US2021926A - Treatment of waxes - Google Patents
Treatment of waxes Download PDFInfo
- Publication number
- US2021926A US2021926A US661176A US66117633A US2021926A US 2021926 A US2021926 A US 2021926A US 661176 A US661176 A US 661176A US 66117633 A US66117633 A US 66117633A US 2021926 A US2021926 A US 2021926A
- Authority
- US
- United States
- Prior art keywords
- parts
- mixture
- alcohol
- waxes
- distillation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000001993 wax Substances 0.000 title description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 235000011118 potassium hydroxide Nutrition 0.000 description 15
- 239000000203 mixture Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000003921 oil Substances 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- 238000004821 distillation Methods 0.000 description 10
- 239000000344 soap Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012177 spermaceti Substances 0.000 description 5
- 229940084106 spermaceti Drugs 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000374 eutectic mixture Substances 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- REZQBEBOWJAQKS-UHFFFAOYSA-N triacontan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO REZQBEBOWJAQKS-UHFFFAOYSA-N 0.000 description 2
- 239000004163 Spermaceti wax Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 239000012174 chinese wax Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 239000010685 fatty oil Substances 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 235000019385 spermaceti wax Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B11/00—Recovery or refining of other fatty substances, e.g. lanolin or waxes
Definitions
- True fats and fatty oils consist essentially of glyoerides of higher fatty acids and, as is well known are easily saponified to give soaps and glycerine.
- Waxes also consist of or contain esters of fatty acids, but these esters are not glycerides; they are the esters of higher monohydric alcohols.
- the present invention relates to a treatment of waxes, liquid or solid, whereby the esters present are saponified and the alcohols are separated in a technically advantageous way.
- the distillation is preferably carried out by use of superheated steam, and it can then be carried out usually at atmospheric pressure. Distillation may also be effected under diminished pressure, with or without simultaneous use of steam.
- distillation proceeds smoothly because the material in the still is liquid. So that distillation may take place at the lowest convenient temperature it is advantageous to use not caustic potash alone, but a mixture of caustic potash and caustic soda, the proportions of caustic potash and caustic soda being so chosen that preferably the soap remaining at the end of the distillation is a eutectic mixture.
- Example 1 241 parts of spermaceti are melted and heated to 200 C. 42 parts of powdered potassium hydroxide are now added with agitation in half an hour, during which time the temperature is allowed torise to 240 C. It is held at this temperature for half an hour when superheated steam is passed in. There distils over with the steam a colourless oil which sets on cooling to a crystalline waxy solid which is entirely free from fatty acid and from unsaponified spermaceti. The yield is approximately parts by weight, the proportion of water to oil in the distillate being approximately 10:1.
- Example 2 241 parts of spermaceti are treated as in Example l with a mixture of 21 parts powdered potassium hydroxide and 15 parts of powdered sodium hydroxide. After reaction, the molten mixture of soaps and fatty alcohol is subjected to superheated steam distillation at about 250 C., eventually at 280 C. until no more oil distils. The yield is approximately 100 parts of the pure alcohol from spermaceti, the ratio of water to oil in the distillate being approximately 10:1.
- Example 3 268 parts of sperm oil are treated as in Example 1 with a mixture of 21 parts of caustic potash and 15 parts of caustic soda. After reaction the mass is subjected to superheated steam distillation until no more oil distils. The yield is 90 parts of a semi-solid alcohol, free from unsaponified wax or free fatty acid. The ratio of water to oil in the distillate is approximately 4:1.
- Example 4 290 parts of beeswax are heated to C. 50 and a mixture of 16 parts of powdered caustic potash and 11% parts of powdered caustic soda is added. The mixture is then treated with superheated steam as described in the preceding examples. Myricyl alcohol is obtained, the ratio 55 of water to alcohol in the distillate being about 25:1.
- waxes e. g. chinese wax, wool fat, carnauba wax may be treated in the same way.
- Process for the manufacture of an alcohol from spermaceti wax which comprises heating substantially 241 parts of the Wax with a mixture of about 21 parts of dry caustic potash and about 15 parts of dry caustic soda at about 200-240 (3., and thereafter distilling oi? the alcohol in a current of superheated steam.
- Process for the manufacture of an alcohol from sperm oil which comprises heating substantially 268 parts of the liquid war; with a mixture of about 21 parts of dry caustic potash and about 15 parts of dry caustic soda at about ZOO-240 C., and thereafter distilling oil the alcohol in a current of superheated steam.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
- Fats And Perfumes (AREA)
Description
Patented Nov. 26, 1935 UNITED STATES iATENT OFFICE TREATMENT (PF WAXES No Drawing. Application March 16, 1933, Serial No. 661,176. In Great Britain March 1'7, 1932 4 Claims.
True fats and fatty oils consist essentially of glyoerides of higher fatty acids and, as is well known are easily saponified to give soaps and glycerine. Waxes also consist of or contain esters of fatty acids, but these esters are not glycerides; they are the esters of higher monohydric alcohols. When the distinction between fats and Waxes is thus drawn on a chemical basis, there come to be classed among the waxes the the so-called liquid waxes, sperm oil and arctic sperm oil.
The present invention relates to a treatment of waxes, liquid or solid, whereby the esters present are saponified and the alcohols are separated in a technically advantageous way.
Known methods of saponifying waxes are not adapted to be performed on a manufacturing scale. When aqueous alkali is used much troublesome-froth is formed and it is difficult to separate the alcohol from the soap. To saponify with alcoholic alkali is too costly. It has been proposed to separate alcoholic material, adapted for pharmaceutical use, from spermaceti by a treatment with lime, followed by distillation (Axelrad, Journal of Industrial and Engineering Chemistry, 1917, 9, 1123) but this process is not free from technical disadvantages because the lime, lime soaps, etc. of which the mass to be distilled consists do not melt.
According to the present invention we heat together a liquid or solid wax and either dry caustic potash or a dry mixture of caustic potash and caustic soda and separate the alcohol from the molten reaction mass by a distillation process.
When a wax and dry caustic potash or a dry mixture of caustic potash and caustic soda are heated together in accordance with the invention a mixture of fatty alcohol and anhydrous soap is formed. This is molten at a temperature such that the alcohol can be separated by distillation.
The distillation is preferably carried out by use of superheated steam, and it can then be carried out usually at atmospheric pressure. Distillation may also be effected under diminished pressure, with or without simultaneous use of steam.
In using superheated steam it is not necessary that the steam should be superheated before it is admitted to the distillation vessel, it suffices that dry steam such as is commonly available in factory processes, be passed into the vessel, the contents of which are kept at the desired temperature by appropriate external heating.
Distillation proceeds smoothly because the material in the still is liquid. So that distillation may take place at the lowest convenient temperature it is advantageous to use not caustic potash alone, but a mixture of caustic potash and caustic soda, the proportions of caustic potash and caustic soda being so chosen that preferably the soap remaining at the end of the distillation is a eutectic mixture.
The invention is illustrated but not limited by the following examples, the parts are by weight.
Example 1 241 parts of spermaceti are melted and heated to 200 C. 42 parts of powdered potassium hydroxide are now added with agitation in half an hour, during which time the temperature is allowed torise to 240 C. It is held at this temperature for half an hour when superheated steam is passed in. There distils over with the steam a colourless oil which sets on cooling to a crystalline waxy solid which is entirely free from fatty acid and from unsaponified spermaceti. The yield is approximately parts by weight, the proportion of water to oil in the distillate being approximately 10:1.
Example 2 241 parts of spermaceti are treated as in Example l with a mixture of 21 parts powdered potassium hydroxide and 15 parts of powdered sodium hydroxide. After reaction, the molten mixture of soaps and fatty alcohol is subjected to superheated steam distillation at about 250 C., eventually at 280 C. until no more oil distils. The yield is approximately 100 parts of the pure alcohol from spermaceti, the ratio of water to oil in the distillate being approximately 10:1.
Example 3 268 parts of sperm oil are treated as in Example 1 with a mixture of 21 parts of caustic potash and 15 parts of caustic soda. After reaction the mass is subjected to superheated steam distillation until no more oil distils. The yield is 90 parts of a semi-solid alcohol, free from unsaponified wax or free fatty acid. The ratio of water to oil in the distillate is approximately 4:1.
Example 4 290 parts of beeswax are heated to C. 50 and a mixture of 16 parts of powdered caustic potash and 11% parts of powdered caustic soda is added. The mixture is then treated with superheated steam as described in the preceding examples. Myricyl alcohol is obtained, the ratio 55 of water to alcohol in the distillate being about 25:1.
Other waxes, e. g. chinese wax, wool fat, carnauba wax may be treated in the same way.
We claim:
1, Process for the manufacture of higher alcohols comprising heating a wax with a dry mixture of caustic potash and caustic soda in proportions such as to give a eutectic mixture of the corresponding soaps.
2. Process for the manufacture of higher alcohols comprising heating a Wax with a dry mixture of caustic potash and caustic soda in proportions such as to give a eutectic mixture of the corresponding soaps and separating the alcohol by distillation.
3. Process for the manufacture of an alcohol from spermaceti wax which comprises heating substantially 241 parts of the Wax with a mixture of about 21 parts of dry caustic potash and about 15 parts of dry caustic soda at about 200-240 (3., and thereafter distilling oi? the alcohol in a current of superheated steam.
4. Process for the manufacture of an alcohol from sperm oil which comprises heating substantially 268 parts of the liquid war; with a mixture of about 21 parts of dry caustic potash and about 15 parts of dry caustic soda at about ZOO-240 C., and thereafter distilling oil the alcohol in a current of superheated steam.
WILFRED ARCHIBALD SEXTON. DENIS WARD.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB2021926X | 1932-03-17 |
Publications (1)
Publication Number | Publication Date |
---|---|
US2021926A true US2021926A (en) | 1935-11-26 |
Family
ID=10896335
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US661176A Expired - Lifetime US2021926A (en) | 1932-03-17 | 1933-03-16 | Treatment of waxes |
Country Status (1)
Country | Link |
---|---|
US (1) | US2021926A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2506473A (en) * | 1948-06-10 | 1950-05-02 | Richards Chemical Works | Metod of obtaining fatty alcohols from their esters |
US5663156A (en) * | 1992-09-29 | 1997-09-02 | Laboratorios Dalmer Sa | Mixture of higher primary aliphatic alcohols, its obtention from sugar cane wax and its pharmaceutical uses |
-
1933
- 1933-03-16 US US661176A patent/US2021926A/en not_active Expired - Lifetime
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2506473A (en) * | 1948-06-10 | 1950-05-02 | Richards Chemical Works | Metod of obtaining fatty alcohols from their esters |
US5663156A (en) * | 1992-09-29 | 1997-09-02 | Laboratorios Dalmer Sa | Mixture of higher primary aliphatic alcohols, its obtention from sugar cane wax and its pharmaceutical uses |
US5856316A (en) * | 1992-09-29 | 1999-01-05 | Laboratorios Dalmer Sa | Mixture of higher primary aliphatic alcohols, its obtention from sugar cane wax and its pharmaceutical uses |
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