Process for preparing sucrose fatty acid ester powder

• US 4,996,309 A
• Filed: 10/03/1989
• Issued: 02/26/1991
• Est. Priority Date: 11/14/1988
• Status: Expired due to Fees

• Current Assignee: Dai-Ichi Kogyo Seiyaku Company Limited (DKS Co., Ltd.)
• Original Assignee: Dai-Ichi Kogyo Seiyaku Company Limited (DKS Co., Ltd.)
• Inventors: Nakajima, Akihiko, Matsumoto, Shusaku, Hatakawa, Yoshio
• Primary Examiner(s): Griffin, Ronald W.
• Assistant Examiner(s): White, Everett
• Application Number:
  US07/416,611
• Time in Patent Office: 511 Days
• Field of Search: 536/119, 536/127, 536/124, 536/115, 536/120, 536/116, 514/951, 426/658
• US Class Current: 536/119
• CPC Class Codes: C07H 13/06 Fatty acids

Abstract

A process for preparing sucrose fatty acid esters by reacting sucrose and a fatty acid alkyl ester in an aqueous reaction system in the presence of a catalyst, adding water to the reaction mixture to dissolve it, adjusting the reaction mixture to a neutral ph region, adding a neutral salt to the solution to precipitate the sucrose fatty acid esters, separating and washing the precipitate with an acidic water, and subjecting the washing liquid to ultrafiltration. The precipitate washed with the acidic water is spray-dried in the form of an aqueous slurry to give a dry powder of the sucrose esters having low HLB, and the concentrate obtained by ultrafiltration is spray-dried to form a dry powder of the sucrose esters having high HLB, and the liquid obtained by separating the precipitate is contacted with a reverse osmosis membrane to recover sucrose. According to the invention, purifed sucrose fatty acid esters can be obtained without using an organic solvent, while sucrose can be recovered in high yield.

Claims

1. A process for preparing a powder of sucrose fatty acid esters, which comprises reacting sucrose with a fatty acid alkyl ester in an aqueous reaction system containing a catalyst to produce a sucrose fatty acid ester, adjusting the resulting reaction mixture to a neutral pH region, adding water and a neutral salt to the reaction mixture to precipitate the sucrose fatty acid ester product, separating the resulting precipitate from the liquid phase, washing the precipitate with an acidic water, subjecting the washing liquid to ultrafiltration, spray drying the resulting concentrate in the form of an aqueous solution, and recovering the unreacted sucrose by subjecting the liquid phase to reverse osmosis.

2. The process of claim 1, wherein said reaction mixture to be treated consists essentially of 15 to 74% by weight of sucrose fatty acid esters, 1.0 to 80% by weight of unreacted sucrose, 0.5 to 10% by weight of unreacted fatty acid methyl ester, 0.05 to 7.0% by weight of a catalyst, 1.0 to 60% by weight of a soap, and 0.5 to 10% by weight of a fatty acid.

3. The process of claim 1, wherein said neutral pH region is from pH 6.2 to pH 8.2.

4. The process of claim 1, wherein after the addition of water and neutral salt, the reaction mixture is heated to a temperature of 50°

to 80°

C.

5. The process of claim 1, wherein said water is added to the reaction mixture in a water/reaction mixture ratio of 5:

1 to 40;

1 by weight.

6. The process of claim 1, wherein the pH adjustment of the reaction mixture is made with an acid selected from the group consisting of lactic acid, acetic acid, hydrochloric acid and sulfuric acid.

7. The process of claim 1, wherein the fatty acid radical mainly included in each of the fatty acid alkyl ester, soap and fatty acid is a saturated fatty acid radical having 16 to 22 carbon atoms common to them.

8. The process of claim 1, wherein said neutral salt to be added to the reaction mixture is a salt selected from the group consisting of sodium chloride, Glauber'"'"'s salt, potassium lactate and potassium acetate

9. The process of claim 1, wherein said sucrose fatty acid ester is composed of 10 to 75% by weight of the monoester and 90 to 25% by weight of the di- and higher esters.

10. The process of claim 1, wherein said acidic water has a pH of 3.0 to 5.5.

11. The process of claim 1, wherein said acidic water is maintained at a temperature of 10°

to 40°

C.

12. The process of claim 1, wherein the membrane used for the ultrafiltration is made of a polysulfone or a polyvinylidene fluoride

13. The process of claim 1, wherein the membrane for the ultrafiltration has a fractionation molecular weight of 1,000 to 100,000.

14. The process of claim 1, wherein said ultrafiltration is carried out under a pressure of 1.0 to 20.0 kg/cm² G.

15. The process of claim 1, wherein the washing liquid is neutralized to pH 6.2 to 8.2.

16. The process of claim 1, wherein the washing liquid subjected to ultrafiltration is maintained at a temperature of 40°

to 60°

C.

17. The process of claim 1, wherein a membrane used for the reverse osmosis has a fractionation molecular weight of 150 to 200.

18. The process of claim 1, wherein said liquid phase is maintained at a temperature of 40°

to 60°

C. and at a pH of 6.2 to 8.2.

19. The process of claim 1, wherein said liquid phase has a sucrose content of 10 to 20% by weight.

20. The process of claim 1, wherein said concentrate to be spray-dried has a solid content of 4 to 40% by weight.

21. The process of claim 1, wherein said spray-drying is conducted in an air stream having an absolute humidity of 0.008 to 0.05 kg water/kg dry air and a temperature of 10°

to 100°

C.

22. The process of claim 1, wherein the precipitate washed with an acidic water is spray-dried.

23. The process of claim 22, wherein the precipitate to be spray-dried is in the form of an aqueous slurry having a solid content of 4 to 40% by weight.