A method for producing powder thermosetting composition

 

(57) Abstract:

The invention can be used for corrosion protection of various metal structures. How is that a composition obtained by mixing epoxy oligomer, curing agent, curing accelerator, pigments, fillers and diphenylolpropane as the target additives. The combination of components in a certain ratio and the sequence of their introduction increases the glass transition temperature of up to 10oAnd sheen covering up to 10%. 1 C.p. f-crystals, 6 ill.

The invention relates to the field of development of coatings based on thermosetting powder compositions used for corrosion protection of various metal structures, including industrial and domestic refrigerators, microwave ovens, medical equipment, building construction, oil and gas, metal furniture, radiators, gas stoves, spare parts, etc.

The composition obtained by the above method, designed for applying electrostatic, triboelectric, flame methods of deposition, and deposition in a fluidized bed.

Known powder composition for pokrytiya oligoether, fillers, pigments and additives purpose (the agents for improving the filling, protivokrazhnye agents, agents for improving the filling, and many others). The coating on the basis of this composition has an almost complete set of physico-chemical and mechanical properties that meet the varied demands of consumers coating, however the appearance of this coating is of low quality because of the relatively weak gloss (about 70-75% when the angle of incidence 60o), and has a relatively low softening temperature (glass transition Tc), the method of differential scanning calorimetry (DCK), covering 68-70othat limits the operational capabilities of the coating at elevated temperatures (radiators, gas stoves, building construction, automotive parts and others).

In addition, a method of obtaining powder thermosetting composition for coating carried out by mixing in the melt (extrusion) epoxy oligomer, curing accelerator, pigments, fillers and special additives, curing agent [2].

The coating on the basis of this epoxy composition has a relatively high physical-mechanical and chemical charactera coverage. However, this softening temperature is not the limit for this type of coating (epoxy). Also leaves much to be desired and the rate of gloss 69-70% at an angle of inclination of the light beam 60o.

The aim of the invention is to increase the softening temperature (glass transition Tc) of the cured coating while enhancing Shine of its surface.

This objective is achieved in that in the process of preparation (dry mixed raw components) powder (epoxy or epoxy-polyester) composition in its composition is administered 0.001 to 0.1 mol of diphenylpropane (bisphenol A) 1 mol of epoxy oligomer. The use of this monomer connection allows the first stage curing of the powder composition to improve its spill due to the low molecular weight of DMF, which ultimately leads to an increase of gloss on average from 0 to 10%, and in the second stage of the curing process allows to increase the molecular weight of the coating, which ultimately leads to an increase of the glass transition temperature of the cured under the same conditions (temperature and time) coatings on average from 0 to 10oC.

The proposed method is the W components) in its composition is administered from about 0.001 to 0.1 mol of diphenylolpropane on 1 mol of epoxy oligomer. Then an integral part of the composition pereshivayut, ekstragiruyut at a temperature of 100-130oC, cooled and crushed in accordance with the classical method of obtaining powder compositions.

Example 1. The recipe given in the book by A. D. Yakovlev "Powder paint" [2].

The temperature-time regime of the curing composition: 220oC - 40 minutes

The glass transition temperature Tc= 91oC (Fig. 1).

Example 2. Prigotavlivaemy epoxy-polyester (hybrid) composition of the following composition, wt.1:

Epoxy oligomer with amoxicillinum weight of from 500 to 1200 g, for example, brands GT E-7004 (Ciba-Geigy), Switzerland, E 3003 or E-3004 (Shell), England, and D. E. R. 663, 664 (DOW), the USA and other similar type 200-400.

Carboxyl-containing saturated oligomer with acid number 45-85, for example, Crylcoat 380, 370, 314, 316 (UCB), Belgium, Uralac 5980 P, P 5981 (DSM), the Netherlands or other similar type - 400-200.

Titanium dioxide rutile form R-TC4 (Tioxide), England, 2160, 2310, 2200 (Kronos), Germany, R-902 (Dupont), USA, and other similar type - 275.

Additive for filling, for example, BYK 365P or 366P (BYK Chemic), Germany, Resiflow P-88, PV-88, PV-5 (Worlee), Germany or other similar type - 10.

Benzoin (DSM), the Netherlands (BASF), Germany and others-time mode of curing of the composition: 160oC - 20 minutes

The glass transition temperature Tc= 69oC (Fig. 2).

Example 3. Epoxy powder composition Beckrymix D112-508 firm "Herberts" unknown composition.

The temperature-time regime of the curing composition in accordance with the mode specified in specification: 180oC-12 minutes (see Fig. 3).

The glass transition temperature Tc= 96,2oC.

Example 4. In the composition of example 1 are added in the course of its preparation of 0.001 mol diphenylpropane (Suite) per 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 1.

Example 5. In the composition of example 1 are added in the course of its preparation of 0.005 mol DMF) per 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 1.

The results of measurements of Tcand gloss of the coating shown in Fig. 4.

Example 6. In the composition of example 1 is added during cooking, 0.01 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 1.

The results of measurements of Tcand gloss coating provides * epoxy oligomer.

The temperature-time regime of the curing composition as described in example 1.

The results of measurements of Tcand gloss of the coating shown in Fig. 4.

Example 8. In the composition of example 1 are added to the cooking process to 0.1 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 1.

The results of measurements of Tcand gloss of the coating shown in Fig. 4.

Example 9. In the composition according to example 2 are added in the preparation of 0.001 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 2.

The results of measurements of Tcand gloss of the coating shown in Fig. 5.

Example 10. In the composition according to example 2 are added in the preparation of 0.005 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 2.

The results of measurements of Tcand gloss of the coating shown in Fig. 5.

Example 11. In the composition according to example 2 are added in the preparation of 0.01 mol Suite 1 mol of epoxy oligomer.

Temperature-Veska cover shown in Fig. 5.

Example 12. In the composition according to example 2 are added in the cooking process of 0.05 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 2.

The results of measurements of Tcand gloss of the coating shown in Fig. 5.

Example 13. In the composition according to example 2 are added in the preparation of a 0.1 mol Suite 1 mol of epoxy oligomer.

The temperature-time regime of the curing composition as described in example 2.

The results of measurements of Tcand gloss of the coating shown in Fig. 5.

Example 14. In the powder composition of the company "Herberts" example 3 is added 0.01 mol Suite 1 mol of epoxy oligomer (in this case approximately, since we only know the approximate content of the epoxy oligomer in the composition). Next, the powder composition is mixed, ekstradiruet at a temperature of 100oC, cooled and ground.

The temperature-time regime of the curing composition as described in example 3.

The results of measurements of Tcand gloss of the coating shown in Fig. 6.

Example 15. In the composition according to example 3 is added in the cooking process 0,005 Denia composition as described in example 3.

The results of measurements of Tcand gloss of the coating shown in Fig. 6.

Example 16. In the composition according to example 3 is added during cooking, 0.01 mol Suite 1 mol of epoxy oligomer. Further according to the example 14.

The temperature-time regime of the curing composition as described in example 3.

The results of measurements of Tcand gloss of the coating shown in Fig. 6.

Example 17. In the composition according to example 3 is added in the cooking process of 0.05 mol Suite 1 mol of epoxy oligomer. Further according to the example 14.

The temperature-time regime of the curing composition as described in example 3.

The results of measurements of Tcand gloss of the coating shown in Fig. 6.

Example 18. In the composition according to example 3 are added in the preparation of a 0.1 mol Suite 1 mol of epoxy oligomer. Further according to the example 14.

The temperature-time regime of the curing composition as described in example 3.

The results of measurements of Tcand gloss of the coating shown in Fig. 6.

Powder compositions (examples 1-18) was applied onto the pre-prepared metal plate with a thickness of 0.8 mm steel 3 electrostatic method. The thickness of the coating somaclone light beam 60o.

To determine the glass transition temperature of the powder compositions prepared in accordance with examples 1-18, used the method of differential scanning calorimetry (DSC) using a calorimeter company Mettler TA 3000 and (Dupont 9900). The scanning speed was 10o/min (see Fig. 1, 2 and 3).

1. A method for producing powder thermosetting composition for coating a mixture of epoxy oligomer, curing agent, curing accelerator, pigments, fillers and special additives, characterized in that the additives used as the target of 0.001 - 0.1 mol diphenylolpropane on 1 mol of epoxy oligomer.

2. The method according to p. 1, characterized in that in the initial mixture further added oligoether.

 

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FIELD: hydraulic insulating materials for hydraulic insulation and corrosion prevention of concrete, metal and reinforced concrete structural surfaces.

SUBSTANCE: claimed composition contains: butadiene-styrene thermoelastomer, diepoxy resin, filler (carbon black), solvent (toluene), pigment filler, containing aluminum and iron hydroxides and additionally indene-coumarone resin, waterproofing agent (liquid polymethylsiloxane), and stabilizer.

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2 tbl

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2 tbl, 4 ex

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