US3481783A - Molasses purification - Google Patents
Molasses purification Download PDFInfo
- Publication number
- US3481783A US3481783A US662878A US3481783DA US3481783A US 3481783 A US3481783 A US 3481783A US 662878 A US662878 A US 662878A US 3481783D A US3481783D A US 3481783DA US 3481783 A US3481783 A US 3481783A
- Authority
- US
- United States
- Prior art keywords
- molasses
- mud
- sugars
- sugar
- lime
- 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
- 235000013379 molasses Nutrition 0.000 title description 35
- 238000000746 purification Methods 0.000 title description 9
- 235000000346 sugar Nutrition 0.000 description 33
- 150000008163 sugars Chemical class 0.000 description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 16
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 14
- 235000011941 Tilia x europaea Nutrition 0.000 description 14
- 239000004571 lime Substances 0.000 description 14
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 13
- 239000000126 substance Substances 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 239000001569 carbon dioxide Substances 0.000 description 8
- 238000004040 coloring Methods 0.000 description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000005342 ion exchange Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000011282 treatment Methods 0.000 description 5
- 239000003086 colorant Substances 0.000 description 4
- 229960004903 invert sugar Drugs 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- CZMRCDWAGMRECN-UHFFFAOYSA-N 2-{[3,4-dihydroxy-2,5-bis(hydroxymethyl)oxolan-2-yl]oxy}-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 description 1
- DSLZVSRJTYRBFB-LLEIAEIESA-N D-glucaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O DSLZVSRJTYRBFB-LLEIAEIESA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 235000013681 dietary sucrose Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000019988 mead Nutrition 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229960004793 sucrose Drugs 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B35/00—Extraction of sucrose from molasses
- C13B35/02—Extraction of sucrose from molasses by chemical means
- C13B35/06—Extraction of sucrose from molasses by chemical means using ion exchange
Definitions
- Liquid sugar is obtained from cane molasses by subecting the molasses to two defeco-saturation treatments at different pH before they are passed into an ion exchanger.
- This invention relates to the production of an only slightly colored liquid sugar of high purity from cane molasses by means of ion exchange resins.
- molasses contain a number of various coloring agents the constitution of which is not completely known. Part of such coloring agents is retained by ion exchangers; however, certain coloring agents which are found especially in cane molasses, are not bound by ion exchangers and impart an intense yellow color to the juices from which the salts have been removed by ion exchangers.
- said objects are attained by applying to the cane molasses, before they are subjected to an ion exchanger purification, the following pretreatment:
- the molasses is diluted to about 35 Bx. and the mud substances contained therein are removed, preferably by separation;
- a defeco-saturation is carried out at a temperature up to 45 C., preferably below 40 C., with lime and carbon dioxide at a pH of -12, preferably about 10.5, with an amount of lime corresponding to 30 to 60 percent of CaO, calcu- 3,481,783 Patented Dec.
- the formed mud is filtered off, and finally the filtrate is brought, by a second defecosaturation with lime and carbon dioxide, to a pH of 8- 8.5, whereby 3 to 6, preferably 5% of lime, calculated on the non-sugars of the original molasses, are used and filtered again.
- the invention is based on the discovery that it is possible to remove, prior to the treatment with ion exchange resins, a considerable amount of the non-sugars and the major part of coloring substances not removed by the ion exchangers, when the juice is subjected to a specific prepurification procedure.
- the first step the removal of the mud substances contained in the molasses by dilution of the molasses to about 35 Bx. and subsequent separation, filtration, or decantation can be carried out in apparatus known for this purpose, preferably in separators, and with advantage at room temperature.
- the second step i.e. the defecosaturation with lime and carbon dioxide at a pH of 10-12, preferably 10.5
- a pH of 10-12 preferably 10.5
- a temperature adjustment to a bout 45 C., preferably below 40 C. has the result that a decomposition of the invert sugar in the alkaline range, in which new coloring substances and water soluble calcium salts are formed, is substantially avoided.
- the subsequent treatment of the juice consists in a treatment with cation-anion exchangers, as described for instance, in the journal Zucker, vol. 15 (1962), pp. 340-345.
- the deionized juice is concentrated to about BX., e.g., by means of flash boilers.
- the sugar containing waste waters of the muds below about Bx. and those of the ion exchange plant, as far as not incorporated in the purified juice, are used to dilute the molasses.
- a single defeco-saturation at a pH below 10 does not retain sufiiciently those coloring substances which are difiiculty removed in the ion exchangers.
- the degree of the nonsugar removal and juice decoloration can be widely varied during the pre-purification by the amount of the lime added.
- liquid sugar of a purity up to 99% total sugar/TS and a color of 3-5 St. are obtained.
- Such products known on the market as Golden syrup, are used in the food and beverage industry.
- the solutions fed into the ion exchangers are completely free of colloids, fats, and waxes, thereby preventing capacity losses of the ion exchange plant by irreversible loads.
- the solution is separated in a mud separator at C. After removal of the mud, the solution has still 44.4%
- the solution is defeco-saturated with 50% CaO, calculated on the non-sugars of the starting molasses at a pH of 10.7 and a temperature of 2532 C., and with CO and the mud is filtered ofi.
- the filtrate contains of non-sugars/TS and has a color of 320 St.
- the removed amount of non-sugars corresponds to percent of the original content.
- the filtrate is defeco-saturated with 3% of CaO, calculated on non-sugars of the starting molasses, and CO thereby, the pH value gradually drops to 8.5.
- the filtrate of the mud contains 32.5 percent of non-sugars/TS and has a color of 330 St.
- the thus obtained juice is desalted in cation-anion exchangers, concentrated in vacuo at 70 to 80 C. to 75 Bx. and produces a liquid sugar of 98.9 percent total sugar purity and a color of 7.4 St.
- a process of preparing liquid sugar of high purity and low color from cane molasses comprising diluting cane molasses to 35 Brix, removing mud substances, then subjecting the diluted molasses to a defeco-saturation at a temperature not higher than C.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB0088619 | 1966-08-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3481783A true US3481783A (en) | 1969-12-02 |
Family
ID=6984387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US662878A Expired - Lifetime US3481783A (en) | 1966-08-25 | 1967-08-24 | Molasses purification |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US3481783A (de) |
| AT (1) | AT268165B (de) |
| DE (1) | DE1567248A1 (de) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3975205A (en) * | 1973-12-14 | 1976-08-17 | Suddeutsche Zucker-Aktiengesellschaft | Process for working up molasses |
| US4193817A (en) * | 1979-03-22 | 1980-03-18 | Illinois Water Treatment | Production of bottler's liquid sugar |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1727738A (en) * | 1926-09-13 | 1929-09-10 | Gerhard Elias Van Nes | Purification of liquids containing sugar |
| US2075127A (en) * | 1936-04-27 | 1937-03-30 | Nat Grain Yeast Corp | Clarification of molasses |
| US2093759A (en) * | 1936-04-14 | 1937-09-21 | Petree & Dorr Engineers Inc | Sugar juice clarification |
| US2697049A (en) * | 1949-06-03 | 1954-12-14 | Brieghel-Muller Arne Vigand | Lime-carbonation method of refining sugar solutions |
| US2774693A (en) * | 1950-03-24 | 1956-12-18 | Danske Sukkerfab | Method for purifying sugar juices by liming and carbonation |
| US2868677A (en) * | 1956-07-30 | 1959-01-13 | Ultra Sucro Company | Clarification and demineralization process for b-molasses and similar materials containing concentrated impurities |
| US2916404A (en) * | 1954-12-06 | 1959-12-08 | Battistoni Giovanni | Process for extracting sugar from molasses |
| US3257236A (en) * | 1964-07-07 | 1966-06-21 | Nat Sugar Refining Company | Method of making sugar |
-
1966
- 1966-08-25 DE DE19661567248 patent/DE1567248A1/de active Pending
- 1966-09-09 AT AT854566A patent/AT268165B/de active
-
1967
- 1967-08-24 US US662878A patent/US3481783A/en not_active Expired - Lifetime
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1727738A (en) * | 1926-09-13 | 1929-09-10 | Gerhard Elias Van Nes | Purification of liquids containing sugar |
| US2093759A (en) * | 1936-04-14 | 1937-09-21 | Petree & Dorr Engineers Inc | Sugar juice clarification |
| US2075127A (en) * | 1936-04-27 | 1937-03-30 | Nat Grain Yeast Corp | Clarification of molasses |
| US2697049A (en) * | 1949-06-03 | 1954-12-14 | Brieghel-Muller Arne Vigand | Lime-carbonation method of refining sugar solutions |
| US2774693A (en) * | 1950-03-24 | 1956-12-18 | Danske Sukkerfab | Method for purifying sugar juices by liming and carbonation |
| US2916404A (en) * | 1954-12-06 | 1959-12-08 | Battistoni Giovanni | Process for extracting sugar from molasses |
| US2868677A (en) * | 1956-07-30 | 1959-01-13 | Ultra Sucro Company | Clarification and demineralization process for b-molasses and similar materials containing concentrated impurities |
| US3257236A (en) * | 1964-07-07 | 1966-06-21 | Nat Sugar Refining Company | Method of making sugar |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3975205A (en) * | 1973-12-14 | 1976-08-17 | Suddeutsche Zucker-Aktiengesellschaft | Process for working up molasses |
| US4193817A (en) * | 1979-03-22 | 1980-03-18 | Illinois Water Treatment | Production of bottler's liquid sugar |
Also Published As
| Publication number | Publication date |
|---|---|
| DE1567248A1 (de) | 1970-06-25 |
| AT268165B (de) | 1969-02-10 |
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