completely neutralize the soap Solohjrf a process reduces the build-up of silica as the aging process occurs Powder.

The tendency to clump was measured by applying the following tests which are intentionally the Schleohtestmögliehe Wasehteohnik represent. There is no direct connection between the obtained Results from the two tests, but each test is an indication in itself of the effect of the additive on the tendency to clump

Wasohmasohin test.

This is carried out in a Simpson AD5 washing machine. The machine will be filtered with 14 gallons What atr like 125 ^{Ο Ϊ} and 31715 g (Q | 5 £ 14 gallons) de · to be tested Powders are halfway "wipe in a heap on the surface of fiührwelle and dtm

109808/1948 bad original

-6- 16172U

Container edge clogged. The stirrer will stop immediately switched on and allowed to run for one minute. The solution is then drained during 5 minutes ditched. The foam τοη the surface of the water is removed and the presence τοη floating lumps noted. The hose from another The AD5 machine or the inlet hose of a transfer pump will then go just below the surface of the water brought and removed the water from the testing machine. Am piece of gauze τοη about 10 stitches will be over the end the inlet tube held during this operation

When no more water can be removed τοη above, τοη the best heats up as much as possible . removed with the pump of the testing machine Any lumps on the sides or bottom of the empty machine are left undisturbed for 20 minutes, then collected and immediately weighed

This procedure weighs the lumps · All non-lumped * powder had ample opportunity to dissolve »

Cup test.

125 ml of water τοη 125 ⁰ P are poured into a 250 ml beaker and 5 g of the PulTermuster are added, which are brought to the center of the water surface in a heap. The contents of the beaker were left to stand for 15 seconds; then swirled for 15 seconds with a circular movement of the hand to ensure that all the powder is submerged.The contents of the beaker are then poured into another 250 ml beaker, the opening of which is covered with a slightly concave piece of copper gauze τοη about 10 meshes "The solid material is allowed to drain for 30 seconds and then immediately weighed"

The invention is further described in the examples, in which the given approaches are nominal are due to the reaction of an excess of fatty acid with an available alkali · BAD

109108/1141

example 1

A finely divided compilation of nominal values ▼ on 609t total fat (soap base derived from a fat ana ate τοη 95 ^ XaIg and 59 * coconut oil), 10.59 » alkaline sodium silicate, 5109 * sodium tripolyphosphate » 2.59 * sodium toluenesulfonate, 16.59 * water, was put into a Spray tower as control blown. Another Compilation where 5) 1 and 2.679 »of total fat τοη caprylic acid was shown in the same Blow way * clumping tests using the cup test showed:

Hit lump area weight (g)

control 6.5 4.1-8.5 59 * caprylic acid 0.03 0.00-0.06 2,679 * caprylic acid 0.7 0.1-1.0 Example 2

A finely divided compilation of the nominal amount τοη 57t4 ^ fatty acids (soap base from a fatty compound τοη 959 * tallow / 5Jt coconut oil), 11,19) »alkaline »Atrium silicate, 4» 34! * Satrlnstslpolyphoephat, 2,329 » Sodium toluenesulfonate, 24> 7! 59 * water and miscellaneous, as a control, and compilations which τοη the control by replacing the specified amount of fat component with caprylic acid, see were subjected to the machine and Becker lump test. The mean lump weights in grams were as follows

- machine - 2.0 cups Konirolle 28.0 6.5 5J * caprylic acid - 0.0 49 * caprylic acid 0.3 - 2,679 * caprylic acid 0.7 29 * caprylic acid Example 3

Butyric acid was incorporated as the carboxylic acid into a soap powder similar to that of the control in Example 2. This powder hardly shows any reduction in the tendency to lump, even if with the higher content τοη

109808/1948 bad

Butyric acid used. The cup clumping test gave the following values:

Control (as in Example 2) 6.5 1.6396 butyric acid 5.0

556 butyric acid 6.3

Similarly insignificant improvements in the tendency to clump of the soap powder of Example 2 with 2j6 myristic acid or 2 $> falmitic acid therein were noted.

Example 4

This example shows the comparative tendency of compilations to clump together in which finished Particles sprayed with a fatty acid according to FIG Invention, are compared with finished particles which have the same fatty acid homogeneously dispersed therein in the same amount by adding the acid to the fat base or to the mixer.

The particles dee control powder of Example 2 were sprayed with Zi »caprylic acid by heating 1500 g of powder to 14O ⁰ F in a closed vessel, followed by contacting in a 40 pound drum on a Hollmaschine · the engine has been started and the fatty acid was converted to the Drum sprayed with a household fly syringe. When the correct amount of acid was added, the drum was sealed and tumbled for 20 minutes. Three batches of powder were prepared.

The machine clumping tests were as follows:

Medium lump weight

control

■ it 2j> Caprylic acid sprays onto the particle surface

■ with gjf caprylic acid homogeneous the dispersed

34 , 3 34 , 5 45 , 6 ■ ORfG !TIMES β , 0 11 , 6 9 , 6 2 , 0 1 , 9 2 , 0 BATH

109808/1948

ο 16172U

The powders in this example had the following particle size distribution:

Retained by 22 meshes (British) 5 »Oj6

»» 60 "72.55 *

Passage through 60 ^M 22,

Example 5

Soap powder of nominal composition as follows were made by spray cooling:

(a) control (b) control

Fatty acids (soap based) as previously defined

Pelargonic acid Uatriumtrip olypho s phat 5.0

Alkaline urosodium silicate

Water and miscellaneous

Sodium carbonate lump weight (g)

Example 6

A finely divided composition as in Example 2 was used as a control in which 2 # and 3j6 pelargonic acid were entrapped by incorporation in the mixer. The machine clumping test gave the following Worth

Control 9.0 g mean lump weight

(a) with yfa pelargon

acid 0-0., 5

(b) with $ 1> pelargon

acid 2.0.

57.0 60 37.0 40.0 3.0 - 3.0 - at 5.0 5.0 - - 10.0 10.0 5.0 5.0 25.0 25.0 35.0 35.0 - - 20.0 20.0 0.5 28.0 0.2 8.0

Each of the powders with pelargonic acid was satisfactory after L <2 months
and sunlight

after 2 months of storage at 4 ° 0, room temperature, 37 ° O

09808/1

Belapiel 7 "

A soap powder of the following composition was made manufactured:

Sodium soap (anhydrous)

_auegedrück from Pettsäure 55.4) t ■

/ ale soap od ₉ da pelargonic acid 2.0 I * ¹ * ^öeire

Sodium hydroxide * ' Builders, 15.53 Water, salts, impurities 19.12 Additives (Einsonlies8Iioh Matrium-

toluenesulfonate) to 100

The clap and position tests were satisfactory

Example 8

itttüUU, a product of the following composition:

5 £ Na soap of hardened tallow fatty acid 10 i » alkylbenzenesulphonate

5Ji Honylphenol-10 B 0
4-0 i » ! Cripolyphosphate

5fi water glass
15 Ji sodium perborate

1? Ί OMO

3 ^ pelargonic acid

Remainder water, salts, brighteners

showed significantly better wettability when introduced into water than a corresponding product without Pelargonic acid additive

BATH ORIGINAL

109808/1941

Claims (1)

■ TCT72H -11 patent claims 1. Powdery, soap-containing detergent, the soap content of which consists of coconut oil soap up to a maximum of $ 25 , characterized by an additional content of at least 2% of saturated fatty acids with 5-11 carbon atoms in the molecule or their water-soluble salts 2. Methods for Improving the Wettability of Syndet-Based Detergents With Low Soap Levels from fatty acids with predominantly at least 16 carbon atoms, g e kennz e i c h η · t through an addition according to Claim 1 * 3. Method for reducing the tendency to clump in finely divided soap products which are up to 25S < Contain nut oil soaps, characterized that homogeneous through the particles a saturated aliphatic carboxylic acid is dispersed, which carbon atoms, single in the molecule of inggeeeat 5-11 contains or an alkali salt thereof, plus any acid (or salt) with 5-11 carbon atoms, which in the soap product due to the nut oil soap is available· 4. The method according to the preceding claims, characterized in that additional acid or salt is present in an amount of at least 2% (expressed as acid) by weight of the total agent » 5 · Method according to the preceding claims, characterized in that pelargonic acid as Addition is used « 6 · method according to the preceding claims, characterized i that caprylic acid 'is used · 7. Verfahr s according to the preceding claims, _{characterized in that e} »indicates that the additional 108801/194« 6AD ORIGINAL 16172H is added to a soap base. 8 ·! One-part soap products containing up to $ 25 nut oil soaps with through all of the particles homogeneously dispersed salt of a saturated aliphatic carboxylic acid with a total of 5-11 carbon atoms in the molecule, in addition to the salt derived from the nut oil component of the soap base an amount of 2-10% by weight of the soap product. 9β fine-particle soap products according to claim 8, in that the salt of pelargonic acid is used. 10. Compound soap products according to claim 8, characterized in that the Salt of caprylic acid is used. 109808/1946