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CN1526738A - Method for preparing pectin from citrus peel - Google Patents

Method for preparing pectin from citrus peel Download PDF

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Publication number
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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filter cake
minutes
filter
ethanol
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王存文
王为国
吴元欣
张俊峰
徐汶
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Wuhan Chemistry College
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Wuhan Chemistry College
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Abstract

本发明涉及一种柑桔皮制备果胶的方法，以柑桔皮为原料，经原料处理、酸萃取、盐析、脱盐和干燥步骤制备果胶。其中所采用的新方法：酸萃取过程中，在其后期，加入果胶助溶剂，提高了其后期的果胶溶出速率；盐析过程中，用含相同金属离子的盐水稀溶液洗涤纯化果胶盐沉淀，提高了果胶产品质量；脱盐过程中，用起始浓度较高的乙醇多级逆流方法脱盐，降低了乙醇使用量与损耗量。本发明具有果胶产品的质量好，综合成本低等优点。

Figure 03125441

The invention relates to a method for preparing pectin from citrus peels. The citrus peels are used as raw materials to prepare pectin through the steps of raw material treatment, acid extraction, salting out, desalting and drying. The new method used: in the acid extraction process, in the later stage, pectin co-solvent is added to improve the dissolution rate of pectin in the later stage; in the salting out process, the purified pectin is washed with a dilute brine solution containing the same metal ions Salt precipitation improves the quality of pectin products; in the desalination process, the multi-stage countercurrent method of ethanol with a higher initial concentration is used for desalination, which reduces the use and loss of ethanol. The invention has the advantages of good quality of pectin products, low overall cost and the like.

Figure 03125441

Description

Orange peel prepares the method for pectin
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、柑桔皮制备果胶的方法，主要包括原料处理、酸萃取、盐析、脱盐和干燥步骤，A、原料处理：干柑桔皮(含水10～14％)粉碎后，用清水浸泡1小时，滤去水，再用水漂洗至水基本无色；B、酸萃取：将处理后的柑桔皮粉置入25倍水中，加盐酸，在pH1.4～1.6、温度80～85℃的条件下搅拌，萃取30分钟后，加入0.2％水量的果胶助溶剂，再萃取20分钟，过滤得萃取液；C、盐析：边搅拌边加入硫酸铝溶液至萃取液中，氨水调pH至4.0～4.5，静置，压滤，滤饼为控湿90％的果胶铝沉淀，将滤饼粉碎至粒度1mm；D、脱盐：①脱铝离子：将粉碎后的果胶铝沉淀置入75％的乙醇中，加36～38％盐酸后，搅拌15分钟，压滤，滤饼控湿90％；②脱铝离子：将①步的滤饼置入75％的乙醇中，加36～38％盐酸后，搅拌10～15分钟，压滤，滤饼控湿90％；③脱铝离子：将②步的滤饼置入75％的乙醇中，加36～38％盐酸后，搅拌15分钟，压滤，滤饼控湿90％；④脱氯化氢：将③步的滤饼置入90％的乙醇中，搅拌15分钟，压滤，滤饼控湿90％；⑤脱氯化氢：将④步的滤饼置入90％的乙醇中，滴加20～22％氨水调溶液pH至3.5～4.0，搅拌15分钟，压滤，滤饼控湿90％；⑥脱氯化铵：将⑤步的滤饼置入90％的乙醇中，搅拌30分钟，压滤，滤饼为控湿70％湿果胶；E、干燥：将湿果胶粉碎至粒度1mm，装盘，置入烘厢，在50℃、真空度为0.08MPa条件下，干燥4小时得干果胶，将干果胶粉碎至60～80目得果胶产品。1. The method for preparing pectin from citrus peels mainly includes raw material processing, acid extraction, salting out, desalination and drying steps. A. Raw material processing: after crushing dried citrus peels (water content 10-14%), soak them in water for 1 hour, filter the water, then rinse with water until the water is basically colorless; B, acid extraction: put the treated citrus peel powder into 25 times of water, add hydrochloric acid, at pH 1.4～1.6, temperature 80～85 ℃ Stir under conditions, extract after 30 minutes, add 0.2% water as a pectin co-solvent, extract for another 20 minutes, and filter to obtain the extract; C, salting out: add aluminum sulfate solution to the extract while stirring, and adjust the pH to 4.0～4.5, stand still, press filter, the filter cake is pectin aluminum precipitation with humidity control 90%, crush the filter cake to a particle size of 1mm; D, desalination: ①dealuminum ion: put the pulverized pectin aluminum precipitation into In 75% ethanol, add 36-38% hydrochloric acid, stir for 15 minutes, press filter, and the humidity of the filter cake is 90%; After 38% hydrochloric acid, stir for 10-15 minutes, press filter, and the filter cake has a humidity control of 90%; ③dealuminum ion: put the filter cake in step ② into 75% ethanol, add 36-38% hydrochloric acid, and stir for 15 Minutes, pressure filtration, filter cake humidity control 90%; ④ dehydrochlorination: put the filter cake in step ③ into 90% ethanol, stir for 15 minutes, press filtration, filter cake humidity control 90%; ⑤ dehydrochlorination: put ④ Put the filter cake in the first step into 90% ethanol, add 20-22% ammonia water dropwise to adjust the pH of the solution to 3.5-4.0, stir for 15 minutes, press filter, and the filter cake will control the humidity to 90%; Put the filter cake in 90% ethanol, stir for 30 minutes, press filter, the filter cake is 70% wet pectin for humidity control; E, drying: crush the wet pectin to a particle size of 1mm, put it into a tray, and put it into a drying chamber. Under the conditions of 50° C. and a vacuum degree of 0.08 MPa, dry pectin for 4 hours to obtain dry pectin, and crush the dried pectin to 60-80 mesh to obtain pectin products. 2、根据权利要求1所述柑桔皮制备果胶的方法，其特征在于：果胶助溶剂为碳酸氨、碳酸氢氨、碳酸钠或碳酸氢钠。2. The method for preparing pectin from citrus peels according to claim 1, characterized in that: the pectin cosolvent is ammonium carbonate, ammonium bicarbonate, sodium carbonate or sodium bicarbonate. 3、根据权利要求1所述柑桔皮制备果胶的方法，其特征在于：所述盐析，边搅拌边加入20％硫酸铝溶液至萃取液中，用20～22％氨水调pH至4.0～4.5，静置30分钟，压滤并将滤饼粉碎，用0.3％硫酸铝溶液洗涤数次，至洗涤液呈淡黄绿色，压滤，滤饼为控湿90％的果胶铝沉淀，将滤饼粉碎至粒度1mm。3. The method for preparing pectin from citrus peels according to claim 1, characterized in that: for the salting out, add 20% aluminum sulfate solution to the extract while stirring, and adjust the pH to 4.0 with 20-22% ammonia water ~4.5, let it stand for 30 minutes, press filter and crush the filter cake, wash with 0.3% aluminum sulfate solution several times until the washing liquid is light yellow-green, press filter, the filter cake is precipitated by pectin aluminum with 90% humidity control, The filter cake was crushed to a particle size of 1 mm. 4、根据权利要求1所述柑桔皮制备果胶的方法，其特征在于：所述脱盐，①脱铝离子：将粉碎后的果胶铝沉淀置入前一次②步排出液(含乙醇约75％)中，搅拌15分钟，压滤，滤饼控湿90％；②脱铝离子：将①步的滤饼置入前一次③步排出液(含乙醇约80％)，加36～38％盐酸后，搅拌15分钟，压滤，滤饼控湿90％；③脱铝离子：将②步的滤饼置入前一次④步排出液(含乙醇约83％)，加36～38％盐酸后，搅拌15分钟，压滤，滤饼控湿90％；④脱氯化氢：将③步的滤饼置入前一次⑤步排出液(含乙醇约85％)，搅拌15分钟，压滤，滤饼控湿90％；⑤脱氯化氢：将④步的滤饼置入前一次⑥步排出液(含乙醇约88％)，滴加20～22％氨水调溶液pH至3.5～4.0，搅拌15分钟，压滤，滤饼控湿90％；⑥脱氯化铵：将⑤步的滤饼置入90％的乙醇中，搅拌30分钟，压滤，滤饼为控湿70％湿果胶。4. The method for preparing pectin from citrus peels according to claim 1, characterized in that: the desalination, ① dealumination: put the pulverized aluminum pectin precipitate into the previous ② step discharge liquid (containing ethanol about 75%), stirred for 15 minutes, press-filtered, the filter cake humidity control was 90%; After 1% hydrochloric acid, stir for 15 minutes, press filter, filter cake humidity control 90%; ③dealuminum ion: put the filter cake of step ② into the discharge liquid of step ④ (containing about 83% ethanol), add 36-38% After hydrochloric acid, stir for 15 minutes, press filter, filter cake humidity control 90%; ④ dehydrochlorination: put the filter cake of step ③ into the discharge liquid of the previous step ⑤ (containing about 85% ethanol), stir for 15 minutes, press filter, Filter cake humidity control 90%; ⑤ dehydrochlorination: put the filter cake in step ④ into the discharge liquid of step ⑥ (containing about 88% ethanol), add dropwise 20-22% ammonia water to adjust the pH of the solution to 3.5-4.0, stir for 15 Minutes, pressure filtration, filter cake humidity control 90%; 6. Deammonium chloride: put the filter cake of step 5 in 90% ethanol, stir for 30 minutes, pressure filtration, filter cake is humidity control 70% wet pectin.
CNA031254411A 2003-09-23 2003-09-23 Method for preparing pectin from citrus peel Pending CN1526738A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100443504C (en) * 2006-09-26 2008-12-17 陕西科技大学 A method for extracting pectin from pulping and cooking waste liquor of white cork
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

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100443504C (en) * 2006-09-26 2008-12-17 陕西科技大学 A method for extracting pectin from pulping and cooking waste liquor of white cork
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 A method of using a decanter centrifuge 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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