CN103981294A - Process for preparing pectinose from pea pods used as raw materials - Google Patents
Process for preparing pectinose from pea pods used as raw materials Download PDFInfo
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- CN103981294A CN103981294A CN201410215271.9A CN201410215271A CN103981294A CN 103981294 A CN103981294 A CN 103981294A CN 201410215271 A CN201410215271 A CN 201410215271A CN 103981294 A CN103981294 A CN 103981294A
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- pectinose
- hydrolysis
- hydrolyzed
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- 239000002994 raw material Substances 0.000 title claims abstract description 13
- SRBFZHDQGSBBOR-QMKXCQHVSA-N alpha-L-arabinopyranose Chemical compound O[C@H]1CO[C@@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-QMKXCQHVSA-N 0.000 title abstract description 7
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 34
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000007670 refining Methods 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 53
- 239000002253 acid Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- NAOLWIGVYRIGTP-UHFFFAOYSA-N 1,3,5-trihydroxyanthracene-9,10-dione Chemical compound C1=CC(O)=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1 NAOLWIGVYRIGTP-UHFFFAOYSA-N 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000002203 pretreatment Methods 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 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 description 5
- 239000003456 ion exchange resin Substances 0.000 claims description 5
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- 206010030113 Oedema Diseases 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000010411 cooking Methods 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 210000000952 spleen Anatomy 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 abstract description 4
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 2
- 229920002488 Hemicellulose Polymers 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 239000000413 hydrolysate Substances 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000010612 desalination reaction Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 235000014666 liquid concentrate Nutrition 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 235000000346 sugar Nutrition 0.000 description 3
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 238000013375 chromatographic separation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000001727 glucose Nutrition 0.000 description 2
- 229960003487 xylose Drugs 0.000 description 2
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000008504 concentrate Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000002304 glucoses Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a process for preparing pectinose from pea pods used as raw materials. The process comprises the following steps: preprocessing the raw materials, performing primary hydrolysis to extract hemicellulose, and performing secondary hydrolysis to extract pectinose. According to the process, a pectinose liquid obtained by adopting the process of extracting pectinose by virtue of two-step acid hydrolysis does not need to be filtered by virtue of an ultrafiltration membrane, a high-purity pectinose hydrolysate can be obtained by adopting a process of decolorizing in one step, desalting, refining and concentrating only, the operation is simple, and the production cost is reduced; in addition, the product quality can be remarkably improved by adopting the process.
Description
Technical field
The invention belongs to functional sugar preparing technical field, relate to a kind of pea skin that utilizes and prepare the technique of l-pectinose for raw material.
Background technology
Pea belongs to leguminous plants, in pea skin, be rich in robust fibre, there is reported in literature to learn that by the pectin in acidolysis pea skin it is rich in the research of wood sugar abroad, and utilize research that pea skin produces l-pectinose seldom, and production content due to pectinose in raw material in industrial production of l-pectinose is very low at present, be difficult to direct crystallization, the chromatographic separation modes that adopt go out other assorted sugars more, just can obtain highly purified crystallized arabinose, by test, find, although contain more l-pectinose in pea skin, but adopt a step direct hydrolysis still to can not get enough highly purified Arabic liquid glucoses and make its crystallization, middle-chain still needs to remove glucose, after chromatographic separation, just can obtain crystallization l-pectinose.Chinese patent application 201410166232.4(denomination of invention: a kind ofly take pea skin and prepare the technique of l-pectinose by-product wood sugar as raw material) in, mentioned a kind of method that l-pectinose is extracted in low acid hydrolysis, adopt after the acid solution hydrolysis of low concentration, by saccharic acid separatory membrane, hydrolyzed solution is carried out to saccharic acid separation, carry out activated carbon decolorizing, then destainer is carried out to ultrafiltration-desalination-refining, ultrafiltration adopts the ultra-filtration membrane that molecular weight cut-off is 300-10000, isolate other assorted sugar, thereby improve the purity of l-pectinose, just can obtain crystallization l-pectinose, and membrane sepn cost is high, separation efficiency is low, so these two kinds of processing sequencees are all more complicated, operation easier is high, become the high bottleneck of restriction l-pectinose production cost.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, provide a kind of pea skin that utilizes to prepare the technique of l-pectinose for raw material.
According to the present invention, described technique mainly comprises the steps:
(1) pre-treatment: pea skin is added to the aqueous solution by solid-to-liquid ratio 1:10-20, and boiling 30-60min at 90-100 ℃, obtains the pea severe edema due to hypofunction of the spleen and boil mixed solution, filters mixed solution, discards water cooking liquid, obtains pea skin filter residue;
(2) once hydrolysis: the pea skin filter residue that above-mentioned pre-treatment is obtained adds acid solution to be once hydrolyzed, wherein: acid solution used is a kind of in sulfuric acid, phosphoric acid; Its hydrolysising condition is: solid-to-liquid ratio 1:8-20; Acid mass concentration 0.1-0.3%; Hydrolysis temperature 110-120 ℃; Hydrolysis time 100-120min;
(3) hydrolyzed solution secondaries hydrolysis: an above-mentioned hydrolyzed solution is carried out to secondary hydrolysis, wherein: acid solution used is a kind of in sulfuric acid, phosphoric acid; Its hydrolysising condition is: sour mass concentration 1.5-2.5%; Hydrolysis temperature 110-125 ℃; Hydrolysis time 100-150min;
Hydrolyzed solution is processed: the method that hydrolyzed solution is processed is as follows:
The first step, carries out saccharic acid separation by saccharic acid separatory membrane to hydrolyzed solution, obtains part acid solution and liquid glucose; Acid solution is reclaimed standby;
Second step, carries out activated carbon decolorizing by liquid glucose, decolorization condition: by 100ml liquid glucose, add 1-6g gac, temperature is 50-80 ℃, insulation 20-50min;
The 3rd step, carries out desalination-refining to destainer, and except salt refining adopts ion exchange resin to cross negative and positive negative and positive negative resin technique or adopts the cloudy technique of electrodialysis-negative and positive, wherein negative resin all adopts D301, and positive resin all adopts 001*7; The refined liquid obtaining concentrate, crystallization, obtain l-pectinose.
Saccharic acid separatory membrane of the present invention is a kind ofly to monose, can hold back and the selectively film that allows acid group to see through, and it can be held back monose molecule and allow small molecules acid pass through.
Beneficial effect of the present invention is: adopt two step acid hydrolysiss to extract the technique of l-pectinose, the Arabic liquid glucose of l-obtaining is without process ultrafiltration membrance filter, only adopt the step salt refining-concentration technology that decolours-remove, just can obtain highly purified l-pectinose hydrolyzed solution, simple to operate, reduced production cost.And, adopt this technique can obviously improve the quality of product.
Embodiment
Embodiment 1
1) get 100g pea skin raw material, add purified water 2000g, boiling 60min in 100 ℃ of steam cookers; Pre-treatment mixed solution filters, and filtrate is outwelled, and obtains filter residue 92.4g;
2) once hydrolysis: adding 1000g mass concentration in filter residue 92.4g obtained above is 0.2% dilution heat of sulfuric acid, the 120min that is hydrolyzed in 120 ℃ of steam cookers filters, and obtains hydrolyzed solution 960ml one time, obtains hydrolysis residue 74.0g;
3) secondary hydrolysis a: hydrolyzed solution is adjusted to acidity 1.5% with sulfuric acid and carries out secondary hydrolysis, hydrolysising condition: 120 ℃ of temperature, time 150min;
The processing of secondary hydrolyzed solution: hydrolyzed solution, by saccharic acid separatory membrane, is obtained to acid solution 608ml, liquid glucose 330ml, acid solution reclaims standby, and liquid glucose is through activated carbon decolorizing-desalination-refining liquid glucose that obtains being rich in l-pectinose;
Decolouring adopts activated carbon decolorizing, in every 100ml hydrolyzed solution, adds 5g gac, 75 ℃ of insulation 40min; Desalination adopts ion exchange resin to cross negative and positive technique; To except saline solution further the refining ion exchange resin that adopts cross the cloudy technique of negative and positive, to refined liquid concentrate, to obtain purity be 98.26% l-pectinose in crystallization.
Embodiment 2
1) get 100g pea skin raw material, add purified water 1600g, boiling 60min in 90 ℃ of steam cookers; Pre-treatment mixed solution filters, and filtrate is outwelled, and obtains filter residue 90.21g;
2) once hydrolysis: adding 1000g mass concentration in filter residue 90.21g obtained above is 0.3% dilution heat of sulfuric acid, the 100min that is hydrolyzed in 110 ℃ of steam cookers filters, and obtains hydrolyzed solution 956ml one time, obtains hydrolysis residue 70.28g one time;
3) secondary hydrolysis a: hydrolyzed solution is adjusted to acidity 1.8% with sulfuric acid and carries out secondary hydrolysis, hydrolysising condition: 125 ℃ of temperature, time 120min;
The processing of secondary hydrolyzed solution: hydrolyzed solution by saccharic acid separatory membrane, is obtained to acid solution 610ml, liquid glucose 336ml, acid solution reclaims standby, and liquid glucose is through activated carbon decolorizing-desalination-refining liquid glucose that obtains being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing, in every 100ml hydrolyzed solution, adds 5g gac, 75 ℃ of insulation 50min; Desalination adopts ion exchange resin to cross negative and positive technique; To except the further refining negative and positive anionite-exchange resin technique that adopted of saline solution, to refined liquid concentrate, to obtain purity be 97.88% l-pectinose in crystallization.
Embodiment 3
1) get 100g pea skin raw material, add purified water 1800g, boiling 30min in 100 ℃ of steam cookers; Pre-treatment mixed solution filters, and filtrate is outwelled, and obtains filter residue 91.37g;
2) once hydrolysis: adding 1000g mass concentration in filter residue 91.37g obtained above is 0.2% dilute phosphoric acid solution, the 120min that is hydrolyzed in 115 ℃ of steam cookers filters, and obtains hydrolyzed solution 942ml one time, obtains hydrolysis residue 72.10g one time;
3) secondary hydrolysis a: hydrolyzed solution is adjusted to acidity 1.8% with phosphoric acid and carries out secondary hydrolysis, hydrolysising condition: 125 ℃ of temperature, time 120min;
The processing of secondary hydrolyzed solution: hydrolyzed solution by saccharic acid separatory membrane, is obtained to acid solution 598ml, liquid glucose 339ml, acid solution reclaims standby, and liquid glucose is through activated carbon decolorizing-desalination-refining liquid glucose that obtains being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing: in every 100ml hydrolyzed solution, add 4g gac, 75 ℃ of insulation 50min, desalination adopted anion-cation exchange resin technique, to except the further refining negative and positive anionite-exchange resin technique that adopted of saline solution, to refined liquid concentrate, to obtain purity be 98.12% l-pectinose in crystallization.
Embodiment 4
1) get 100g pea skin raw material, add purified water 1000g, boiling 60min in 100 ℃ of steam cookers; Pre-treatment mixed solution filters, and filtrate is outwelled, and obtains filter residue 91.80g;
2) once hydrolysis: adding mass concentration in filter residue 91.80g obtained above is 0.1% dilution heat of sulfuric acid 1100g, the 150min that is hydrolyzed in 115 ℃ of steam cookers filters, and obtains hydrolyzed solution 1028ml one time, obtains hydrolysis residue 68.00g one time;
3) secondary hydrolysis a: hydrolyzed solution is adjusted to acidity 2.5% with sulfuric acid and carries out secondary hydrolysis, hydrolysising condition: 120 ℃ of temperature, time 120min;
The processing of hydrolyzed solution: hydrolyzed solution by saccharic acid separatory membrane, is obtained to acid solution 626ml, liquid glucose 349ml, acid solution reclaims standby, and hydrolyzed solution is through activated carbon decolorizing-desalination-refining liquid glucose that obtains being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing, in every 100ml hydrolyzed solution, adds 5g gac, 75 ℃ of insulation 40min, and desalination adopted anion-cation exchange resin technique; To except the further refining negative and positive anionite-exchange resin technique that adopted of saline solution, to refined liquid concentrate, to obtain purity be 98.46% l-pectinose in crystallization.
Claims (1)
1. utilize pea skin to prepare the technique of l-pectinose for raw material, it is characterized in that, mainly comprise the steps:
(1) pre-treatment: pea skin is added to the aqueous solution by solid-to-liquid ratio 1:10-20, and boiling 30-60min at 90-100 ℃, obtains the pea severe edema due to hypofunction of the spleen and boil mixed solution, filters mixed solution, discards water cooking liquid, obtains pea skin filter residue;
(2) once hydrolysis: the pea skin filter residue that above-mentioned pre-treatment is obtained adds acid solution to be once hydrolyzed, wherein: acid solution used is a kind of in sulfuric acid, phosphoric acid; Its hydrolysising condition is: solid-to-liquid ratio 1:8-20; Acid mass concentration 0.1-0.3%; Hydrolysis temperature 110-120 ℃; Hydrolysis time 100-120min;
(3) hydrolyzed solution secondaries hydrolysis: an above-mentioned hydrolyzed solution is carried out to secondary hydrolysis, wherein: acid solution used is a kind of in sulfuric acid, phosphoric acid; Its hydrolysising condition is: sour mass concentration 1.5-2.5%; Hydrolysis temperature 110-125 ℃; Hydrolysis time 100-150min;
Hydrolyzed solution is processed: the method that hydrolyzed solution is processed is as follows:
The first step, carries out saccharic acid separation by saccharic acid separatory membrane to hydrolyzed solution, obtains part acid solution and liquid glucose; Acid solution is reclaimed standby;
Second step, carries out activated carbon decolorizing by liquid glucose, decolorization condition: by 100ml liquid glucose, add 1-6g gac, temperature is 50-80 ℃, insulation 20-50min;
The 3rd step, carries out desalination-refining to destainer, and except salt refining adopts ion exchange resin to cross negative and positive negative and positive negative resin technique or adopts the cloudy technique of electrodialysis-negative and positive, wherein negative resin all adopts D301, and positive resin all adopts 001*7; The refined liquid obtaining concentrate, crystallization, obtain l-pectinose.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410215271.9A CN103981294B (en) | 2014-05-21 | 2014-05-21 | A kind of pea skin that utilizes prepares the technique of l-pectinose for raw material |
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| CN201410215271.9A CN103981294B (en) | 2014-05-21 | 2014-05-21 | A kind of pea skin that utilizes prepares the technique of l-pectinose for raw material |
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| CN103981294A true CN103981294A (en) | 2014-08-13 |
| CN103981294B CN103981294B (en) | 2015-09-30 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11313700A (en) * | 1998-05-01 | 1999-11-16 | Sanwa Kosan Kk | Production of l-arabinose by acid hydrolysis |
| EP1002782A2 (en) * | 1998-11-18 | 2000-05-24 | Xyrofin Oy | Method of producing polyols from arabinoxylan-containing material |
| JP2009207462A (en) * | 2008-03-06 | 2009-09-17 | Unitika Ltd | Method for producing sugar for synthetic raw material |
| CN101643795A (en) * | 2009-08-28 | 2010-02-10 | 长宁县泰宁化工有限公司 | Method for preparing xylose and xylitol by using bamboo |
| CN102660606A (en) * | 2012-05-04 | 2012-09-12 | 山东龙力生物科技股份有限公司 | Bio-preparation method for production of high-purity xylo-oligosaccharide and coproduction of arabinose and xylose |
| CN103468761A (en) * | 2013-09-25 | 2013-12-25 | 重庆工商大学 | Method for preparing L-arabinose by using rape cake |
| CN103608360A (en) * | 2011-06-24 | 2014-02-26 | 不二制油株式会社 | Pectic polysaccharides and process for producing the same |
| CN103667365A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for preparing dihydric alcohol from crop straw |
-
2014
- 2014-05-21 CN CN201410215271.9A patent/CN103981294B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11313700A (en) * | 1998-05-01 | 1999-11-16 | Sanwa Kosan Kk | Production of l-arabinose by acid hydrolysis |
| EP1002782A2 (en) * | 1998-11-18 | 2000-05-24 | Xyrofin Oy | Method of producing polyols from arabinoxylan-containing material |
| JP2009207462A (en) * | 2008-03-06 | 2009-09-17 | Unitika Ltd | Method for producing sugar for synthetic raw material |
| CN101643795A (en) * | 2009-08-28 | 2010-02-10 | 长宁县泰宁化工有限公司 | Method for preparing xylose and xylitol by using bamboo |
| CN103608360A (en) * | 2011-06-24 | 2014-02-26 | 不二制油株式会社 | Pectic polysaccharides and process for producing the same |
| CN102660606A (en) * | 2012-05-04 | 2012-09-12 | 山东龙力生物科技股份有限公司 | Bio-preparation method for production of high-purity xylo-oligosaccharide and coproduction of arabinose and xylose |
| CN103667365A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for preparing dihydric alcohol from crop straw |
| CN103468761A (en) * | 2013-09-25 | 2013-12-25 | 重庆工商大学 | Method for preparing L-arabinose by using rape cake |
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