CN106519066A - Method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues) - Google Patents
Method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues) Download PDFInfo
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- CN106519066A CN106519066A CN201610851996.6A CN201610851996A CN106519066A CN 106519066 A CN106519066 A CN 106519066A CN 201610851996 A CN201610851996 A CN 201610851996A CN 106519066 A CN106519066 A CN 106519066A
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- filter residue
- filtrate
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- ethanol
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- 239000001814 pectin Substances 0.000 title claims abstract description 64
- 229920001277 pectin Polymers 0.000 title claims abstract description 64
- 235000010987 pectin Nutrition 0.000 title claims abstract description 64
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 44
- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 229920005610 lignin Polymers 0.000 claims abstract description 45
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 102000004190 Enzymes Human genes 0.000 claims abstract description 24
- 108090000790 Enzymes Proteins 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 142
- 239000000706 filtrate Substances 0.000 claims description 100
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 62
- 239000007788 liquid Substances 0.000 claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 43
- 239000007787 solid Substances 0.000 claims description 32
- 108091005804 Peptidases Proteins 0.000 claims description 29
- 239000004365 Protease Substances 0.000 claims description 29
- 230000000694 effects Effects 0.000 claims description 29
- 235000019419 proteases Nutrition 0.000 claims description 29
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 24
- 229940088598 enzyme Drugs 0.000 claims description 23
- 239000012043 crude product Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 241000194108 Bacillus licheniformis Species 0.000 claims description 21
- 238000001556 precipitation Methods 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 17
- 239000002893 slag Substances 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 16
- 235000015097 nutrients Nutrition 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 13
- 102000004139 alpha-Amylases Human genes 0.000 claims description 13
- 108090000637 alpha-Amylases Proteins 0.000 claims description 13
- 229940024171 alpha-amylase Drugs 0.000 claims description 13
- 238000005267 amalgamation Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 13
- 238000009835 boiling Methods 0.000 claims description 11
- 108010067770 Endopeptidase K Proteins 0.000 claims description 10
- 108010059378 Endopeptidases Proteins 0.000 claims description 10
- 102000005593 Endopeptidases Human genes 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000004061 bleaching Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 6
- 241000894006 Bacteria Species 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 230000003321 amplification Effects 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 230000000937 inactivator Effects 0.000 claims description 5
- 239000006210 lotion Substances 0.000 claims description 5
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 230000028327 secretion Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims 6
- 238000001816 cooling Methods 0.000 claims 1
- 239000001913 cellulose Substances 0.000 abstract description 18
- 229920002678 cellulose Polymers 0.000 abstract description 18
- 235000005911 diet Nutrition 0.000 abstract description 3
- 230000000378 dietary effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 102000035195 Peptidases Human genes 0.000 description 23
- 239000003337 fertilizer Substances 0.000 description 13
- 229920002472 Starch Polymers 0.000 description 10
- 239000008107 starch Substances 0.000 description 10
- 235000019698 starch Nutrition 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 102000004169 proteins and genes Human genes 0.000 description 7
- 108090000623 proteins and genes Proteins 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000008635 plant growth Effects 0.000 description 6
- 150000003384 small molecules Chemical class 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 241000193830 Bacillus <bacterium> Species 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 3
- 108010059892 Cellulase Proteins 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 3
- 210000000170 cell membrane Anatomy 0.000 description 3
- 229940106157 cellulase Drugs 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000008030 elimination Effects 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 230000002779 inactivation Effects 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000010297 mechanical methods and process Methods 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000021049 nutrient content Nutrition 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 102000004196 processed proteins & peptides Human genes 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 235000015203 fruit juice Nutrition 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000013138 pruning Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Sustainable Development (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues), belonging to the technical field of biology. According to the invention, in accordance with biomass comprehensive utilization principles of multistage separation and multilevel utilization, main components like dietary cellulose, pectin, hemicellulose and lignin are successfully separated and refined from the fruit branches, the fruit peels and the fruit residues; meanwhile, obtained dietary cellulose, pectin, hemicellulose and lignin have high extraction rate, good integrity and high quality; and a foundation is laid for high-value-added development and utilization of the fruit branches, the fruit peels and the fruit residues. The method provided by the invention utilizes a steam explosion separation technology in the prior art, adopts conditions of low temperature and high pressure (provided by inert gas), and applies a special biological enzyme, thereby guaranteeing high efficiency, high quality and high benefits in utilization of the fruit branches, the fruit peels and the fruit residues.
Description
Technical field
The present invention relates to biological technical field, more particularly to a kind of to utilize fruit tree branch, pericarp（Slag）Production dietary fiber is simultaneously
The method of coproduction pectin.
Background technology
With the development of China's forestry, planting fruit trees area is increasing.According to statistics, nearly 20,000 hectares of cultivated area, fruit
Nearly 200,000,000 tons of product total output；Thus corresponding fruit deep processing industry, such as fruit juice etc., also develop.Pruning fruit tree gets off
Brush wood, all pile up by orchard every year, it is impossible to utilize；Fruit juice factory fruit squeeze the juice after remaining pomace, pericarp etc., by random
Process as feed or fertilizer.Therefore, we only focus on the wastes and pollution of crop material every year, in fact, fruit branch, pericarp,
The waste of pomace etc., pollution are equally very serious.
Containing high added value compositions such as abundant fiber, pectin in fruit branch, pericarp, pomace, these compositions are separated, is refined
Out, great economic worth not only can be created, also environmental pollution and the wasting of resources can be avoided simultaneously.
The content of the invention
In order to make up the deficiencies in the prior art, the invention provides a kind of utilize fruit tree branch, pericarp（Slag）Production meals are fine
The method of dimension co-production pectin.
The technical scheme is that：
It is a kind of to utilize fruit tree branch, pericarp（Slag）The method of production dietary fiber co-production pectin, including step：
The preparation of A hemicelluloses
A1）Digester is dried and moved into after crushing to fruit tree branch, pericarp or pomace, adds fruit tree branch, pericarp or pomace quality 1-20
Times water, add alkali to concentration of lye to be 1%-10%, logical steam stops logical steam after being warming up to 60-100 DEG C, is passed through indifferent gas
Body, will seal after air emptying in digester；Then intermittence is passed through steam and inert gas in digester, to maintain to steam
Boil kettle temperature for 60-100 DEG C, pressure be 0.5-1MPa, heat-insulation pressure keeping spurted after 10-120 minutes；
A2）By step 1）Gained spurts during slurry is transferred to grinding mill and grinds；
A3）Separation of solid and liquid, obtains filter residue one and filtrate one；
A4）The ethanol of one 1-10 times of volume of filtrate is added in filtrate one, after stirring, is stood complete to precipitation；
A5）Precipitation and separation and supernatant, obtain filter residue two and filtrate two；
A6）Filter residue two is dissolved using sig water, is subsequently adding the ethanol of 1-10 times of volume of sig water, it is to be precipitated completely after, separate
Precipitation and supernatant, repeat operation 1-5 time, obtain filter residue three and filtrate three；
A7）Three drying of filter residue, crushing obtain final product hemicellulose finished product.
The preparation of B lignin
B1）Filter residue one is placed in into digester, the water of one 1-20 times of quality of filter residue is added, is passed through inert gas, filter residue is uniformly divided
Cloth is in water；Compound protease is subsequently adding, interval 1-3 minute, inert gas is passed through, is digested 10-80 minutes；Often it is subsequently added
Warm type AMS, digests 10-80 minutes；Then pass to steam and be warming up to 60-70 DEG C, be incubated the work of 2-20 minute inactivators
Property；The compound protease is made up of the alkali protease for possessing endopeptidase activity and the Proteinase K for possessing peptide ending enzyme activity；Institute
Normal temperature type AMS is stated by microwave induced gained variation bacillus licheniformis secretion gained AMS, the normal temperature type α-shallow lake
The preference temperature of powder enzyme is 22-35 DEG C；
B2）Go out after enzyme, the mass fraction for adding ethanol to ethanol in digester is 30%-80%, is then intermittently passed through water
Steam and inert gas, are 80-120 DEG C, pressure for 0.5-2 MPa to maintain boiling kettle temperature, heat-insulation pressure keeping 60-120 point
Spurt after clock；
B3）Step B2）Gained spurts slurry separation of solid and liquid, obtains filter residue four and filtrate four；Ethanol of the filter residue four using 40%-90%
Washing, ethanol washing lotion are merged with filtrate four, obtain amalgamation liquid one；
B4）Amalgamation liquid one is concentrated by evaporation, and obtains lignin crude product；After lignin crude product is washed with water, Jing is dried, crushes to obtain lignin
Finished product.
The preparation of C dietary fibers
C1）Filter residue four is placed in into extractor, the water of four 3-30 times of filter residue is added, diluted acid after stirring evenly, is added, and pH is adjusted to 1-5, is led to
Enter water vapour, temperature stops water flowing steam after rising to 30-100 DEG C, is then passed through inert gas, sealed in emptying tank after air；
Water vapour and inert gas is intermittently passed through, and temperature is maintained in tank as 30-100 DEG C, and material is uniformly distributed in tank,
Insulation extracting 30-300 minutes；
C2）After extracting is finished, the material in extractor is carried out into separation of solid and liquid, filter residue five and filtrate five is obtained；
C3）The water of five 1-10 times of filter residue during filter residue five adds bleaching tank, is added, the concentration of hydrogen peroxide to hydrogen peroxide after stirring evenly, is added
For 1%-5%, 50-80 DEG C is warming up to, is incubated 10-120 minutes；
C4）Separation of solid and liquid, and wash filter residue with water, obtain filter residue six and filtrate six；
C5）Filter residue the six channels is dried, crushes to obtain dietary fiber finished product.
The preparation of D pectin
D1）The filtrate Five Classics decolourizes, filters filtrate five of must decolourizing；
D2）To in decolouring filtrate five, the mass fraction of the hydrochloric ethanol to ethanol of five 1-10 times of volumes of addition decolouring filtrate is
30%-80%, after stirring, stands 20-100 minutes, and separation of solid and liquid obtains filter residue seven and filtrate seven；
D3）Filter residue seven, repeat step D1 is dissolved with diluted acid）And D2）, last gained solid pectin as after purification；
D4）Step D3）Gained pectin drying after purification, crushing obtain final product pectin finished product.
Preferably, step A1, A6）In, the alkali is potassium hydroxide, NaOH, ammoniacal liquor or calcium hydroxide.
Preferably, step B1）In, the obtaining step of the microwave induced gained variation bacillus licheniformis is concrete
For：The nutrient solution of bacillus licheniformis is placed in into microwave generator, setting microwave power is 850-950W, pulse frequency is
2300MHz, microwave treatment 20s cool down 20s, reciprocal 25-35 time according to this；Nutrient solution after microwave treatment is coated on into solid training
On foster base, cultivate 1-2 days under the conditions of 30 DEG C, by the high ground of alpha-amylase activity under four plants of normal temperature of screening in the bacterium colony for surviving
The dissociant of clothing bacillus.
Further, the dissociant Amplification Culture of alpha-amylase activity highest bacillus licheniformis under normal temperature is selected,
So as to obtain the normal temperature type AMS.The normal temperature type AMS obtained using the method, at normal temperatures can efficient enzyme
Solution starch, had both reduced energy consumption, turn avoid the generation of side reaction.
Preferably, possess the alkali protease of endopeptidase activity in the compound protease and possess peptide ending enzyme work
Property Proteinase K ratio be 1:1-3；The addition of the compound protease meets every kilogram of one 400-800U of butt filter residue,
The addition of the normal temperature type AMS meets every kilogram of one 300-700U of butt filter residue.
Preferably, step C1）And D3）In, the acid is sulfuric acid, nitric acid, hydrochloric acid, sulfurous acid, in acetic acid one
Kind.
Preferably, the inert gas is nitrogen, helium or argon gas.
Preferably, step A7）、B4）、C5）、D4）Described in be dried as spray drying, heated-air drying, fluid bed
It is dried or freeze-drying；Baking temperature is less than 120 DEG C.
Preferably, step D2）In hydrochloric ethanol, the volume fraction of ethanol is 95%, and the concentration of hydrochloric acid is
0.5mol/L。
In addition, merging some filtrates and waste water, pH and nutrient content is adjusted, the liquid of plant growth needs can be prepared
Fertilizer, makes full use of filtrate and waste water, reduces discharge.
Beneficial effects of the present invention are：
The present invention adheres to the principle that the biomass comprehensive of " multi-layer is separated, utilized at many levels " is utilized, by fruit branch, pericarp, pomace
In Main Components dietary cellulosic, pectin, hemicellulose, lignin etc. be successfully separated, refine out, and meals for being obtained
Cellulose, pectin, hemicellulose, lignin extraction rate are high, integrality is good, quality is high；Height for fruit branch, pericarp, pomace is added
Value exploitation are laid a good foundation.
Although the present invention also utilizes steam explosion isolation technics of the prior art, employ in present invention process low
Temperature, high pressure（Inert gas is provided）Condition, and apply special biology enzyme, it is ensured that the present invention is to fruit branch, pericarp and pomace
The high efficiency that utilizes, high-quality, high yield.
Specific embodiment
Embodiment 1
It is a kind of to utilize fruit tree branch, pericarp（Slag）The method of production dietary fiber co-production pectin, including step：
The preparation of A hemicelluloses
A1）Apple branch impurity elimination, section, drying（Inactivation pectase, cellulase, zytase）And boiling is added after crushing
Pot, adds the water of 10 times of apple branch quality, adds ammoniacal liquor to concentration of lye to be 4%, and logical steam stops logical steaming after being warming up to 90 DEG C
Vapour, is passed through nitrogen, will seal after air emptying in digester；Then intermittence is passed through steam and nitrogen in digester, with
Boiling kettle temperature is maintained to be 93 DEG C, pressure is 0.8MPa, heat-insulation pressure keeping was spurted after 70 minutes.
The step extracts hemicellulose with diluted alkaline；Using relatively low boiling temperature（93℃）, higher pot inner pressure（0.8MPa）
And inert gas environment, it is therefore intended that ensure that the components such as hemicellulose, cellulose, lignin, pectin avoid high temperature, aerobic bar
Decomposition, oxidation, peeling, esterification under part etc. are reacted, and the integrality and product quality effect to ensureing molecular radical is obvious；Compared with
High pressure（0.8MPa）Ensure that alkali lye the effective infiltration between apple branch cell membrane and the dissolution of macromolecular.
A2）By step 1）Gained spurts during slurry is transferred to mill and grinds 20 minutes.With Mechanical Method crack macromolecular it
Between part be connected chemically key, further increase the yield of each material.
A3）Separation of solid and liquid, obtains filter residue one and filtrate one.Filter residue one is containing compositions such as cellulose, lignin, pectin
Slurry；First filtrate be thick liquid of hemicellulose.
A4）The 95% of one 4 times of volumes of filtrate ethanol is added in filtrate one, after stirring, is stood complete to precipitation.
A5）Precipitation and separation and supernatant, obtain filter residue two and filtrate two.
A6）Filter residue two is dissolved using weak aqua ammonia, is subsequently adding the 95% of 5 times of volumes of weak aqua ammonia ethanol, to be precipitated complete
Afterwards, precipitation and separation and supernatant, repeat operation 3 times, and sleeping spiral shell centrifugation obtains filter residue three and filtrate three.
Step A4）、A5）、A6）For the purification step of hemicellulose.Step A4）Filter residue two obtained by alcohol precipitation is mainly half fiber
Plain crude product, the water phase being mainly in filtrate two in ethanol and filtrate one, the ethanol whole recycling in filtrate two；Step
A6）Purified, alcohol precipitation again after gained hemicellulose crude product is dissolved again, should used in the process of ethanol also all reclaim
Recycle.
A7）Filter residue three is spray-dried（115 DEG C of outlet temperature）, crush obtain final product hemicellulose finished product.After testing, this enforcement
The quality of hemicellulose obtained by apple branch for butt apple branch quality 18.4% in example, purity is 96.7%.
The preparation of B lignin
B1）Filter residue one is placed in into digester, the water of one 10 times of quality of filter residue is added, is passed through nitrogen, makes filter residue be evenly distributed on water
In；It is subsequently adding compound protease（500U/Kg butts filter residue one）, intermittently 1 minute, nitrogen is passed through, is digested 40 minutes；Subsequently add
Enter normal temperature type AMS（400U/Kg butts filter residue one）, digest 30 minutes；Then pass to steam and be warming up to 65 DEG C, insulation 10
The activity of minute inactivator.
Wherein, compound protease is by the alkali protease for possessing endopeptidase activity and possesses the active Proteinase K of peptide ending enzyme
Composition, the alkali protease for possessing endopeptidase activity in compound protease and the ratio for possessing the active Proteinase K of peptide ending enzyme are
1:1；The compound protease can effectively hydrolyzing protein at normal temperatures.
Normal temperature type AMS is by microwave induced gained variation bacillus licheniformis secretion gained AMS；It is microwave induced
The obtaining step of gained variation bacillus licheniformis is specially：The nutrient solution of bacillus licheniformis is placed in into microwave generator, if
Microwave power is put for 900W, pulse frequency is 2300MHz, microwave treatment 20s, cool down 20s, reciprocal 30 times according to this；At microwave
Nutrient solution after reason is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, screens four plants by the bacterium colony for surviving
The dissociant of the high bacillus licheniformis of alpha-amylase activity under normal temperature.Select alpha-amylase activity highest lichens under normal temperature
The dissociant Amplification Culture of bacillus, so that obtain normal temperature type AMS；Normal temperature type AMS is in 22-35 DEG C of temperature
Under expeditiously hydrolysis starch, it is not necessary to as the thermal-stable α-amylase for adopting mostly at present needs high temperature（80-90℃）Condition, because
And reduce energy consumption and also reduce the requirement to equipment, while greatly reduce the generation of side reaction；Herein can be with soft with enzyme process
Protein, Starch Hydrolysis are entered in filtrate, so as to success into the peptides of small molecule, amino acid, maltose, glucose etc. with ground
Deproteination matter and starch；To ensure the purity of lignin.
B2）Go out after enzyme, the mass fraction for adding 95% ethanol to ethanol in digester is 60%, is then intermittently led to
Enter water vapour and nitrogen, boiling kettle temperature is maintained as 110 DEG C, pressure is 1.5MPa, and heat-insulation pressure keeping was spurted after 100 minutes.
Vapours containing ethanol all enters ethanol recovery system by cover mouth.
B3）Step B2）Gained spurts slurry separation of solid and liquid, obtains filter residue four and filtrate four；Filter residue four adopts 60% ethanol
Washing, ethanol washing lotion are merged with filtrate four, obtain amalgamation liquid one.
Filter residue four is the slurry containing cellulose and pectin, and filtrate four is the molten lignin of alcohol.
B4）Amalgamation liquid one is concentrated by evaporation, and obtains lignin crude product；After lignin crude product is washed with water, Jing is spray-dried（Outlet
105 DEG C of temperature）, crush to obtain lignin finished product.After testing, in the present embodiment, the quality of lignin obtained by apple branch is butt apple
The 28.6% of branch quality, purity is 96.3%.
The preparation of C dietary fibers
C1）Filter residue four is placed in into extractor, the water of 4 20 times of filter residue is added, dilute sulfurous acid after stirring evenly, is added, and pH is adjusted to 1.5,
Water vapour is passed through, temperature stops water flowing steam after rising to 90 DEG C, is then passed through nitrogen, sealed in emptying tank after air；It is intermittent
Be passed through water vapour and nitrogen, to maintain in tank temperature as 90 DEG C, and material is uniformly distributed in tank, 100 points of insulation extracting
Clock.
C2）After extracting is finished, the material in extractor is carried out into sleeping spiral shell centrifugation, filter residue five and filtrate five is obtained.
Filter residue five is dietary fiber crude product, and filtrate five is pectin extracting soln.
C3）The water of 55 times of filter residue during filter residue five adds bleaching tank, is added, after stirring evenly, adds hydrogen peroxide dense to hydrogen peroxide
Spend for 2.5%, be warming up to 60 DEG C, be incubated 60 minutes.
This step mainly, while bleaching, is dissolved under weak basic condition with hydrogen peroxide and remains in the half of cellulose surface
Cellulose and lignin, to ensure the purity of dietary fiber.
C4）Separation of solid and liquid, and wash filter residue with water, obtain filter residue six and filtrate six.The step is walked for the purifying of dietary fiber
Suddenly.
C5）Filter residue the six channels fluidized bed drying（Temperature is less than 105 DEG C）, crush to obtain dietary fiber finished product.After testing, this enforcement
The quality of dietary fiber obtained by apple branch for butt apple branch quality 37.7% in example, purity is 96.9%.
The preparation of D pectin
D1）The filtrate Five Classics decolourizes, filters filtrate five of must decolourizing.
D2）The hydrochloric ethanol of decolouring 56 times of volumes of filtrate is added in decolouring filtrate five（The volume fraction of ethanol is
95%, the concentration of hydrochloric acid is 0.5mol/L, and sleeping spiral shell centrifugation obtains filter residue seven and filtrate seven.Filter residue seven is pectin crude product.
D3）Filter residue seven, repeat step D1 is dissolved with dilute sulfurous acid）And D2）3 times, last gained solid is after purification
Pectin.
Step D3）For the purification step of pectin, alcohol dissolubility impurity is removed.
D4）Step D3）Gained pectin after purification is spray-dried（115 DEG C of outlet temperature）, crush obtain final product pectin finished product.
After testing, in the present embodiment, the quality of pectin obtained by apple branch is the 4.7% of butt apple branch quality, and purity is 97.2%.
In addition, merging some filtrates and waste water, pH and nutrient content is adjusted, the liquid of plant growth needs can be prepared
Fertilizer, makes full use of filtrate and waste water, reduces discharge.
The preparation of E liquid fertilizers
Ammoniacal liquor, sulfurous acid used in the present embodiment；Raffinate after ethanol is reclaimed in merging filtrate six and hemicellulose preparation
In prepared by body and lignin, amalgamation liquid one reclaims remaining liquid after ethanol, adjusts pH to 6.5, and barrelling is used as plant nutrient
Foliage fertilizer or punching fertilising.
The Liquid Fertilizer contains required for the plant growths such as a certain amount of N, P, K, mineral matter and small molecule organic material
Nutrient.
Embodiment 2
It is a kind of to utilize fruit tree branch, pericarp（Slag）The method of production dietary fiber co-production pectin, including step：
The preparation of A hemicelluloses
A1）Pomace impurity elimination, drying（Inactivation pectase, cellulase, zytase）And digester after crushing, is added, add fruit
The water that 6 times of pomace quality, adds potassium hydroxide to concentration of lye to be 6%, and logical steam stops logical steam after being warming up to 85 DEG C, be passed through
Nitrogen, will seal after air emptying in digester；Then intermittence is passed through steam and nitrogen in digester, to maintain boiling
Kettle temperature is 92 DEG C, pressure is 0.7MPa, and heat-insulation pressure keeping spurted after 60 minutes.
The step extracts hemicellulose with diluted alkaline；Using relatively low boiling temperature（92℃）, higher pot inner pressure（0.7MPa）
And inert gas environment, it is therefore intended that ensure that the components such as hemicellulose, cellulose, lignin, pectin avoid high temperature, aerobic bar
Decomposition, oxidation, peeling, esterification under part etc. are reacted, and the integrality and product quality effect to ensureing molecular radical is obvious；Compared with
High pressure（0.7MPa）Ensure that alkali lye the effective infiltration between pomace cell membrane and the dissolution of macromolecular.
A2）By step 1）Gained spurts during slurry is transferred to colloid mill and grinds 25 minutes.Macromolecular is cracked with Mechanical Method
Between part be connected chemically key, further increase the yield of each material.
A3）Separation of solid and liquid, obtains filter residue one and filtrate one.Filter residue one is containing compositions such as cellulose, lignin, pectin
Slurry；First filtrate be thick liquid of hemicellulose.
A4）The ethanol of one 3 times of volumes of filtrate is added in filtrate one, after stirring, is stood complete to precipitation.
A5）Precipitation and separation and supernatant, obtain filter residue two and filtrate two.
A6）Filter residue two is dissolved using dilute potassium hydroxide solution, is subsequently adding the 95% of 6 times of volumes of sig water ethanol, is waited to sink
After forming sediment completely, precipitation and separation and supernatant are repeated operation 4 times, obtain filter residue three and filtrate three.
Step A4）、A5）、A6）For the purification step of hemicellulose.Step A4）Filter residue two obtained by alcohol precipitation is mainly half fiber
Plain crude product, the water phase being mainly in filtrate two in ethanol and filtrate one, the ethanol whole recycling in filtrate two；Step
A6）Purified, alcohol precipitation again after gained hemicellulose crude product is dissolved again, should used in the process of ethanol also all reclaim
Recycle.
A7）Three Jing heated-air dryings of filter residue（95 DEG C of temperature）, crush obtain final product hemicellulose finished product.After testing, in the present embodiment
The quality of hemicellulose obtained by pomace for butt pomace quality 19.5%, purity is 97.5%.
The preparation of B lignin
B1）Filter residue one is placed in into digester, the water of one 6 times of quality of filter residue is added, is passed through nitrogen, makes filter residue be evenly distributed on water
In；It is subsequently adding compound protease（550U/Kg butts filter residue one）, intermittently 2 minutes, nitrogen is passed through, is digested 30 minutes；Subsequently add
Enter normal temperature type AMS（450U/Kg butts filter residue one）, digest 20 minutes；Then pass to steam and be warming up to 68 DEG C, be incubated 8 points
The activity of clock inactivator.
Wherein, compound protease is by the alkali protease for possessing endopeptidase activity and possesses the active Proteinase K of peptide ending enzyme
Composition, the alkali protease for possessing endopeptidase activity in compound protease and the ratio for possessing the active Proteinase K of peptide ending enzyme are
1:3；The compound protease can effectively hydrolyzing protein at normal temperatures.
Normal temperature type AMS is by microwave induced gained variation bacillus licheniformis secretion gained AMS；It is microwave induced
The obtaining step of gained variation bacillus licheniformis is specially：The nutrient solution of bacillus licheniformis is placed in into microwave generator, if
Microwave power is put for 900W, pulse frequency is 2300MHz, microwave treatment 20s, cool down 20s, reciprocal 30 times according to this；At microwave
Nutrient solution after reason is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, screens four plants by the bacterium colony for surviving
The dissociant of the high bacillus licheniformis of alpha-amylase activity under normal temperature.Select alpha-amylase activity highest lichens under normal temperature
The dissociant Amplification Culture of bacillus, so that obtain normal temperature type AMS；Normal temperature type AMS is in 22-35 DEG C of temperature
Under expeditiously hydrolysis starch, it is not necessary to as the thermal-stable α-amylase for adopting mostly at present needs high temperature（80-90℃）Condition, because
And reduce energy consumption and also reduce the requirement to equipment, while greatly reduce the generation of side reaction；Herein can be with soft with enzyme process
Protein, Starch Hydrolysis are entered in filtrate, so as to success into the peptides of small molecule, amino acid, maltose, glucose etc. with ground
Deproteination matter and starch；To ensure the purity of lignin.
B2）Go out after enzyme, the mass fraction for adding 95% ethanol to ethanol in digester is 55%, is then intermittently led to
Enter water vapour and nitrogen, to maintain boiling kettle temperature to be 115 DEG C, pressure for 1.3 MPa, heat-insulation pressure keeping spurted after 90 minutes.
Vapours containing ethanol all enters ethanol recovery system by cover mouth.
B3）Step B2）Gained spurts slurry separation of solid and liquid, obtains filter residue four and filtrate four；Filter residue four adopts 55% ethanol
Washing, ethanol washing lotion are merged with filtrate four, obtain amalgamation liquid one.
Filter residue four is the slurry containing cellulose and pectin, and filtrate four is the molten lignin of alcohol.
B4）Amalgamation liquid one is concentrated by evaporation, and obtains lignin crude product；Lignin crude product wash with water after Jing heated-air dryings（Temperature
90℃）, crush to obtain lignin finished product.After testing, in the present embodiment, the quality of lignin obtained by pomace is butt apple slag
The 29.5% of amount, purity is 97.1%.
The preparation of C dietary fibers
C1）Filter residue four is placed in into extractor, the water of 4 10 times of filter residue is added, dilute sulfuric acid after stirring evenly, is added, and pH is adjusted to 3, is passed through
Water vapour, temperature stop water flowing steam after rising to 90 DEG C, are then passed through nitrogen, are sealed in emptying tank after air；Intermittently lead to
Enter water vapour and nitrogen, temperature is maintained in tank as 92 DEG C, and material is uniformly distributed in tank, insulation extracting 120 minutes.
C2）After extracting is finished, the material in extractor is carried out into separation of solid and liquid, filter residue five and filtrate five is obtained.
Filter residue five is dietary fiber crude product, and filtrate five is pectin extracting soln.
C3）The water of 53 times of filter residue during filter residue five adds bleaching tank, is added, after stirring evenly, adds hydrogen peroxide dense to hydrogen peroxide
Spend for 3%, be warming up to 70 DEG C, be incubated 40 minutes.
This step mainly, while bleaching, is dissolved under weak basic condition with hydrogen peroxide and remains in the half of cellulose surface
Cellulose and lignin, to ensure the purity of dietary fiber.
C4）Separation of solid and liquid, and wash filter residue with water, obtain filter residue six and filtrate six.The step is walked for the purifying of dietary fiber
Suddenly.
C5）Filter residue the six channels heated-air drying（105 DEG C of temperature）, crush to obtain dietary fiber finished product.After testing, apple in the present embodiment
The quality of dietary fiber obtained by pomace for butt pomace quality 42.7%, purity is 97.6%.
The preparation of D pectin
D1）The filtrate Five Classics decolourizes, filters filtrate five of must decolourizing.
D2）The hydrochloric ethanol of decolouring 59 times of volumes of filtrate is added in decolouring filtrate five（The volume fraction of ethanol is
95%, the concentration of hydrochloric acid is 0.5mol/L）Mass fraction to ethanol is 55%, after stirring, stands 60 minutes, separation of solid and liquid
Obtain filter residue seven and filtrate seven.Filter residue seven is pectin crude product.
D3）Filter residue seven, repeat step D1 is dissolved with dilute sulfuric acid）And D2）, last gained solid pectin as after purification.
Step D3）For the purification step of pectin, alcohol dissolubility impurity is removed.
D4）Step D3）Gained pectin Jing heated-air dryings after purification（95 DEG C of temperature）, crush obtain final product pectin finished product.Jing is examined
Survey, the quality of pectin obtained by pomace for butt pomace quality 5.7% in the present embodiment, purity is 96.4%.
The preparation of E liquid fertilizers
Potassium hydroxide, sulfuric acid used in the present embodiment；In merging filtrate six and hemicellulose preparation, ethanol is remaining after reclaiming
In prepared by liquid and lignin, amalgamation liquid one reclaims remaining liquid after ethanol, adjusts pH to 6.5, and barrelling, as plant nutrient
Foliage fertilizer or punching fertilising.
The Liquid Fertilizer contains required for the plant growths such as a certain amount of N, P, K, mineral matter and small molecule organic material
Nutrient.
Embodiment 3
It is a kind of to utilize fruit tree branch, pericarp（Slag）The method of production dietary fiber co-production pectin, including step：
The preparation of A hemicelluloses
A1）Orange peel impurity elimination, section drying（Inactivation pectase, cellulase, zytase）And digester is added after crushing, add
The water that 12 times of orange peel quality, adds ammoniacal liquor to concentration of lye to be 5%, and logical steam stops logical steam after being warming up to 90 DEG C, be passed through nitrogen
Gas, will seal after air emptying in digester；Then intermittence is passed through steam and nitrogen in digester, to maintain digester
Interior temperature is 91 DEG C, pressure is 0.8MPa, and heat-insulation pressure keeping spurted after 80 minutes.
Step diluted alkaline extracts hemicellulose and the inorganic salts such as most of siliceous in removing ash content；Using relatively low boiling
Temperature（91℃）, higher pot inner pressure（0.8MPa）And inert gas environment, it is therefore intended that ensure hemicellulose, cellulose,
The components such as lignin, pectin avoid the reaction such as decomposition under high temperature, aerobic conditions, oxidation, peeling, esterification, to ensureing molecule base
The integrality and product quality effect of group is obvious；Elevated pressures（0.8MPa）Ensure that alkali lye effective between orange peel cell membrane
Infiltration and the dissolution of macromolecular.
A2）By step 1）Gained spurts during slurry is transferred to and grinds 15 minutes in dense mill.Macromolecular is cracked with Mechanical Method
Between part be connected chemically key, further increase the yield of each material.
A3）Filter press press filtration is separated, and obtains filter residue one and filtrate one.Filter residue one is as containing cellulose, lignin, pectin etc.
The slurry of composition；First filtrate be thick liquid of hemicellulose.
A4）The 95% of one 4 times of volumes of filtrate ethanol is added in filtrate one, after stirring, is stood complete to precipitation.
A5）Precipitation and separation and supernatant, obtain filter residue two and filtrate two.
A6）Filter residue two is dissolved using weak aqua ammonia, is subsequently adding the 95% of 4 times of volumes of weak aqua ammonia ethanol, to be precipitated complete
Afterwards, precipitation and separation and supernatant, repeat operation 2 times, obtain filter residue three and filtrate three.
Step A4）、A5）、A6）For the purification step of hemicellulose.Step A4）Filter residue two obtained by alcohol precipitation is mainly half fiber
Plain crude product, the water phase being mainly in filtrate two in ethanol and filtrate one, the ethanol whole recycling in filtrate two；Step
A6）Purified, alcohol precipitation again after gained hemicellulose crude product is dissolved again, should used in the process of ethanol also all reclaim
Recycle.
A7）Three Jing fluidized bed dryings of filter residue（100 DEG C of temperature）, crush obtain final product hemicellulose finished product.After testing, the present embodiment
The quality of hemicellulose obtained by middle orange peel for butt orange peel quality 17.2%, purity is 96.6%.
The preparation of B lignin
B1）Filter residue one is placed in into digester, the water of one 10 times of quality of filter residue is added, is passed through nitrogen, makes filter residue be evenly distributed on water
In；It is subsequently adding compound protein 50 minutes；It is subsequently added normal temperature type AMS（500U/Kg butts filter residue one）, digest 40 points
Clock；Then pass to steam and be warming up to 62 DEG C, be incubated the activity of 12 minutes inactivators.
Wherein, compound protease is by the alkali protease for possessing endopeptidase activity and possesses the active Proteinase K of peptide ending enzyme
Composition, the alkali protease for possessing endopeptidase activity in compound protease and the ratio for possessing the active Proteinase K of peptide ending enzyme are
1:2；The compound protease can effectively hydrolyzing protein at normal temperatures.
Normal temperature type AMS is by microwave induced gained variation bacillus licheniformis secretion gained AMS；It is microwave induced
The obtaining step of gained variation bacillus licheniformis is specially：The nutrient solution of bacillus licheniformis is placed in into microwave generator, if
Microwave power is put for 900W, pulse frequency is 2300MHz, microwave treatment 20s, cool down 20s, reciprocal 30 times according to this；At microwave
Nutrient solution after reason is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, screens four plants by the bacterium colony for surviving
The dissociant of the high bacillus licheniformis of alpha-amylase activity under normal temperature.Select alpha-amylase activity highest lichens under normal temperature
The dissociant Amplification Culture of bacillus, so that obtain normal temperature type AMS；Normal temperature type AMS is in 22-35 DEG C of temperature
Under expeditiously hydrolysis starch, it is not necessary to as the thermal-stable α-amylase for adopting mostly at present needs high temperature（80-90℃）Condition, because
And reduce energy consumption and also reduce the requirement to equipment, while greatly reduce the generation of side reaction；Herein can be with soft with enzyme process
Protein, Starch Hydrolysis are entered in filtrate, so as to success into the peptides of small molecule, amino acid, maltose, glucose etc. with ground
Deproteination matter and starch；To ensure the purity of lignin.
B2）Go out after enzyme, the mass fraction for adding 95% ethanol to ethanol in digester is 50%, is then intermittently led to
Enter water vapour and nitrogen, boiling kettle temperature is maintained as 105 DEG C, pressure is 1.6MPa, and heat-insulation pressure keeping was spurted after 100 minutes.
Vapours containing ethanol all enters ethanol recovery system by cover mouth.
B3）Step B2）Gained spurts slurry separation of solid and liquid, obtains filter residue four and filtrate four；Filter residue four adopts 50% ethanol
Washing, ethanol washing lotion are merged with filtrate four, obtain amalgamation liquid one.
Filter residue four is the slurry containing cellulose and pectin, and filtrate four is the molten lignin of alcohol.
B4）Amalgamation liquid one is concentrated by evaporation, and obtains lignin crude product；Lignin crude product wash with water after Jing fluidized bed dryings（Temperature
100 DEG C of degree）, crush to obtain lignin finished product.After testing, in the present embodiment, the quality of lignin obtained by orange peel is butt orange peel quality
14.8%, purity is 96.8%.
The preparation of C dietary fibers
C1）Filter residue four is placed in into extractor, the water of 48 times of filter residue is added, dust technology after stirring evenly, is added, and pH is adjusted to 4, is passed through water
Steam, temperature stop water flowing steam after rising to 85 DEG C, are then passed through nitrogen, are sealed in emptying tank after air；Intermittently it is passed through
Water vapour and nitrogen, to maintain in tank temperature as 90 DEG C, and make material be uniformly distributed in tank, insulation extracting 150 minutes.
C2）After extracting is finished, the material in extractor is carried out into separation of solid and liquid, filter residue five and filtrate five is obtained.
Filter residue five is dietary fiber crude product, and filtrate five is pectin extracting soln.
C3）The water of 53 times of filter residue during filter residue five adds bleaching tank, is added, after stirring evenly, adds hydrogen peroxide dense to hydrogen peroxide
Spend for 4.5%, be warming up to 55 DEG C, be incubated 70 minutes.
This step mainly, while bleaching, is dissolved under weak basic condition with hydrogen peroxide and remains in the half of cellulose surface
Cellulose and lignin, to ensure the purity of dietary fiber.
C4）Separation of solid and liquid, and wash filter residue with water, obtain filter residue six and filtrate six.The step is walked for the purifying of dietary fiber
Suddenly.
C5）Filter residue the six channels fluidized bed drying（95 DEG C of temperature）, crush to obtain dietary fiber finished product.After testing, in the present embodiment
The quality of dietary fiber obtained by orange peel for butt orange peel quality 29.5%, purity is 97.7%.
The preparation of D pectin
D1）The filtrate Five Classics decolourizes, filters filtrate five of must decolourizing.
D2）The hydrochloric ethanol of decolouring 57 times of volumes of filtrate is added in decolouring filtrate five（The volume fraction of ethanol is
95%, the concentration of hydrochloric acid is 0.5mol/L）Mass fraction to ethanol is 50%, after stirring, stands 60 minutes, separation of solid and liquid
Obtain filter residue seven and filtrate seven.Filter residue seven is pectin crude product.
D3）With dilute nitric acid dissolution filter residue seven, repeat step D1）And D2）, last gained solid pectin as after purification.
Step D3）For the purification step of pectin, alcohol dissolubility impurity is removed.
D4）Step D3）Gained pectin Jing fluidized bed dryings after purification（100 DEG C of temperature）, crush obtain final product pectin finished product.Jing
Detection, the quality of pectin obtained by orange peel for butt orange peel quality 27.8% in the present embodiment, purity is 96.1%.
In addition, merging some filtrates and waste water, pH and nutrient content is adjusted, the liquid of plant growth needs can be prepared
Fertilizer, makes full use of filtrate and waste water, reduces discharge.
The preparation of E liquid fertilizers
Ammoniacal liquor, nitric acid used in the present embodiment；Remaining liq after ethanol is reclaimed in merging filtrate six and hemicellulose preparation
In preparing with lignin, amalgamation liquid one reclaims remaining liquid after ethanol, adjusts pH to 6.5, and barrelling, as plant nutrient
Foliage fertilizer or punching fertilising.
The Liquid Fertilizer contains required for the plant growths such as a certain amount of N, P, K, mineral matter and small molecule organic material
Nutrient.
Claims (9)
1. it is a kind of to utilize fruit tree branch, pericarp（Slag）The method of production dietary fiber co-production pectin, it is characterised in that including step
Suddenly：
The preparation of A hemicelluloses
A1）Digester is dried and moved into after crushing to fruit tree branch, pericarp or pomace, adds fruit tree branch, pericarp or pomace quality 1-20
Times water, add alkali to concentration of lye to be 1%-10%, logical steam stops logical steam after being warming up to 60-100 DEG C, is passed through indifferent gas
Body, will seal after air emptying in digester；Then intermittence is passed through steam and inert gas in digester, to maintain to steam
Boil kettle temperature for 60-100 DEG C, pressure be 0.5-1MPa, heat-insulation pressure keeping spurted after 10-120 minutes；
A2）By step 1）Gained spurts during slurry is transferred to grinding mill and grinds；
A3）Separation of solid and liquid, obtains filter residue one and filtrate one；
A4）The ethanol of one 1-10 times of volume of filtrate is added in filtrate one, after stirring, is stood complete to precipitation；
A5）Precipitation and separation and supernatant, obtain filter residue two and filtrate two；
A6）Filter residue two is dissolved using sig water, is subsequently adding the ethanol of 1-10 times of volume of sig water, it is to be precipitated completely after, separate
Precipitation and supernatant, repeat operation 1-5 time, obtain filter residue three and filtrate three；
A7）Three drying of filter residue, crushing obtain final product hemicellulose finished product；
The preparation of B lignin
B1）Filter residue one is placed in into digester, the water of one 1-20 times of quality of filter residue is added, is passed through inert gas, filter residue is uniformly divided
Cloth is in water；Compound protease is subsequently adding, interval 1-3 minute, inert gas is passed through, is digested 10-80 minutes；Often it is subsequently added
Warm type AMS, digests 10-80 minutes；Then pass to steam and be warming up to 60-70 DEG C, be incubated the work of 2-20 minute inactivators
Property；The compound protease is made up of the alkali protease for possessing endopeptidase activity and the Proteinase K for possessing peptide ending enzyme activity；Institute
Normal temperature type AMS is stated by microwave induced gained variation bacillus licheniformis secretion gained AMS, the normal temperature type α-shallow lake
The preference temperature of powder enzyme is 22-35 DEG C；
B2）Go out after enzyme, the mass fraction for adding ethanol to ethanol in digester is 30%-80%, is then intermittently passed through water
Steam and inert gas, are 80-120 DEG C, pressure for 0.5-2 MPa to maintain boiling kettle temperature, heat-insulation pressure keeping 60-120 point
Spurt after clock；
B3）Step B2）Gained spurts slurry separation of solid and liquid, obtains filter residue four and filtrate four；Ethanol of the filter residue four using 40%-90%
Washing, ethanol washing lotion are merged with filtrate four, obtain amalgamation liquid one；
B4）Amalgamation liquid one is concentrated by evaporation, and obtains lignin crude product；After lignin crude product is washed with water, Jing is dried, crushes to obtain lignin
Finished product；
The preparation of C dietary fibers
C1）Filter residue four is placed in into extractor, the water of four 3-30 times of filter residue is added, diluted acid after stirring evenly, is added, and pH is adjusted to 1-5, is led to
Enter water vapour, temperature stops water flowing steam after rising to 30-100 DEG C, is then passed through inert gas, sealed in emptying tank after air；
Water vapour and inert gas is intermittently passed through, and temperature is maintained in tank as 30-100 DEG C, and material is uniformly distributed in tank,
Insulation extracting 30-300 minutes；
C2）After extracting is finished, the material in extractor is carried out into separation of solid and liquid, filter residue five and filtrate five is obtained；
C3）The water of five 1-10 times of filter residue during filter residue five adds bleaching tank, is added, the concentration of hydrogen peroxide to hydrogen peroxide after stirring evenly, is added
For 1%-5%, 50-80 DEG C is warming up to, is incubated 10-120 minutes；
C4）Separation of solid and liquid, and wash filter residue with water, obtain filter residue six and filtrate six；
C5）Filter residue the six channels is dried, crushes to obtain dietary fiber finished product；
The preparation of D pectin
D1）The filtrate Five Classics decolourizes, filters filtrate five of must decolourizing；
D2）To in decolouring filtrate five, the mass fraction of the hydrochloric ethanol to ethanol of five 1-10 times of volumes of addition decolouring filtrate is
30%-80%, after stirring, stands 20-100 minutes, and separation of solid and liquid obtains filter residue seven and filtrate seven；
D3）Filter residue seven, repeat step D1 is dissolved with diluted acid）And D2）, last gained solid pectin as after purification；
D4）Step D3）Gained pectin drying after purification, crushing obtain final product pectin finished product.
2. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：Step A1, A6）In, the alkali is potassium hydroxide, NaOH, ammoniacal liquor or calcium hydroxide.
3. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In step B1）In, the obtaining step of the microwave induced gained variation bacillus licheniformis is specially：By bacillus licheniformis
Nutrient solution be placed in microwave generator, setting microwave power is 850-950W, and pulse frequency is 2300MHz, microwave treatment 20s,
Cooling 20s, it is reciprocal 25-35 time according to this；Nutrient solution after microwave treatment is coated on solid medium, is cultivated under the conditions of 30 DEG C
1-2 days, by the dissociant for screening the high bacillus licheniformis of alpha-amylase activity under four plants of normal temperature in the bacterium colony for surviving.
4. fruit tree branch, pericarp are utilized as claimed in claim 3（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：The dissociant Amplification Culture of alpha-amylase activity highest bacillus licheniformis under normal temperature is selected, it is described normal so as to obtain
Warm type AMS.
5. using fruit tree branch, pericarp as described in claim 1 or 3（Slag）The method of production dietary fiber co-production pectin, which is special
Levy and be：Possess the alkali protease and the Proteinase K for possessing peptide ending enzyme activity of endopeptidase activity in the compound protease
Ratio is 1:1-3；The addition of the compound protease meets every kilogram of one 400-800U of butt filter residue, the normal temperature type α-shallow lake
The addition of powder enzyme meets every kilogram of one 300-700U of butt filter residue.
6. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：Step C1）And D3）In, described sour one kind in sulfuric acid, nitric acid, hydrochloric acid, sulfurous acid, acetic acid.
7. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：The inert gas is nitrogen, helium or argon gas.
8. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：Step A7）、B4）、C5）、D4）Described in be dried as spray drying, heated-air drying, fluidized bed drying or freeze-drying；It is dried
Temperature is less than 120 DEG C.
9. fruit tree branch, pericarp are utilized as claimed in claim 1（Slag）The method of production dietary fiber co-production pectin, its feature exist
In：Step D2）In hydrochloric ethanol, the volume fraction of ethanol is 95%, and the concentration of hydrochloric acid is 0.5mol/L.
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| CN107319509A (en) * | 2017-05-22 | 2017-11-07 | 石家庄市兄弟伊兰食品配料有限公司 | A kind of method for preparing pectin and fiber continuous from fruit |
| CN107692066A (en) * | 2017-09-26 | 2018-02-16 | 大连工业大学 | A kind of high fine fish sausage product and its processing method |
| CN108373513A (en) * | 2018-02-24 | 2018-08-07 | 天津科技大学 | A kind of method of the steam and nitrogen collaboration gas explosion separation hemicellulose of poplar |
| CN108623710A (en) * | 2018-05-03 | 2018-10-09 | 昆明理工大学 | A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose |
| CN109887762A (en) * | 2019-02-15 | 2019-06-14 | 上海应用技术大学 | A kind of preparation method of the nitrogen sulphur codope carbon material based on hemicellulose |
| CN110041446A (en) * | 2019-03-20 | 2019-07-23 | 肖兵 | A kind of biomass comprehensive method for refining |
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| RU2763401C1 (en) * | 2021-03-09 | 2021-12-28 | Евгений Михайлович Герасимов | Method for obtaining a pectin-containing composition |
| RU2806822C2 (en) * | 2021-10-05 | 2023-11-07 | Евгений Михайлович Герасимов | Method for processing gourds with obtaining pectin-containing compositions |
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| CN107319509A (en) * | 2017-05-22 | 2017-11-07 | 石家庄市兄弟伊兰食品配料有限公司 | A kind of method for preparing pectin and fiber continuous from fruit |
| WO2018214753A1 (en) * | 2017-05-22 | 2018-11-29 | 河北兄弟伊兰食品科技股份有限公司 | Method for continuously preparing pectin and fiber from fruits |
| CN107692066A (en) * | 2017-09-26 | 2018-02-16 | 大连工业大学 | A kind of high fine fish sausage product and its processing method |
| CN108373513A (en) * | 2018-02-24 | 2018-08-07 | 天津科技大学 | A kind of method of the steam and nitrogen collaboration gas explosion separation hemicellulose of poplar |
| CN108623710A (en) * | 2018-05-03 | 2018-10-09 | 昆明理工大学 | A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose |
| CN109887762A (en) * | 2019-02-15 | 2019-06-14 | 上海应用技术大学 | A kind of preparation method of the nitrogen sulphur codope carbon material based on hemicellulose |
| CN110041446A (en) * | 2019-03-20 | 2019-07-23 | 肖兵 | A kind of biomass comprehensive method for refining |
| CN112029012A (en) * | 2020-08-06 | 2020-12-04 | 湖南华诚生物资源股份有限公司 | Comprehensive utilization method of siraitia grosvenorii horizontal snail centrifugal slag |
| RU2763401C1 (en) * | 2021-03-09 | 2021-12-28 | Евгений Михайлович Герасимов | Method for obtaining a pectin-containing composition |
| RU2806822C2 (en) * | 2021-10-05 | 2023-11-07 | Евгений Михайлович Герасимов | Method for processing gourds with obtaining pectin-containing compositions |
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