Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
  • C11D13/02—Boiling soap; Refining
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
  • C07C51/42—Separation; Purification; Stabilisation; Use of additives
  • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
  • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
  • C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
  • C11C1/08—Refining
  • C11C1/10—Refining by distillation

Definitions

• the present invention relates to the separation of volatile constituents from crude soaps.
• aqueous crude alkali metal soaps prepared from materials containing fatty acids of high molecular weight, e. g. thosexhaving at least 10 carbon atoms, or mixtures thereof, such as products or the oxidation of aliphatic hydrocarbons of high molecular weight and of mixtures thereof, or fats, oils or waxes 01 natural origin can be freed from volatile substances of.
• the minimum pressure necessary to produce this effect during the heating up to the melting temperature depends on the nature of the saponiflcation products to be worked up; in most cases pressures of from about 10 to about 30 atmospheres are suflicient, but higher pressures may be'employed.
• the melting temperatures which lie generally between about 200 and about 300 C.
• non-saponifiable constituents of high boiling point are also dependent on the nature of the initial materials; they'may be readf materials containing non-saponifiable constituents of high boiling point, as for example natural waxes, such as mineral waxes containing esters such as crude Montan wax, physically or chemically bleached Montan wax, or vegetal, i. e. animal or vegetable waxes, such as wool grease, sperm oil, spermaceti and the like.
• oxidation products of liquid or solid non-aromatic hydrocarbons such as parafiln wax, paraflln oil or high-boiling mineral oil fractions, which oxidation products contain high molecular fatty acids,
• the quantity of water in the said crude soaps is generally so high that a mass is obtained in the saponification which can be easily stirred by mechanical means as are usual in the soap industries.
• the quantity of alkali present in the crude soaps may .be equivalent to those of fatty acid present but it may. be higher or lower, the saponiilcation requiring often an excess 01' alkali and, on the other hand, may be often carried out with a lower quantity of alkali depending ,on the resistance to saponification of the initial materials and on the nature of the alkali employed.
• the process may be carried out for example by first heating the aqueous saponiflcation product in a closed vessel, preferably while stirring or otherwise causing movement, until the necessary minimum pressure ascertained by a preliminary test with a small quantity in a small vessel has been produced then 'while maintaining the said pressure, which may be eflected by periodically releasing the pressure, heating the mass to the melting temperature of the anhydrous saponiflcation products and removing the water contained in the saponiilcation products in the to of water vapor by releasing the pressure.
• The'heating of the saponiflcation products to the melting temperature, the releasing of the pressure and the distillation of the volatile constituents may be carried out in batches in a pressure-tight stirring vessel capable of being heated and provided with the necessary supply and withdrawal pipes for supplying and withdrawing the saponification products and for distilling off the vapors and if desired also for blowing in steam or gases. It is of especial advantage, however, to carry out the process in a continuous manner and only to expose the product for a very short time to the high and, during a too protracted action,.
• the saponification product may be heated in a closed stirring vessel as hereinbefore described only to such an extent that the necessary minimum pressure is attained. While making use of the pressure, the mass is then led from the stirring vessel through a tube system heated to the said or higher temperatures at the end of which the fused mass is released from pressure and at the same time freed from water vapor in a chamber which is likewise heated to the said temperatures and in which the mass is subjected to distillation for the removal of impurities.-
• the heating of the apparatus is preferably carried out while avoiding injurious overheating, as for example by means of metal baths the temperature of which is not allowed'to exceed the predetermined lim-- its.
• the melt of soaps freed from volatile con stituents may be rapidly removed from the hot distillation zone by its own weight or by employ ⁇ ,
• the process according to the present invention is especially suitable for separating unsaponifiable constituents of high boiling point from saponiflcation products of substances containing fatty acids, especially of oxdiation. products of aliphatic hydrocarbons of high molecular weight.
• Efrainplei 1500 parts of an oxidation product obtained by the treatment of 1350 parts of hard paraffin wax'with a per cent nitric acid at C. for about 8 hours) having an acid value of 128, a
• saponification value of 243 a content of 17.5 per cent of unsaponiflable material and 3.1! per cent of nitrogen are mixed with 1800 parts of a 20 per cent aqueous caustic soda solution and heated to 230 C. in an autoclave while stirring. A pressure of 25 atmospheres lSzthllS produced.
• the soap solution is led under pressure through a spiral tube which is situated in a lead bath heated to 340 C, and is introduced, with the simultaneous release of pressure, into a vessel provided with a stirring device, a temperature of 320 C. being maintained in the said vessel.
• the fused saponification product leaves the vessel through a siphon arranged in the lower part thereof, while the vapors of the unsaponiflable substances to-' gether with the steam escape through an outlet pipe and are condensed. In this way 300 parts of unsaponiflable substances are obtained.
• the pure saponiflcation product is dissolved in water and decomposed by means of hydrochloric acid.
• the fatty acids which separate have the following characteristlcsj acid value 265, saponification value 2'11. content of 'unsaponiflable substances 3.1 per cent, nitrogen 0.49 per cent. distillation of these fatty acids, a part of the unsaponifiable substances remains behind in the distillation residue so. that, calculated on the initial amount, 77 per cent of fatty acids contain- During a ing only 1.6 per cent of unsaponiflable substances are finally obtained.
• Example 2 nitrogen thus produced is regulated to 5 atmospheres and kept constant by periodically releasing After separating off the nitric acid,
• Example 3 100 parts of wool tat having a saponification va1ue of 88 are heated while stirring in an autoclave with parts of a 20 per cent aqueous caustic soda solution and '75 parts of water. As soon as a pressure of 30 atmospheres is attained heating is continued while blowing oil steamin such a quantity that the pressure remains constant. As soon as the mass has attained a temperature of from 250 to 260 C. the pressure is completely released whereby the steam is wholly blown off. The soap in the autoclave is then heated to 350 C. while blowing through steam for facilitating the distillation oi the volatile constituents. The vapors are passed through a condenser heated to from about 70 to about 80 C. so that volatile matter distilled off is condensed.
• Example 4 1000 parts oi sperm oil having a saponii'lcation.
• oi! 150 are heated in an autoclave while stirring to 200- C.-'together with 590 parts oi a 20 per cent aqueous caustic soda'solution and 530 parts of water, whereby a pressure oi 18 atmospheres is attained. The whole is then kept for 3 hours at the said temperature for rendering completethe saponiflcation, passed by the prevailing pressure into a pipe system in which it is heated to 300 C. while maintaining the pressure and then released through a second pipe system connected into a separator in which .the
• the separator is provided at its bottom with a siphon from which the molten, soap is drawn oi! while the vapors are drawn oil through an outlet pipe connected to the top 0! the separator and then led to a-condenser in which they are precipitated by indirect cooling with the aid of water warmed to from 70 to C.
• vunsaponiiiable matter from crude soaps the step which comprises heating an aqueous, crude soap containing volatile, unsaponifiable substances at a pressure between 10 and about 30 atmospheres to the melting point of the soap, when in the anhydrous state, releasing the pressure and then distilling on the said volatile, unsaponiiiable substances at a temperature at least as high as the aforesaid temperature.
• the step which comprises heating an aqueous, crude soap containing volatile, unsaponifiable substances to from about 250 to about 300 C., at a pressure between 10 and, about 30 atmospheres, releasing the pressure and then distilling of! the said volatile, unsaponifiable substances at a "temperature at least as high as the aforesaid temperature.
• the step unsaponifla'ble matter from crude coaps, the step which comprises heating an aqueous, crude alkali metal soap; from the products of an oxidation of ditlicultly volatile, non-aromatic hydrocarbons and containing volatile, unsaponiflable substances, at a pressure betweenlo and about 30 atmospheres to the melting point of the soap when in the anhydrous state, releasing the pressure and then distilling oil the said volatile, unsaponiflable substances at a temperature at least as high as the aforesaid temperature.
• the step which comprises heating an aqueous, crude alkali metal so'ap, irom the products oi an oxidation of difllcultly volatile, non-aromatic hydrocarbons and containing volatile, unsaponiflable substances, at .a pressure between 10 and about 30 atmospheres to the melting point of the soap when in the anhydrous state, releasing the pressure and then distilling oil the said volatile, unsaponifiable substances with the aid of steam at a temperature at least as high as the ai'oresid temperature.
• the step which comprises heating an aqueous, crude sodium soap from the saponiflcation of products of an oxidation of paraffin and containing volatile. ,unsaponiflable" substances, to from about 250 to about 300 C. at a pressure I and about 30 atmospheres, releasing the pressure and then distilling of! the said volatile, unsaponiflable substances at a temperature at least as high between 10 .145
• the step which comprises heating an aqueous, crude sodium soap from the saponiflcation of sperm oil and containing alcohols of sperm oil esters to 5 about 200 C. at a' pressure of about 18 atmospheres, heating the whole to about 300 (3., while maintaining the said pressure, releasing the pressure and separating the vapors formed ⁇ mm the liquid soap.

Landscapes

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Life Sciences & Earth Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Wood Science & Technology (AREA)
• Crystallography & Structural Chemistry (AREA)
• Microbiology (AREA)
• General Chemical & Material Sciences (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Detergent Compositions (AREA)

Applications Claiming Priority (1)

Publications (1)

Family

ID=7816509

Family Applications (1)

Country Status (2)

Cited By (1)

• 0
  • NL NL32545D patent/NL32545C/xx active
• 1932
  • 1932-02-12 US US592648A patent/US1965566A/en not_active Expired - Lifetime

Also Published As

Similar Documents