CN103981294B - A kind of pea skin that utilizes prepares the technique of l-pectinose for raw material - Google Patents
A kind of pea skin that utilizes prepares the technique of l-pectinose for raw material Download PDFInfo
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- CN103981294B CN103981294B CN201410215271.9A CN201410215271A CN103981294B CN 103981294 B CN103981294 B CN 103981294B CN 201410215271 A CN201410215271 A CN 201410215271A CN 103981294 B CN103981294 B CN 103981294B
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002994 raw material Substances 0.000 title claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 28
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 28
- 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 abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 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
- 238000007670 refining Methods 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 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
- 239000012528 membrane Substances 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 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
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 206010030113 Oedema Diseases 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000010411 cooking Methods 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 210000000952 spleen Anatomy 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000108 ultra-filtration Methods 0.000 abstract description 4
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229920002488 Hemicellulose Polymers 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 150000004676 glycans Chemical class 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
- 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
- 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
- 229960003487 xylose Drugs 0.000 description 2
- 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 1
- 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 description 1
- 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
- 230000007812 deficiency Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 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
- 239000000047 product Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a kind of pea skin that utilizes and prepare the technique of l-pectinose for raw material, comprise raw materials pretreatment, once hydrolysis and extract hemicellulose glycan, secondary hydrolysis extraction l-pectinose, the present invention adopts two-stage acid hydrolysis to extract the technique of l-pectinose, the Arabic liquid glucose of the l-that obtains is without the need to through ultrafiltration membrance filter, only adopt a step decolour-except salt refining-concentration technology, just can obtain highly purified l-pectinose hydrolyzed solution, simple to operate, reduce production cost.And, adopt this technique can significantly improve the quality of product.
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, robust fibre is rich in pea skin, reported in literature is had to learn that it is rich in the research of wood sugar by the pectin in acidolysis pea skin abroad, and utilize pea skin little to the research of producing l-pectinose, and the content of production in the industrial production due to pectinose in raw material of l-pectinose is very low at present, be difficult to direct crystallization, other assorted sugars go out by many employings chromatographic separation mode, just can obtain highly purified crystallized arabinose, found by test, although containing more l-pectinose in pea skin, but adopt a step direct hydrolysis still to can not get enough highly purified Arabic liquid glucose and make its crystallization, middle-chain still needs to carry out removal glucose, crystallization l-pectinose just can be obtained after chromatographic separation.Chinese patent application 201410166232.4(denomination of invention: a kind of with pea skin for raw material prepares l-pectinose and the technique of by-product wood sugar) in refer to a kind of method that l-pectinose is extracted in low acid hydrolysis, after adopting the acid solution hydrolysis of low concentration, by saccharic acid separatory membrane, saccharic acid separation is carried out to hydrolyzed solution, carry out activated carbon decolorizing, then ultrafiltration-desalination-refining is carried out to destainer, ultrafiltration adopts molecular weight cut-off to be the ultra-filtration membrane of 300-10000, isolate other assorted sugar, thus 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 bottleneck that restriction l-pectinose production cost is high.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, provide a kind of pea skin that utilizes and 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 the aqueous solution by solid-to-liquid ratio 1:10-20, boiling 30-60min at 90-100 DEG C, obtains the pea severe edema due to hypofunction of the spleen and boils mixed solution, is filtered by mixed solution, discards water cooking liquid, obtain pea skin filter residue;
(2) be once hydrolyzed: the pea skin filter residue above-mentioned pre-treatment obtained adds acid solution and is once hydrolyzed, wherein: acid solution used is the one 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 DEG C; Hydrolysis time 100-120min;
(3) hydrolyzed solution secondary hydrolysis: an above-mentioned hydrolyzed solution is carried out secondary hydrolysis, wherein: acid solution used is the one in sulfuric acid, phosphoric acid; Its hydrolysising condition is: sour mass concentration 1.5-2.5%; Hydrolysis temperature 110-125 DEG C; Hydrolysis time 100-150min;
Hydrolyzed solution process: the method processed hydrolyzed solution 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; Recovery is carried out to acid solution for subsequent use;
Second step, carries out activated carbon decolorizing by liquid glucose, decolorization condition: add 1-6g gac by 100ml liquid glucose, and temperature is 50-80 DEG C, insulation 20-50min;
3rd step, carry out desalination-refining to destainer, adopt ion exchange resin to cross negative and positive negative and positive negative resin technique except salt refining or adopt the cloudy technique of electrodialysis-negative and positive, wherein negative resin all adopts D301, and positive resin all adopts 001*7; The refined liquid obtained is carried out concentrating, crystallization, obtain l-pectinose.
Saccharic acid separatory membrane of the present invention be a kind of can retaining monose and allow acid group through selectively film, it can retain monosaccharide molecule and allow small molecules acid pass through.
Beneficial effect of the present invention is: adopt two-stage acid hydrolysis to extract the technique of l-pectinose, the Arabic liquid glucose of the l-that obtains is without the need to through ultrafiltration membrance filter, only adopt a step decolour-except salt refining-concentration technology, just can obtain highly purified l-pectinose hydrolyzed solution, simple to operate, reduce production cost.And, adopt this technique can significantly improve the quality of product.
Embodiment
Embodiment 1
1) get 100g pea skin raw material, add purified water 2000g, boiling 60min in 100 DEG C of steam cookers; Pretreatment Mixed Liauid filters, and filtrate is outwelled, and obtains filter residue 92.4g;
2) be once hydrolyzed: in filter residue 92.4g obtained above, add the dilution heat of sulfuric acid that 1000g mass concentration is 0.2%, be hydrolyzed 120min in 120 DEG C of steam cookers, filter, obtain a hydrolyzed solution 960ml, obtain hydrolysis residue 74.0g;
3) secondary hydrolysis: a hydrolyzed solution sulfuric acid is adjusted to acidity 1.5% and carries out secondary hydrolysis, hydrolysising condition: temperature 120 DEG C, time 150min;
The process of secondary hydrolyzed solution: by hydrolyzed solution by saccharic acid separatory membrane, obtain acid solution 608ml, liquid glucose 330ml, acid solution reclaims for subsequent use, and liquid glucose obtains through activated carbon decolorizing-desalination-refining the liquid glucose being rich in l-pectinose;
Decolouring adopts activated carbon decolorizing, adds 5g gac in every 100ml hydrolyzed solution, 75 DEG C 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, refined liquid is concentrated, crystallization obtains the l-pectinose that purity is 98.26%.
Embodiment 2
1) get 100g pea skin raw material, add purified water 1600g, boiling 60min in 90 DEG C of steam cookers; Pretreatment Mixed Liauid filters, and filtrate is outwelled, and obtains filter residue 90.21g;
2) be once hydrolyzed: in filter residue 90.21g obtained above, add the dilution heat of sulfuric acid that 1000g mass concentration is 0.3%, be hydrolyzed 100min in 110 DEG C of steam cookers, filter, obtain a hydrolyzed solution 956ml, obtain a hydrolysis residue 70.28g;
3) secondary hydrolysis: a hydrolyzed solution sulfuric acid is adjusted to acidity 1.8% and carries out secondary hydrolysis, hydrolysising condition: temperature 125 DEG C, time 120min;
The process of secondary hydrolyzed solution: by hydrolyzed solution by saccharic acid separatory membrane, obtain acid solution 610ml, liquid glucose 336ml, acid solution reclaims for subsequent use, and liquid glucose obtains through activated carbon decolorizing-desalination-refining the liquid glucose being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing, adds 5g gac in every 100ml hydrolyzed solution, 75 DEG C of insulation 50min; Desalination adopts ion exchange resin to cross negative and positive technique; Adopted negative and positive anionite-exchange resin technique to except saline solution is refining further, refined liquid was concentrated, crystallization obtained the l-pectinose that purity is 97.88%.
Embodiment 3
1) get 100g pea skin raw material, add purified water 1800g, boiling 30min in 100 DEG C of steam cookers; Pretreatment Mixed Liauid filters, and filtrate is outwelled, and obtains filter residue 91.37g;
2) be once hydrolyzed: in filter residue 91.37g obtained above, add the dilute phosphoric acid solution that 1000g mass concentration is 0.2%, be hydrolyzed 120min in 115 DEG C of steam cookers, filter, obtain a hydrolyzed solution 942ml, obtain a hydrolysis residue 72.10g;
3) secondary hydrolysis: a hydrolyzed solution phosphoric acid is adjusted to acidity 1.8% and carries out secondary hydrolysis, hydrolysising condition: temperature 125 DEG C, time 120min;
The process of secondary hydrolyzed solution: by hydrolyzed solution by saccharic acid separatory membrane, obtain acid solution 598ml, liquid glucose 339ml, acid solution reclaims for subsequent use, and liquid glucose obtains through activated carbon decolorizing-desalination-refining the liquid glucose being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing: add 4g gac in every 100ml hydrolyzed solution, 75 DEG C of insulation 50min, desalination adopted anion-cation exchange resin technique, adopted negative and positive anionite-exchange resin technique to except saline solution is refining further, refined liquid was concentrated, crystallization obtained the l-pectinose that purity is 98.12%.
Embodiment 4
1) get 100g pea skin raw material, add purified water 1000g, boiling 60min in 100 DEG C of steam cookers; Pretreatment Mixed Liauid filters, and filtrate is outwelled, and obtains filter residue 91.80g;
2) be once hydrolyzed: in filter residue 91.80g obtained above, add the dilution heat of sulfuric acid 1100g that mass concentration is 0.1%, be hydrolyzed 150min in 115 DEG C of steam cookers, filter, obtain a hydrolyzed solution 1028ml, obtain a hydrolysis residue 68.00g;
3) secondary hydrolysis: a hydrolyzed solution sulfuric acid is adjusted to acidity 2.5% and carries out secondary hydrolysis, hydrolysising condition: temperature 120 DEG C, time 120min;
The process of hydrolyzed solution: by hydrolyzed solution by saccharic acid separatory membrane, obtain acid solution 626ml, liquid glucose 349ml, acid solution reclaims for subsequent use, and hydrolyzed solution obtains through activated carbon decolorizing-desalination-refining the liquid glucose being rich in l-pectinose:
Decolouring adopts activated carbon decolorizing, adds 5g gac in every 100ml hydrolyzed solution, 75 DEG C of insulation 40min, and desalination adopted anion-cation exchange resin technique; Adopted negative and positive anionite-exchange resin technique to except saline solution is refining further, refined liquid was concentrated, crystallization obtained the l-pectinose that purity is 98.46%.
Claims (1)
1. utilize pea skin to prepare a technique for l-pectinose for raw material, it is characterized in that, mainly comprise the steps:
(1) pre-treatment: pea skin is added the aqueous solution by solid-to-liquid ratio 1:10-20, boiling 30-60min at 90-100 DEG C, obtains the pea severe edema due to hypofunction of the spleen and boils mixed solution, is filtered by mixed solution, discards water cooking liquid, obtain pea skin filter residue;
(2) be once hydrolyzed: the pea skin filter residue above-mentioned pre-treatment obtained adds acid solution and is once hydrolyzed, wherein: acid solution used is the one 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 DEG C; Hydrolysis time 100-120min;
(3) hydrolyzed solution secondary hydrolysis: an above-mentioned hydrolyzed solution is carried out secondary hydrolysis, wherein: acid solution used is the one in sulfuric acid, phosphoric acid; Its hydrolysising condition is: sour mass concentration 1.5-2.5%; Hydrolysis temperature 110-125 DEG C; Hydrolysis time 100-150min;
Secondary hydrolyzed solution process: the method processed secondary hydrolyzed solution is as follows:
The first step, carries out saccharic acid separation by saccharic acid separatory membrane to secondary hydrolyzed solution, obtains part acid solution and liquid glucose; Recovery is carried out to acid solution for subsequent use;
Second step, carries out activated carbon decolorizing by liquid glucose, decolorization condition: add 1-6g gac by 100ml liquid glucose, and temperature is 50-80 DEG C, insulation 20-50min;
3rd step, carry out desalination-refining to destainer, adopt ion exchange resin to cross negative and positive negative and positive negative resin technique except salt refining or adopt the cloudy technique of electrodialysis-negative and positive, wherein negative resin all adopts D301, and positive resin all adopts 001*7; The refined liquid obtained is carried out concentrating, 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 CN103981294A (en) | 2014-08-13 |
| CN103981294B true CN103981294B (en) | 2015-09-30 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 polysaccharide and method for producing 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3834152B2 (en) * | 1998-05-01 | 2006-10-18 | 三和興産株式会社 | Method for producing L-arabinose by acid hydrolysis method |
-
2014
- 2014-05-21 CN CN201410215271.9A patent/CN103981294B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 polysaccharide and method for producing 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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