CS257138B1 - A method of producing ashless emulsifier - Google Patents

Abstract

The solution relates to the production of an ashless emulsifier intended for the production of machining and cooling fluids and additives to lubricating oils. It is prepared from the distillation residue from the production of alkylbenzene with alkyl from 9 to 16 carbon atoms by refining with refining clay and one or two-stage sulfonation with sulfur trioxide. After removal of acid resins, the sulfoacid is neutralized with mono*, dl*, triethanolamine or a mixture thereof to pH 7 to 12.

Description

The invention relates to the production of a ashless emulsifier for machining and cooling fluids used in the treatment and machining of metals and additives for lubricating oils.

Alkylbenzene with an alkyl chain of 10 to 13 carbon atoms is the most widely used raw material for the manufacture of synthetic detergents. Monoalkylbenzenesulfonates are a permanent major component of detergents. Monoalkylbenzene is produced from linear olefins and benzene under the catalytic action of HF, or A1CL ·, or linear bromoicans and benzene under Friedel-Crafts reaction conditions.

By-products are diphenylalkanes, dialkylindanes and tetralines and dialkylbenzenes. The formation of dialkylbenzenes cannot be prevented because the reaction is equilibrium. The formation of other by-products can be partially suppressed by the use of olelins or by a suitable choice of reaction conditions and chlorination equipment. After separation of the catalyst, the reaction mixture is washed and distilled off. Unreacted products are returned to the process, the monoalkylbenzene is sulfonated and the distillation residue is utilized differently. Dialylbenzenes and diphenylalkanes and other complicated, undefined substances remain in the distillation residue.

US P 3,272,881 recommends disproportionating the distillation residue to yield monoalkylbenzene, possibly returning to the process as described in Czechoslovak AO 199 342. Dialkylbenzenes are also produced intentionally to obtain high-quality, low-freezing oils.

These processes are described in U.S. Pat. No. 3,538,177, 3,538,178, 3,316,294 and Japanese Patent 81,169,630. The distillation residue from the production of monoalkylbenzene and intentionally prepared dialkyl benzene has also been shown to be a very good raw material for the production of surfactants. The calcium or barium salts of the sulfoacids prepared therefrom are recommended to be used as additives to lubricating oils and to Australian patent 414 540 and Pofi patent 68 269.

In Pofi 117 117 the authors recommend to produce a sulfoacid from a distillation residue from the production of monoalkylbenzene or dialkylbenzene from monoalkylbenzene by alkylation with chloroalkanes. Gudron-like sulfo acids are removed in the raffinate after extraction with hexane or petrol. They produced barium, calcium and magnesium sulfonates from the sulfo acids thus prepared. The water must boil from them. Sulfonates of this type are not suitable for the production of machining and cooling fluids in the metal industry.

The process for the production of a new ashless emulsifier from the distillation residue from the production of monoalkylbenzene from both chloroalkanes and olefins was tested. The distillation residue is sulfonated with sulfur trioxide at a temperature of 10 to 80 degrees Celsius, preferably 20 to 50 ° C, such that the product contains 65 to 95% by weight. sulfonic acid. After settling, the acid pitch is separated. It is useful to refine the distillation residue before the sulfonation with refining clay for 10 to 60 minutes in an amount of 1 to 10 washes. wt. %, preferably 3 to 5 wt. at a temperature of 80 to 150 ° C, preferably 90 to 120 ° C and then filter the clay.

Sulfonation may be carried out in one or two stages. The acid pitch is allowed to settle and is separated after the first sulfonation or after it has been sulfonated in only one stage. The sulfoacid is neutralized with monoethanolamine, diethanolamine, triethanolamine, a mixture of di- and triethanolamine, or a mixture of all three amines so that the pH of the reaction mixture is 7-12.

Example 1

300 g of the distillation residue from the production of monoalkylbenzene from olefins were sulfonated with sulfur dioxide up to 310 g. 30 grams of acid pitch were separated from the reaction mixture by sedimentation and the mixture was sulfonated to a final 306 g. The temperature of the exothermic reaction reached 56 ° C.

Example 2

500 g of the distillation residue from the production of alkylbenzene from chloroalkanes was refined for 30 minutes at 95-110 ° C with 3 wt. Refining clay and after filtration 400 g of the filtrate were sulfonated once with sulfur trioxide at a temperature as in Example 1. 410 g of sulfoacid and 37 g of acid pitch were obtained.

Example 3 g of the sulfo acid of Examples 1 and 2 were mixed and neutralized with monoethanolamine to pH 12. The neutralization temperature was 20 to 50 ° C. The neutralization point was indicated by visual clarification of the reaction mixture. 114 g of emulsifier were obtained.

Example 4 g of the sulfo acid of Example 1 was neutralized with diethanolamine as in Example

3. 74 g of emulsifier were obtained.

Example 5 g of the sulfo acid of Example 2 was neutralized with a mixture of di- and triethanolamine as in Example 3. 79 g of an emulsifier were obtained.

Claims (3)

SUBJECT 1. A process for producing a ash-free emulsifier from a distillation residue from the production of alkylbenzene from 9 to 16 carbon atoms olefins or chloroalkanes, characterized in that the distillation residue is sulfonated at 10 to 80 [deg.] C. is neutralized at 20 to 60 degrees Celsius with monoethanolamine, diethanolamine, triethanolamine, a mixture of dia triethanolamine, a mixture of mono- and diethanolamine, or a mixture of all three alkanolamine nolamines until the mixture clears until the pH of the emulsifier reaches 7-12. 2. The process according to claim 1, wherein the distillation residue is refined for 10 to 60 minutes with 1 to 10% by weight of clay before the sulfonation. at 80 to 150 ° C and the refining clay is filtered off. 3. The process according to claim 1, wherein the sulfonation is carried out in one or two stages and the acid pitch is separated after the first sulfonation stage.