CN1157400C - Dealcoholizing process for preparing alkylglucoside - Google Patents
Dealcoholizing process for preparing alkylglucoside Download PDFInfo
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- CN1157400C CN1157400C CNB001055232A CN00105523A CN1157400C CN 1157400 C CN1157400 C CN 1157400C CN B001055232 A CNB001055232 A CN B001055232A CN 00105523 A CN00105523 A CN 00105523A CN 1157400 C CN1157400 C CN 1157400C
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- alkyl glycoside
- alcohol
- molecular distillation
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Abstract
The present invention discloses a dealcoholizing process for obtaining solid alkyl glycoside. Excessive alcohol and dextrose are adopted for an acetalation reaction under the condition that an acidic catalyst exists for obtaining a coarse product of alkyl glycoside; then, the excessive alcohol is vaporized by a distillation device; obtained solid alkyl glycoside is slightly bleached or is not bleached for preparing the solid alkyl glycoside with a stable color in an alkali state. The product can be widely applied to food and daily chemical chemicals.
Description
What the present invention relates to is the pure method of removing that is used for direct synthesizing alkyl polyglycoside process, in particular uses the pure method of removing of distillation plant.
Have more research for the pure method of removing in the direct building-up process of alkyl glycoside, narrated with the extractive method of critical gas as Japanese 02-103202 and from the mixture of alkyl glycoside, removed higher alcohols; DEAplication3932173 adopts the mode of falling liquid film and thin-film evaporator two-step distillation that higher alcohols are separated from the alkyl glycoside mixture to remove; What US5633359 narrated is after alcohol and sugared acetalation, and excessive alcohol is removed with the thin-film evaporator evaporation.Above-mentioned separation of adopting removes pure method and very easily produces undesirable foreign pigment, the foreign pigment that produces can increase gradually, the color burn that causes alkyl glycoside, thereby influence the quality and the range of application of alkyl glycoside, and the alcohol of Separation and Recovery can't use without just handling in recirculation, and the key of dealing with problems is selecting appropriate separation to remove pure mode.
The purpose of this invention is to provide be used for direct synthesizing alkyl polyglycoside after, the separation of removing alcohol excess from the alkyl glycoside mixture removes pure method, the alcohol after the separation need not handled and can recycle.
The preparation method of alkyl glycoside of the present invention mixes the pure and mild glucose of excess fats especially glucose in reactor, Fatty Alcohol(C12-C14 and C12-C18) is 10 with the weight ratio of sugar: 1-1: 1, add suitable an acidic catalyst in reactor, temperature in the kettle remains on 80 ℃--and 150 ℃ acetalation take place generate alkyl glycoside.By the alkyl glycoside that above-mentioned reaction obtains, be actually alkyl glycoside and pure mixture, the treatment stage of also needing process to remove alcohol, slough excessive alcohol and just can obtain final alkyl glycoside.The pure method of removing that the present invention adopts is the alkyl glycoside that reaction generates directly to be entered in the molecular distillation equipment distill, the vacuum tightness of molecular distillation equipment remains on 0.90-0.01KPa, distillation temperature is 100 ℃--180 ℃, steam excessive high fatty alcohol, distillation time is controlled at and steams till the extremely not discharging, contain the alcohol amount in the reactant less than 5% weight percentage, obtain final product solid alkyl glycoside.Before using the molecular distillation equipment dealcoholysis, alkyl glycoside can be evaporated part alcohol through common evaporation equipment earlier, and then the process molecular distillation equipment evaporates remainder alcohol, distillation time is controlled at and steams till the extremely not discharging, contain the alcohol amount in the reactant less than 5% weight percentage, obtain final product solid alkyl glycoside, the vacuum tightness of molecular distillation equipment still is 0.90-0.01KPa, and distillation temperature is 100-180 ℃.
Adopt the molecular distillation equipment distillation temperature low, alkyl glycoside residence time in equipment is short, and the impurity that product produces is few, so the color and luster of product meets the requirements.When separating alcohol, can obtain final product solid alkyl glycoside, remaining alcohol＜0.2%-5% wherein, the alcohol after the separation can directly recycle.Present method technology is simple, is easy to operate and control.
Fig. 1 is a process flow sheet of the present invention.
By embodiment, be described in detail implementation process of the present invention.
Embodiment one: add dextrose anhydrous 200 grams, lauryl alcohol 1102 grams, tosic acid 3.75 grams, stearic acid 0.309 gram in a band stirs, is equipped with 2 liters of there-necked flasks of water trap, open stirring and be heated to 120 ℃, heating was kept 2 hours, and to the reaction solution clarification, reaction finishes.Can collect the water that generates in the reaction with the liquid nitrogen cooling, to determine whether reaction reaches terminal point.Reaction solution APHA＜150.Reaction solution joins in the molecular distillation equipment, and control molecular distillation equipment vacuum tightness is at 0.90-0.01KPa, and distillation temperature is 100 ℃--and 180 ℃, steam alcohol excess, steam till the extremely not discharging, reactant contains the alcohol amount less than 5% weight percent, obtains the solid alkyl glycoside.The solid alkyl glycoside is dissolved in the water at 80 ℃, its APHA＜150, and accent PH is 11-12, drips 30%H
2O
24 milliliters of APHA＜30 of bleaching to alkylglycoside.
Embodiment two: add glucose 300 grams, ten alcohol, 810 grams, sulfuric acid 0.904 gram, methylsulfonic acid 0.876 gram, stearic acid 0.238 gram, propanedioic acid 0.0869 gram that contain a crystal water in aforesaid device, stirring also is heated to 110 ℃, keep 2 hours to the reaction solution clarification, reaction finishes.Can collect the water that generates in the reaction with the liquid nitrogen cooling, to determine whether reaction reaches terminal point.Reaction solution APHA＜150.In this equipment, continue to slough part alcohol, then reaction solution is poured in the molecular distillation equipment, press the method operation of embodiment one, obtain the solid alkyl glycoside at 130-150 ℃.
Claims (2)
1. pure method of removing that is used to prepare alkyl glycoside, be that the pure and mild glucose of excess fats especially glucose is mixed in proportion, under an acidic catalyst existence condition, maintain the temperature at more than 80 ℃, acetalation takes place generate alkyl glycoside, obtain the solid alkyl glycoside through removing pure treating processes, it is characterized in that: the alkyl glycoside that will react generation directly enters in the molecular distillation equipment distills, the vacuum tightness of molecular distillation equipment remains on 0.90-0.01KPa, distillation temperature is 100 ℃---180 ℃, steam excessive high fatty alcohol, distillation time is controlled at and steams till the extremely not discharging, contain the alcohol amount in the reactant less than 5% weight percentage, obtain final product solid alkyl glycoside
2. according to claim 1 except that pure method, feature is before using the molecular distillation equipment dealcoholysis, alkyl glycoside can be evaporated part alcohol through common evaporation equipment earlier, and then the process molecular distillation equipment evaporates remainder alcohol, distillation time is controlled at and steams till the extremely not discharging, contains the alcohol amount in the reactant less than 5% weight percentage, obtains final product solid alkyl glycoside, the vacuum tightness of molecular distillation equipment still is 0.90-0.01KPa, and distillation temperature is 100-180 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001055232A CN1157400C (en) | 2000-03-30 | 2000-03-30 | Dealcoholizing process for preparing alkylglucoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001055232A CN1157400C (en) | 2000-03-30 | 2000-03-30 | Dealcoholizing process for preparing alkylglucoside |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1315327A CN1315327A (en) | 2001-10-03 |
| CN1157400C true CN1157400C (en) | 2004-07-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001055232A Expired - Fee Related CN1157400C (en) | 2000-03-30 | 2000-03-30 | Dealcoholizing process for preparing alkylglucoside |
Country Status (1)
| Country | Link |
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| CN (1) | CN1157400C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314695C (en) * | 2003-12-04 | 2007-05-09 | 兰州鸿卉生物科技有限公司 | Method for preparing alkyl glucoside |
| CN105461764A (en) * | 2015-12-11 | 2016-04-06 | 苏州华周胶带有限公司 | Method for refining alkyl polyglycoside |
| CN105418699B (en) * | 2015-12-29 | 2018-11-23 | 河北合佳医药科技集团有限公司 | The method of continuous production alkyl glycosides |
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2000
- 2000-03-30 CN CNB001055232A patent/CN1157400C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1315327A (en) | 2001-10-03 |
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Legal Events
| Date | Code | Title | Description |
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| PB01 | Publication | ||
| ASS | Succession or assignment of patent right |
Owner name: CHINA PETROLEUM CO., LTD. Free format text: FORMER OWNER: JILIN PETRIFICATION BRANCH ACADEMY, CHINA PETROLEUM AND NATURAL GAS STOCK CO., LTD. Effective date: 20020712 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20020712 Applicant after: China Petroleum & Natural Gas Co., Ltd. Applicant before: Research Inst of Jilin Petro-Chemical Branch, China National Petroleum Co., Ltd. |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040714 Termination date: 20160330 |