CN1078111A - The preparation technology of Citrus reticuiata Blano series of products - Google Patents
The preparation technology of Citrus reticuiata Blano series of products Download PDFInfo
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- CN1078111A CN1078111A CN93110827A CN93110827A CN1078111A CN 1078111 A CN1078111 A CN 1078111A CN 93110827 A CN93110827 A CN 93110827A CN 93110827 A CN93110827 A CN 93110827A CN 1078111 A CN1078111 A CN 1078111A
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- 241000207199 Citrus Species 0.000 title claims abstract description 21
- 235000020971 citrus fruits Nutrition 0.000 title claims abstract description 21
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000001814 pectin Substances 0.000 claims abstract description 34
- 235000010987 pectin Nutrition 0.000 claims abstract description 34
- 229920001277 pectin Polymers 0.000 claims abstract description 34
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 241000675108 Citrus tangerina Species 0.000 claims abstract description 19
- 239000012141 concentrate Substances 0.000 claims abstract description 19
- 230000006837 decompression Effects 0.000 claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 13
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- 238000001291 vacuum drying Methods 0.000 claims description 15
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- 238000001035 drying Methods 0.000 claims description 5
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A kind of preparation technology of Citrus reticuiata Blano series of products is characterized in that through cleaning, pulverizing, immersion, decompression distillation, lixiviate, precipitation with alcohol, press filtration, step such as concentrates, and can prepare products such as tangerine oil, pectin, uranidin, feed addictive from Citrus reticuiata Blano.Technology of the present invention is simple and easy to grasp, and equipment is few, non-environmental-pollution, with short production cycle, good product quality, yield height, citrous fruit peels such as Citrus reticuiata Blano obtain comprehensive utilization, and remarkable in economical benefits is applicable to that middle-size and small-size producer, township enterprise, school-run enterprise and specialist use.
Description
The present invention relates to the preparation of foodstuff, spices etc., feature relates to the preparation technology who prepares series of products such as tangerine oil, pectin, uranidin, feed addictive from scarlet tangerine peel.
Red tangerine, peculiar flavour and nutritive peculiarity because of its fruit are subjected to liking of men and women, old and young deeply, and the red tangerine resource of China is very abundant, surplus only the annual production in Sichuan promptly reaches 20 ten thousand tons.For a long time, Citrus reticuiata Blano is general all through drying as medicinal material.The someone adopts cold-press or vapor distillation method to extract tangerine oil from Citrus reticuiata Blano at present, but, the tangerine oil oil yield that these methods are produced is low, product is single, other composition in the Citrus reticuiata Blano or destroyed or be wasted, Citrus reticuiata Blano does not have to such an extent that make full use of, and equipment investment is bigger, and economic benefit is low.
The preparation technology of the Citrus reticuiata Blano series of products that purpose of the present invention aims to provide that a kind of technology is simple, cost is low, good product quality, yield height, Citrus reticuiata Blano can obtain fully utilizing.
Content of the present invention is: a kind of preparation technology of Citrus reticuiata Blano series of products, and comprise fresh orange peel is cleaned, pulverizes, it is characterized in that also comprising the following steps:
After the fresh orange peel of a, pulverizing placed 60～90 ℃ of hot water of 3～8 times of weight to soak 2～12 hours, (pressure was that 13.33Pa～533.32Pa) does not distillate to having grease substantially, must oil-water mixture (1) and residue (2) in decompression distillation;
Add 70～100 ℃ of hot water of 10～30 times of weight in b, the residue (2), transferring PH with inorganic acid (3) is 2～6, soaks after 1～6 hour, gets filtrate (4) and filter residue (5) through the filter press press filtration;
C, filter residue (5) are 20～35 ℃ of following spontaneous fermentations 3～5 days, again through 60～80 ℃ of dry feed addictives that get;
(pressure is 1.2 * 10 through decompression distillation for d, filtrate (4)
4Pa～3.99 * 10
4Pa) get oil-water mixture (6) and concentrate (7);
E, oil-water mixture (6) and oil-water mixture (1) merge through oil water separator separate tangerine oil;
Add 95% edible ethanol among the f, concentrate (7) and mix, and control ethanol weight accounts for 40～70% of this mixture weight, make the pectin precipitation, get pectin (8) and filtrate (9) through the filter press press filtration;
G, pectin (8) get the powdery pectin product through vacuum desiccator drying, pulverizing, mistake 60 mesh sieves;
H, filtrate (9) are concentrated through reducing pressure, and (pressure is 2.67 * 10
4Pa～6.67 * 10
4Pa) get uranidin medicinal extract,, cross 60 mesh sieves, get powdery uranidin product again through the vacuum desiccator drying.
Be 2～6 times 70～100 ℃ of hot-water soak residues (2) with 10～30 times of weight at PH described in the step b in the content of the present invention, this hot water can be divided into 2～4 immersions, merging filtrate after the filter press press filtration (4).
The volume of concentrate described in the steps d (7) is controlled to be 1/4～1/5 of filtrate (4) volume preferably in the content of the present invention.
Inorganic acid described in the step b (3) can be hydrochloric acid, acetate, oxalic acid or phosphoric acid in the content of the present invention.
Step f gained pectin (8) can also add the absolute ethyl alcohol of 1～4 times of weight in the content of the present invention, through mixing, filtration, vacuum drying, pulverizing, mistake 60 mesh sieves, must make with extra care pectin.
Edible ethanol described in the content of the present invention can also be the ethanol of absolute ethyl alcohol or other concentration, only needs consumption is done corresponding suitable adjustment.
Filter press described in the content of the present invention can be plate and frame, spiral or other filter press of the prior art.
The product that obtains by the present invention has following properties:
(1) tangerine oil: main component is octanal, capraldehyde, linalool etc., brownish translucent liquid, and tool orange fragrance, density is about 0.85～0.856 kilograms per cubic meter;
(2) Chinese herbal feed additive: be powdered granule, contain trace elements such as phosphorus, potassium, calcium, compositions such as citrin, dihydrochalcone (can make sweetening agent), vitamin C, amino acid, titanium, sugar, cellulose, hemicellulose; 20～35 ℃ of following spontaneous fermentations 3～5 days, further pathogenic microbe killing not only, and each active ingredient reacts each other, produce some organic acids etc., and the bitter taste that makes color coordinate to increase palatability and remove feed, as feed addictive, have nutrition, disease-resistant, abirritate livestock alimentary canal, promote that gastric secretion helps effects such as digestion:
(3) pectin: i.e. D one galacturonic acid polymer, molecular weight 10～200,000 are the yellowish white powder, and are water-soluble, are insoluble to ethanol, free from extraneous odour, water content 7%, degree of gelation can be applicable to food industry, medical industry etc. greater than 180 degree;
(4) uranidin: mainly contain tangerine peel, and contain a small amount of luteole etc., be yellow powder, water-soluble and ethanol is insoluble to ether, chloroform, and is nontoxic, can be used as food additives, antioxidant and natural edible flavochrome, good stability, strong coloring force.
The present invention has following characteristics:
(1) Citrus reticuiata Blano obtains comprehensive utilization.Tangerine oil, pectin, uranidin by the present invention's preparation can be widely used in food industry, daily chemical industry and medical industry etc.; Accessory substance-filter residue can be made Chinese herbal feed additive through fermentation process, to the livestock effect of preventing and curing diseases; The liquid that oil-water mixture separates behind the tangerine oil is the distilled water that contains a small amount of spices and other composition, can be used for formulated drink, also can be recycled;
(2) technology is simple.The present invention only relates to technology such as pulverizing, immersion, decompression distillation, filtration, vacuum drying, and is simple and practical, easily grasps, and easily promotes;
(3) equipment is gone into operation and is lacked, and only adopts equipment such as cold boiler, filter press, pulverizer, vacuum desiccator, and small investment is easily purchased, low production cost;
(4) package unit can recycle, and prepares series of products continuously; In the production process, the preparation of front product does not have destruction to subsequent product and influences, and has both guaranteed continuity, the simplicity of technology, has guaranteed the yield and the quality of series of products again, product yield height, and quality better meets the quality sanitary standard;
(5) safe, free from environmental pollution.Raw material related among the present invention only have Citrus reticuiata Blano, water and edible ethanol, do not have other any harmful substance, environmentally safe, and most ethanol recyclable (rate of recovery 70～80%) is fully used;
(6) the raw material source is very abundant, and technology is simple, and is with low cost, with short production cycle, has wide development prospect and value, and will bring comparatively remarkable economic efficiency and social benefit;
(7) the present invention also can be used for the comprehensive exploitation of agricultural byproducts such as other citrous fruit peel except that the comprehensive utilization that is applicable to Citrus reticuiata Blano.
Accompanying drawing is a process flow diagram of the present invention.
Below by embodiment the present invention is further described:
Embodiment 1:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders～80 orders), add 70 ℃ of hot-water soaks 4 hours of 6 times of weight, decompression distillation (pressure 533.32Pa) 3 hours, get oil-water mixture and slag, oil-water mixture through oil water separator separate tangerine oil (product I), yield 1.04%.90 ℃ of hot water that add 20 times of weight in the slag, transferring PH with oxalic acid is 3, lixiviate 6 hours, the plate and frame filter filter slag and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry the powdery product as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 2 * 10
4Pa) to 1/5 of stoste volume, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 70%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60～70 ℃) (and reclaiming ethanol), pulverize, cross 60 mesh sieves, get pectin (powder) (product III), yield 7.5%; Concentrated (the pressure: 5.334 * 10 of filtrate through reducing pressure
4Pa) get uranidin medicinal extract, reclaim ethanol (rate of recovery 70-80%), uranidin medicinal extract is through vacuum drying (60 ℃), and 60 orders sieve, and gets uranidin (powder) (product IV), yield 0.04%.
Embodiment 2:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders～80 orders), add 90 ℃ of hot-water soaks of 3 times of weight 2 hours, decompression distillation (pressure 66.67Pa) 2 hours gets oil-water mixture and slag, oil-water mixture through oil water separator separate tangerine oil (product I), yield 1.45%; 90 ℃ of hot water that add 30 times of weight in the slag, transferring PH with oxalic acid is 3, lixiviate 6 hours, the plate and frame filter press press filtration gets slag and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry the powdery product as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 1.2 * 10
4Pa) to stoste volume 1/4, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 70%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60 ℃-70 ℃), (and reclaiming ethanol) pulverizes, and crosses 60 mesh sieves, get pectin (powder) (product III), yield 7.8%; Concentrated (the pressure: 5.334 * 10 of filtrate through reducing pressure
4Pa) uranidin medicinal extract, reclaim ethanol (rate of recovery 70%～80%), uranidin medicinal extract is through vacuum drying (60 ℃), 60 orders sieve uranidin (powder) (product IV), yield 0.03%.
Embodiment 3:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders-80 order), add 75 ℃ of hot-water soaks of 8 times of weight 4 hours, decompression distillation (pressure: 13.33Pa) 3 hours, get oil-water mixture and slag, oil-water mixture gets tangerine oil (product I), yield 2.2% through water-oil separating; 80 ℃ the hot water that adds 10 times of weight in the slag, transferring PH with phosphoric acid is 2.5, lixiviate 6 hours, the plate and frame filter press press filtration gets slag and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry powdery as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 1.2 * 10
4Pa) to stoste volume 1/4, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 70%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60 ℃-70 ℃), (and reclaiming ethanol) pulverizes, and crosses 60 mesh sieves, get pectin (powder) (product III), yield 5%; Concentrated (the pressure: 2.67 * 10 of filtrate through reducing pressure
4) uranidin medicinal extract, reclaim ethanol (rate of recovery 70-80%), uranidin medicinal extract is through vacuum drying (60 ℃), 60 orders sieve uranidin (powder) (product) IV), yield 0.22%.
Embodiment 4:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders～80 orders), add 75 ℃ of hot-water soaks of 8 times of weight 4 hours, decompression distillation (pressure 66.67Pa) 3 hours gets oil-water mixture and slag, oil-water mixture gets tangerine oil (product I), yield 2.07% through water-oil separating; 85 ℃ the hot water that adds 30 times of weight in the slag, PH is 2.5 with 1N hydrochloric acid accent, lixiviate 3 hours, the plate and frame filter press press filtration gets filter residue and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry powder product as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 2 * 10
4Pa) to 1/4 of stoste volume, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 70%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60 ℃-70 ℃) (and reclaiming ethanol), pulverize, cross 60 mesh sieves, get pectin (powder) (product III), yield 7%; Concentrated (the pressure: 5.334 * 10 of filtrate through reducing pressure
4Pa), get uranidin medicinal extract, reclaim ethanol (rate of recovery 70%～80%), uranidin medicinal extract is through vacuum drying (60 ℃), and 60 orders sieve, and gets uranidin (powder) (product IV), yield 0.2%.
Embodiment 5:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders-80 order), add 60 ℃ of hot-water soaks of 8 times of weight 12 hours, decompression distillation (pressure 66.67Pa) 3 hours gets oil-water mixture and slag, oil-water mixture through oil water separator separate tangerine oil (product I), yield 1.30%; 85 ℃ the hot water that adds 30 times of weight in the slag, PH is 2.5 with 1N hydrochloric acid accent, lixiviate 1 hour, the plate and frame filter press press filtration gets filter residue and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry powder product as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 3.99 * 10
4Pa) to stoste volume 1/4, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 50%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60 ℃～70 ℃) (and reclaiming ethanol), pulverize, cross 60 mesh sieves, get pectin (powder) (product III), yield 6%; Concentrated (the pressure: 6.67 * 10 of filtrate through reducing pressure
4Pa) get uranidin medicinal extract, reclaim ethanol (rate of recovery 70%～80%), uranidin medicinal extract is through vacuum drying (60 ℃), and 60 orders sieve, and gets uranidin (powder) (product IV), yield 0.1%.
Embodiment 6:
Take by weighing fresh orange peel 10Kg, clean, be ground into graininess (40 orders～80 orders), add 75 ℃ of hot-water soaks of 8 times of weight 4 hours, decompression distillation (pressure 533.32Pa) 3 hours gets oil-water mixture and slag, oil-water mixture through oil water separator separate tangerine oil (product I), yield 1.15%; 85 ℃ the hot water that adds 30 times of weight in the slag is transferred PH2.5 with 1N hydrochloric acid, lixiviate 3 hours, the plate and frame type filter-press press filtration gets filter residue and filtrate, slag spontaneous fermentation 3～4 days, 60～80 ℃ dry powder product as Chinese herbal feed additive (product II); Filtrate decompression concentrates (pressure 2 * 10
4Pa) to stoste volume 1/4, the gained concentrate precipitates with 95% edible ethanol, concentration of alcohol is controlled at 40%(weight % in the precipitation mixture), through flame filter press press filtration must wet pectin and filtrate, pectin is refining with absolute ethyl alcohol, vacuum drying (60 ℃～70 ℃) (and reclaiming ethanol), pulverize, cross 60 mesh sieves, get pectin (powder) (product III), yield 4%; Concentrated (the pressure 6.67 * 10 of filtrate through reducing pressure
4Pa), get uranidin medicinal extract, reclaim ethanol (rate of recovery 70%～80%), uranidin medicinal extract is through vacuum drying (60 ℃), and 60 orders sieve, and gets uranidin (powder) (product IV), yield 0.15%.
The invention is not restricted to the foregoing description, content of the present invention all can be implemented.
Claims (6)
1, a kind of preparation technology of Citrus reticuiata Blano series of products comprises fresh orange peel is cleaned, pulverizes, and it is characterized in that also comprising the following steps:
After the fresh orange peel of a, pulverizing placed 60-90 ℃ of hot water of 3～8 times of weight to soak 2～12 hours, decompression distillation (pressure is 13.33Pa-533.32Pa) did not distillate to having grease substantially, got oil-water mixture (1) and residue (2);
Add 70～100 ℃ of hot water of 10～30 times of weight in b, the residue (2), transferring PH with inorganic acid (3) is 2-6, soaks after 1～6 hour, gets filtrate (4) and filter residue (5) through the filter press press filtration;
C, filter residue (5) are 20-35 ℃ of following spontaneous fermentation 3～5 days, again through 60～80 ℃ of dry feed addictives that get;
(pressure is 1.2 * 10 through decompression distillation for d, filtrate (4)
4Pa～3.99 * 10
4Pa) get oil-water mixture (6) and concentrate (7);
E, oil-water mixture (6) and oil-water mixture (1) merge through oil water separator separate tangerine oil;
Add 95% edible ethanol among the f, concentrate (7) and mix, and control ethanol weight accounts for this mixture weight 40-70%, make the pectin precipitation, get pectin (8) and filtrate (9) through the filter press press filtration;
G, pectin (8) get the powdery pectin product through vacuum desiccator drying, pulverizing, mistake 60 mesh sieves;
H, filtrate (9) are concentrated through reducing pressure, and (pressure is 2.67 * 10
4Pa～6.67 * 10
4Pa) get uranidin medicinal extract,, cross 60 mesh sieves, get powdery uranidin product again through the vacuum desiccator drying.
2, press the preparation technology of the described Citrus reticuiata Blano series of products of claim 1, it is characterized in that described in the step b at PH being 2～6 times 70～100 ℃ of hot-water soak residues (2) with 10～30 times of weight, this hot water can be divided into 2～4 immersions, merging filtrate after the filter press press filtration (4).
3, by the preparation technology of claim 1 or 2 described Citrus reticuiata Blano series of products, it is characterized in that the volume of concentrate described in the steps d (7) is controlled to be 1/4～1/5 of filtrate (4) volume preferably.
4, by the preparation technology of claim 1 or 2 described Citrus reticuiata Blano series of products, it is characterized in that inorganic acid described in the step b (3) can be hydrochloric acid, acetate, oxalic acid or phosphoric acid.
5, by the preparation technology of the described Citrus reticuiata Blano series of products of claim 3, it is characterized in that inorganic acid described in the step b (3) can be hydrochloric acid, acetate, oxalic acid or phosphoric acid.
6, press the preparation technology of claim 1,2 or 5 described Citrus reticuiata Blano series of products, it is characterized in that gained pectin (8) among the step f can also add the absolute ethyl alcohol of 1～4 times of weight, through mixing, filtration, vacuum drying, pulverizing, mistake 60 mesh sieves, must make with extra care pectin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN93110827A CN1078111A (en) | 1993-01-01 | 1993-01-01 | The preparation technology of Citrus reticuiata Blano series of products |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110827A CN1078111A (en) | 1993-01-01 | 1993-01-01 | The preparation technology of Citrus reticuiata Blano series of products |
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| CN1078111A true CN1078111A (en) | 1993-11-10 |
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|---|---|---|---|
| CN93110827A Pending CN1078111A (en) | 1993-01-01 | 1993-01-01 | The preparation technology of Citrus reticuiata Blano series of products |
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| CN101884405A (en) * | 2009-05-14 | 2010-11-17 | 马立同 | Process for manufacturing fruit cakes |
| CN101248841B (en) * | 2008-03-31 | 2011-07-20 | 天津天农康嘉生态养殖有限公司 | Feedstuff additive nutriment |
| CN102268327A (en) * | 2010-06-01 | 2011-12-07 | 浙江省柑桔研究所 | Method for orange peel essential oil and pectin combined production |
| CN102690724A (en) * | 2012-06-25 | 2012-09-26 | 天宁香料（江苏）有限公司 | Preparation method of concentrated tangerine oil, and application of prepared product |
| CN103913046A (en) * | 2014-02-19 | 2014-07-09 | 南充佳美食品工业有限公司 | Orange pomace and peel drying method |
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| US11623967B2 (en) | 2010-07-30 | 2023-04-11 | Cargill, Incorporated | Process for obtaining citrus fiber from citrus pulp |
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- 1993-01-01 CN CN93110827A patent/CN1078111A/en active Pending
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| CN101884405A (en) * | 2009-05-14 | 2010-11-17 | 马立同 | Process for manufacturing fruit cakes |
| CN104059249A (en) * | 2009-07-28 | 2014-09-24 | Cp凯可股份公司 | Dewatering biomass material comprising polysaccharide, method for extracting polysaccharide from biomass material, and dewatered biomass material |
| CN102268327A (en) * | 2010-06-01 | 2011-12-07 | 浙江省柑桔研究所 | Method for orange peel essential oil and pectin combined production |
| CN102268327B (en) * | 2010-06-01 | 2013-07-24 | 浙江省柑桔研究所 | Method for orange peel essential oil and pectin combined production |
| US11623967B2 (en) | 2010-07-30 | 2023-04-11 | Cargill, Incorporated | Process for obtaining citrus fiber from citrus pulp |
| AU2013209799B2 (en) * | 2012-01-20 | 2016-10-13 | Cargill, Incorporated | Process for obtaining citrus fiber from citrus peel |
| CN102690724B (en) * | 2012-06-25 | 2013-09-25 | 天宁香料（江苏）有限公司 | Preparation method of concentrated tangerine oil, and application of prepared product |
| CN102690724A (en) * | 2012-06-25 | 2012-09-26 | 天宁香料（江苏）有限公司 | Preparation method of concentrated tangerine oil, and application of prepared product |
| CN103913046A (en) * | 2014-02-19 | 2014-07-09 | 南充佳美食品工业有限公司 | Orange pomace and peel drying method |
| CN104560394A (en) * | 2014-12-29 | 2015-04-29 | 上海万香日化有限公司 | Method for comprehensively utilizing sweet orange oil terpene by-products |
| CN109480114A (en) * | 2018-12-18 | 2019-03-19 | 山东汉欧生物科技有限公司 | A kind of food and preparation method of pre- anti-pet obesity |
| WO2022029152A1 (en) * | 2020-08-05 | 2022-02-10 | Herbstreith & Fox Gmbh & Co. Kg Pektin-Fabriken | Activatable, deesterified fruit fiber |
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