CN1749379A - Method for extracting orange oil and pectin from organic skin - Google Patents
Method for extracting orange oil and pectin from organic skin Download PDFInfo
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- CN1749379A CN1749379A CN 200510032262 CN200510032262A CN1749379A CN 1749379 A CN1749379 A CN 1749379A CN 200510032262 CN200510032262 CN 200510032262 CN 200510032262 A CN200510032262 A CN 200510032262A CN 1749379 A CN1749379 A CN 1749379A
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Abstract
The process of extracting orange oil and pectin from orange peel includes the steps of: microwave aided water extraction of orange peel material, the subsequent vacuum suction filtering, extracting the filtrate with organic extractant to obtain orange oil and extracting filter residue to obtain pectin. Owing to powerful heat effect of microwave, the material is heated fast to boiling state and the pectinase is deactivated fully without need of special pectinase deactivating step, resulting in greatly raised pectin extracting rate. During pectin extraction, microwave aided lixiviation and ion exchange resin adsorption of metal cation are adopted to result in fast dissolving of pectin, and raised pectin quality and yield. During orange oil production, the microwave aided water extraction results in greatly lowered organic solvent consumption and high recovery rate.
Description
Technical field
The present invention relates to a kind of method of from citrous fruit peel, extracting mandarin oil and pectin.
Background technology
CN1075729 discloses a kind of " extracting the method for natural yellow pigment, mandarin oil and pectin from orange peel simultaneously ".This method flow is long, needs to use a large amount of sherwood oils in leaching process, because the sherwood oil consumption is big, volatile, causes in the production process solvent loss very big, and economic benefit is not high.And pericarp is a large amount of to be absorbed and residual organic solvent, follow-up pectin is extracted bring inconvenience.CN1078111 discloses a kind of " extracting the method for tangerine oil, pectin, yellow pigment, fodder additives from orange peel simultaneously ".Adopt steam distillation at leaching process, energy expenditure is big, and the product extraction yield is not high.CN1100106 discloses that " method of extracting low ester pectin from citrus waste, this method has been abandoned the extraction to mandarin oil in the citrous fruit peel, has caused underutilization of resources and unnecessary waste, and calcium ion be difficult to remove totally in the product, influences quality product.
Summary of the invention
The object of the present invention is to provide a kind of a large amount of energy of saving, reduce production costs, simplify technical process, improve the high a kind of microwave-assisted technology comprehensive method of extracting mandarin oil and pectin from Citrus (citrus, lemon, shaddock etc.) pericarp of utilizing of the rate of recovery.
Technical scheme of the present invention is: adopt microwave-assisted water abstraction technique to handle the pericarp raw material, and vacuum filtration then, filtrate is used for extracting mandarin oil with organic extractant, and filter residue is used for extracting pectin.In pectous extracting method, adopt the microwave-assisted extracting technology, and when acid is carried, adopted ion exchange resin absorption metallic cation.
Specifically may further comprise the steps:
(1) raw material crushing: earlier citrous fruit peel is crushed to granularity 3～10mm; ,
(2) microwave auxiliary extraction: add the water of 2～30 times of volumes, heat 3～15 minutes to the 3 minutes final vacuum suction filtrations that seethe with excitement in microwave reactor, filtrate being used for extracted mandarin oil, and the tangerine peel slag is used for extracting pectin;
(3) extraction of mandarin oil:
1. extraction: the organic extractant that adds 1/4～1 times of volume of gained filtrate stirred 3～5 minutes, behind the standing demix, got the upper strata oily liquids and extracted mandarin oil, and the filter excess extracts pectin;
2. fractionation by distillation mandarin oil: upper strata liquid 80～85 ℃ of about 30 minutes of distillations down, is obtained faint yellow mandarin oil, and distillate is colourless organic extractant, can be recycled;
3., decolouring, dehydration: faint yellow mandarin oil is through conventional activated carbon decolorizing and anhydrous Na
2SO
4After the dehydration, must contain the mandarin oil product of limonene 92～95%;
(4) extraction of pectin:
1. microwave-assisted lixiviate+ion-exchange: collect the tangerine peel slag as raw material, adding hydrochloric acid, to transfer pH value of solution be 1.5～2.0, and add the Zeo-karb that accounts for raw material total mass 10～30%, with microwave heating to 80～95 ℃, in constantly stirring, keep constant temperature 15～60min, get liquid pectin;
2. decolouring: add and to account for the pectin gac of solution total mass 5～25% just, stir 5～20min down at 80 ℃, filter colourless pectin extracting soln;
3. ultrafiltration and concentration: under temperature is 40～50 ℃, pH2-4, pressure 0.15～0.3Mpa condition, be the tubular type acrylonitril membrane ultra-fine filter of 50000 μ, pectin extracting soln is concentrated into 4～6% with molecular weight cut off;
4. precipitating: under 50 ℃～65 ℃, the technical hydrochloric acid that in fructose concentrating liquid, adds the 1-2% that accounts for the concentrated solution gross weight, weight ethanol contents such as adding and concentrated solution are 95% alcohol again, mixed 5 minutes, and made the pectin precipitating, and filter, be the washing of 80% alcohol with ethanol content again after the filtration, remove alcohol dissolubility impurity, with the ethanolic soln washing that contains 0.3mol/LHCI 2 times, get the pectin primary products after the squeezing then;
5. dry: the pectin primary products are put into loft drier is inherent to carry out drying below 60 ℃, until water content below 10%, the pectin porphyrize, pack the pectin powder finished product.
Described organic extractant is sherwood oil, normal hexane, Virahol.
The present invention adopts microwave-assisted water abstraction technique to handle the pericarp raw material, because microwave intensive heat effect, raw material will soon be heated to boiling state, thereby makes the abundant passivation of polygalacturonase, necessary polygalacturonase passivation step in the time of can saving pectin like this and extract; Follow-up pectin extraction yield is increased greatly, in pectous extracting method, adopted the microwave-assisted extracting technology, and when acid is carried, adopt ion exchange resin absorption metallic cation, thereby quicken the dissolving of protopectin-, improve the quality and the productive rate of pectin.In the mandarin oil production process, after employing microwave-assisted water abstraction technique is handled the pericarp raw material, can reduce the consumption of organic extractant greatly; Make the usage quantity of sherwood oil, normal hexane, Virahol have only 1/5～1/3 of background technology, and rate of recovery height, reach more than 95%; And saved a large amount of energy, and simplified technical process, reduced production cost.
Embodiment
Embodiment 1:
Get fresh orange peel 145.2 grams, be crushed to 3～5mm, add 600 gram water, place Glass Containers, put into the special microwave oven of adjustable power frequency fixing, microwave heating 5 minutes is to the 3 minutes final vacuum suction filtrations that seethe with excitement, filtrate being used for extracted mandarin oil, and filter residue is used for extracting pectin.
Mandarin oil extracts: filter the 390mL mixed solution, add the 168mL petroleum ether extraction and separate, get upper strata liquid, in 85 ℃ of water-baths, add thermal distillation half an hour, reclaim sherwood oil 162mL, the rate of recovery reaches 96.43%; Heat up in a steamer excess behind activated carbon decolorizing and anhydrous Na2SO4 dehydration, get mandarin oil product 5.85 grams, mandarin oil extraction rate reached to 4.03%.
Pectin extracts: filter 258 gram tangerine peel slags, add 28 grams, 717 type ion exchange resin absorption metallic cation, add 600mL 1%HCl, transferring pH is 2.0, heating, lixiviate in the special microwave oven of adjustable power frequency fixing are stirred insulation 45 minutes down at 95 ℃; After taking out filtration, get pectin solution just, add 10 gram gacs again, stir 8 minutes final vacuum suction filtrations, liquid pectin 400mL must decolour; Under temperature is 45 ℃, PH3.0, pressure 0.2Mpa condition, be the tubular type acrylonitril membrane ultra-fine filter of 50000 μ with molecular weight cut off, concentration of pectin is concentrated into 4.21%; The ethanol content that adds 400mL under being heated to 65 ℃ is 95% alcohol, and after precipitating was complete, the ethanolic soln with 0.3mol/LHCl washed again, filter, be the washing of 80% alcohol with ethanol content again after the filtration, then with the ethanolic soln washing that contains 0.3mol/LHCl 2 times, the pectin colloid.55 ℃ of following vacuum-dryings 3 hours, grind to such an extent that pectin powder 17.3 restrains pectin extraction rate reached to 11.9% at last this colloid.
Embodiment 2 gets fresh orange peel 125 grams, is crushed to 3～5mm, adds 550 gram water, put into the special microwave oven of adjustable power frequency fixing, microwave heating 8 minutes is to 3 minutes final vacuum suction filtrations, the vacuum filtrations then of seething with excitement, filtrate being used for extracted mandarin oil, and filter residue is used for extracting pectin.
Mandarin oil extracts: filter the 340mL mixed solution, add 150mL n-hexane extraction separating layer, get upper strata liquid, in 90 ℃ of water-baths, add thermal distillation half an hour, reclaim normal hexane 144mL, the rate of recovery reaches 96.0%; After heating up in a steamer excess process decolouring dehydration, get mandarin oil product 4.55 grams, mandarin oil extraction rate reached to 3.64%.
Pectin extracts: filter 230 gram tangerine peel slags, add 25 grams, 711 type ion exchange resin, add 550mLl%HCl, transferring pH is 1.8, heating, lixiviate in microwave oven are stirred insulation 40 minutes down at 95 ℃; After taking out filtration, add 10 gram gacs again, stir 8 minutes final vacuum suction filtrations, liquid pectin 360mL must decolour; Under temperature is 45 ℃, pH3.0, pressure 0.2Mpa condition, be the tubular type acrylonitril membrane ultra-fine filter of 50000 μ with molecular weight cut off, concentration of pectin is concentrated into 4.35%; The ethanol content that adds 350mL under being heated to 65 ℃ is 95% alcohol, and after precipitating was complete, the ethanolic soln with 0.3mol/LHCl washed again, filter, be the washing of 80% alcohol with ethanol content again after the filtration, then with the ethanolic soln washing that contains 0.3mol/LHCl 2 times, the pectin colloid.55 ℃ of vacuum-dryings 3 hours, grind to such an extent that pectin powder 15.1 restrains pectin extraction rate reached to 12.08% at last this colloid.
Embodiment 3 gets fresh orange peel 200 grams, is crushed to 3～5mm, adds 800 gram water, put into the special microwave oven of adjustable power frequency fixing, microwave heating 6 minutes is to 3 minutes final vacuum suction filtrations, the vacuum filtrations then of seething with excitement, filtrate being used for extracted mandarin oil, and filter residue is used for extracting pectin.
Mandarin oil extracts: filter the 590mL mixed solution, add 200mL Virahol extracting and separating layer, get upper strata liquid, in 90 ℃ of water-baths, add thermal distillation half an hour, reclaim Virahol 193.5mL, the rate of recovery reaches 96.75%; After heating up in a steamer excess process decolouring dehydration, get mandarin oil product 7.6 grams, mandarin oil extraction rate reached to 3.80%.
Pectin extracts: filter 312 gram tangerine peel slags, add 35 grams, 717 type ion exchange resin, add 700mLl%HCl, transferring pH is 1.5, heating, lixiviate in microwave oven are stirred insulation 30 minutes down at 90 ℃; After taking out filtration, add 12 gram gacs again, stir 8 minutes final vacuum suction filtrations, liquid pectin 500mL must decolour; Under temperature is 50 ℃, pH3.0, pressure 0.2Mpa condition, be the tubular type acrylonitril membrane ultra-fine filter of 50000 μ with molecular weight cut off, concentration of pectin is concentrated into 4.42%; The ethanol content that adds 500mL under being heated to 65 ℃ is 95% alcohol, and after precipitating was complete, the ethanolic soln with 0.3mol/LHCl washed again, filter, be the washing of 80% alcohol with ethanol content again after the filtration, then with the ethanolic soln washing that contains 0.3mol/LHCl 2 times, the pectin colloid.55 ℃ of vacuum-dryings 3 hours, grind to such an extent that pectin powder 24.5 restrains pectin extraction rate reached to 12.25% at last this colloid.
Claims (2)
1. from citrous fruit peel, extract the method for mandarin oil and pectin, it is characterized in that may further comprise the steps:
(1) raw material crushing: earlier citrous fruit peel is crushed to granularity 3～10mm; ,
(2) microwave auxiliary extraction: add the water of 2～30 times of volumes, heat 3～15 minutes to the 3 minutes final vacuum suction filtrations that seethe with excitement in microwave reactor, filtrate being used for extracted mandarin oil, and the tangerine peel slag is used for extracting pectin;
(3) extraction of mandarin oil:
1. extraction: the organic extractant that adds 1/4～1 times of volume of gained filtrate stirred 3～5 minutes, behind the standing demix, got the upper strata oily liquids and extracted mandarin oil, and the filter excess extracts pectin;
2. fractionation by distillation mandarin oil: upper strata liquid 80～85 ℃ of about 30 minutes of distillations down, is obtained faint yellow mandarin oil, and distillate is colourless organic extractant, can be recycled;
3., decolouring, dehydration: faint yellow mandarin oil is through conventional activated carbon decolorizing and anhydrous Na
2SO
4After the dehydration, must contain the mandarin oil product of limonene 92～95%;
(4) extraction of pectin:
1. microwave-assisted lixiviate+ion-exchange: collect the tangerine peel slag as raw material, adding hydrochloric acid conditioning solution pH is 1.5～2.0, and adds the Zeo-karb that accounts for raw material total mass 10～30%, with microwave heating to 80～95 ℃, in constantly stirring, keep constant temperature 15～60min, get liquid pectin;
2. decolouring: add and to account for the pectin gac of solution total mass 5～25% just, stir 5～20min down at 80 ℃, filter colourless pectin extracting soln;
3. ultrafiltration and concentration: under temperature is 40～50 ℃, pH2-4, pressure 0.15～0.3Mpa condition, be the tubular type acrylonitril membrane ultra-fine filter of 50000 μ, pectin extracting soln is concentrated into 4～6% with molecular weight cut off;
4. precipitating: under 50 ℃～65 ℃, the technical hydrochloric acid that in fructose concentrating liquid, adds the 1-2% that accounts for the concentrated solution gross weight, weight ethanol contents such as adding and concentrated solution are 95% alcohol again, mixed 5 minutes, and made the pectin precipitating, and filter, be the washing of 80% alcohol with ethanol content again after the filtration, remove alcohol dissolubility impurity, with the ethanolic soln washing that contains 0.3mol/LHCI 2 times, get the pectin primary products after the squeezing then;
5. dry: the pectin primary products are put into loft drier is inherent to carry out drying below 60 ℃, until water content below 10%, the pectin porphyrize, pack the pectin powder finished product.
2. method according to claim 1 is characterized in that described organic extractant is sherwood oil, normal hexane, Virahol.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100322627A CN1304544C (en) | 2005-10-18 | 2005-10-18 | Method for extracting orange oil and pectin from organic skin |
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| CNB2005100322627A CN1304544C (en) | 2005-10-18 | 2005-10-18 | Method for extracting orange oil and pectin from organic skin |
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| CN1749379A true CN1749379A (en) | 2006-03-22 |
| CN1304544C CN1304544C (en) | 2007-03-14 |
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Cited By (21)
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| CN101037485B (en) * | 2007-04-20 | 2010-06-09 | 兰州大学 | Pectin extraction method |
| CN101074270B (en) * | 2006-05-17 | 2010-09-22 | 烟台安德利果胶有限公司 | Production of polymer apple pectin |
| CN101857648A (en) * | 2010-06-30 | 2010-10-13 | 李恒勇 | Process for producing pectin without using alcohol |
| CN101935361A (en) * | 2010-08-31 | 2011-01-05 | 中国农业大学 | Method for preparing pectin by high static pressure technology |
| CN102174121A (en) * | 2011-02-15 | 2011-09-07 | 江苏九久环境科技有限公司 | Process for extracting pectin from citrus peel and producing organic fertilizer by using waste residues |
| CN102285862A (en) * | 2011-06-20 | 2011-12-21 | 成都蓉药集团四川长威制药有限公司 | Method for extracting limonene from fruit skin of citrus |
| CN101731748B (en) * | 2008-11-05 | 2012-07-18 | 湖北中烟工业有限责任公司 | Method for extracting Dendranthema indium leaves and application of extractive thereof in cigarettes |
| CN102702379A (en) * | 2012-04-26 | 2012-10-03 | 赛珂睿德生物医药科技(上海)有限公司 | Extraction and preparation process of citrus pectin |
| CN103204954A (en) * | 2013-03-22 | 2013-07-17 | 安徽亿源生物工程有限公司 | Continuous countercurrent extraction method of pectin in Chinese medicine residue by microwave |
| CN103265650A (en) * | 2013-05-14 | 2013-08-28 | 安徽金枫果胶有限公司 | Method for extracting pectin from orange peel |
| CN104974274A (en) * | 2015-07-01 | 2015-10-14 | 安徽亿源生物工程有限公司 | Preparation method of high esterification degree super slow set pectin |
| CN105176682A (en) * | 2015-09-21 | 2015-12-23 | 华中农业大学 | Sweet orange essential oil decoloring and aroma conserving method |
| CN105440155A (en) * | 2015-12-28 | 2016-03-30 | 西北农林科技大学 | Pectin extraction method |
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| CN106433987A (en) * | 2016-10-31 | 2017-02-22 | 湖北中烟工业有限责任公司 | Preparation method of refined sweet-orange spice and application thereof |
| CN106496355A (en) * | 2016-11-07 | 2017-03-15 | 涟源康麓生物科技有限公司 | A kind of preparation method of pectin |
| CN108219028A (en) * | 2018-01-22 | 2018-06-29 | 重庆汇达柠檬科技集团有限公司 | The extracting method of pectin in a kind of lemon peel slag |
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| CN111543629A (en) * | 2020-04-07 | 2020-08-18 | 杭州莱恩纳尔生物科技有限公司 | Method for simultaneously preparing pectin, fruit vinegar, ferment, probiotics and carbon black from peel residues |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1003208B (en) * | 1985-04-01 | 1989-02-08 | 四川大学 | Method for obtaining pectine from peels of oranges and tangerines and producing wine, essential oil, jam, pigment and peel glucoside simultaneously |
| JPS644602A (en) * | 1987-06-26 | 1989-01-09 | Niochiyou | Extraction of pectin by means of microwave irradiation |
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- 2005-10-18 CN CNB2005100322627A patent/CN1304544C/en not_active Expired - Fee Related
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| CN101074270B (en) * | 2006-05-17 | 2010-09-22 | 烟台安德利果胶有限公司 | Production of polymer apple pectin |
| CN101037485B (en) * | 2007-04-20 | 2010-06-09 | 兰州大学 | Pectin extraction method |
| CN101731748B (en) * | 2008-11-05 | 2012-07-18 | 湖北中烟工业有限责任公司 | Method for extracting Dendranthema indium leaves and application of extractive thereof in cigarettes |
| CN101857648A (en) * | 2010-06-30 | 2010-10-13 | 李恒勇 | Process for producing pectin without using alcohol |
| CN101935361B (en) * | 2010-08-31 | 2012-06-20 | 中国农业大学 | Method for preparing pectin by high static pressure technology |
| CN101935361A (en) * | 2010-08-31 | 2011-01-05 | 中国农业大学 | Method for preparing pectin by high static pressure technology |
| CN102174121B (en) * | 2011-02-15 | 2012-05-30 | 江苏九久环境科技有限公司 | Process for extracting pectin from citrus peel |
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| CN102285862B (en) * | 2011-06-20 | 2014-07-16 | 成都蓉药集团四川长威制药有限公司 | Method for extracting limonene from fruit skin of citrus |
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| CN106496355B (en) * | 2016-11-07 | 2018-11-20 | 涟源康麓生物科技有限公司 | A kind of preparation method of pectin |
| CN108219028A (en) * | 2018-01-22 | 2018-06-29 | 重庆汇达柠檬科技集团有限公司 | The extracting method of pectin in a kind of lemon peel slag |
| CN108715619A (en) * | 2018-04-28 | 2018-10-30 | 广东李金柚农业科技有限公司 | A method of for extracting naringin and pectin |
| CN110615857A (en) * | 2019-08-28 | 2019-12-27 | 浙江环耀环境建设有限公司 | Method for recycling waste in orange can processing production |
| CN111543629A (en) * | 2020-04-07 | 2020-08-18 | 杭州莱恩纳尔生物科技有限公司 | Method for simultaneously preparing pectin, fruit vinegar, ferment, probiotics and carbon black from peel residues |
| CN112876581A (en) * | 2021-02-07 | 2021-06-01 | 西南大学 | Premna microphylla low-ester pectin and preparation method and application thereof |
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