CN107056964A - A kind of method that utilization zanthoxylum slag prepares pectin - Google Patents
A kind of method that utilization zanthoxylum slag prepares pectin Download PDFInfo
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- CN107056964A CN107056964A CN201710076130.7A CN201710076130A CN107056964A CN 107056964 A CN107056964 A CN 107056964A CN 201710076130 A CN201710076130 A CN 201710076130A CN 107056964 A CN107056964 A CN 107056964A
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- pectin
- utilization
- zanthoxylum slag
- zanthoxylum
- prepares
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a kind of method that utilization zanthoxylum slag prepares pectin, comprise the following steps：Pretreatment, pectin extraction, centrifugation removal of impurities, activated carbon decolorizing, vacuum concentration, alcohol precipitation, pectin separation, dry pectin finished product.The process operation that the present invention prepares pectin is simple, and auxiliary material used in whole process is food-grade processing aid, is remained in finished product pectin, and finished product pectin is applied to food processing field, while providing one kind for industrial waste zanthoxylum slag utilizes new way.
Description
Technical field
The present invention relates to pectin production technical field, and in particular to one kind prepares pectin using Wastage of food industry zanthoxylum slag
Method.
Background technology
Chinese prickly ash has higher economic value and ecological protection function, implementation and the market demand with project of conceding the land to forestry
Pulling, China's Chinese prickly ash cultivated area expands rapidly in recent years, and the speed with annual 2 times increases.The Chinese prickly ash total yield of current China
Amount is at 400,000 tons or so, pricklyash bark and each 200,000 tons or so of wild pepper seed (2012 annual data), and the deep processing of Chinese prickly ash is concentrated mainly on
It is more and more extensive with the deep processing of Chinese prickly ash in terms of Zanthoxylum essential oil, pepper volatile oil, xanthoxylum oleoresin, Fructus Zanthoxyli oil, zanthoxylum slag
As a big industrial waste, but its utilization rate is low, and substantial amounts of zanthoxylum slag is discarded to cause environmental pollution.With supercritical CO2Extraction
Application popularization of the technology in spice extraction, has been extracted after xanthoxylum oleoresin, remaining zanthoxylum slag does not have any solvent residual
The pollution such as stay, because the macromolecular substances such as protein, carbohydrate, dietary fiber are very severe for extraction conditions in Chinese prickly ash
Carve, their contents in zanthoxylum slag are also very high, do not have preferable utilization ways to cause the larger wasting of resources these materials.
The content of the invention
The problem to be solved in the present invention is to provide one kind for the above-mentioned deficiency in the presence of prior art and utilize Chinese prickly ash
Slag prepares the extraction from zanthoxylum slag of the method for pectin and prepares pectin.
To achieve the above object, present invention employs following technical scheme：A kind of utilization zanthoxylum slag prepares the side of pectin
Method, comprises the following steps：
[1] pre-process：Add 8-10 times of water to boil 10-15min into zanthoxylum slag and obtain mixed liquor；
[2] pectin is tentatively extracted：The mixed liquor pH value is adjusted to 3-4, heating, in 70-90 DEG C with food grade organic acid
Filtrate is obtained after insulated and stirred 1-2h, filtering；
[3] removal of impurities is centrifuged：Filtrate centrifuges in tube centrifuge, collects clear liquid；
[4] activated carbon decolorizing：Add in clear liquid and stir 1h at 2-5% food grade active charcoal, 40-50 DEG C, filter, obtain de-
Pectin extracting soln after color
[5] it is concentrated in vacuo：Pectin extracting soln after decolouring is in concentration at vacuum 0.75-0.95MPa, 45-60 DEG C of temperature
To 3-5 times of raw material weight；
[6] alcohol precipitation：Consumption is added to alcohol precipitation pectin in concentrate for 2-3 times of edible alcohol of concentrate weight；
[7] pectin is separated：Pectin is cleaned 2-3 times with 60-70% alcoholic solution, filtering；
[8] dry：Pectin is freeze-dried, and obtains pectin finished product.
Further, the zanthoxylum slag is that supercritical carbon dioxide extraction technology has extracted the zanthoxylum slag after pigment and numb monosodium glutamate.
Further, step 2) in filter after filter residue repeating said steps 2) operation 2-3 times, merging filtrate；
Further, step 2) in the organic acid be food-grade citric acid.
Further, 16000r/min is centrifuged in tube centrifuge.
Further, step 4) in the pectin extracting soln decolorising agent used that decolourizes be food grade active charcoal.
Further, step 6) in pectin prepare the edible alcohol that alcohol used is at least 95% and the above for concentration.
Compared to prior art, the present invention has the advantages that：The present invention is by the use of zanthoxylum slag as raw material, by pre-
Processing, acid adjustment are extracted, centrifugation removal of impurities, activated carbon decolorizing, vacuum concentration, separated, be dried to obtain pectin finished product, reduce resource
Waste；The process operation that the present invention prepares pectin is simple, and auxiliary material used in whole process is food-grade processing aid, finished product
Pectin is applied to food processing field, while providing one kind for industrial waste zanthoxylum slag utilizes new way.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Embodiment
In order that technological means, creation characteristic, reached purpose that the present invention is realized more understand and are apparent to effect,
With reference to embodiment, the present invention is further elaborated：
Embodiment 1
The present invention proposes a kind of method that utilization zanthoxylum slag prepares pectin, comprises the following steps：
[1] pre-process：Add 8-10 times of water to boil 10-15min into zanthoxylum slag and obtain mixed liquor.
[2] pectin is tentatively extracted：Make the solubility of pectin more with organic food acids adjustment mixed liquor pH value to 3-4
Height, heating, in 70-90 DEG C of insulation, stirs 1-2h, filtrate is obtained after filtering；
[3] removal of impurities is centrifuged：Filtrate centrifuges in tube centrifuge, collects clear liquid；
[4] activated carbon decolorizing：Add in clear liquid and stir 1h at 2-5% food grade active charcoal, 40-50 DEG C, filter, obtain de-
Pectin extracting soln after color；
[5] it is concentrated in vacuo：Pectin extracting soln after decolouring is in concentration at vacuum 0.75-0.95MPa, 45-60 DEG C of temperature
To 3-5 times of raw material weight；
[6] alcohol precipitation：Consumption is added to alcohol precipitation pectin in concentrate for 2-3 times of edible alcohol of concentrate weight；
[7] pectin is separated：Pectin is cleaned 2-3 times with 60-70% alcoholic solution, filtering；
[8] dry：Pectin is freeze-dried, and obtains pectin finished product.
The present invention is by the way that zanthoxylum slag as raw material, is extracted by pretreatment, acid adjustment, centrifugation removal of impurities, activated carbon decolorizing, true
Sky is concentrated, separated, being dried to obtain pectin finished product；Reduce the waste of resource.
As specific embodiment, the zanthoxylum slag is that supercritical carbon dioxide extraction technology has been extracted after pigment and numb monosodium glutamate
Zanthoxylum slag, nontoxic solvent-free residual zanthoxylum slag can be left afterwards, using these residual zanthoxylum slag, take mesh number in 40-
60 mesh are one group and prepare pectin to zanthoxylum slag residual progress.
As specific embodiment, 1kg supercritical carbon dioxide extraction technologies are taken to extract the Chinese prickly ash after pigment and numb monosodium glutamate
Slag, adds the stirring of 8kg water and boils 15min, be cooled to normal temperature；Then with the pH value of the above-mentioned mixed liquor of citric acid adjustment to 3.25,
Heating, in insulated and stirred 1h in 90 DEG C, filtrate is collected in filtering；Repetition is operated as above 3 times, merges 3 filtrates.Filtrate is passed through
16000r/min tube centrifuge centrifugation, collects clear liquid；30g food grade active charcoals are added thereto, and 1h is stirred at 40 DEG C,
Filtering；Filtrate is concentrated to 3.8kg and stops concentration in being concentrated at vacuum 0.85MPa, 55 DEG C of temperature；Added into concentrate
8kg95% edible alcohols, stand 12h.Filtering, pectin is cleaned 2 times with 65% edible alcohol solution；By pectin be freeze-dried into
Product.
As specific embodiment, in order to improve the utilization rate of zanthoxylum slag residue, in step 2) in filter after filter residue weight
The multiple step 2) operation 2-3 time, the filtrate repeatedly obtained mixing is subjected to step 3 together and then again)；
Be used as specific embodiment, step 2) in the organic acid be food-grade citric acid；Auxiliary material used is food-grade,
Ensure safety.
As specific embodiment, 16000r/min is centrifuged in tube centrifuge.
Be used as specific embodiment, step 4) in the pectin extracting soln decolorising agent used that decolourizes be food grade active charcoal.
Be used as specific embodiment, step 6) in pectin prepare alcohol used for concentration be at least 95% and the above it is edible
Alcohol.
Embodiment 2
As specific embodiment, 1kg supercritical carbon dioxide extraction technologies are taken to extract the Chinese prickly ash after pigment and numb monosodium glutamate
Slag, adds the stirring of 9kg water and boils 10min, be cooled to normal temperature；Then with the pH value of the above-mentioned mixed liquor of citric acid adjustment to 3.52,
Heating, in insulated and stirred 1h in 85 DEG C, filtrate is collected in filtering；Repetition is operated as above 3 times, merges 3 filtrates.Filtrate is passed through
16000r/min tube centrifuge centrifugation, collects clear liquid.50g food grade active charcoals are added thereto, and 1h is stirred at 45 DEG C,
Filtering.Filtrate is concentrated to 3.5kg and stops concentration in being concentrated under vacuum 0.9MPa, temperature 50 C；Added into concentrate
10kg95% edible alcohols, stand 12h；Filtering, pectin is cleaned 2 times with 67% edible alcohol solution；Pectin is freeze-dried
Finished product.
Other are same as Example 1.
Embodiment 3
As specific embodiment, 1kg supercritical carbon dioxide extraction technologies are taken to extract the Chinese prickly ash after pigment and numb monosodium glutamate
Slag, adds the stirring of 10kg water and boils 10min, be cooled to normal temperature；Then with the pH value of the above-mentioned mixed liquor of citric acid adjustment to 3.89,
Heating, in insulated and stirred 1.5h in 80 DEG C, filtrate is collected in filtering；Repetition is operated as above 3 times, merges 3 filtrates.Filtrate is led to
16000r/min tube centrifuge centrifugation is crossed, clear liquid is collected；45g food grade active charcoals are added thereto, are stirred at 50 DEG C
1h, filtering.Filtrate is concentrated to 4.6kg and stops concentration in being concentrated at vacuum 0.75MPa, 65 DEG C of temperature；Added into concentrate
13kg95% edible alcohols, stand 12h；Filtering, pectin is cleaned 2 times with 62% edible alcohol solution；Pectin is freeze-dried
Finished product.
Other are same as Example 1.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover at this
Among the right of invention.
Claims (7)
1. a kind of method that utilization zanthoxylum slag prepares pectin, it is characterised in that comprise the following steps：
[1] pre-process：Add 8-10 times of water to boil 10-15min into zanthoxylum slag and obtain mixed liquor；
[2] pectin is tentatively extracted：The mixed liquor pH value is adjusted to 3-4 with food grade organic acid, and heating is incubated in 70-90 DEG C,
1-2h is stirred, filtrate is obtained after filtering；
[3] removal of impurities is centrifuged：Filtrate centrifuges in tube centrifuge, collects clear liquid；
[4] activated carbon decolorizing：Add in clear liquid and stir 1h at 2-5% food grade active charcoal, 40-50 DEG C, filter, obtain after decolouring
Pectin extracting soln；
[5] it is concentrated in vacuo：Pectin extracting soln after decolouring at vacuum 0.75-0.95MPa, 45-60 DEG C of temperature in being concentrated into original
Expect weight 3-5 times；
[6] alcohol precipitation：Consumption is added to alcohol precipitation pectin in concentrate for 2-3 times of edible alcohol of concentrate weight；
[7] pectin is separated：Pectin is cleaned 2-3 times with 60-70% alcoholic solution, filtering；
[8] dry：Pectin is freeze-dried, and obtains pectin finished product.
2. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：The zanthoxylum slag is
Supercritical carbon dioxide extraction technology has extracted the zanthoxylum slag after pigment and numb monosodium glutamate.
3. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：Step 2) middle filtering
Filter residue repeating said steps 2 afterwards) operation 2-3 times, merging filtrate.
4. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：Step 2) in institute
Organic acid is stated for food-grade citric acid.
5. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：In tube centrifuge
16000r/min is centrifuged.
6. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：Step 4) in pectin
Decolorising agent used in extracting liquid decoloration is food grade active charcoal.
7. the method that a kind of utilization zanthoxylum slag according to claim 1 prepares pectin, it is characterised in that：Step 6) in pectin
Prepare the edible alcohol that alcohol used is at least 95% and the above for concentration.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710076130.7A CN107056964A (en) | 2017-02-13 | 2017-02-13 | A kind of method that utilization zanthoxylum slag prepares pectin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710076130.7A CN107056964A (en) | 2017-02-13 | 2017-02-13 | A kind of method that utilization zanthoxylum slag prepares pectin |
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| CN107056964A true CN107056964A (en) | 2017-08-18 |
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| CN201710076130.7A Pending CN107056964A (en) | 2017-02-13 | 2017-02-13 | A kind of method that utilization zanthoxylum slag prepares pectin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115226893A (en) * | 2022-07-26 | 2022-10-25 | 云南汉木森生物科技有限责任公司 | Pepper peel residue and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN103641930A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue by enzymatic process |
| CN104017105A (en) * | 2014-06-19 | 2014-09-03 | 中国农业大学 | Method for extracting pectin from pepper skin slag |
| CN105273433A (en) * | 2014-07-18 | 2016-01-27 | 周子童 | Natural pigment extraction technology |
| CN106174378A (en) * | 2016-07-15 | 2016-12-07 | 天宁香料（江苏）有限公司 | Flos Caryophylli, Zanthoxylum schinifolium compound the preparation method of extract and the application of product with pericarpium zanthoxyli bungeani |
-
2017
- 2017-02-13 CN CN201710076130.7A patent/CN107056964A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN103641930A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue by enzymatic process |
| CN104017105A (en) * | 2014-06-19 | 2014-09-03 | 中国农业大学 | Method for extracting pectin from pepper skin slag |
| CN105273433A (en) * | 2014-07-18 | 2016-01-27 | 周子童 | Natural pigment extraction technology |
| CN106174378A (en) * | 2016-07-15 | 2016-12-07 | 天宁香料（江苏）有限公司 | Flos Caryophylli, Zanthoxylum schinifolium compound the preparation method of extract and the application of product with pericarpium zanthoxyli bungeani |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115226893A (en) * | 2022-07-26 | 2022-10-25 | 云南汉木森生物科技有限责任公司 | Pepper peel residue and preparation method and application thereof |
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Application publication date: 20170818 |