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Technical Information LuwaxT OA Pastilles

TI/ES 1178 e
February 1994 (DFC)

Supersedes TI/P 2991 e dated April 1987

Emulsifiable polyethylene wax used to prepare wax emulsions for


industrial use.

Specialty Chemicals
Luwax OA Pastilles

Chemical nature Oxidized polyethylene wax

Properties
Test methods
DGF 1 DIN ASTM

Colour Off-white

Physical form Pastilles

Melting point °C 53736 D-2117 94 –104


(Microscope with heated stage)

Melting point (DSC) °C 51007 D-3418 94 –104

Congealing point °C M-III 4 a ISO 2207 D-938 90 – 97


(Rotating thermometer)

Dropping point (Ubbelohde) °C M-III 3 51801 D-566 101 –107

Penetrometer value at 23 °C dmm M-III 9 b 51579 D-1321 3–4

Ball hardness at 23 °C bar M-III 9 a 150 – 300

Acid number mg KOH/g M-IV 2 53402 D-1386 19 – 25

Saponification number mg KOH/g M-IV 2 53401 D-1387 30 – 50

Melt viscosity mm 2/s M-III 8 51562 D-2162 250 – 500

Density at 23 °C g/cm 3 M-III 2a 53479 D-792 ca. 0.96


1 Standard methods devised by the Deutsche Gesellschaft für Fettwissenschaft e. V, Münster.

The above information is correct at the time of going to press. It does not
necessarily form part of the product specification.

A detailed product specification is available from your local BASF


representative.

Storage The shelf life of Luwax OA Pastilles is virtually unlimited, provided they are
stored properly in their sealed original packaging.

Solubility The following table shows the “cloud point” of Luwax OA Pastilles, dissol-
ved in selected solvents at a concentration of 10 %. This is the tempera-
ture at which the wax just begins to precipitate out of solution on cooling.
The temperature at which it forms a clear solution is virtually the same,
depending on the rate at which it is heated.

Solvent Boiling point Cloud


of solvent ( °C) point ( °C)

Mineral spirits 140 – 200 ca. 63


Tetrachloroethylene 121 ca. 52
Toluene 111 ca. 56
Xylene 135.5 –141 ca. 58
Xylene/n-butanol (60 : 40) ca. 68

Miscibility The miscibility of Luwax OA Pastilles with the substances listed below was
determined by melting them and mixing them together in the ratios 9 :1
and 1: 9. The wax forms a homogeneous mixture with the following sub-
stances in molten and solid form.

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Carnauba wax
Fischer-Tropsch wax
Hard microcrystalline wax
Laropal ® K 80
Luwax E Flakes
Luwax LG Flakes
Luwax V Flakes
Montan wax, crude
Oppanol ® B 15
Oxidized microcrystalline wax
Paraffin wax
Plastic microcrystalline wax (Ozokerite)

Emulsification It is easy to prepare very stable emulsions from Luwax OA Pastilles.


Anionic emulsions are the most finely divided and, depending on the type
and quantity of amine soap used to emulsify them, they can be transpar-
ent to crystal-clear. Cationic and nonionic emulsions are less finely divided
and are milky white in appearance, but anionic-nonionic emulsions can be
prepared which are transparent. Emulsions of Luwax OA Pastilles, espe-
cially anionic and anionic-nonionic emulsions dry to form high-gloss films.

Preparing emulsions Because of the wax’s high melting point, the following method has to be
used to prepare emulsions at atmospheric pressure. The wax and emulsi-
fier are melted together at 120 –130 °C. The mixture is then poured into
the water in the form of a thin jet, and stirred vigorously. The water has to
be heated to as near to boiling point as possible. The dimensions of the
stirrer and the speed at which it rotates should be such that the water
forms a deep vortex. The hot wax can then be poured into the vortex to
prevent it from touching the stirrer or the sides of the vessel and forming
specks. Emulsifiers such as alkali hydroxides or acetic acid, etc., can also
be added to the hot water.

After all the wax has been added, the emulsion should be stirred for a fur-
ther 5 –15 minutes at 96 – 98 °C. It then has to be cooled to 40 – 50 °C as
quickly as possible, preferably by passing cold water through coils or a
jacket fitted to the vessel.

Generally speaking, emulsions with solids contents of up to 40 % can be


prepared from Luwax OA Pastilles. They are stable and pumpable at this
concentration. The viscosity of emulsions with a solids content of greater
than 40 % is too high for them to be handled at room temperature.

A less energy-intensive method is to prepare a concentrated emulsion with


a solids content of ca. 40 %, and then to dilute it down to its final
concentration with cold water.

Luwax OA Pastilles can also be emulsified under pressure in an autoclave.


However, it is easier to control the properties of the emulsion if the various
ingredients are added one at a time at atmospheric pressure.

Coemulsions can be prepared with other waxes such as paraffin wax,


microcrystalline waxes (hard, plastic or oxidized), montanic ester waxes
and carnauba wax.

Types of emulsion The following points are important when preparing emulsions of Luwax OA
Pastilles.

Anionic Emulsifiers: Salts of oleic acid or other long-chain fatty acids together with
high-boiling amines such as morpholine (b. p. 127 –130 °C),
diethylethanolamine (b. p. 160 –163 °C) and 2-amino-2-
methylpropanol (b. p. 165 –168 °C).

The wax and the oleic acid are melted together at 120 –130 °C. The mix-
ture is then stirred and cooled to 100 °C, during which time the amine
forms a salt. The mixture is then reheated to 120 –130 °C and poured into
the water.

Anionic-nonionic Emulsifiers: Ethoxylated fatty alcohols such as Lutensol ® AT 11, Lutensol


ON 70 or Lutensol TO 8, together with small quantities of
alkali hydroxide.

The alkali hydroxide forms a salt with the acid groups of the wax, which
makes it very easy to emulsify. The best method is to dissolve the

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hydroxide in the water. A slightly more transparent emulsion is obtained if
the hydroxide is added to the molten wax/emulsifier mixture, but the emul-
sion does not form a more transparent film on drying, and any benefits are
outweighed by disadvantages such as foaming, spitting and the formation
of specks.

If emulsions of this type are to be used for finishing textiles, small quan-
tities of highly ethoxylated fatty alcohols such as Lutensol AT 25 or
Emulan ® OC are usually added to improve their stability towards metal
salts such as magnesium chloride and zinc nitrate.

Cationic Emulsifiers: Salts of ethoxylated amines such as Lutensol FA 12 or Armo-


blen ® 110 1 and short-chain monocarboxylic acids such as
acetic acid.

The acetic acid is added to the water. A cationic emulsifier is formed when
the molten wax/amine mixture is poured in.

Nonionic Emulsifiers: Ethoxylated fatty alcohols such as Lutensol AT 25.

Some guideline formulations for preparing emulsions of Luwax OA


Pastilles are shown in the tables below.

Guideline formulations for preparing emulsions of Luwax OA Pastilles

Type of emulsion Anionic Cationic Non-


ionic

Formulation No. 1 2 3 4 5 6 7 8 9 10 11

Luwax OA Pastilles 13.0 20.0 13.0 20.0 2.6 10.0 22.4 20.0 20.0 20.0 20.0

Paraffin wax (m.p. 52 – 54 °C) 10.4 3.0

Oleic acid 2.0 3.5 2.0 2.5 2.0 2.0 4.8

Diethylethanolamine 3.0 3.5 3.0 3.0

Methylpropanolamine 3.0

Morpholine 3.5

Ammonia, 25 % 7.2

Lutensol AT 25 4.2

Lutensol FA 12 4.0

Armoblen 110 1 4.0 6.0

Acetic acid, 10 % 0.6 0.6

Lactic acid 0.1

Hot water (96 –100 °C) 82.0 73.0 82.0 74.0 82.0 82.0 75.4 75.4 73.9 60.0
+15.8

Water – 1st increment 17.2

Water – 2nd increment 48.4

Notes Prepared at atmosheric pressure 4 bar Prepared at atmosheric pressure

Transmission
(%, 1: 400, 533 nm) 96.3 90.0 89.2 43.7 00.0 92.1 52.9 10.4 32.5 74.0 00.0

pH at room temperature 10.3 10.5 10.4 9.2 10.0 10.1 10.4 4.8 6.3 6.7 3.5

Viscosity
(sec, 4 mm flow cup) 11.0 12.3 11.6 15.3 11.4 11.3 13.2 11.2 11.6 13.1 10.6

1 Supplied by Akzo Chemicals

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Type of emulsion Anionic-nonionic

Formulation No. 12 13 14 15 16 17 18 19 20 21 22

Luwax OA Pastilles 25.0 25.0 25.8 20.0 23.0 20.0 8.0 16.4 11.0 14.0 30.0

Hard microcrystalline
wax (m. p. 68 – 80 °C) 18.0

Paraffin wax (m. p. 52 – 54 °C) 16.4 7.0 6.0

Potassium hydroxide soln.,


50 % 0.8 0.8 0.6 0.7 0.7 0.9 0.3 0.2

Potassium hydroxide, solid 0.5 0.4 1.0

Lutensol AO 8 6.0 3.0

Lutensol AO 10 3.0

Lutensol TO 8 8.5

Lutensol ON 70 4.0 7.0 9.0

Lutensol AT 11 3.0 6.0 6.5 9.0

Lutensol AT 25 1.2

Lutensol AT 80 0.3

Emulan® OC 6.0

Ethylene glycol 0.7

Sodium metabisulfite 0.2 0.3

Hot water (96 –100 °C) 68.2 68.2 65.0 75.4 69.9 74.8 67.3 59.8 72.7 72.8

Cold water 59.7

Notes Prepared at atmospheric pressure 2 bar

Transmission
(%, 1: 400, 533 nm) 31.6 49.6 84.1 66.8 3.9 52.8 0.0 0.0 83.4 5.4 34.9

pH at room temperature 8.6 8.6 9.5 8.7 8.0 9.4 12.4 11.1 7.7 7.1 9.9

Viscosity 17.7 20.0 29.3 10.9 11.9 12.8 13.7 Viscous 15.2 11.7 126.0
(sec, 4 mm flow cup) Viscous

Applications
Floor polishes, leather polishes Emulsions prepared from Luwax OA Pastilles, especially anionic and
anionic-nonionic emulsions, dry to form tough, glossy films which can be
used to protect a variety of substrates. Luwax OA Pastilles perform well in
dry-bright emulsion-type polishes. Coemulsions with montanic ester
waxes, carnauba wax, microcrystalline wax and paraffin wax can also be
prepared if necessary. Solvents such as mineral spirits can also be added
in special cases.

Solvents such as mineral spirits and solvent naphtha can be added to car
polishes and furniture polishes in order to provide an added cleaning
effect. Silicone oils improve the gloss, buffability and toughness of
protective films.

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Furniture polish 5.0 Luwax OA Pastilles ü
3.0 Luwax S Flakes ý (1) 100 °C
1.0 Oleic acid þ
5.0
45.0
Silicone oil (1000 mm 2/s)
Solvent naphtha (b. p. 100/140 °C) % (2)
1.0 Diethylethanolamine (3)
40.0 Water (80 °C) (4)

Automotive wax 25.0 Cationic wax emulsion 1 (1)


(for car washes) 25.0 Water (2)
5.0 Diethylene glycol monobutyl ether (3)
1.5 Emulan OC (4)

Mix (1) and (2), and then heat (3) and (4) until a liquid mixture is formed.
Slowly stir (3) and (4) into (1) and (2) at room temperature. The emulsion
remains stable for several days.

Leather polish 16.0 Luwax OA Pastilles ü


6.0 Paraffin wax (m.p 52 – 54 °C) ï
4.0 Oleic acid ý (1) Emulsion:
5.0 Diethylethanolamine ï Add wax to water
69.0 Water þ
2.0 Collacral ® PU 85
2.0 Silicone oil AK 35 % Stir into (1)

Shoe polish Finely dispersed wax shoe polishes that form a very flexible, high-gloss
film can be prepared from anionic-nonionic emulsions of Luwax OA Pastil-
les and Poligen ® MA. Cationic emulsions of Luwax OA Pastilles are more
resistant to water.

53.2 Water
5.3 Isopropanol
3.0 Diethylene glycol monoethyl ether
1.5 Palatinol ® C
2.0 FC 129, (1%)
15.0 Poligen MA
20.0 Cationic wax emulsion 1

Textile finishing Anionic-nonionic, cationic and nonionic emulsions of Luwax OA Pastilles


are used in textile finishing, often in combination with paraffin wax. They
impart a smooth, soft, full handle to fabrics such as cotton and linen, and
they increase the fabrics’ water repellancy. They can be added to crease-
resistant resin finishes to improve their abrasion resistance, sewability and
tearing resistance. Emulsions of this type can also be used to reduce the
susceptibility of fabrics to soiling and improve their washability and water
resistance, especially if the emulsions have a low emulsifier content.

In textile applications, it is very important that wax emulsions are resistant


to electrolytes and salts that act as catalysts. The resistance of anionic-
nonionic emulsions of Luwax OA Pastilles to 5 % solutions of ammonium
dihydrogen phosphate, zinc nitrate and magnesium chloride at 20 °C is
particularly good.

Other applications Emulsions prepared from Luwax OA Pastilles and large proportions of par-
affin wax dry to form tough, water-repellent films. These have a variety of
applications.

Formwork emulsions

Emulsions of Luwax OA Pastilles can be applied to wooden and metal


forms for concrete. They have the advantage over oils that they do not
penetrate into the concrete, which causes problems when renderings and
finishes are applied.

Water repellants for particle board

Wax emulsions are added to the adhesives used to bind particle board to
prevent particles of wood from absorbing moisture and swelling.

1 See Formulation No. 8 on page 4

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Temporary protective coatings for metal

Emulsions can be applied to new cars and machine parts, etc., to protect
them from corrosion during transport and storage.

Size for paper

Applied to paper in the size press, emulsions of this type give improved
water resistance, smoothness and gloss.

Food-contact legislation The composition of Luwax OA Pastilles conforms to the the recommenda-
tions issued by the German Bundesgesundheitsamt listed in the following
table.

BGA Approved
Recommendations

I Lubricants for plasticized high polymers Up to 3 %


and for special plasticized PVC film used
to wrap fresh meat

II Lubricants for rigid PVC Up to 3 %

V Slip agents and mould release agents Up to 3 %


for polystyrene

VI Slip agents for copolymers and graft Up to 3 %


polymers of styrene and mixtures of
polystyrene and other polymers

German Citrus fruit Up to


additives 140 mg
legislation per kg
of fruit

The composition of Luwax OA Pastilles also conforms to the requirements


of the following paragraphs of legislation administered by the United
States FDA.

FDA, Title 21 CFR

175.105 Adhesives
176.200 Defoaming agents used in coatings
176.210 Defoaming agents used in the manufacture of paper
and paperboard
177.1210 Closures with sealing gaskets for food containers
177.1390 High-temperature laminates
177.2600 Rubber articles intended for repeated use
178.3120 Animal glue

The following paragraphs also apply if the acid number of the wax is less
than 19 mg KOH/g.

172.260 Oxidized polyethylene


175.125 Pressure-sensitive adhesives
175.300 Resinous and polymeric coatings
175.320 Resinous and polymeric coatings for polyolefin films
175.350 Vinyl acetate/crotonic acid copolymer
176.170 Components of paper and paperboard in contact with
aqueous and fatty foods
176.180 Components of paper and paperboard in contact with dry
food
176.300 Slimicides
177.1200 Cellophane
177.1400 Hydroxyethyl cellulose film, water-insoluble
177.1620 Polyethylene, oxidized
177.2800 Textiles and textile fibers
177.2910 Ultra-filtration membranes

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Safety
We know of no ill effects that could have resulted from using Luwax OA
Pastilles for the purposes for which they are intended and from processing
them in accordance with current practice.

According to the experience we have gained over many years and the
other information at our disposal, Luwax OA Pastilles do not exert any
harmful effects on health, provided they are used properly, due attention is
given to the precautions necessary for handling chemicals, and the infor-
mation and advice given in our Safety Data Sheet is observed.

Note
The information submitted in this publication is based on our current
knowledge and experience. In view of the many factors that may affect
processing and application, these data do not relieve processors of the
responsibility of carrying out their own tests and experiments; neither do
they imply any legally binding assurance of certain properties or of suit-
ability for a specific purpose. It is the responsibility of those to whom we
supply our products to ensure that any proprietary rights and existing laws
and legislation are observed.

BASF Aktiengesellschaft
Marketing Spezialchemikalien I
Printed in Germany

67056 Ludwigshafen
Rahmenrezepturen für die Emulgierung von Luwax OA Pastillen

Komponenten/ anionisch kationisch nicht-


Emulsionstyp ionisch

Formulierung Nr. 1 2 3 4 5 6 7 8 9 10 11

Luwax OA Pastillen 13,0 20,0 13,0 20,0 2,6 10,0 22,4 20,0 20,0 20,0 20,0

Paraffin (52/54) 10,4 3,0

Ölsäure 2,0 3,5 2,0 2,5 2,0 2,0 4,8

Diethylethanolamin 3,0 3,5 3,0 3,0

Aminomethylpropanol 3,0

Morpholin 3,5

Ammoniak, 25 %ig 7,2

Lutensol AT 25 4,2

Lutensol FA 12 4,0

Armoblen 110 4,0 6,0

Essigsäure 10 %ig 0,6 0,6

Milchsäure 0,1

Wasser, heiß (96 –100 °C) 82,0 73,0 82,0 74,0 82,0 82,0 75,4 75,4 73,9 60,0
+15,8

Wasser I 17,2

Wasser II 48,4

Bemerkungen Drucklose Emulsionen 4 bar Drucklose Emulsionen

LD-Wert (1: 400, 533 nm) 96,3 90,0 89,2 43,7 00,0 92,1 52,9 10,4 32,5 74,0 00,0

pH-Wert (RT) 10,3 10,5 10,4 9,2 10,0 10,1 10,4 4,8 6,3 6,7 3,5

Viskosität (Ford, 4 mm) 11,0 12,3 11,6 15,3 11,4 11,3 13,2 11,2 11,6 13,1 10,6
Komponenten/Emulsionstyp anionisch-nichtionisch

Formulierung Nr. 12 13 14 15 16 17 18 19 20 21 22

Luwax OA Pastillen 25,0 25,0 25,8 20,0 23,0 20,0 8,0 16,4 11,0 14,0 30,0

Mikrohartwachs (Fp 68 – 80 °C) 18,0

Paraffin (52/54) 16,4 7,0 6,0

KOH 50 %ig 0,8 0,8 0,6 0,7 0,7 0,9 0,3 0,2

KOH, fest 0,5 0,4 1,0

Lutensol AO 8 6,0 3,0

Lutensol AO 10 3,0

Lutensol TO 8 8,5

Lutensol ON 70 4,0 7,0 9,0

Lutensol AT 11 3,0 6,0 6,5 9,0

Lutensol AT 25 1,2

Lutensol AT 80 0,3

Emulan OC 6,0

Ethylenglykol 0,7

Natriumdisulfit 0,2 0,3

Wasser, heiß (96 –100 °C) 68,2 68,2 65,0 75,4 69,9 74,8 67,3 59,8 72,7 72,8

Wasser kalt 59,7

Bemerkungen Drucklose Emulsionen 2 bar

LD-Wert 31,6 49,6 84,1 66,8 3,9 52,8 0,0 0,0 83,4 5,4 34,9

pH-Wert 8,6 8,6 9,5 8,7 8,0 9,4 12,4 11,1 7,7 7,1 9,9

Viskosität 17,7 20,0 29,3 10,9 11,9 12,8 13,7 viskos 15,2 11,7 126,0
(viskos)
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