CS224025B1 - Method of preparation of adducts based on epoxy bitumens - Google Patents

Description

The present invention relates to a process for the preparation of epoxy resin adducts.

To prepare lubricating compositions! For the treatment of glass fibers and mineral fibers, various adducts based on epoxy resins and amines have found wide application. Of the wide variety of adducts, the most widespread use is the adduct of dialkanolamines with epoxy resins based on dianes, either alone or further] modified according to the desired fiber application properties.

The synthesis of these basic adducts, mainly based on diethanolamine and dian-type epoxy resins, was first described by R. Wong and P. W. Sullivan [U.S. Pat.

449 281, Germany Pat. no. 1,494,881, franc. pat. no. 1,371,900, 1,371,901, 1,436,219, brit. pat. no. 1,103,325). The authors have thus solved the possibility of using these resins in lubricating compositions! based on water as the carrier medium. The preparation of the adducts is carried out in an organic water-dilutable solvent such as diacetone alcohol, acetone, isopropyl alcohol and the like. When applying these adduct solutions to the fiber treatment lubricants, the solvents used in their synthesis in drying the fibers are volatile. j. they are depreciated. This also causes air pollution. In addition to this possibility, the authors also mention the possibility of obtaining adducts without organic solvents so that the synthesis can be conducted in an environment of water-insoluble solvents, e.g. toluene and the resulting adduct are extracted with water after acidification. However, industrial use of this method is demanding in terms of equipment and prolonged production cycle. The described disadvantages of these solutions are overcome by the method of the invention.

The invention discloses a solvent-free process for the preparation of adducts based on epoxy resins based on dianos containing 0.20 to 0.58 epoxies / 100g and secondary C 4 -C 6 dialkanolamines by addition, with a molar ratio between epoxy group and amine hydrogen of 1: 0, 2 to 1.2. SUMMARY OF THE INVENTION The reaction is carried out in the melt of an epoxy resin at 30 to 100 ° C in the presence of saturated aliphatic monocarboxylic acids having 1 to 3 carbon atoms in an amount corresponding to 10 to 110% of the stoichiometric amount required for neutralization. dialkanolamine.

For the industrial preparation of adducts, formic, acetic or propionic acid and dialkanolamine are added to the melt of the epoxy resin. The batch is homogenized and the reaction is allowed to proceed

at elevated temperature Dian and epichlorohydrin based resins o sets until addition is complete. Nakolko pri ho- content of 0.53 epoxy / 100 g, which is mogenization leads to exothermic heated to 50 ° C. To 42 g of diethanolamine was added the heat caused by neutralization acetic acid and after tempering amine acid is preferred in the laboratory. Addition salt to 50 ° C with stirring research of technological conditions to the epoxy resin. Amount of acids- prepare separately an amine-acid solution The exotherm T _e and its time S _e are given in and after adding it to the resin, Table. to avoid distortion of measurement results. Adducts can be diluted with water to the desired consistency T _e = T _ma . ₍ T _n The invention is further illustrated by way of example. T _ma ·. - maximum temperature at time S _e perm. T _n - initial temperature of the handle Example 1 The flask was charged with 76 g of epoxy acid T _e S _e (G) (° C) (Min] 0 98 5.5 2.4 82 7.5 4.8 64 10.5 7.2 41 15.0 12, Q 12 45.0 The resin with 12 g of acetic acid was diluted 1 with the difference that to neutralize diet- water to a 50% solution with a viscosity of 605 mPa. Nolamine was used formic acid. quantities . s at 20 ° C and a color of 5 mg. J2. acidity, exotherm T _e and its time are shown in the table. Example 2 Preparation of adducts as in the example acid T _e with (G) (° C) (Min) 0 98 5.5 2.2 78 8.0 6.5 49 14.0 10.9 11 35.0 Dissolve 10,9 g of formic acid in the resin. 1, except that to neutralize diet- 50% solution with a viscosity of 210 nolamine was used propionic acid and mPa. s at 20 ° C and a color of 4 mg. J2. the batch temperature T _n was 80 ° C. The results are shown in the table. Example 3 Preparation of adducts as in the example acid T _e S _e (G) (° C) (Min) 0 102 1.5 8.9 67 2.0 14.8 57 3.0 The resin with 14.8 g of propionic acid was Dian and epichlorohydrin based resins o diluted with water to a 50% viscosity solution content 0,21 epoxy / 100 g, 21 g diethanol- 461 mPa. s / 20 ° C and color 7 mg. J2. amine and 6 g acetic acid. The addition was performed at 100 ° C for 40 minutes. the preparedness Example 4 The adduct is of solid consistency with temperature

mp 56-58 ° C.

The flask was charged with 90 g of epoxy

Example 5

To the flask was charged 76 g of epoxy resin based on diane and epichlorohydrin containing 0.51 epoxy / 100 g, 53.3 g of diisopropanolamine, 16.8 g of acetic acid. The addition was carried out at 70 ° C for 50 minutes. The adduct prepared is a clear mass with a melting point of 58-60 ° C.

Example 6

The resin solution of Example 1 was used to treat the glass fibers in the form of the lubrication shown in the table.

% wt.

polyvinyl acetate dispersion (50 ° / o) 6.0 resin solution (50 ° / o) 5.0 3-metakryloyloxipropyltrimetoxy- lan 0.2 polyethylene glycol 300 0.1 acetic acid 0.1 Water

The glass fibers were dried at 130 ° C for 4 hours after treatment. On the surface, they contained 1.2% of a lube of elastic character, which improves their processing by mowing to produce prepregs. Without the use of resin, the glass strands 1 ' are easily fiberized, resulting in their worse chopping.

Claims (1)

předm ' Process for the preparation of adducts based on epoxy resins based on dianes containing 0.20 to 0.58 epoxies / 100 g and secondary dialkanolamines of 4 to 6 carbon atoms by addition, while maintaining a molar ratio between epoxide group and amine hydrogen of 1: 0.2 to 1, 2, characterized in that the reaction The invention is carried out in an epoxy resin melt at 30 to 100 ° C in the presence of saturated aliphatic monocarboxylic acids having 1 to 3 carbon atoms in an amount corresponding to 10 to 110% of the stoichiometric amount required to neutralize dlalkanolamine.