CN1526738A - Method of preparing pectin with orange peel - Google Patents
Method of preparing pectin with orange peel Download PDFInfo
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- CN1526738A CN1526738A CNA031254411A CN03125441A CN1526738A CN 1526738 A CN1526738 A CN 1526738A CN A031254411 A CNA031254411 A CN A031254411A CN 03125441 A CN03125441 A CN 03125441A CN 1526738 A CN1526738 A CN 1526738A
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Abstract
The present invention is method of preparing pectin with orange peel. Orange peel as material is produced into pectin through the steps of material processing, acid extraction, salt separation, desalting and drying. During the production, pectin cosolvent is added in the later acid extraction steps to raise the pectin leaching rate; dilute salt solution is used to wash and purify pectin salt precipitate and raise pectin product quality in the salt separation step; and multistage reflux desalting method with higher initial concentration is adopted during desalting step to lower the use amount and consumption of ethanol. The present invention has the advantages of high pectin product quality, low comprehensive cost, etc.
Description
Technical field
The present invention relates to foodstuff additive manufacture field, particularly process for producing pectin.
Background technology
With the orange peel is that feedstock production pectin method comparatively commonly used has: the pure precipitator method and salting-out process.Alcohol precipitation legal system is equipped with pectin and comprises that raw material processing, acid extraction, vacuum concentration, alcohol analyses and drying and other steps.This technology major defect is: for the usage quantity of the alcohol that reduces pure precipitation process, must carry out vacuum concentration to extraction liquid, and vacuum Concentrating Process is a large amount of water-soluble and be insoluble to impurity (comprising pigment) enrichment in concentrated solution of alcohol, and pectin molecule has to a certain degree degraded in vacuum Concentrating Process, is difficult to obtain the high quality pectin product.Salting-out process prepares that pectin comprises raw material processing, acid extraction, saltouts, desalination and drying and other steps.Compare with the pure precipitator method, salting-out process is to realize at low temperatures, and removes a large amount of water-solublely and be insoluble to the impurity (comprising pigment) of alcohol at salting-out process, and therefore, pectin product quality improves.But during metal ion, the alcoholic acid usage quantity is bigger in removing pectin salt, and ethanol waste and its usage quantity positive correlation, therefore, comprehensive cost is than higher.
Summary of the invention
Technical problem to be solved by this invention is: overcome the defective that aforesaid method exists, prepare orange peel pectin quality simultaneously at the raising salting-out process, reduce its comprehensive cost.
The technical scheme that technical problem adopted that the present invention solves: with the orange peel is that raw material adopts salting-out process to prepare pectin.In its acid extraction process, in its later stage, add the pectin solubility promoter, improved the pectin dissolution rate in its later stage.In its salting-out process,, improved the pectin product quality with containing same metal ionic salt solution dilute solution washing purifying pectin salt precipitation.Under identical suitable salting-out condition, can make the galacturonic acid content in the pectin product increase by 4～6% to pectin salt washing purifying.In its demineralising process,, ethanol usage quantity and waste have been reduced with the higher ethanol multi-stage countercurrent method desalination of initial concentration.Keeping under desalting effect the same terms, with the higher ethanol multi-stage countercurrent desalination more stages cross-flow method desalination of initial concentration, the ethanol usage quantity reduces more than 50%.Major advantage of the present invention is: 1. the pectin quality is good, and pectin product is beige, galacturonic acid content 75～80%, 200～250 ° of degree of gelation.2. comprehensive cost is low, prepare employing novel method of the present invention in the orange peel pectin technology at salting-out process, the yield of pectin and the pure precipitator method are basic identical, the cost (account for total cost of production 10%) in this step of saltouing in the salting-out process is 40～50% of the cost in this step of vacuum concentration in the pure precipitator method, in the salting-out process in the cost in this step of desalination and the pure precipitator method cost in this step of alcohol precipitation basic identical, and other step both are identical.Therefore, salting-out process prepare in the orange peel pectin technology adopt novel method of the present invention after, the production cost of pectin product is lower than the pure precipitator method.
Description of drawings
Accompanying drawing is this bright process flow diagram.
Embodiment
Hereinafter the invention will be further described in conjunction with example and accompanying drawing.
As shown in drawings: with the orange peel is raw material, through raw material processing, acid extraction, saltout, desalination and drying step prepare pectin.
Embodiment one
1. raw material is handled: after the dried orange peel of 1000 grams (moisture 10～14%, stored 6 months) is pulverized, in clear water, soaked 1 hour, elimination water, again with water rinse extremely water base colourless.
2. acid extraction: the citrus peel meal after will handling insert in the water (dried citrus peel meal: water=1: 25), add hydrochloric acid, stir under 80～85 ℃ the condition, extracted 50 minutes in pH1.4～1.6, temperature, filter extraction liquid.
3. saltout: add 0.5 liter of 20% alum liquor while stirring to extraction liquid, transfer pH to 4.0～4.5, left standstill 30 minutes with 20～22% ammoniacal liquor, press filtration, filter cake is crushed to filter cake about granularity 1mm for the pectin aluminum precipitation of control wet 90%.
4. desalination:
1. dealuminzation ion: the pectin aluminum precipitation after will pulverizing is inserted in 6 liter 75% the ethanol, add 0.3 liter of 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes.
2. dealuminzation ion: the filter cake that will 1. go on foot is inserted in 6 liter 75% the ethanol, add 0.3 liter of 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 10～15 minutes.
3. dealuminzation ion: the filter cake that will 2. go on foot is inserted in 6 liter 75% the ethanol, add 0.3 liter of 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes.
4. dehydrochlorination: the filter cake that will 3. go on foot is inserted in 3 liter 90% the ethanol, stirs press filtration, filter cake control wet 90% 15 minutes.
5. dehydrochlorination: the filter cake that will 4. go on foot is inserted in 3 liter 90% the ethanol, drips 20～22% ammoniacal liquor and transfers pH value of solution to 3.5～4.0, stirred 15 minutes, and press filtration, the filter cake control wets 90%.
6. dechlorination ammonium: the filter cake that will 5. go on foot is inserted in 3 liter 90% the ethanol, stirs press filtration, filter cake control wet 70% 30 minutes.
5. dry: the pectin powder that will wet is broken to about granularity 1mm, and the baking railway carriage or compartment is inserted in sabot, is under the 0.08MPa condition at 50 ℃, vacuum tightness, dry 4 hours dry fruit glue.The dry fruit rubber powder is broken to 60～80 orders gets pectin product.
Pectin product is beige, galacturonic acid content 65～70%, and aluminium composition is less than 0.04%, 150～170 ° of degree of gelation.Yield 9～11% (in dried orange peel).
Embodiment two
In the acid extraction process, if improve temperature, or time expand, the yield of pectin is increased to some extent, but pectin product quality reduce (mainly show as: the pectin product degree of gelation reduces, color burn).If residue after the acid extraction first time is extracted again, the pectin product that is obtained, quality is very low, does not have commodity value substantially.Therefore, the comparatively reasonable method that improves the pectin yield is: in the acid extraction process, do not change the acid extraction condition, in its later stage, add the pectin solubility promoter, improve the pectin dissolution rate in its later stage.Example is as follows:
1. raw material is handled: with embodiment one
2. acid extraction: the citrus peel meal after will handling is inserted in the water (dried citrus peel meal: water=1: 25), add hydrochloric acid, stir under 80～85 ℃ the condition in pH1.4～1.6, temperature, extracted 30 minutes.After adding pectin solubility promoter (add-on be the water yield 0.2%), extracted again 20 minutes, filter extraction liquid.
3. saltout: with embodiment one.
4. desalination: with embodiment one.
5. dry: with embodiment one.
Pectin product is beige, galacturonic acid content 70～75%, 170～200 ° of degree of gelation.Aluminium composition is less than 0.04%, yield 12～14% (in dried orange peel).
Embodiment three
Contain a large amount of wet part in the pectin salt precipitation that obtains after extraction liquid is saltoutd, these wet part is by water, water-soluble and water-soluble but be insoluble to the impurity (comprising pigment) of alcohol, the pectin salt precipitation is also wrapped up water-soluble in a large number and is insoluble to pure impurity (comprising pigment), if remove these water-soluble impurity (especially being insoluble to the impurity of alcohol) before desalination, pectin product quality will increase.Fully compress pectin salt precipitation its wet part content is reduced, but can not remove a large amount of water-soluble of parcel wherein and be insoluble to pure impurity (comprising pigment).Therefore, the sedimentary comparatively reasonable method of purifying pectin salt is: with containing the washing of same metal ionic salt solution dilute solution.Example is as follows:
1. raw material is handled: with example one.
2. acid extraction: with example two.
3. saltout: add 0.5 liter of 20% alum liquor while stirring to extraction liquid, transfer pH to 4.0～4.5 with 20～22% ammoniacal liquor, left standstill 30 minutes, press filtration is also pulverized filter cake, with 0.3% alum liquor washing for several times, be pistac, press filtration to washings, filter cake is crushed to filter cake about granularity 1mm for the pectin aluminium of control wet 90% is heavy.
4. desalination: with example one.
5. dry: with example one.
Pectin product is beige, galacturonic acid content 75～80%, and aluminium composition is less than 0.04%, 200～250 ° of degree of gelation, yield 11～13% (in dried orange peel).
Embodiment four
Salting-out process is produced the cost in this step of desalination in the pectin process in (as: the multistage cross flow method desalination of introducing in the previous examples of the shared large percentage of total cost of production, the cost in this step of desalination accounts for more than 60% in total cost of production), prime cost is the loss of ethanol use and the recovery cost after the use, in general, ethanol waste and usage quantity positive correlation, therefore, the alcoholic acid usage quantity that reduces in the demineralising process will reduce the comprehensive cost that salting-out process is produced pectin effectively.The rational method that reduces the ethanol usage quantity is: adopt the higher ethanol multi-stage countercurrent method desalination of initial concentration.Example is as follows:
1. raw material is handled: with example one.
2. acid extraction: with example two.
3. saltout: with example three.
4. desalination:
1. dealuminzation ion: once 2. go on foot before the pectin aluminum precipitation after will pulverizing is inserted 8 liters in the liquid effluent (containing ethanol about 75%), stirred 15 minutes, press filtration, filter cake control wet 90%.
2. dealuminzation ion: once 3. go on foot liquid effluent (containing ethanol about 80%) before the filter cake that will 1. go on foot is inserted 8 liters, add 0.3 liter of 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes.
3. dealuminzation ion: once 4. go on foot liquid effluent (containing ethanol about 83%) before the filter cake that will 2. go on foot is inserted 8 liters, add 0.3 liter of 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes.
4. dehydrochlorination: once 5. go on foot liquid effluent (containing ethanol about 85%) before the filter cake that will 3. go on foot is inserted 8 liters, stirred 15 minutes, press filtration, filter cake control wet 90%.
5. dehydrochlorination: once 6. go on foot liquid effluent (containing ethanol about 88%) before the filter cake that will 4. go on foot is inserted 8 liters, drip 20～22% ammoniacal liquor and transfer pH value of solution to 3.5～4.0, stirred 15 minutes, press filtration, the filter cake control wets about 90%.
6. dechlorination ammonium: the filter cake that will 5. go on foot is inserted in 8 liter 90% the ethanol, stirred 30 minutes, and press filtration, filter cake is control wet 70% wet pectin.
5. dry: with example one.
Pectin product quality and yield are with example three.
Adopting acid extraction method of the present invention in alcohol deposition method also can make the quality of its product and yield all be improved.
Claims (4)
1, orange peel prepares the method for pectin, mainly comprise raw material processing, acid extraction, saltout, desalination and drying step, A, raw material are handled: after dried orange peel (moisture 10～14%) is pulverized, soaked 1 hour with clear water, elimination water, again with water rinse to water base colourless; B, acid extraction: the citrus peel meal after will handling is inserted in 25 times of water, adds hydrochloric acid, stirs under 80～85 ℃ the condition in pH1.4～1.6, temperature, extracts after 30 minutes, adds the pectin solubility promoter of 0.2% water yield, extracts 20 minutes again, filter extraction liquid; C, saltout: add alum liquor while stirring to extraction liquid, ammoniacal liquor is transferred pH to 4.0～4.5, leave standstill, and press filtration, filter cake is crushed to granularity 1mm for the pectin aluminum precipitation of control wet 90% with filter cake; D, desalination: 1. dealuminzation ion: the pectin aluminum precipitation after will pulverizing is inserted in 75% the ethanol, add 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes; 2. dealuminzation ion: the filter cake that will 1. go on foot is inserted in 75% the ethanol, add 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 10～15 minutes; 3. dealuminzation ion: the filter cake that will 2. go on foot is inserted in 75% the ethanol, add 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes; 4. dehydrochlorination: the filter cake that will 3. go on foot is inserted in 90% the ethanol, stirs press filtration, filter cake control wet 90% 15 minutes; 5. dehydrochlorination: the filter cake that will 4. go on foot is inserted in 90% the ethanol, drips 20～22% ammoniacal liquor and transfers pH value of solution to 3.5～4.0, stirred 15 minutes, and press filtration, the filter cake control wets 90%; 6. dechlorination ammonium: the filter cake that will 5. go on foot is inserted in 90% the ethanol, stirred 30 minutes, and press filtration, filter cake is control wet 70% wet pectin; E, drying: the pectin powder that will wet is broken to granularity 1mm, and the baking railway carriage or compartment is inserted in sabot, is 0.08MP at 50 ℃, vacuum tightness
aUnder the condition, got dry fruit glue, and the dry fruit rubber powder was broken to 60～80 orders gets pectin product in dry 4 hours.
2, prepare the method for pectin according to the described orange peel of claim 1, it is characterized in that: the pectin solubility promoter is carbonic acid ammonia, ammonium hydrogencarbonate, yellow soda ash or sodium bicarbonate.
3, the method for preparing pectin according to the described orange peel of claim 1, it is characterized in that: described saltouing, add 20% alum liquor while stirring to extraction liquid, transfer pH to 4.0～4.5, left standstill 30 minutes with 20～22% ammoniacal liquor, press filtration is also pulverized filter cake, with 0.3% alum liquor washing for several times, be pistac, press filtration to washings, filter cake is crushed to granularity 1mm for the pectin aluminum precipitation of control wet 90% with filter cake.
4, the method for preparing pectin according to the described orange peel of claim 1, it is characterized in that: described desalination, 1. dealuminzation ion: once 2. go on foot before the pectin aluminum precipitation after will pulverizing is inserted in the liquid effluent (containing ethanol about 75%), stirred 15 minutes, press filtration, filter cake control wet 90%; 2. dealuminzation ion: once 3. go on foot liquid effluent (containing ethanol about 80%) before the filter cake that will 1. go on foot is inserted, add 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes; 3. dealuminzation ion: once 4. go on foot liquid effluent (containing ethanol about 83%) before the filter cake that will 2. go on foot is inserted, add 36～38% hydrochloric acid after, stirred press filtration, filter cake control wet 90% 15 minutes; 4. dehydrochlorination: once 5. go on foot liquid effluent (containing ethanol about 85%) before the filter cake that will 3. go on foot is inserted, stirred 15 minutes, press filtration, filter cake control wet 90%; 5. dehydrochlorination: once 6. go on foot liquid effluent (containing ethanol about 88%) before the filter cake that will 4. go on foot is inserted, drip 20～22% ammoniacal liquor and transfer pH value of solution to 3.5～4.0, stirred 15 minutes, press filtration, the filter cake control wets 90%; 6. dechlorination ammonium: the filter cake that will 5. go on foot is inserted in 90% the ethanol, stirred 30 minutes, and press filtration, filter cake is control wet 70% wet pectin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031254411A CN1526738A (en) | 2003-09-23 | 2003-09-23 | Method of preparing pectin with orange peel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031254411A CN1526738A (en) | 2003-09-23 | 2003-09-23 | Method of preparing pectin with orange peel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443504C (en) * | 2006-09-26 | 2008-12-17 | 陕西科技大学 | Method of extracting pectin from waste liquor of white paper mulberry bast pulping |
| CN101791593A (en) * | 2010-03-10 | 2010-08-04 | 砀山宇宁生物科技有限公司 | Horizontal screw centrifugal machine for solid-liquid separation of pectin and use method thereof |
| 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 |
| CN114014951A (en) * | 2021-11-30 | 2022-02-08 | 张东坡 | Production process of alcohol-free instant pectin |
-
2003
- 2003-09-23 CN CNA031254411A patent/CN1526738A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443504C (en) * | 2006-09-26 | 2008-12-17 | 陕西科技大学 | Method of extracting pectin from waste liquor of white paper mulberry bast pulping |
| CN101791593A (en) * | 2010-03-10 | 2010-08-04 | 砀山宇宁生物科技有限公司 | Horizontal screw centrifugal machine for solid-liquid separation of pectin and use method thereof |
| CN101791593B (en) * | 2010-03-10 | 2013-05-29 | 砀山宇宁生物科技有限公司 | Use method of horizontal screw centrifugal machine for solid-liquid separation of 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 |
| CN114014951A (en) * | 2021-11-30 | 2022-02-08 | 张东坡 | Production process of alcohol-free instant pectin |
| CN114014951B (en) * | 2021-11-30 | 2022-08-30 | 张东坡 | Production process of alcohol-free instant pectin |
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