DE2031165C3 - Process for the preparation of coating-forming wax emulsions - Google Patents

Description

The invention relates to a process for the production of coating-forming wax emulsions for oils Surface protection against corrosive influences during storage. Use and transport of metallic materials. Machines and years. in particular for the underbody protection of motor vehicles.

Such coating agents have been known for a long time. There are dispersions of waxes. Bitumen. Pitch and other plastic materials as well as their mixtures in solvents with different Solid hook and different consistency that are partly sprayable, partly applied manually have to. On the other hand, aqueous dispersions are also known in which the organic substance with the help are dispersed in water by emulsifiers or organic or inorganic protective colloids. These underbody protection agents can also be produced in different consistencies.

ίο Both groups of the aforementioned glazing agents have Disadvantage. The solvent-based coating agents have an intense and detrimental effect Odor and are either flammable - or if non-flammable solvents have been used - harmful to health or have a narcotic effect. There are therefore when processing this Products require special protective measures. Furthermore, it is necessary to apply the order surface, e.g. B. Carefully dry the underbody of a vehicle before application. They lead with rubber parts and seals for loosening the plasticizer and making it brittle quickly. Spray units and spray contamination on vehicles and the workplace are only allowed with solvents clean, with the risk of fire or a health impairment of the workforce again and again consists. In addition, these cleaning agents are indifferent to the vehicle paintwork must be relatively expensive. The drying

This coating agent can usually only process can be followed by scanning the treated areas.

The aqueous dispersions dry very slowly and are not suitable for bare iron parts because dry them up, showing signs of rust. Due to these rust phenomena, the protective film is insufficient adherent. Even with the coating agents of this group, the drying process must be controlled manually. In addition, there is no way to determine when the protective film will become waterproof has reached.

In addition, the aqueous dispersions are not sufficiently frost-proof. They are attempts carried out by adding water-soluble solvents such as low molecular weight mono-, Di- and tri-alcohols to achieve frost protection, but which have remained unsuccessful, since this addition as a result of increasing instability of the dispersions on so had to remain limited to small proportions that frost protection was insufficient.

The object of the present invention now exists therein, a process for the production of stable coating-forming, non-flammable wax emulsions to create that avoid the disadvantages of the known emulsions and are easy to process are. This includes good sprayability, among other things. Opacity and frost resistance.

This object is achieved according to the invention in that a mixture of bituminous Substances, hydrocarbon waxes, resins, oxidized Waxes may contain chlorinated paraffin Solid above the melting temperature of the mixture and then stirred homogeneously above its melting temperature an er

^ft 5 warmed mixture of amines, which can optionally / by part be replaced by ammonia, preferably by aminoir.ctlnlpropanol, diethylaminoiithanol and monoithanolamine and water in the

3 4

Weight ratio from 1: 1 to 1:10, preferably from 65 to 80 ⁰ C, according to DIN 51 180 and an acid number about 1: 7.5, offset from 0 to 150, preferably from 10 to 80 mg KOH / g at a minimum stirrer speed which has a Reynolds number in the range from 30,000 to ASTM D 465, these mixtures can be 150,000, preferably 44,000 to 120,000 guaranteed. Improvement of the adhesion to metallic surfaces is added that, after the subsequent addition of 5 surfaces, a chlorinated paraffin with a chlorine content of water of at least 90 ° C is below 40 to 70%, preferably 63 to 65%, after half the melting temperature of the mixture DIN 63 474 can be added. As an emulsifier, the ammonium salts from oxidized waxes are cooled to a temperature, preferably about 60 ° C, e.g. a stirrer speed is set that of oxidized montan wax with a solidification point of the Reynolds i ₀ , which ensures the emulsion stability, of 60 to 85 ° C according to DIN 51 556 and an acid number in the range from 30,000 to 150,000, preferably from SO to 160 mg KOH / g according to ASTM D 465 and from 44,000 to 120,000, depends on that subsequently used with the aforementioned volatile amines. The continued stirring to the batch a mixture of 15 emulsifier is formed during the manufacturing process up to 30%, based on the total weight, preferably of the dispersion.

about 16 to 20%, water-soluble alcohols, preferably 15 The mixture of bitumen, hydrocarbon isopropanol, and water in a weight ratio wax, resins, chlorinated paraffin and oxidized wax of at least 1: 1, preferably about 1.6: 1, is drawn in a stirred tank and one above and the batch is brought to room temperature by cooling and adding the temperature of the melting temperature of the mixture of water. temperature, the z. B. 110 to 120 ⁰ C, homo-

A health impairment at work was stirred. Then also above the

personals is not given. The dispersion can be heated to the melting temperature of the mixture

sprayed, brushed on or by dipping the mixture of the aforementioned amines and

parts to be treated are applied to the dispersion water in a weight ratio of 1: 1 to 1:10,

the, whereby the spraying is preferable, however, because preferably in a weight ratio of 1: 7.5,

due to the thixotropic setting of the dispersion one added as quickly as possible with stirring and still

on the other hand, low-air pressure spray units or spray units are stirred for about 15 minutes. The minimum speed of the

sufficient handguns and other hand uie dispersion stirrer, after emulsification for. "rforder--

Can also be applied in a thick layer, set borrowed Reynolds number. It will subsequently

without the fear of dripping. The dispersant about 90 ⁰ C hot condensate water added and

sion can be applied to parts that are still wet. Stirred for a further 15 minutes and the batch then

There are no signs of rust. Parts and seals quickly cool down to around 60 ° C,

rubber genes are not attacked. Contaminant- A mixture of isopropanol and water in the

on the vehicle, on the working scale: and on the weight ratio of 1: 1 to 2: 1, preferably

Spraying units can be very light and cost-effective, but in a weight ratio of 1.6: 1, with one

To save on cleaning or washing with water, the stirrer speed is 35 added to reduce the emulsion

the. In the gasoline separator of gas stations and the stability it depends on the Reynolds number.

The dispersion that has reached the plant is coagulated by the dispersion. The dispersion is cooled to room temperature

the existing excess water so quickly that and stir in a residual amount of cold water.

Wastewater pollution does not occur. The dispersion can also be produced in this way.

Through a combination of specially selected 40 organic solids added to the water at a higher temperature, a very low film temperature with a temperature of about 90 ⁰ C in two part formation temperature can be achieved, so that the steps are added (see embodiment 2).
Drying the dispersion and the beginning water _.,. .
Strength of the protective film slightly visually through an exemplary embodiment 1
Color change of the protective film from light brown to 45 The dispersion according to the invention has, for example, black that can be observed. have the following composition:

The solid of the dispersion consists of an Oewichisicile

Mixture of bituminous substances with hydrocarbons I. Standard bitumen B 200 according to DIN 1995

fabric waxes and resins. The bituminous substances are (softening point 37 to 44 "C) .... 7.0

Petroleum bitumina with a softening point (ring 50 microwax (solidification point

and ball) from 27 to 50 ^° C., preferably from 37 to 82 ^° C., penetration 8) 4.0

44 ° C, and a breaking point according to F r a a s s of - 15 Montanharz 5.0

to -20 "C or blown bitumina with an Er-Oxidized montan wax 3.0

softening point (ring and ball) from 80 to 90 ° C and chlorinated paraffin 1.0

a Fraass breaking point of -15 to 55 II. Diethylamine ethanol 1.5

-20 "C. The hydrocarbon waxes are 10.0

Asphalting of mineral oil distillation residues III. Condensate water 20.0

Hydrocarbon waxes obtained (so-called Pe- IV. Isopropanol 25.0

trolate) or condensate water obtained by de-oiling the petrolatum 15.0

Hydrocarbon waxes (so-called micro waxes), fio V. Condensate water 8.5

which can also be refined, with a solidification point of 40 to 95 ° C., preferably 65 to 85 ° C. In a heated stirred reactor with a diameter of 770 mm DIN 51 556 and a penetration at 25 C by knife with a cross bar stirrer of 400 mm 3 to 200, preferably from 6 to 70 according to DIN 51 579. Diameter is equipped. components I The resins are charged with these substances in the melt 65 and melted at 110 "C. Under Riihmischbarc Products, e.g. B. hydrocarbon resins. The homogeneous melt rises at 168 rpm Colophony resins and montan resins are cooled to 100 ° C, and the components II are Softening point of 40 to 140 C. preferably added, with a Reynolds number of about

\ 5,000 results. At the same speed r temperature with III ejn? Added of about 90 ^c C, and subsequent-3End Leaving the mixture to about 60 'C is cooled. Components IV and V are then added with further stirring.

Embodiment 2

The dispersion according to the invention has the following composition, for example:

Wichlsieile

I. Blown bitumen (softening point 80 to 90 ° C) 7.0

Microwax (freezing point

70 ° C, penetration 25) 3.0

Rosin resin 5.0

Oxidized polyethylene 3.0

Chlorinated paraffin 2.0

II. Diethylaminoethanol 1.5

Water 1.5

III. Water 30.0

IV. Water 17.0

V. Isopropanoi 18.0

Water 12.0

Manufacture example after outh
I. Solids content in 25.0 Weight percent .... 21.5 I.sopropanol content in 17.8 Weight percent ... 24.6 Expiry time after 4 DIN 53 211 (according to 33 sec. 10 hour storage) 28 sec. Expiry time after 4 DIN 53 2! I (immediately after vigorous 23 sec. Stir) 22 sec.

The advantages of the dispersions over the dispersions known per se for the intended use can be taken from the following numerical values.

Manufacture

Ϊ according to the example

45 _{| 0} drying time of

Dispersion
with a wet film thickness of 60 μ

with a wet film thickness of 100 μ

Freezing point of

Dispersion

Pour point of

Dispersion

Drying process

30 min.

60 min.

-18 C

-22'- C

40 min.

70 min.

-14 C

-20-

The components I are charged and melted at 120.degree. C. in a heated stirred reactor with a diameter of 1080 mm and equipped with a frame stirrer with a diameter of 1000 mm. While stirring at a stirrer speed of 88 rpm, the homogeneous melt is cooled to 95 ° C., and components II are added. ^{The mixture is then kept at about 90 °} C. for about 15 minutes, with continued stirring, and III is then added at a temperature of about 90 ^° C., resulting in a Reynolds number of about 120,000. With further stirring, IV is added and the mixture cooled to about 6O ⁰ C. Then the components V are mixed in.

The dispersions according to Examples 1 and 2 are light brown in color and completely homogeneous with ihixotropic inclination, as the following flow times show.

Water resistance of the
dried wax fihies

through color change before ·. -Light brown after] swan, recognizable

available immediately after the color change, the film can no longer be re-emulsified with water

The excellent properties of the protective film that is created by drying the dispersion and the make it suitable as an underbody protection agent can be seen from the following numerical values.

Melting point of
Wax film. ..

Temperature resistance of the wax film
(The wax film runs off the sheet metal) ....

Cold flexibility of the
Wax film
-35 ° C

Corrosion protection (salt spray chamber)

Stone chip resistance ...

Shareholding

according to embodiment I.

WC

given

at least 240 hours

80C

75 C

given

at least 240 hours

with a dry film thickness of I / O μ none Breakthroughs

Claims (5)

Patent claims: 1. Process for the production of coating-forming Wax emulsions, characterized in that a mixture of bituminous substances, hydrocarbon waxes, Resins, oxidized waxes and optionally chlorinated paraffin existing solid above the melting temperature of the mixture stirred homogeneously and this then above his Melting temperature a heated mixture of amines, optionally partially replaced by ammonia can be replaced, and water in a weight ratio of 1: 1 to 1:10 for one Minimum stirrer speed that has a Reynolds number im Range from 30,000 to 150,000, preferably 44,000 to 120,000, ensured, is added, that after the subsequent addition of water of at least 90 C, the approach to a below The temperature lying below the melting temperature of the mixture, preferably about 60 ° C., is cooled is set, a stirrer speed is set, which ensures the emulsion stability Reynolds number in the range from 30,000 to 150,000, preferably 44,000 to 120,000, depends on that subsequently with continued stirring the approach a mixture of 15 to 30%, based on the Total weight, preferably about 16 to 20%, water-soluble alcohols and water in a weight ratio of at least I: 1 and the batch by cooling and adding water is brought to room temperature. 2. The method according to claim 1, characterized in that that as amines aminomethylpropanol, diethylaminoethanol and monoethanolamine and used as the water-soluble alcohol is isopropanol will. 3. The method according to claim I or 2, characterized in that the heated. Amines and Mixture of water-soluble alcohol containing water, preferably in a ratio of 1: 7.5 with water, preferably in a weight ratio of 1.6: 1, is added. 4. The method according to any one of the preceding claims, characterized in that the mixture from bituminous substances, carbon hydrogen waxes, oxidized waxes and resins, chlorinated paraffin is admitted. 5. The method according to any one of the preceding claims, characterized in that according to the Addition of the mixture of amines and water added amount of water in two staggered periods Sub-steps, between which the batch is stirred, is supplied.