CN1076187A - The preparation method of high-purity monostearin - Google Patents
The preparation method of high-purity monostearin Download PDFInfo
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- CN1076187A CN1076187A CN 93101063 CN93101063A CN1076187A CN 1076187 A CN1076187 A CN 1076187A CN 93101063 CN93101063 CN 93101063 CN 93101063 A CN93101063 A CN 93101063A CN 1076187 A CN1076187 A CN 1076187A
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Abstract
The invention provides a kind of preparation method of high-purity monostearin.Be raw material wherein, with NaHCO with winterized stearin and glycerine
3-CO
2Mixture is a catalyzer, with CO
2Gas is shielding gas, carries out transesterification reaction under 230-260 ℃, obtains content and be the mixed ester of 40-60% glyceryl monostearate; be solvent with 95% ethanol then, after carrying out carrying in twice minute, mechanical separation; drying is made powder, gained glyceryl monostearate content 〉=90%.
Description
The present invention relates to a kind of organic chemical industry's product preparation, relate in particular to the preparation of glyceryl monostearate.
At present, " the preparation technology of " glyceryl monostearate " in the Chemicals handbook is adopted in the preparation of industrial glyceryl monostearate mostly, be that stearic acid and glycerine carry out esterification under the effect of NaOH catalyzer, cooling then, water dish, packing is a finished product, though the prepared product of technology also can directly apply to foodstuffs industry thus, daily chemical industry and medicine industry, but because it is a glyceryl monostearate, distearin, the mixture of Tristearoylglycerol, the content of its mono stearate glyceryl ester only reaches about 40%, thereby the effect that is used as emulsifying agent is relatively poor, the external employing carried out molecular distillation and isolated glyceryl monostearate product mixtures, its purity can reach more than 90%, according to " Guangdong chemical industry " 1989,3 introduce, and the Guangdong chemical institute is also successfully isolated glyceryl monostearate product more than 90% with molecular distillation method, still, the equipment complexity of this technology, processing difficulties is invested greatlyyer, make to use and to be restricted.
The purpose of this invention is to provide glyceryl monostearate content height in the elementary product of a kind of building-up reactions, separating device is simple, the preparation method of a kind of high-purity monostearin of good separating effect.
Technical scheme of the present invention is realized by following manner:
With winterized stearin and glycerine is raw material, NaHCO and CO
2The gas-solid mixture that forms is a catalyzer, with CO
2Be shielding gas, under 230-260 ℃, carry out transesterification reaction.Make solvent with ethanol then the reaction solid product is divided and carries, again through mechanical separation with dryly make powder promptly to obtain purity be 〉=90% mono stearate glyceryl ester.
Winterized stearin: NaHCO
3: CO
2=100(g): 0.4-0.5(g): 0.8-1.0(l).
Winterized stearin is preferably h-tallow, hydrogenated lard.
The solvent branch is carried preferably and is carried out twice, and dividing temperature raising for the first time is 35-30 ℃, and dividing the temperature raising degree for the second time is 29-25 ℃, and the solute ratio is preferably 1: 8-1: 10.
The preferred centrifugation of mechanical separation, rotating speed are 6000-8000r.pm.
Positively effect of the present invention is: mono stearate glyceryl ester content can reach 50-62% in the product of transesterification reaction, separating device is simple, processing ease, separate back glyceryl monostearate purity and can reach more than 90%, meet the ISO7366 standard, reduced production cost of products.
Under the normal temperature, glycerine solubleness in grease is about 4%, the theoretical requirement of glycerine in the alcoholysis reaction, and high temperature can significantly increase the solubleness of glycerine in grease, but then can cause the stock oil oxidation if temperature is too high, thereby preferable reaction temperature of the present invention is 255 ° ± 5 ℃, this temperature down glycerine solubleness in winterized stearin than improving more than 10 times under the normal temperature.
The present invention feeds CO
2Gas has the effect of two aspects.The one, get rid of reactive system hollow G﹠W part; The 2nd, the CO in the reaction solution
2Gas and NaHCO
3Form gas one solid mixed catalyst.Its catalytic mechanism is under the winterized stearin hot conditions and NaHCO
3Saponification reaction takes place emit CO
2Gas, CO
2Meet with soap lye the acidification reaction that carbonic acid decomposes soda soap, i.e. CO take place
2Can make sodium soap be decomposed into lipid acid and produce NaHCO
3, NaHCO
3Through thermal conversion is Na
2CO
3, reaction formula is as follows:
R-C
17H
15, above-mentioned reaction is yellow soda ash saponification-carbonic acid gas acidifying-yellow soda ash saponification.Can form a circulation catalysis system like this, thereby guarantee the transesterification reaction of winterized stearin with glycerine.
Fig. 1 is preparation technology's schema of the present invention.
Below in conjunction with accompanying drawing the present invention is described in further detail.
With the pre-heat fusing of winterized stearin, add glycerine then and mix, add NaHCO again
3, and feed CO
2Gas starts to stir and continues to heat up, and when temperature reaches 230-260 ℃, is incubated 25-35 minute.After then reaction product directly being carried out centrifugation and removed unreacted glycerine, be the dissolution with solvents reaction product with ethanol.The solute ratio is 1: 10, carries in twice minute 35-31 ℃ and 29-25 ℃ and separates out two, behind the Tristearoylglycerol.Solution continues cold analysis to temperature and separates out glyceryl monostearate-10 ℃-15 ℃ the time.Isolate ethanolic soln with whizzer then, rotating speed is 6000 8000r.pm, with the solid reheat fusion after separating, make powder.Promptly getting glyceryl monostearate purity is 〉=90%.
Embodiment 1,100 gram sclerosis lards are put into four-hole boiling flask, heating and melting adds 40 gram glycerine again to 70-80 ℃, continues to be warming up to 240 ℃, adds 0.5 gram NaHCO then
3, start and stir and feed CO
2Gas, flow is 0.61/min, makes temperature rise to 255 ℃, constant temperature 25 minutes, cooling discharging is isolated glycerine with above-mentioned reaction product with supercentrifuge, and its rotating speed is 6000r.pm, obtains glyceryl monostearate content and be 52% mixed ester.Take by weighing 50 gram mixed esters then, by the solute ratio is 1: 10 adding 95% ethanol 400ml, and the heating for dissolving mixed ester then makes its naturally cooling, carry out dividing to carry the first time isolating solid at 31 ℃, continue to be cooled to divide 25 ℃ of second time and propose separate solid, the solution cold analysis again after proposing in twice minute, in the time of-10 ℃, separate out glyceryl monostearate, centrifugation goes out ethanolic soln, and rotating speed is 8000r.pm, to solid heating, fusion after separating, making powder, promptly to get glyceryl monostearate content be 91%.
Embodiment 2: 100 gram hardened tallow heating and meltings to 70-80 ℃, are added glycerine 40 grams, and continuing to heat up mixes its reactant, adds 0.5 gram NaHCO
3, and feed CO
2Gas, flow is 0.81/min, stir, be warming up to 255 ℃, constant temperature 28 minutes, cooling, isolate glycerine with supercentrifuge, rotating speed is 7000rpm, obtains content and be the mixed ester of 58% glyceryl monostearate, takes by weighing 50 gram mixed esters then, press solute and added 95% ethanol 400ml than 1: 8, the heating for dissolving mixed ester makes its naturally cooling, 32 ℃ and 26 ℃ of propositions two in twice minute, Tristearoylglycerol, then with solution cold analysis again, temperature is separated out glyceryl monostearate in the time of 15 ℃, centrifugation goes out ethanolic soln, and rotating speed is the solid heating and melting after 7000rpm separates, making powder gained glyceryl monostearate content is 95%.
Embodiment 3: 100 gram sclerosis lard heating and meltings to 70-80 ℃, are added 30 gram glycerine, be heated to 240 ℃ and make its mixing, feed CO
2Gas, flow are 1l/min, add 0.5 gram NaHCO
3Stir, be warming up to 260 ℃, constant temperature cooling in 30 minutes, centrifugation goes out glycerine, and rotating speed is 7000r.pm, glyceryl monostearate content is 53% mixed ester, take by weighing 50 gram mixed esters then, press solute and added 95% ethanol 500ml, behind the heating for dissolving mixed ester than 1: 10, naturally cooling, proposed two in twice minute 33 ℃ and 26 ℃, Tristearoylglycerol, when solution continues cold analysis to 7 ℃, separate out glyceryl monostearate, centrifugation goes out ethanolic soln, rotating speed is 8000r.pm, and the solid heating and melting after separating is made powder, and getting the sweet fat ester content of Stearinsaeure is 93%.
Embodiment 4: 100 gram winterized stearin heating and meltings to 70-80 ℃, are added 35 gram glycerine, be heated to 240 ℃, add 0.5 gram NaHCO
3, feed CO
2, flow is 0.9l/min, stirs and is warming up to 258 ℃, constant temperature 30 minutes, cooling.Centrifugation goes out glycerine, and rotating speed is 7500r.pm, glyceryl monostearate content is 52.5% mixed ester.Then, take by weighing 50 gram mixed esters, press solute and added 95% ethanol 500ml, behind the heating for dissolving mixed ester, make its naturally cooling than 1: 10, at 35 ℃ of time-divisions propositions two, Tristearoylglycerol, behind 25 ℃ of time-divisions propositions two, Tristearoylglycerol, solution continues cooling, separates out mono stearate glyceryl ester in the time of 10 ℃, then, centrifugation goes out alcohol solvent.Rotating speed is 6000r.pm, and the solid heating and melting after the separation, making powder, promptly to get glyceryl stearate content be 92%.
Claims (7)
1, a kind of preparation method of high-purity monostearin, it comprises with winterized stearin and glycerine is that raw material carries out transesterification reaction, it is characterized in that it is catalyzer that gas-solid mixture is adopted in reaction, CO
2Gas is shielding gas, is reflected under 230-260 ℃ to carry out, directly reaction mixture is isolated glycerine then after, make the solid of solvent after with ethanol and carry out carrying in twice minute separation of glycerin, make powder through mechanical separation and drying again.
2, a kind of preparation method of high-purity monostearin according to claim 1 is characterized in that described winterized stearin is hardened tallow or sclerosis lard.
3, a kind of preparation method as high-purity monostearin as described in the claim 2 is characterized in that described gas one solid mixture is NaHCO
3-CO
2The mixture of (gas).
4, a kind of preparation method as high-purity monostearin as described in the claim 3 is characterized in that winterized stearin (g): NaHCO
3(g): CO
2(l)=100: 0.4-0.5: 0.8-1.0.
5, a kind of preparation method as any high-purity monostearin as described in the claim 1-4 is characterized in that carrying to dividing the temperature raising degree for the first time in described twice minute is 35-31 ℃, and dividing the temperature raising degree for the second time is 28-25 ℃.
6, a kind of preparation method as high-purity monostearin as described in the claim 5 is characterized in that described mechanical separation is centrifugation, and rotating speed is 6000-8000r.pm.
7, a kind of preparation method as high-purity glycerol monostearate as described in the claim 5 is characterized in that the described solute ratio of carrying in twice minute is 1: 8-1: 10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101063 CN1076187A (en) | 1993-01-19 | 1993-01-19 | The preparation method of high-purity monostearin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101063 CN1076187A (en) | 1993-01-19 | 1993-01-19 | The preparation method of high-purity monostearin |
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| CN1076187A true CN1076187A (en) | 1993-09-15 |
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ID=4983390
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| CN 93101063 Pending CN1076187A (en) | 1993-01-19 | 1993-01-19 | The preparation method of high-purity monostearin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914016A (en) * | 2010-08-17 | 2010-12-15 | 聊城大学 | Quick preparation method of glycerin monostearate |
| CN102964245A (en) * | 2012-11-28 | 2013-03-13 | 广州嘉德乐生化科技有限公司 | Preparation method of high-quality glycerin monostearate |
| CN103205315A (en) * | 2012-01-12 | 2013-07-17 | 江西永友化工助剂有限公司 | Monoglyceride production technology and residue separation and purification technology |
| CN105418414A (en) * | 2015-12-22 | 2016-03-23 | 杭州富春食品添加剂有限公司 | Production method for glycerol monostearate and glycerol distearate |
| US20180105685A1 (en) * | 2015-05-07 | 2018-04-19 | Fine Organics Industries Ptv. Ltd. | Polypropylene cap or film composition |
-
1993
- 1993-01-19 CN CN 93101063 patent/CN1076187A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914016A (en) * | 2010-08-17 | 2010-12-15 | 聊城大学 | Quick preparation method of glycerin monostearate |
| CN101914016B (en) * | 2010-08-17 | 2013-01-02 | 聊城大学 | Quick preparation method of glycerin monostearate |
| CN103205315A (en) * | 2012-01-12 | 2013-07-17 | 江西永友化工助剂有限公司 | Monoglyceride production technology and residue separation and purification technology |
| CN103205315B (en) * | 2012-01-12 | 2017-12-22 | 江西益普畅新材料应用研究推广有限公司 | A kind of production technology of monoglyceride and the separation purifying technique of slag charge |
| CN102964245A (en) * | 2012-11-28 | 2013-03-13 | 广州嘉德乐生化科技有限公司 | Preparation method of high-quality glycerin monostearate |
| US20180105685A1 (en) * | 2015-05-07 | 2018-04-19 | Fine Organics Industries Ptv. Ltd. | Polypropylene cap or film composition |
| US10557025B2 (en) * | 2015-05-07 | 2020-02-11 | Fine Organics Industries Pvt Ltd. | Polypropylene cap or film composition |
| CN105418414A (en) * | 2015-12-22 | 2016-03-23 | 杭州富春食品添加剂有限公司 | Production method for glycerol monostearate and glycerol distearate |
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