CN101092359A - Method for extracting diglyceride from tailings of molecular distillation of glyceride - Google Patents
Method for extracting diglyceride from tailings of molecular distillation of glyceride Download PDFInfo
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- CN101092359A CN101092359A CNA2007100288979A CN200710028897A CN101092359A CN 101092359 A CN101092359 A CN 101092359A CN A2007100288979 A CNA2007100288979 A CN A2007100288979A CN 200710028897 A CN200710028897 A CN 200710028897A CN 101092359 A CN101092359 A CN 101092359A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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Abstract
This invention discloses a method for extracting diglyceride from trash of monoglyceride production by molecular distillation. The method comprises: adding a certain amount of trash into a reaction kettle, adding reductant and decolorant (0.1-10 wt. % of trash) for reduction and decolorization, filtering, and extracting the filtrate by three-stage molecular distillation to obtain diglyceride. The low molecular reductant is H2O2 or ozone compound. The decolorant is activated carbon or diatomite. The content of the obtained diglyceride is higher than 90%.
Description
Technical field
The present invention relates to a kind of production method of triglyceride, particularly a kind of method of from the tankage of molecule distillating monoglyceride, extracting triglyceride.
Background technology
Chinese patent (application number) ZL200310112327.X, ZL03113862.4, ZL200410015348.4, ZL200610049242.5 are disclosed all to be about adopting solidification lipase to carry out the technology of synthetic triglyceride at low temperatures.Chinese patent ZL200410015388.9 and Chinese patent ZL200410015388.9 are disclosed to be about producing the production technique of the triglyceride that unsaturated fatty acids occupies the majority, the diglyceride content of producing does not reach more than 90% yet, does not adopt reductive agent to decolour yet.The PCTWO999119 disclosed method is to be hydrolyzed at 240 ℃ by immobilized enzyme, and the source of lipid acid does not comprise plam oil, PCTWO2003060139 is disclosed to be to adopt the immobilization partial glyceride lipase, produce lipid acid then, make lipid acid and glycerine reaction and obtain triglyceride, the production method of these triglycerides all is to produce this product specially, is not that the tankage of the present molecule distillating monoglyceride of employing are the method that raw material is purified.
The domestic bibliographical information of publishing is crossed a kind of purification techniques of triglyceride, and this technology is triglyceride and the by product mono-glycerides that obtains purifying from the mixture of enzyme process triglyceride by liquid abstraction technique; In addition, enzyme process glycerine is separated synthetic triglyceride, fixed lipase catalyzed synthetic triglyceride, glycerolysis and is produced the research of the water vapour purification techniques of triglyceride, triglyceride and enzyme process reaction purification techniques etc. bibliographical information is also arranged, but the shortcoming of this employing enzyme method is must be through the separation of lipid acid, purification, carry out the selective enzymatic reaction again, and it is infeasible adopting these methods in industrial actual production.Present technical disadvantages is to carry out industrialized production, all is to rest on breadboard conceptual phase, because the raw material and the technology that adopt all are that industrial production is beyond one's reach, can operate and control is wanting in.Do not have at present any as yet about from the by product of molecular distillation, extracting the correlation technique of triglyceride.
Summary of the invention
The objective of the invention is to solve the problem of above-mentioned existence, a kind of method that can extract triglyceride from present molecule distillating monoglyceride industry repeatedly the round-robin tankage is provided.Utilize the resultant triglyceride of this method not only color be very shallow, content surpasses 90%, but and outward appearance and color meet requirement, and the suitability for industrialized production of food grade fully.This method has been started the novel process of triglyceride industrialization.
Technical scheme of the present invention is achieved in that
A kind of method of extracting triglyceride from the tankage of molecule distillating monoglyceride comprises the steps:
(1), will put into the vacuum reaction still and the vacuum reaction still heated from the tankage raw material that molecule distillating monoglyceride obtains described tankage raw material is melted by with filtration unit that described vacuum reaction still directly is connected the tankage raw material being filtered, to remove the tankage impurities in raw materials again;
(2), add 0.1%～10% the reductive agent that accounts for the tankage raw material weight in the vacuum reaction still and carry out reduction-decolor and handle, the vacuum pressure that this moment, described reduction-decolor was handled is-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～150 ℃, and the time is 10～600 minutes;
(3), add 0.2%～20% the discoloring agent that accounts for the tankage raw material weight processings of decolouring in the vacuum reaction still, this moment the vacuum pressure of described decolouring processing be-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～200 ℃, and the time is 10～600 minutes;
(4), by the material in the vacuum reaction still being filtered to remove the impurity in the material with the direct-connected filtration unit of vacuum reaction still;
(5), will carry out the two-stage molecular distillation through the material in the reactor after filtering and extract filtered liquid, resulting distillate is triglyceride.
Wherein the vacuum pressure of the first step molecular distillation in the above-mentioned steps (five) is that 30～100Pa, temperature are 160～250 ℃, its objective is the glycerol content in the tankage is dropped to below 1%, the vacuum pressure of second stage molecular distillation is that 20～100Pa, temperature are 150～250 ℃, its objective is the free acid in the tankage is removed that free acid content is reduced to below 1.0%.
In order further the mono-glycerides in the tankage being removed, and content of monoglyceride to be reduced to below 5.0%, also to include third stage molecular distillation in the above-mentioned steps (five) and purify, this grade molecule distillatory vacuum pressure is 0.1～10.0Pa, and temperature is 140～250 ℃.
Advantage of the present invention is:
1, utilized the tankage of present molecule distillating monoglyceride fully, it is turned waste into wealth.
2, proposed to adopt low molecule reductive agent (as hydrogen peroxide, ozonide) and discoloring agent (as gac and diatomite) bonded method to carry out the comprehensive decolouring processing of chemistry and physics.
3, adopt three grades of molecule distillatory methods to make the content of the triglyceride that obtains by the tankage purification greater than 90%.
The invention will be further described below in conjunction with drawings and Examples:
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The method of extracting triglyceride from the tankage of molecule distillating monoglyceride of the present invention comprises the steps:
(1), will put into the vacuum reaction still and the vacuum reaction still heated from the tankage raw material that molecule distillating monoglyceride obtains described tankage raw material is melted by with filtration unit that described vacuum reaction still directly is connected the tankage raw material being filtered, to remove the tankage impurities in raw materials again;
(2), add 0.1%～10% the reductive agent that accounts for the tankage raw material weight in the vacuum reaction still and carry out reduction-decolor and handle, the vacuum pressure that this moment, described reduction-decolor was handled is-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～150 ℃, and the time is 10～600 minutes;
(3), add 0.2%～20% the discoloring agent that accounts for the tankage raw material weight processings of decolouring in the vacuum reaction still, this moment the vacuum pressure of described decolouring processing be-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～200 ℃, and the time is 10～600 minutes;
Wherein above-mentioned reductive agent is hydrogen peroxide or superoxide or ozonide or other low molecule reductive agent.Above-mentioned discoloring agent is gac or diatomite or carclazyte or its both mixture.It is that 30～100Pa, temperature are 160～250 ℃ that first step molecule in the above-mentioned steps (five) steams the vacuum pressure that stays, and the vacuum pressure of second stage molecular distillation is that 20～100Pa, temperature are 150～250 ℃.
(4), by the material in the vacuum reaction still being filtered to remove the impurity in the material with the direct-connected filtration unit of vacuum reaction still;
(5), will carry out the two-stage molecular distillation through the material in the reactor after filtering and extract filtered liquid, resulting distillate is triglyceride.
Wherein the vacuum pressure of the first step molecular distillation in the above-mentioned steps (five) is that 30～100Pa, temperature are 160～250 ℃, its objective is the glycerol content in the tankage is dropped to below 1%, the vacuum pressure of second stage molecular distillation is that 20～100Pa, temperature are 150～250 ℃, its objective is the free acid in the tankage is removed that free acid content is reduced to below 1.0%.Its preferable embodiment is: the vacuum pressure of first step molecular distillation is that 40Pa, temperature are 200 ℃, and the vacuum of second stage molecular distillation is that 35Pa, temperature are 190 ℃.In order will to remove the mono-glycerides in the tankage, and content of monoglyceride is reduced to below 5.0%, above-mentioned steps (five) also includes third stage molecular distillation and purifies, and this grade molecule distillatory vacuum pressure is 0.1～10.0Pa, and temperature is 140～250 ℃.The preferred version that molecule steaming is this time stayed is vacuum 1.0Pa, and temperature is 200 ℃.
The tankage of molecule distillating monoglyceride of the present invention comprise the saturated or unsaturated of industries such as molecular distillation glyceryl monostearate, molecular distillation monopalmitin, molecular distillation glyceryl monolaurate, molecular distillation Dan Xinkui acid glyceride, perhydro-or partial hydrogenation, the mixture of one or several in the tankage of hydrogenated raw material oil not even.The raw material of above-mentioned production molecular distillation glyceryl monostearate, molecular distillation monopalmitin, molecular distillation glyceryl monolaurate, molecular distillation Dan Xinkui acid glyceride can be from the oil of natural animal-plant oil and transesterify as a result, modification, as: a kind of oil in soya-bean oil, plam oil, palm-kernel oil, lard, butter, sheep oil, peanut oil, Trisun Oil R 80, Thistle oil, fish oil, theobroma oil, Oleum Gossypii semen, sardine oil, sea-buckthorn wet goods perhydro-or the partial hydrogenation oil or the mixing oil thing of several oil.
The invention belongs to the foodstuff additive industry, its key equipment is to adopt the molecular distillation technique of Ministry of Science and Technology's keypoint recommendation and " energy-efficient consumption-reducing technological and the related products " that country advocates, thereby guarantee that effectively the present invention can completely realize the green circulation of industry reliably, thereby promote molecule distillating monoglyceride industry competitive capacity in the world comprehensively.And provide a triglyceride product that can carry out extensive industrialization.
Embodiment 1:
With molecule distillating monoglyceride tankage double centner, place the reactor of 200L, heating and melting to 100 ℃, filter 2 times by the pressure filter that is connected then, connect vacuum system, make vacuum reach-0.1Mpa, add thermal material to 110 ℃, add 1 kilogram of concentration and be 30% hydrogen peroxide, keep this temperature to stir 30 minutes.Temperature is reduced to 100 ℃, utilize vacuum to suck 1 kilogram of gac and 1 kilogram of diatomite and stirred 30 minutes, temperature is filtered after being reduced to 80 ℃ repeatedly, up to clear excessively, do not have till the impurity, enter three grades of molecule Distallation systms, keeping the vacuum pressure of first step molecular distillation is 40Pa, temperature is 200 ℃, keeping the vacuum pressure of second stage molecular distillation is 35Pa, temperature is 190 ℃, and keeping the vacuum pressure of third stage molecular distillation is 1.0Pa, and temperature is 200 ℃, the triglyceride that distilled in 10 minutes that begins the most distillation that refluxes again, begin to collect distillage then.Get about 89 kilograms of triglyceride (being not included in ducted material) at last, detection level is a triglyceride 94.7%.
Embodiment 2:
With 500 kilograms of molecule distillating monoglyceride tankage, place the reactor of 5000L, heating and melting to 100 ℃, filter 2 times by the pressure filter that is connected then, connect vacuum system, make vacuum reach-0.1Mpa, add thermal material to 105 ℃, add 10 kilograms of concentration and be 30% hydrogen peroxide, keep this temperature to stir 60 minutes.Temperature is reduced to 85 ℃, utilize vacuum to suck 20 kilograms of gacs and 20 kilograms of diatomite, stirred 60 minutes, filter repeatedly after temperature is reduced to 80 ℃, up to clear excessively, do not have till the impurity, enter three grades of molecule Distallation systms, keeping the vacuum pressure of first step molecular distillation is 40Pa, temperature is 200 ℃, and keeping the vacuum pressure of second stage molecular distillation is 35Pa, and temperature is 190 ℃, keeping the vacuum pressure of third stage molecular distillation is 0.8Pa, temperature is 198 ℃, the triglyceride that distilled in 20 minutes that begins is most refluxed distill again, begins to collect distillage then.Get about 465 kilograms of triglyceride (being not included in ducted material) at last, detection level is a triglyceride 92.3%.
Embodiment 3:
With molecule distillating monoglyceride tankage double centner, place the reactor of 200L, heating and melting to 100 ℃, filter 2 times by the pressure filter that is connected then, connect vacuum system, make vacuum reach-0.001Mpa, add thermal material to 150 ℃, add 10 kilograms of concentration and be 30% hydrogen peroxide, keep this temperature to stir 10 minutes.Temperature is reduced to 100 ℃, utilize vacuum to suck 0.1 kilogram of gac and 0.1 kilogram of diatomite and stirred 600 minutes, temperature is filtered after being reduced to 50 ℃ repeatedly, up to clear excessively, do not have till the impurity, enter three grades of molecule Distallation systms, keeping the vacuum pressure of first step molecular distillation is 30Pa, temperature is 250 ℃, keeping the vacuum pressure of second stage molecular distillation is 20Pa, temperature is 250 ℃, and keeping the vacuum pressure of third stage molecular distillation is 0.1Pa, and temperature is 250 ℃, the triglyceride that distilled in 20 minutes that begins the most distillation that refluxes again, begin to collect distillage then.Get about 89 kilograms of triglyceride (being not included in ducted material) at last, detection level is a triglyceride 94.7%.
Embodiment 4:
With molecule distillating monoglyceride tankage double centner, place the reactor of 200L, heating and melting to 100 ℃, filter 2 times by the pressure filter that is connected then, connect vacuum system, make vacuum reach-0.1Mpa, add thermal material to 200 ℃, add 1 kilogram of concentration and be 30% superoxide, keep this temperature to stir 30 minutes.Temperature is reduced to 100 ℃, utilize vacuum to suck 1 kilogram of gac and 1 kilogram of diatomite and stirred 100 minutes, temperature is filtered after being reduced to 80 ℃ repeatedly, up to clear excessively, do not have till the impurity, enter three grades of molecule Distallation systms, keeping the vacuum pressure of first step molecular distillation is 100Pa, temperature is 160 ℃, keeping the vacuum pressure of second stage molecular distillation is 100Pa, temperature is 150 ℃, and keeping the vacuum pressure of third stage molecular distillation is 10Pa, and temperature is 140 ℃, the triglyceride that distilled in 10 minutes that begins the most distillation that refluxes again, begin to collect distillage then.Get about 90 kilograms of triglyceride (being not included in ducted material) at last, detection level is a triglyceride 94.7%.
Embodiment 5:
With molecule distillating monoglyceride tankage double centner, place the reactor of 200L, heating and melting to 100 ℃, filter 2 times by the pressure filter that is connected then, connect vacuum system, make vacuum reach-0.1Mpa, add thermal material to 110 ℃, add 1 kilogram of concentration and be 30% ozonide, keep this temperature to stir 30 minutes.Temperature is reduced to 100 ℃, utilize vacuum to suck 1 kilogram of gac and 1 kilogram of diatomite and stirred 30 minutes, temperature is filtered after being reduced to 80 ℃ repeatedly, up to clear excessively, do not have till the impurity, enter three grades of molecule Distallation systms, keeping the vacuum pressure of first step molecular distillation is 40Pa, temperature is 200 ℃, keeping the vacuum pressure of second stage molecular distillation is 35Pa, temperature is 190 ℃, and keeping the vacuum pressure of third stage molecular distillation is 1.0Pa, and temperature is 200 ℃, the triglyceride that distilled in 10 minutes that begins the most distillation that refluxes again, begin to collect distillage then.Get about 88 kilograms of triglyceride (being not included in ducted material) at last, detection level is a triglyceride 94.7%.
Claims (8)
1, a kind of method of extracting triglyceride from the tankage of molecule distillating monoglyceride is characterized in that in turn including the following steps:
(1), will put into the vacuum reaction still and the vacuum reaction still heated from the tankage raw material that molecule distillating monoglyceride obtains described tankage raw material is melted by with filtration unit that described vacuum reaction still directly is connected the tankage raw material being filtered, to remove the tankage impurities in raw materials again;
(2), add 0.1%～10% the reductive agent that accounts for the tankage raw material weight in the vacuum reaction still and carry out reduction-decolor and handle, the vacuum pressure that this moment, described reduction-decolor was handled is-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～150 ℃, and the time is 10～600 minutes;
(3), add 0.2%～20% the discoloring agent that accounts for the tankage raw material weight processings of decolouring in the vacuum reaction still, this moment the vacuum pressure of described decolouring processing be-0.001Mpa～-0.1Mpa; Temperature is 50 ℃～200 ℃, and the time is 10～600 minutes;
(4), by the material in the vacuum reaction still being filtered to remove the impurity in the material with the direct-connected filtration unit of vacuum reaction still;
(5), will carry out the two-stage molecular distillation through the material in the reactor after filtering and extract filtered liquid, resulting distillate is triglyceride.
2, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 1, it is characterized in that above-mentioned reductive agent is hydrogen peroxide or superoxide or ozonide or other low molecule reductive agent.
3, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 1, it is characterized in that above-mentioned discoloring agent is gac or diatomite or carclazyte or its both mixture.
4, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 1, the vacuum pressure that it is characterized in that the first step molecular distillation in above-mentioned steps (five) is that 30～100Pa, temperature are 160～250 ℃, and the vacuum pressure of second stage molecular distillation is that 20～100Pa, temperature are 150～250 ℃.
5, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 4, the vacuum pressure that it is characterized in that above-mentioned first step molecular distillation is that 40Pa, temperature are 200 ℃, and the vacuum pressure of second stage molecular distillation is that 35Pa, temperature are 190 ℃.
6, according to claim 4 or the 5 described methods of from the tankage of molecule distillating monoglyceride, extracting triglyceride, it is characterized in that also comprising in the above-mentioned steps (five) purification of third stage molecular distillation, this grade molecule distillatory vacuum pressure is 0.1～10.0Pa, and temperature is 140～250 ℃.
7, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 6, it is characterized in that the vacuum pressure 1.0Pa of above-mentioned third stage molecular distillation, temperature is 200 ℃.
8, according to the described method of from the tankage of molecule distillating monoglyceride, extracting triglyceride of claim 1, it is characterized in that above-mentioned filter-pressing device is plate and frame(type)filter press or board-like closed filter.
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| CNA2007100288979A CN101092359A (en) | 2007-06-29 | 2007-06-29 | Method for extracting diglyceride from tailings of molecular distillation of glyceride |
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| CNA2007100288979A CN101092359A (en) | 2007-06-29 | 2007-06-29 | Method for extracting diglyceride from tailings of molecular distillation of glyceride |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516056A (en) * | 2011-12-08 | 2012-06-27 | 河北欣奇典生物科技有限公司 | Method for reproduction of fatty acid with molecular distillation distillate of unsaturated fatty acid |
| 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 |
| CN105481891A (en) * | 2015-12-02 | 2016-04-13 | 山东兆圭高分子材料科技有限公司 | Methylphenyl mixed ring purifying and separating method |
| CN105733804A (en) * | 2016-03-25 | 2016-07-06 | 合肥工业大学 | Decoloration method in process for preparing biodiesel from waste cooking oil |
| CN107022404A (en) * | 2017-04-25 | 2017-08-08 | 安徽省华银茶油有限公司 | A kind of processing method of powder formula tea-seed oil |
| CN108690656A (en) * | 2017-04-05 | 2018-10-23 | 中国石油天然气股份有限公司 | A kind of process for purification of ester oil crude product |
| CN109475141A (en) * | 2016-08-17 | 2019-03-15 | 酶学技术有限公司 | Oily admixture and preparation method |
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2007
- 2007-06-29 CN CNA2007100288979A patent/CN101092359A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516056A (en) * | 2011-12-08 | 2012-06-27 | 河北欣奇典生物科技有限公司 | Method for reproduction of fatty acid with molecular distillation distillate of unsaturated fatty acid |
| 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 |
| CN105481891A (en) * | 2015-12-02 | 2016-04-13 | 山东兆圭高分子材料科技有限公司 | Methylphenyl mixed ring purifying and separating method |
| CN105481891B (en) * | 2015-12-02 | 2018-07-20 | 山东兆圭高分子材料科技有限公司 | A kind of method for purifying and separating of aminomethyl phenyl mixed methylcyclosiloxane |
| CN105733804A (en) * | 2016-03-25 | 2016-07-06 | 合肥工业大学 | Decoloration method in process for preparing biodiesel from waste cooking oil |
| CN109475141A (en) * | 2016-08-17 | 2019-03-15 | 酶学技术有限公司 | Oily admixture and preparation method |
| CN108690656A (en) * | 2017-04-05 | 2018-10-23 | 中国石油天然气股份有限公司 | A kind of process for purification of ester oil crude product |
| CN107022404A (en) * | 2017-04-25 | 2017-08-08 | 安徽省华银茶油有限公司 | A kind of processing method of powder formula tea-seed oil |
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Application publication date: 20071226 |