CN1269843C - Process of preparing pectin from Japanese premna leaf - Google Patents
Process of preparing pectin from Japanese premna leaf Download PDFInfo
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- CN1269843C CN1269843C CN 03128055 CN03128055A CN1269843C CN 1269843 C CN1269843 C CN 1269843C CN 03128055 CN03128055 CN 03128055 CN 03128055 A CN03128055 A CN 03128055A CN 1269843 C CN1269843 C CN 1269843C
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- Prior art keywords
- pectin
- ultrafiltration
- bean curd
- ion exchange
- concentration
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- 239000001814 pectin Substances 0.000 title claims abstract description 39
- 229920001277 pectin Polymers 0.000 title claims abstract description 39
- 235000010987 pectin Nutrition 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 18
- 241000131771 Premna Species 0.000 title 1
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 235000013527 bean curd Nutrition 0.000 claims abstract description 11
- 238000004042 decolorization Methods 0.000 claims abstract description 11
- 238000005342 ion exchange Methods 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 8
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims abstract 5
- 239000000701 coagulant Substances 0.000 claims abstract 3
- 238000005345 coagulation Methods 0.000 claims abstract 3
- 230000015271 coagulation Effects 0.000 claims abstract 3
- 238000004332 deodorization Methods 0.000 claims abstract 3
- 239000000047 product Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229920002301 cellulose acetate Polymers 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 description 11
- 239000000796 flavoring agent Substances 0.000 description 11
- 235000019634 flavors Nutrition 0.000 description 11
- 241000531314 Premna microphylla Species 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000005507 spraying Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005189 flocculation Methods 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Images
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
本发明是一种豆腐柴叶制备果胶工艺，以豆腐柴叶为原料，经原料处理、酸萃取、过滤、脱色脱味、喷雾干燥制成果胶，或者，在脱色脱味后，经醇沉淀、洗涤和喷雾干燥制成果胶。其中，过滤后的萃取液通过凝聚、离子交换、超滤浓缩进行脱色脱味和脱糖，即：将浓度为1%的凝聚剂置入过滤后的萃取液中，通过加碱控制pH值，分两步沉淀除杂脱色；凝聚除杂后的提取液，由离子交换树脂在离子交换柱中处理；树脂脱色后的液体在常温常压下，经内压式超滤膜超滤浓缩3～4倍，得超滤浓缩液。本发明具有工序少、除杂率高、果胶损失量小和可低温操作等优点。
The present invention relates to a process for preparing pectin from bean curd leaves. The pectin is made from bean curd leaves as raw materials, through raw material treatment, acid extraction, filtration, decolorization and deodorization, and spray drying, or, after decolorization and deodorization, through alcohol precipitation , washing and spray drying to make pectin. Among them, the filtered extract is decolorized, deodorized and desugared through coagulation, ion exchange, and ultrafiltration concentration, that is, a coagulant with a concentration of 1% is placed in the filtered extract, and the pH value is controlled by adding alkali. Precipitate in two steps to remove impurities and decolorize; coagulate the extract after removing impurities, and use ion exchange resin to process it in an ion exchange column; the liquid after resin decolorization is concentrated by ultrafiltration through an internal pressure ultrafiltration membrane at normal temperature and pressure for 3~ 4 times to obtain the ultrafiltration concentrate. The invention has the advantages of less steps, high impurity removal rate, less pectin loss, low temperature operation and the like.
Description
Technical field
The present invention relates to the foodstuff additive manufacture field, particularly a kind of premna microphylla prepares pectin technology.
Background technology
No. 86105966 (notification number CN1011188B) documents of Chinese patent patent, disclosing a kind of is raw material with the bean curd leaf, through acid extraction, take off the method that flavor, separation, removal of impurities, drying, pulverizing process are made pectin.Because this method adopts foodstuffs industry refinery practice commonly used, prepares pectin with the pure precipitator method or salt precipitation method, thereby has following problem.If adopt alcohol precipitation technology, for reducing the ethanol consumption, pectin extracting soln must be concentrated in vacuo to finite concentration, and its defective is: the one, and vacuum Concentrating Process energy consumption height; The 2nd, make pectin degrading because of heated time is long, influence the pectin product quality.If adopt the salt depositing technology to separate pectin, though can save enrichment step,, the desalination difficulty.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of premna microphylla to prepare pectin technology, simple, the easy row of this technology by the isolation technique of practicality, is produced the high quality pectin product of different stage.
The technical solution adopted for the present invention to solve the technical problems is such: be raw material with the premna microphylla, through raw material processing, acid extraction, filtration, decolouring take off flavor, spraying drying is made pectin.Wherein, by cohesion, ion-exchange, ultrafiltration and concentration to the extraction liquid after filtering decolour flavor and desugar, that is: be in the extraction liquid after 1% flocculation agent is inserted filtration with concentration, by adding alkali control pH value, precipitate the removal of impurities decolouring in two steps, the pH value in the two-step precipitation removal of impurities decolorization is respectively 3,4; Extracting solution after the cohesion removal of impurities is handled in ion exchange column by ion exchange resin; Liquid after the resin decolorization through 3～4 times of inner pressed ultra-filtration membrane ultrafiltration and concentration, gets ultrafiltration and concentration liquid at normal temperatures and pressures.
Major advantage of the present invention is:
One. operation is few: need not to separate pectin with salt precipitation method; If separate pectin with the pure precipitator method, can save the vacuum concentration operation.
They are two years old. and adopt two-step precipitation removal of impurities decoloring method, can remove a large amount of impurity and pigment, thereby reach the impurities removing efficiency height, the effect of improving the quality of products.Extracting solution after the removal of impurities, its total impurities removing efficiency can reach 30～40%.
They are three years old. and reusable behind the ion exchange resin regeneration, and the adsorbed pectin of resin can reclaim more than 90% again in the resin regeneration process, and therefore, the pectin loss amount is little, substantial loss about 1.5%.
They are four years old. and adopt ultrafiltration and concentration to concentrate the method that combines, both can reach concentrated effect, can remove desaccharification part and other impurity effectively simultaneously with dilution.
They are five years old. and easy to operate, but cold operation, energy consumption is low.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
As shown in drawings: the present invention be a kind of be raw material with the premna microphylla, after flavor desugar, spraying drying are taken off in raw material processing, acid extraction, filtration, decolouring, make Powdered pectin product; Perhaps, after the flavor desugar is taken off in decolouring, make Powdered pectin product through alcohol precipitation, washing and spraying drying.Take off the flavor desugar and comprise cohesion, ion-exchange, ultrafiltration concentration process.
The present invention to the extraction liquid after filtering decolour flavor and desugar, that is: is in the extraction liquid after 1% flocculation agent is inserted filtration, by adding alkali control pH value, to precipitate removal of impurities in two steps and decolour concentration by cohesion, ion-exchange, ultrafiltration and concentration; Extracting solution after the cohesion removal of impurities is handled in ion exchange column by ion exchange resin; Liquid after the resin decolorization through 3～4 times of inner pressed ultra-filtration membrane ultrafiltration and concentration, gets ultrafiltration and concentration liquid at normal temperatures and pressures.
Embodiment one.
1. raw material is handled: insert after the dried premna microphylla of 20Kg Yichang product is cleaned and boil 3 minutes in the boiling water, and elimination water, extremely colourless with water rinse.
2. acid extraction: add the HCl aqueous solution by solid-to-liquid ratio 1: 20～35 (be preferably 1: 25～30), under pH1.5～2.0,80～95 ℃ of temperature, 40～60 minutes time condition, extract.
3. filter: extraction liquid is filtered, get brown or chocolate liquid.
4. take off the flavor desugar:
Because the extraction liquid after filtering except that pectin is arranged, also contains a large amount of impurity such as protein, organic acid, carbohydrate, Mierocrystalline cellulose, pigment, color and luster is dark and taste heavy, therefore, must decolour to this liquid and take off the flavor desugar.Concrete grammar is as follows:
1) cohesion: earlier the flocculation agent for preparing is inserted in the extraction liquid after the filtration, flocculation agent adopts inorganic salt solution, and its concentration is 1%.Then, by adding alkali control pH value, precipitate the removal of impurities decolouring in two steps, the pH value in the two-step precipitation removal of impurities decolorization is respectively 3,4.
2) ion-exchange: handle the extracting solution of cohesion after the removal of impurities by ion exchange resin in ion exchange column, percent of decolourization is more than 80%, and the pectin loss amount is no more than 10%.The pectin that resin is adsorbed can reclaim in the resin regeneration process, and the rate of recovery is more than 90%.Ion exchange resin can adopt the macroporous resin of models such as D3520, D4020, or weakly acidic resin, and is reusable after the resin regeneration.
3) ultrafiltration and concentration: the liquid after the resin decolorization through 3～4 times of inner pressed ultra-filtration membrane ultrafiltration and concentration, gets ultrafiltration and concentration liquid at normal temperatures and pressures.The inner pressed ultra-filtration membrane can adopt cellulose acetate film, or polysulfone membrane, or polypropylene screen etc.
5. spraying drying: with ultrafiltration and concentration liquid spray-dried Powdered pectin product, yield is 12～13%, 170～180 ° of degree of gelation.
Embodiment two.
With the ultrafiltration and concentration liquid among the embodiment one dilution, behind the reconcentration, spray-dried Powdered pectin product, yield is 10～11%, 200 ° of degree of gelation.
Embodiment three.
Combine with traditional alcohol precipitation technology (not containing vacuum concentration) if flavor desugar technology is taken off in decolouring of the present invention, both can make high-quality pectin product, can overcome traditional alcohol again and precipitate defective in the technology.Example is as follows:
With among the embodiment one after the ultrafiltration and concentration liquid dilution that flavor desugar technology makes is taken off in decolouring, get Powdered pectin product through alcohol precipitation, washing and spraying drying again, yield is 9～10%, 250～280 ° of degree of gelation.Wherein, during the alcohol precipitation, available ethanol or Virahol precipitate, and its concentration is 60～70%; During washing,, be filtered to finite concentration with the liquid scrubbing of alcoholic solution after 2～3 times to precipitate and separate; Then, with spray of negative pressure moisture eliminator drying.
The premna microphylla that the present invention also can adopt other area to produce.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128055 CN1269843C (en) | 2003-05-29 | 2003-05-29 | Process of preparing pectin from Japanese premna leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128055 CN1269843C (en) | 2003-05-29 | 2003-05-29 | Process of preparing pectin from Japanese premna leaf |
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| Publication Number | Publication Date |
|---|---|
| CN1454905A CN1454905A (en) | 2003-11-12 |
| CN1269843C true CN1269843C (en) | 2006-08-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03128055 Expired - Fee Related CN1269843C (en) | 2003-05-29 | 2003-05-29 | Process of preparing pectin from Japanese premna leaf |
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| Country | Link |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365023C (en) * | 2005-12-15 | 2008-01-30 | 西北农林科技大学 | Decolorization of apple pectin and process for producing white fine powder apple pectin |
| CN101906175B (en) * | 2009-06-03 | 2013-06-12 | 浙江省农业科学院 | Method for preparing premna microphylla turez pectin |
| CN103599566B (en) * | 2013-10-21 | 2015-05-20 | 中山大学 | Tissue engineering natural gel stent material and preparation method and application thereof |
| CN104387498B (en) * | 2014-11-05 | 2017-02-15 | 安徽农业大学 | Technical method for simultaneously preparing premna microphylla pectin and premna microphylla sodium copper chlorophyll from premna microphylla |
| CN104592414A (en) * | 2014-12-10 | 2015-05-06 | 保康原生现代农业有限公司 | Method for extraction of pectin from Daphniphyllum macropodum Miq. |
| CN104788403A (en) * | 2015-04-28 | 2015-07-22 | 王燕燕 | Extraction method for compounds in premna microphylla |
| CN105250234B (en) * | 2015-09-10 | 2018-08-07 | 李厚山 | A kind of capsule shells and preparation method thereof |
| CN105622777A (en) * | 2016-01-27 | 2016-06-01 | 巫山县天煜奇叶农业开发有限公司 | Technology for extracting pectin from premna microphylla turca |
| CN105801721A (en) * | 2016-05-24 | 2016-07-27 | 合肥本盛生物科技有限公司 | Method for extracting low-molecular-weight low-ester pectin from Premna microphylla leaf |
| CN105884929A (en) * | 2016-06-13 | 2016-08-24 | 合肥本盛生物科技有限公司 | Method of extracting pectin from premna microphylla leaves |
| CN112876581A (en) * | 2021-02-07 | 2021-06-01 | 西南大学 | Premna microphylla low-ester pectin and preparation method and application thereof |
| CN115005268B (en) * | 2022-06-30 | 2023-05-26 | 安徽农业大学 | A kind of composite antibacterial strawberry fresh-keeping liquid and preparation method thereof |
-
2003
- 2003-05-29 CN CN 03128055 patent/CN1269843C/en not_active Expired - Fee Related
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| CN1454905A (en) | 2003-11-12 |
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Granted publication date: 20060816 Termination date: 20100529 |