CN102775275A - Refined glycerol purification process - Google Patents
Refined glycerol purification process Download PDFInfo
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- CN102775275A CN102775275A CN2012103261536A CN201210326153A CN102775275A CN 102775275 A CN102775275 A CN 102775275A CN 2012103261536 A CN2012103261536 A CN 2012103261536A CN 201210326153 A CN201210326153 A CN 201210326153A CN 102775275 A CN102775275 A CN 102775275A
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Abstract
The invention discloses a refined glycerol purification process. The purification process comprises the following steps: by taking sweet water which is a fatty acid byproduct as the raw material, performing hydrochloric acid acidification pretreatment, oil-water separation pretreatment and saponification pretreatment to remove impurities; and performing further purification in the subsequent refining process to obtain refined glycerol having a purity of 99.5% or above.
Description
Technical field
The invention belongs to a kind of purifying technique of glycerine, be specifically related to the technology of the smart glycerine of purification from the fatty acid by-products sugar water.
Background technology
CN200910176557.X provides a kind of sweet water fatty acid separation process, before sugar water adds the milk of lime saponification, adopts hydrochloric acid to fatty acid separation, makes sugar water more pure, thereby reaches the purpose that reduces saponification equivalent.The focusing on of this patent described the technological process before the sugar water saponification is handled, to the separation of follow-up glycerine and not mentioned.
Summary of the invention
The object of the present invention is to provide a kind of technology of the smart glycerine of from the fatty acid by-products sugar water, purifying.
In order to solve the problems of the technologies described above; The technical scheme that the present invention adopts is following: a kind of purifying technique of smart glycerine; With the fatty acid by-products sugar water is raw material; Remove impurity through hcl acidifying, oily water separation saponification pre-treatment step, thereby obtain smart glycerine through the treating process glycerine bullion of further purifying again, it is characterized in that: described treating process may further comprise the steps:
1) sugar water after the oily water separation is squeezed in the alkaline purification still, the milk of lime that adds 1-3wt% carries out saponification to be handled, and the pH value of solution value is remained between the 8-9, and reaction solution is transported in the strainer, and the lipid acid calcium deposit is removed in press filtration, obtains the sugar water of concentration at 20-35wt%;
2) adopt the evaporation of multiple-effect self-circulation thickener to dewater in above-mentioned sugar water, after concentrating, obtain the raw glycerine of 90wt%;
3) raw glycerine is sent into the glycerol distillation tower and purify, collection output gets into the deodorization tower to smart glycerine from the tower middle part, and the black pin of glycerine continues to refine smart glycerine from the black pin still kettle of tower still discharging entering;
4) the smart glycerine that black pin still kettle in the step 3) is refined; Send into the rectifying of glycerine rectifying tower; Smart glycerine after the rectifying is returned to the glycerol distillation tower and evaporates once more, and remaining residue then is stored in the residue collection jar in the black pin still kettle, finally is back in the sugar water for use;
5) getting into the smart glycerine of deodorization tower in the step 3), after the deodorization heat exchange, is 80-90 ℃ in temperature, and pressure is the input bleaching tower processing of decolouring under the condition of 0.35MPa, is packaged into smart glycerine finished product after the decolouring.
Preferably, the tower of glycerol distillation described in the step 3, the temperature of heating raw glycerine is 175 ℃, and pressure be-0.098MPa, and the sprinkling that refluxes of whole tops is adopted in the distillation tower middle and upper part, and collecting temperature is 150 ℃, the middle part collecting temperature is 155 ℃.
Preferably, black pin still kettle in the step 3, distillation temperature are 195 ℃ ~ 200 ℃, pressure is-and 0.095MPa ~-0.1MPa.
Preferably, glycerine rectifying tower temperature is 180 ~ 185 ℃ in the step 4, tower press for-0.095MPa ~-0.1MPa.
Preferably, deodorization tower operational condition is 115 ~ 125 ℃ of temperature in the step 5, pressure 0.096MPa, and the bleaching tower operational condition is 80 ~ 90 ℃ of temperature, pressure is 0.2MPa ~ 0.4MPa.
The invention has the advantages that: the present invention is a raw material with the fatty acid by-products sugar water, removes impurity through hcl acidifying, oily water separation saponification pre-treatment step, and further purifying through treating process, to obtain purity be the smart glycerine more than 99.5% again.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The fatty acid by-products sugar water derives from Rugao Shuangma Chemical Co., Ltd..
As shown in Figure 1, the fatty acid by-products sugar water is a raw material, through hcl acidifying; Keep the pH value of solution value between 3.4-4, through water-and-oil separator sugar water, lipid acid and impurity are separated, the sugar water after the processing is squeezed in the alkaline purification still; The milk of lime that adds 1-3wt% carries out saponification to be handled, and the pH value of solution value is remained between the 8-9, and reaction solution is transported in the strainer; The lipid acid calcium deposit is removed in press filtration, obtains the sugar water of concentration at 20-35wt%;
Sugar water adopts the evaporation of multiple-effect self-circulation thickener to dewater, and after concentrating, obtains the raw glycerine of 90wt%; Raw glycerine is sent into the glycerol distillation tower and is purified, and under vacuum pressure-0.098MPa, adds thermal material to 175 ℃ explosive evaporatoin; The distillation tower middle and upper part adopts the backflow of whole tops to spray; Collecting temperature is 150 ℃, and smart glycerine is gathered at the middle part, and collecting temperature is 155 ℃;
The black pin of distillation Tata still discharging glycerine gets into black pin still kettle, is 195 ℃ ~ 200 ℃ in distillation temperature, and pressure be-0.095MPa ~-continue refinement glycerine under the 0.1MPa condition; The glycerine that extracts is sent into the glycerine rectifying tower and is returned to the glycerol distillation tower; Wherein, glycerine rectifying tower operational condition: temperature is 180 ~ 185 ℃, tower press for-0.095MPa ~-0.1MPa; Remaining residue then is stored in the residue collection jar in the black pin still kettle, finally returns in the hydrolysis sugar water for use;
Smart glycerine output after the collection gets into the deodorization tower, 115 ~ 125 ℃ of temperature, under the pressure 0.096MPa condition through after the deodorization heat exchange; And it is 80-90 ℃ in temperature; Pressure is to import bleaching tower under the condition of 0.35MPa, and decolouring is handled, and the decolouring treatment temp is 80 ~ 90 ℃; Pressure is 0.2MPa ~ 0.4MPa, is packaged into smart glycerine finished product after the decolouring.
The quality examination result of finished product is: smart glycerine purity is greater than 99.5%.
Claims (5)
1. the purifying technique of a smart glycerine; With the fatty acid by-products sugar water is raw material; Remove impurity through hcl acidifying, oily water separation saponification pre-treatment step; Thereby obtain smart glycerine through the treating process glycerine bullion of further purifying again, it is characterized in that: described treating process may further comprise the steps:
1) sugar water after the oily water separation is squeezed in the alkaline purification still, the milk of lime that adds 1-3wt% carries out saponification to be handled, and the pH value of solution value is remained between the 8-9, and reaction solution is transported in the strainer, and the lipid acid calcium deposit is removed in press filtration, obtains the sugar water of concentration at 20-35wt%;
2) adopt the evaporation of multiple-effect self-circulation thickener to dewater in above-mentioned sugar water, after concentrating, obtain the raw glycerine of 90wt%;
3) raw glycerine is sent into the glycerol distillation tower and purify, collection output gets into the deodorization tower to smart glycerine from the tower middle part, and the black pin of glycerine continues to refine smart glycerine from the black pin still kettle of tower still discharging entering;
4) the smart glycerine that black pin still kettle in the step 3) is refined; Send into the rectifying of glycerine rectifying tower; Smart glycerine after the rectifying is returned to the glycerol distillation tower and evaporates once more, and remaining residue then is stored in the residue collection jar in the black pin still kettle, finally is back in the sugar water for use;
5) getting into the smart glycerine of deodorization tower in the step 3), after the deodorization heat exchange, is 80-90 ℃ in temperature, and pressure is the input bleaching tower processing of decolouring under the condition of 0.35MPa, is packaged into smart glycerine finished product after the decolouring.
2. the purifying technique of a kind of smart glycerine according to claim 1; It is characterized in that: the tower of glycerol distillation described in the step 3; The temperature of heating raw glycerine is 175 ℃, and pressure is-0.098MPa that the distillation tower middle and upper part adopts the backflow of whole tops to spray; Collecting temperature is 150 ℃, and the middle part collecting temperature is 155 ℃.
3. the purifying technique of a kind of smart glycerine according to claim 1, it is characterized in that: black pin still kettle in the step 3, distillation temperature are 195 ℃ ~ 200 ℃, pressure is-0.095MPa ~-0.1MPa.
4. the purifying technique of a kind of smart glycerine according to claim 1, it is characterized in that: glycerine rectifying tower temperature is 180 ~ 185 ℃ in the step 4, tower press for-0.095MPa ~-0.1MPa.
5. the purifying technique of a kind of smart glycerine according to claim 1, it is characterized in that: deodorization tower operational condition is 115 ~ 125 ℃ of temperature in the step 5, pressure 0.096MPa, the bleaching tower operational condition is 80 ~ 90 ℃ of temperature, pressure is 0.2MPa ~ 0.4MPa.
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| CN2012103261536A CN102775275A (en) | 2012-09-06 | 2012-09-06 | Refined glycerol purification process |
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| CN2012103261536A CN102775275A (en) | 2012-09-06 | 2012-09-06 | Refined glycerol purification process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262104A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104262101A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104707353A (en) * | 2015-02-12 | 2015-06-17 | 浙江华诺化工有限公司 | Glycerin distillation system |
| CN105085171A (en) * | 2015-04-16 | 2015-11-25 | 彭才文 | High purity glycerin refining method by using saponification hydrolysis esterification byproduct |
| CN106866370A (en) * | 2016-12-31 | 2017-06-20 | 衡阳市晨丰生物科技有限公司 | A kind of method of lipid in removing crude glycerine |
| WO2017119007A1 (en) | 2016-01-07 | 2017-07-13 | Institute Of Chemical Technology | Process for purification and refining of glycerol |
| CN115745746A (en) * | 2022-07-29 | 2023-03-07 | 湖北天基生物能源科技发展有限公司 | Glycerol refining method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696155A (en) * | 2009-09-23 | 2010-04-21 | 如皋市双马化工有限公司 | Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same |
| CN102391069A (en) * | 2011-09-05 | 2012-03-28 | 德源(中国)高科有限公司 | Preparation method of high-purity glycerol |
-
2012
- 2012-09-06 CN CN2012103261536A patent/CN102775275A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696155A (en) * | 2009-09-23 | 2010-04-21 | 如皋市双马化工有限公司 | Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same |
| CN102391069A (en) * | 2011-09-05 | 2012-03-28 | 德源(中国)高科有限公司 | Preparation method of high-purity glycerol |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262104A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104262101A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104707353A (en) * | 2015-02-12 | 2015-06-17 | 浙江华诺化工有限公司 | Glycerin distillation system |
| CN105085171A (en) * | 2015-04-16 | 2015-11-25 | 彭才文 | High purity glycerin refining method by using saponification hydrolysis esterification byproduct |
| WO2017119007A1 (en) | 2016-01-07 | 2017-07-13 | Institute Of Chemical Technology | Process for purification and refining of glycerol |
| CN106866370A (en) * | 2016-12-31 | 2017-06-20 | 衡阳市晨丰生物科技有限公司 | A kind of method of lipid in removing crude glycerine |
| CN106866370B (en) * | 2016-12-31 | 2020-10-30 | 衡阳市晨丰生物科技有限公司 | Method for removing lipid in crude glycerol |
| CN115745746A (en) * | 2022-07-29 | 2023-03-07 | 湖北天基生物能源科技发展有限公司 | Glycerol refining method |
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