CN101396051A - Technique for producing edible ethyle ester type chrysalis oil using chrysalis crude-oil - Google Patents
Technique for producing edible ethyle ester type chrysalis oil using chrysalis crude-oil Download PDFInfo
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- CN101396051A CN101396051A CNA2007101326520A CN200710132652A CN101396051A CN 101396051 A CN101396051 A CN 101396051A CN A2007101326520 A CNA2007101326520 A CN A2007101326520A CN 200710132652 A CN200710132652 A CN 200710132652A CN 101396051 A CN101396051 A CN 101396051A
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Abstract
The invention discloses a process used for producing edible ethyl ester-typed silkworm pupa oil by silkworm pupa crude oil, comprising the main steps as follows: silkworm pupa crude oil extracted by organic solvent or squeezed and separated by machines is degummed, dehydrated and esterified; ethanol is recovered, glycerin and sulphuric acid are separated and washed; saturated fatty acids are removed and distilled; during the distillation process, the distillate with the temperature of 120-140 DEG C and the pressure of 1-5Pa is intercepted. The ethyl ester-typed edible silkworm oil produced by the process has good sensory index and the color thereof is buff; no crystals occur at zero DEG C; unsaturated fatty acid has high content; the acid value and peroxide value of the oil reach the edible standard, the quality of the product is good, the safety is high and no solvent remains; the process can be widely applied to the industries such as medicines, health-caring food, nutrition food, high-grade cosmetics and the like.
Description
Technical field
The invention belongs to the technical field of producing of edible silkworm oil
Technical background
Silkworm chrysalis oil contains multiple unrighted acid, content is up to more than 75%, wherein alpha-linolenic acid content is more than 30%, linoleic acid content is about 7%, oleic acid content accounts for about 32%, what deserves to be mentioned is and also contain a certain amount of odd-carbon fatty acid carbon 15 and carbon 17 in the silkworm chrysalis oil, Japan natural pond doctor Tian Guanghong finds that in the exploitation of carrying out cancer therapy drug odd-carbon fatty acid has higher anti-cancer activity, and odd-carbon fatty acid is extremely rare in terrestrial life, and this makes silkworm chrysalis oil open development and utilization and is worth; Have the silkworm chrysalis crude oil of common solvent extraction or mechanical expression, separation now, color is dark brown, acid number and peroxide value height, and unpleasant stench flavor is arranged.
Summary of the invention
For overcoming the shortcoming that prior art exists, the invention provides a kind of technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil, the food grade ethyl ester type silkworm chrysalis oil sense organ of this explained hereafter is good, and color and luster is light yellow, crystallization can not occur when zero degree; The content height of unrighted acid, the quality better of product, safe.
The present invention solves the problems of the technologies described above the technical scheme of being taked to be: a kind of technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil, it comprises the steps:
(1) comes unstuck: after the silkworm chrysalis crude oil that passes through organic solvent extraction or mechanical expression, separation is heated to 65--80 ℃, the phosphoric acid that adds concentration 85% in the ratio of 0.15-0.25%, add 70-90 ℃ hot water in the ratio of 3-5% again and stirred 15-25 minute, standing separation or pump into seperator and separate and come unstuck;
(2) dehydration: the back feed liquid of will coming unstuck is carried out vacuum dehydration, and vacuum is negative pressure 0.05-0.15MPa, and temperature is 90-98 ℃;
(3) esterification: the feed liquid after the dehydration of will coming unstuck is by feed liquid: absolute ethyl alcohol: sulfuric acid (concentration 98%)=(0.8-1.2): (0.6-1): weight ratio (0.02-0.04) adds ethanol, sulfuric acid mixture liquid, add the hot reflux ester exchange, transesterification temperature is 65-75 ℃, reflux time 5--6 hour;
(4) reclaim ethanol: after esterification was finished, the ethanol of inventory 70-75% was reclaimed in distillation.
(5) separation of glycerin and sulfuric acid: about 20 minutes of time of repose;
(6) washing: in the hot water of 75-80 ℃ of feed liquid quality 75-85% ratio adding, agitator treating three times, glycerine that flush away is residual and sulfuric acid;
(7) remove saturated fatty acid: the feed liquid after will wash pumps into freezing equipment, treat that temperature reaches subzero after, press filtration removal saturated fatty acid.
(8) distillation: the feed liquid after will washing is distilled, and intercepts 120-140 ℃, the pressure distillate at 1-5Pa.
In the above-mentioned steps (1), after preferred silkworm chrysalis crude oil was heated to 70--75 ℃, the ratio by 0.2% added the food grade phosphoric acid of concentration 85%, and the hot water in 80 ℃ of 4% ratio addings stirred 20 minutes again;
In the above-mentioned steps (2), preferred vacuum is negative pressure 0.1MPa, and temperature is 93-97 ℃,
In the above-mentioned steps (3), preferably will come unstuck feed liquid after the dehydration by feed liquid: absolute ethyl alcohol: the weight ratio of sulfuric acid (concentration 98%)=1:0.8:0.03 adds ethanol, sulfuric acid mixture liquid, add the hot reflux ester exchange, transesterification temperature is 70 ℃, reflux time 5--6 hour;
In the above-mentioned steps (8), the equipment that takes off flavor and removal feed liquid impurity is molecular distillation equipment.
Advantage of the present invention is: the product quality height, and to decolour, come unstuck, depickling, take off flavor thoroughly, the organoleptic indicator is good, and color and luster is light yellow, crystallization can not occur when zero degree; The content of unrighted acid is compared than with the silkworm chrysalis oil of glyceride type, exceeds 10%, and acid value of lipids, peroxide value reach the food grade standard simultaneously, and the quality better of product is safe, without any dissolvent residual.Because of finished product is rich in especially alpha-linolenic acid of unrighted acid, except that direct edible, also can be widely used in industries such as medicine, health food, nutraceutical and the cosmetics of super quality; Production technology is simple, and the equipment less investment is suitable for large-scale production.
The specific embodiment
Embodiment:
(1) comes unstuck: 100 kilograms of silkworm chrysalis crude oils of learnt from else's experience organic solvent extraction or mechanical expression, separation, after being heated to 65--80 ℃, the food grade phosphoric acid that adds 0.2 kilogram concentration 85%, 4 kilograms of hot water that add 70-90 ℃ again, stirred standing separation or pump into seperator and separate and to come unstuck 15-25 minute;
(2) dehydration: will come unstuck the back feed liquid carry out vacuum dehydration, vacuum be negative pressure at 0.05-0.15MPa, temperature is 90-98 ℃;
(3) esterification: the feed liquid after the dehydration of will coming unstuck adds the hot reflux ester exchange by 3 kilograms of the concentrated sulfuric acids that adds 80 kilograms of absolute ethyl alcohols, concentration 98% in the feed liquid, and transesterification temperature is 65-75 ℃, reflux time 5--6 hour;
(4) reclaim ethanol: after esterification was finished, the ethanol of inventory 70-75%, about 58.3 kilograms were reclaimed in distillation;
(5) separation of glycerin and sulfuric acid: about 20 minutes of time of repose, the glycerine and the sulfuric acid of separation sub-cloud;
(6) washing: add 80 kilograms 75-80 ℃ hot water, agitator treating three times, glycerine that flush away is residual and sulfuric acid;
(7) remove saturated fatty acid: the feed liquid after will washing pumps into freezing equipment, and temperature is set in-5 ℃ to 0 ℃, keeps after 24 hours, and saturated fatty acid is removed in press filtration.
(8) distillation: the feed liquid after will washing is distilled, intercept 120-140 ℃, pressure distillate at 1-5Pa, get 68.6 kilograms of finished products, the finished product color and luster is faint yellow, has the normal smell of grease, no silkworm chrysalis peculiar smell and tapinoma-odour, acid value of lipids is 0.6mg KOH/g, peroxide value is 1.2mmol/kg, and dissolvent residual is zero, and sanitary indexs such as content of beary metal such as lead, inorganic arsenic, total mercury and total number of bacteria, yeast and mould, coliform, pathogenic bacteria all meet the state food specified standard.
The feed liquid that press filtration is come out pumps into molecular distillation equipment and distills, the intercepting temperature at 120 to 140 ℃, pressure at 1 to 5Pa distillate.
Claims (5)
1, a kind of technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil is characterized in that, it comprises the steps:
(1) comes unstuck: after the silkworm chrysalis crude oil that passes through organic solvent extraction or mechanical expression, separation is heated to 65--80 ℃, the phosphoric acid that adds concentration 85% in the ratio of 0.15-0.25%, add 70-90 ℃ hot water in the ratio of 3-5% again and stirred 15-25 minute, standing separation or pump into seperator and separate and come unstuck;
(2) dehydration: the back feed liquid of will coming unstuck is carried out vacuum dehydration, and vacuum is negative pressure 0.05-0.15MPa, and temperature is 90-98 ℃;
(3) esterification: the feed liquid after the dehydration of will coming unstuck is by feed liquid: absolute ethyl alcohol: sulfuric acid (concentration 98%)=(0.8-1.2): (0.6-1): weight ratio (0.02-0.04) adds ethanol, sulfuric acid mixture liquid, add the hot reflux ester exchange, transesterification temperature is 65-75 ℃, reflux time 5--6 hour;
(4) reclaim ethanol: after esterification was finished, the ethanol of inventory 70-75% was reclaimed in distillation.
(5) separation of glycerin and sulfuric acid: about 20 minutes of time of repose;
(6) washing: in the hot water of 75-80 ℃ of feed liquid quality 75-85% ratio adding, agitator treating three times, glycerine that flush away is residual and sulfuric acid;
(7) remove saturated fatty acid: the feed liquid after will wash pumps into freezing equipment, treat that temperature reaches subzero after, press filtration removal saturated fatty acid.
(8) distillation: the feed liquid after will washing is distilled, and intercepts 120-140 ℃, the pressure distillate at 1-5Pa.
2, the technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil according to claim 1, it is characterized in that: in the above-mentioned steps (1), after preferred silkworm chrysalis crude oil is heated to 70--75 ℃, add the food grade phosphoric acid of concentration 85% in 0.2% ratio, add 80 ℃ hot water in 4% ratio again and stirred 20 minutes.
3, the technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil according to claim 1 is characterized in that: in the above-mentioned steps (2), preferred vacuum is negative pressure 0.1MPa, and temperature is 93-97 ℃.
4, the technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil according to claim 1, it is characterized in that: in the above-mentioned steps (3), preferably will come unstuck feed liquid after the dehydration by feed liquid: absolute ethyl alcohol: the weight ratio of sulfuric acid (concentration 98%)=1:0.8:0.03 adds ethanol, sulfuric acid mixture liquid, add the hot reflux ester exchange, transesterification temperature is 70 ℃, reflux time 5--6 hour.
5, the technology of producing edible ethyle ester type chrysalis oil using chrysalis crude-oil according to claim 1 is characterized in that: in the above-mentioned steps (8), the equipment that takes off flavor and removal feed liquid impurity is molecular distillation equipment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101326520A CN101396051A (en) | 2007-09-29 | 2007-09-29 | Technique for producing edible ethyle ester type chrysalis oil using chrysalis crude-oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101326520A CN101396051A (en) | 2007-09-29 | 2007-09-29 | Technique for producing edible ethyle ester type chrysalis oil using chrysalis crude-oil |
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| CN101396051A true CN101396051A (en) | 2009-04-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504503A (en) * | 2018-11-06 | 2019-03-22 | 苏州玖城润滑油有限公司 | A kind of chain grease and preparation method thereof |
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2007
- 2007-09-29 CN CNA2007101326520A patent/CN101396051A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504503A (en) * | 2018-11-06 | 2019-03-22 | 苏州玖城润滑油有限公司 | A kind of chain grease and preparation method thereof |
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Open date: 20090401 |