DE838651C - Process for the production of rubber hydrochlorides - Google Patents

Description

Process for the production of rubber hydrochlorides According to the previously known processes for the production of rubber hydrochlorides in solution, rubber is treated with dry hydrogen chloride gas in benzene hydrocarbons, chloroform or other chewing powder solvents. The properties of this end product largely depend on the concentration with which the hydrogen chloride in the solution acts on the rubber. The lower the temperature, the higher the concentration of hydrogen chloride in the solution and the faster the hydrochlorination takes place, which has an advantageous effect on the properties of the end product. But if you want a costly freezing (- 10 to - 30 °) spare the hydrochlorination so much longer Hydrochlorierungszeiten required by the previously known methods, which adversely affect the properties of the final products.

It has now been found that the hydrochlorination time can also be used Room temperature can be significantly reduced if you carry out the reaction in the presence of Hydrogen chloride dissolves well with the rubber solvent used are miscible. Through the use of rubber solvents Miscible, good solvents for hydrogen chloride succeed in reducing the hydrogen chloride concentration to increase in the rubber solution. Come as a solvent for hydrogen chloride before especially polar substances such as alcohols, ethers and acid anhydrides. As special Acetic anhydride proves to be suitable. It is so effective in promoting hydrochlorination that an exceptionally pale rubber hydrochloride is obtained, as is the case after the previously known processes could not be produced at temperatures above 10 °. In addition, if the hydrogen chloride is left under a slight excess pressure on the rubber solutions have an effect, a further not inconsiderable improvement is thereby achieved, which also allows you to work safely at temperatures above Hauniteniperatur. The neutralized rubber hydrochloride solutions are worked up in the usual way, wherein the additives are either removed from the solution during the neutralization or when processing the rubber hydrochloride, e.g. 1i. on slides, at Pouring with earth.

Example i Heavily niastized crepe rubber becomes a 15 oigen dissolved in benzene solution. 20.0 to 25.0 kg of acetic anhydride are added to every 100.0 kg of crepe with good stirring and conducts a steady stream of dry at io f> is 15v Hydrogen chloride until the viscosity of the solution rises sharply, which is usually reached after 3 to 4 hours. One interrupts the Clilcirwass, erstoffzijfuhr, lets the batch stand for up to 1 hour, warmed to 50 to 60 ° and neutralized with soda or ammonia. After filtration, the product is worked up as usual.

Example 12 Heavily niastized crel> ekautscliuk turns into a 200 per cent 1> wizolischeii solution dissolved. One adds to each i oo, o 1: g crepe io, o to 15, o kg acetic anhydride with thorough stirring. Then one passes at 20 to 25 ° and about 1 to 2 atmospheres overpressure hydrogen chloride into the solution until the viscosity increases sharply, which is the case after 3 to 4 hoursi. The supply of water chloride is interrupted, lets the solution stand for 1/2 to 1 hour, then warmed to 50 to 60 °, neutralized with soda or ammonia and works up as usual. Example3 Heavily masticated Crepe rubber is dissolved to a 15% 1> enzolic solution, for each 100, o kg of crel> e 20.0 to 25, o kg of Ethai101 with good oil added and added 15 to 18 ° a steady stream of dry hydrogen chloride is introduced as long as until the viscosity of the solution rises sharply, which is usually after 3 to 4 hours of the Case is. The supply of hydrogen chloride is interrupted and the batch i / 2 bis is still left Stand for i hour and neutralize with soda or ammonia. After separating the Salt is worked up as usual.

For example 4 heavily masticated crepe rubber becomes a 2oo / oigen Dissolved benzene solution, on each 100.0 kg crepe 50.0 kg butanol under good Stirring added and a steady stream of dried hydrogen chloride at 15 ° to 20 ° initiated until the viscosity of the solution rises sharply, which after about .4 hours is the case. Further work-up as in Example 3.

Example s Heavily masticated crepe rubber becomes a 200% strength dissolved in benzene solution. 15.0 to 20.0 kg of ether are added to every 100.0 kg of crepe with good stirring and passes a uniform stroni of dried at 15 to 20 ° Hydrogen chloride until the viscosity of the solution rises sharply, which is usually the case after about 4 hours. Further work-up as in Example 3.

EXAMPLE 6 Heavily masticated crepe rubber becomes a 200% strength dissolved in benzene solution. 20.0 to 25.0 kg of dioxane are added to every 100.0 kg of crepe with good stirring and passes a steady stream of dried at 15 to 20 ° Hydrogen chloride until the viscosity of the solution rises sharply, which usually after about 4 to 5 hours. Further work-up as in the example 3.

Claims (2)

PATENT CLAIMS: i. Process for the preparation of rubber hydrochlorides by the action of: hydrogen chloride on rubber solutions, characterized in that the reaction is carried out in the presence of substances which dissolve well hydrogen chloride and which are miscible with the rubber solvent used. 2. Procedure according to claim i, characterized in that the unisposition is carried out at increased pressure will.