CN102731681A - Method for extracting pectin from orange peel and shaddock peel - Google Patents
Method for extracting pectin from orange peel and shaddock peel Download PDFInfo
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- CN102731681A CN102731681A CN2011101062425A CN201110106242A CN102731681A CN 102731681 A CN102731681 A CN 102731681A CN 2011101062425 A CN2011101062425 A CN 2011101062425A CN 201110106242 A CN201110106242 A CN 201110106242A CN 102731681 A CN102731681 A CN 102731681A
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- pectin
- nanofiltration
- orange peel
- press filtration
- shaddock skin
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- 229920001277 pectin Polymers 0.000 title claims abstract description 87
- 239000001814 pectin Substances 0.000 title claims abstract description 87
- 235000010987 pectin Nutrition 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 58
- 235000001759 Citrus maxima Nutrition 0.000 title claims abstract description 36
- 244000276331 Citrus maxima Species 0.000 title claims abstract description 36
- 238000001728 nano-filtration Methods 0.000 claims abstract description 58
- 238000001914 filtration Methods 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 8
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 14
- 239000003292 glue Substances 0.000 claims description 14
- 229920002521 macromolecule Polymers 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000010298 pulverizing process Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 10
- 108010059820 Polygalacturonase Proteins 0.000 claims description 7
- 235000019658 bitter taste Nutrition 0.000 claims description 7
- 230000008030 elimination Effects 0.000 claims description 7
- 238000003379 elimination reaction Methods 0.000 claims description 7
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 7
- 238000000265 homogenisation Methods 0.000 claims description 7
- 238000002161 passivation Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 239000007858 starting material Substances 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 230000004071 biological effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 235000021190 leftovers Nutrition 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 150000004676 glycans Chemical class 0.000 description 4
- 229920002230 Pectic acid Polymers 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- -1 methyl alcohol ester Chemical class 0.000 description 3
- 239000010318 polygalacturonic acid Substances 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- AEMOLEFTQBMNLQ-DTEWXJGMSA-N D-Galacturonic acid Natural products O[C@@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-DTEWXJGMSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- AEMOLEFTQBMNLQ-UHFFFAOYSA-N beta-D-galactopyranuronic acid Natural products OC1OC(C(O)=O)C(O)C(O)C1O AEMOLEFTQBMNLQ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000006198 methoxylation reaction Methods 0.000 description 1
- LCLHHZYHLXDRQG-ZNKJPWOQSA-N pectic acid Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)O[C@H](C(O)=O)[C@@H]1OC1[C@H](O)[C@@H](O)[C@@H](OC2[C@@H]([C@@H](O)[C@@H](O)[C@H](O2)C(O)=O)O)[C@@H](C(O)=O)O1 LCLHHZYHLXDRQG-ZNKJPWOQSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for extracting pectin from orange peel and shaddock peel, which relates to the technical field of biochemical pharmacy. A technical scheme provided in the invention is as follows: the method for extracting pectin from orange peel and shaddock peel comprises the successive steps of cleaning leftovers of orange peel and shaddock peel, crushing the leftovers of orange peel and shaddock peel into particles with a particle size of 2 to 3 mm, treating the obtained particles with steam or boiling water for 5 to 8 min to passivate the activity of pectase, steeping the particles in clear water for 30 min, heating an obtained mixture to a temperature of 90 DEG C for 5 min, carrying out rinsing with clear water several times to remove bitter, pigments and soluble impurities, and after the above-mentioned pre-treatment, carrying out mixing and homogenizing, press filtration, ultrafiltration, nanofiltration I, nanofiltration II, stirring for pectin formation, press filtration, distillation and recycling, spray drying and crushing so as to prepare a pure product. Compared with the prior art, the invention has the following striking substantive advantages and remarkable progress: usage of traditional extraction methods and harmful organic solvents is reduced, original biological activity is retained during the process of extraction, the extraction process is simple and environment-friendly, and the method costs little and is applicable to large scale industrial production.
Description
Technical field
The present invention relates to biological chemistry pharmaceutical technology field, relate in particular to a kind of method and technology field of from orange peel, shaddock skin, extracting pectin.
Background technology
Pectin (Pcctin) is one group of polygalacturonic acid.It has water-soluble, and is promptly separable in the industry, its molecular weight about 50,000 one 30 ten thousand.Its solution can form gel and partly methoxylation (esterification just forms the methyl alcohol ester) take place under optimum conditions, and its staple is a (I, a 4) D one polygalacturonic acid of cruelization of part first.Residual carboxyl unit exists with the form of free acid or forms salt such as amine, potassium, sodium and calcium.
Pectin is present in cell walls and the cell internal layer of plant, is the support substance of inner cell.Different vegetables, the fruit mouthfeel is had any different, and mainly is the difference decision of the pectin content pectin molecule that contained by them.By the composition of pectin two types of homogeneity polysaccharide and mixed polysaccharide can be arranged: homogeneity glycan pectin such as D-Polygalactan, L-ARABINANS and D-galacturonic acid glycan etc.; Mixed polysaccharide pectin is the most common, is made up of in varing proportions galacturonic acid glycan, Polygalactan and ARABINANS, is commonly referred to pectic acid.Also each is variant for the pectin of different sources, its ratio.Because pectin is a kind of natural high moleculer eompound, has good gelationization and stable emulsifying effect, food, medicine, daily use chemicals and textile industry therefore have been widely used in.Pectin divides three kinds of liquid pectin, pectin powder and low-methoxy pectins, and is wherein general with the application of pectin powder especially.Just extracting pectin adopts traditional acid, enzyme formula process for extracting always at present; Because its extraction process process is long, more, the residual solvent of the various solvent of adding is unfavorable for HUMAN HEALTH; The method of therefore, seeking a kind of new production pectin is the technical task that the technician in present technique field needs to be resolved hurrily.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes prior art; And a kind of usage quantity new, that can reduce traditional extraction process and harmful organic solvent is provided; In leaching process, keep original biological activity, make that leaching process is simple, environmental protection, cost is low and can carry out the method for from orange peel, shaddock skin, extracting pectin of large-scale industrial production.
For solving the problems of the technologies described above, the present invention is achieved through implementing following technical scheme; A kind of method of from orange peel, shaddock skin, extracting pectin; Its special character is that described method comprises the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.
For further solving the problems of the technologies described above, the preferred version of technique scheme is:
Above-mentioned described mixing homogenate is that the material after handling is placed in the refiner, and be 1 in material and water: the ratio of 1.5-4 adds water, starter, and adding concentration is that its pH value of hydrochloric acid adjustment of 95-99% is 2-3, high-speed homogenization 2-3 hour.
Above-mentioned described press filtration is to be under the air pressure of 0.5-1MPA, to carry out press filtration with mixing homogenate in the basket-hanging air pressure filter, crosses the 300-700 mesh sieve.
Above-mentioned described ultrafiltration be with above-mentioned homogenate can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.01-0.05MPA, adopt cross flow filter to remove waste residue and get just and filtrate.
Above-mentioned said nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.01-0.15MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate.
Above-mentioned described nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, under the pressure of 0.01-0.15MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product.
The above-mentioned described glue that stirs into is to place in the whisking appliance above-mentioned pectin first product and by weight 1: 1.5-2.5 adds 70-98% ethanol, stirs and promptly forms gel in 0.5-1 hour.
Above-mentioned described press filtration is that the gel with pectin places the gelling thing that under the pressure of 0.2-0.3Mpa, makes pectin in the plate-and-frame filter press.
The present invention compared with prior art has following outstanding substantive distinguishing features and obvious improvement: in the first method of the present invention except that in the mixing homogenate that extracts pectin, being added with hydrochloric acid and the ethanol afterwards; No longer add any deleterious organic solvent; All utilize the mechanical-physical method and extract the preparation process; Reach the usage quantity that reduces traditional extraction process and harmful organic solvent fully, make that the preparation process reaches simply, the standard-required of environmental protection; Improved the security of preparation process, eliminated the potential safety hazard of prior art and the pollution of environment.It two is that method of the present invention is all extracted through specific equipment; Or else whole described method is added under the prerequisite of any harmful organic solvent and is separated, purifies; Thereby make pectin of the present invention keep original biological activity; Not only reach and improve pectin, and improved security, the safety used in the range of application that is used for food, medicine, daily use chemicals and textile industry; Its three be extracting pectin of the present invention both for depleted orange peel, shaddock skin found renewable resource high added value utilize method; Take to use mechanical means to exercise the process of extracting pectin again, thereby make that extracting pectin of the present invention has compared with prior art that implementation process is simple, reliable, environmental protection, cost are low, outstanding substantive distinguishing features and the obvious improvement that can carry out large-scale industrial production.
Embodiment
Further specify a kind of concrete implementation process of method of from orange peel, shaddock skin, extracting pectin of the present invention below in conjunction with embodiment.
Embodiment 1:
A kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 1; Comprise the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its concrete enforcement is following:
1. the material 10kg after will handling places in the refiner, is that 1: 1.5 ratio adds water 15kg and starter in material and water, and its pH value of hydrochloric acid adjustment that adds concentration again and be 95-99% is 2, opens machine, carries out high-speed homogenization 2 hours;
2. press filtration is to be that press filtration is carried out in above-mentioned mixing homogenate in the basket-hanging air pressure filter under the air pressure of 0.5MPA, crosses 300 mesh sieves.
Ultrafiltration be with liquid after the above-mentioned press filtration can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.01-0.02MPA, adopt cross flow filter to remove waste residue and get just and filtrate;
4. nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.01-0.02MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate;
Nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, under the pressure of 0.01-0.02MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product;
6. stirring into glue is above-mentioned pectin first product to be placed in the whisking appliance and by weight 1: 1.5 add 98% ethanol, stirs and promptly forms gel in 0.5 hour;
7. press filtration is that gel with pectin places the gelling thing that under the pressure of 0.2Mpa, makes pectin in the plate-and-frame filter press;
8. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
9. above-mentioned gelling thing is carried out spraying drying, be prepared into the pectin dry product; Promptly got the pectin powder finished product through pulverizing 80 mesh sieves.More than be a kind of of the embodiment of the invention 1 from a kind of method of from orange peel, shaddock skin, extracting pectin.
Embodiment 2:
A kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 2; Comprise the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its concrete enforcement is following:
1. the material 10kg after will handling places in the refiner, is that 1: 2 ratio adds water 20kg and starter in material and water, and its pH value of hydrochloric acid adjustment that adds concentration again and be 95-99% is 2.8, opens machine, carries out high-speed homogenization 2.5 hours;
2. press filtration is to be that press filtration is carried out in above-mentioned mixing homogenate in the basket-hanging air pressure filter under the air pressure of 0.6MPA, crosses 400 mesh sieves.
Ultrafiltration be with liquid after the above-mentioned press filtration can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.02-0.03MPA, adopt cross flow filter to remove waste residue and get just and filtrate;
4. nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.03-0.04MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate;
Nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, under the pressure of 0.03-0.04MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product;
6. stirring into glue is above-mentioned pectin first product to be placed in the whisking appliance and by weight 1: 1.8 add 90% ethanol, stirs and promptly forms gel in 1 hour;
7. press filtration is that gel with pectin places the gelling thing that under the pressure of 0.25Mpa, makes pectin in the plate-and-frame filter press;
8. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
9. above-mentioned gelling thing is carried out spraying drying, be prepared into the pectin dry product; Promptly got the pectin powder finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 2.
Embodiment 3:
A kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 3; Comprise the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its concrete enforcement is following:
1. the material 10kg after will handling places in the refiner, is that 1: 3 ratio adds water 30kg and starter in material and water, and its pH value of hydrochloric acid adjustment that adds concentration again and be 95-99% is 3, opens machine, carries out high-speed homogenization 3 hours;
2. press filtration is to be that press filtration is carried out in above-mentioned mixing homogenate in the basket-hanging air pressure filter under the air pressure of 0.7MPA, crosses 500 mesh sieves.
Ultrafiltration be with liquid after the above-mentioned press filtration can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.03-0.04MPA, adopt cross flow filter to remove waste residue and get just and filtrate;
4. nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.06-0.08MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate;
Nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, under the pressure of 0.06-0.08MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product;
6. stirring into glue is above-mentioned pectin first product to be placed in the whisking appliance and by weight 1: 2 add 85% ethanol, stirs and promptly forms gel in 0.5 hour;
7. press filtration is that gel with pectin places the gelling thing that under the pressure of 0.3Mpa, makes pectin in the plate-and-frame filter press;
8. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
9. above-mentioned gelling thing is carried out spraying drying, be prepared into the pectin dry product; Promptly got the pectin powder finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 3.
Embodiment 4:
A kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 4; Comprise the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its concrete enforcement is following:
1. the material 10kg after will handling places in the refiner, is that 1: 3.5 ratio adds water 35kg and starter in material and water, and its pH value of hydrochloric acid adjustment that adds concentration again and be 95-99% is 2.4, opens machine, carries out high-speed homogenization 2.5 hours;
2. press filtration is to be that press filtration is carried out in above-mentioned mixing homogenate in the basket-hanging air pressure filter under the air pressure of 0.9MPA, crosses 600 mesh sieves.
Ultrafiltration be with liquid after the above-mentioned press filtration can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.04-0.05MPA, adopt cross flow filter to remove waste residue and get just and filtrate;
4. nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.1-0.12MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate;
Nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, under the pressure of 0.1-0.12MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product;
6. stirring into glue is above-mentioned pectin first product to be placed in the whisking appliance and by weight 1: 2.2 add 80% ethanol, stirs and promptly forms gel in 1 hour;
7. press filtration is that gel with pectin places the gelling thing that under the pressure of 0.25Mpa, makes pectin in the plate-and-frame filter press;
8. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
9. above-mentioned gelling thing is carried out spraying drying, be prepared into the pectin dry product; Promptly got the pectin powder finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 4.
Embodiment 5:
A kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 5; Comprise the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its concrete enforcement is following:
1. the material 10kg after will handling places in the refiner, is that 1: 4 ratio adds water 40kg and starter in material and water, and its pH value of hydrochloric acid adjustment that adds concentration again and be 95-99% is 2.2, opens machine, carries out high-speed homogenization 2 hours;
2. press filtration is to be that press filtration is carried out in above-mentioned mixing homogenate in the basket-hanging air pressure filter under the air pressure of 1MPA, crosses 700 mesh sieves.
Ultrafiltration be with liquid after the above-mentioned press filtration can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.03-0.04MPA, adopt cross flow filter to remove waste residue and get just and filtrate;
4. nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.14-0.15MPA, carries out a nanofiltration and removes macromolecular substance and must filtrate;
Nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton, at 0.14-0, carry out the secondary nanofiltration under the pressure of 15MPA and remove impurity, its trapped substance is the pectin first product;
6. stirring into glue is above-mentioned pectin first product to be placed in the whisking appliance and by weight 1: 2.5 add 70% ethanol, stirs and promptly forms gel in 0.5 hour;
7. press filtration is that gel with pectin places the gelling thing that under the pressure of 0.2Mpa, makes pectin in the plate-and-frame filter press;
8. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
9. above-mentioned gelling thing is carried out spraying drying, be prepared into the pectin dry product; Promptly got the pectin powder finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from orange peel, shaddock skin, extracting pectin of the embodiment of the invention 5.
Claims (8)
1. method of from orange peel, shaddock skin, extracting pectin; It is characterized in that described method comprises the steps: that successively it is 2-3mm that orange peel, shaddock skin tankage are cleaned and be crushed to particle diameter; Place steam or boiling water to handle 5～8min then; In water, to steep 30min behind the passivation pectinase activity more clearly; And be heated to 90 ℃ of 5min, and with the clear water rinsing for several times, to mix homogenate, press filtration, ultrafiltration, nanofiltration I, nanofiltration II after the pre-process of removing bitter taste and pigment and soluble impurity again, to stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.
2. the method for from orange peel, shaddock skin, extracting pectin according to claim 1; It is characterized in that described mixing homogenate is that the material after handling is placed in the refiner; In material and water is 1: the ratio of 1.5-4 adds water, starter; Adding concentration is that its pH value of hydrochloric acid adjustment of 95-99% is 2-3, high-speed homogenization 2-3 hour.
3. the method for from orange peel, shaddock skin, extracting pectin according to claim 1 and 2 is characterized in that described press filtration is is under the air pressure of 0.5-1MPA, to carry out press filtration with mixing homogenate, crosses the 300-700 mesh sieve in the basket-hanging air pressure filter.
4. the method for from orange peel, shaddock skin, extracting pectin according to claim 1 and 2; It is characterized in that described ultrafiltration be with above-mentioned homogenate can molecular weight cut-off 10000 dalton in the rolling ultra-filtration equipment of above material, under the pressure of 0.01-0.05MPA, adopt cross flow filter to remove waste residue and get just and filtrate.
5. the method for from orange peel, shaddock skin, extracting pectin according to claim 1 and 2; It is characterized in that said nanofiltration I is can molecular weight cut-off be in the nanofiltration device of the above macromolecular substance of 200 dalton with above-mentioned filtrating just, under the pressure of 0.01-0.15MPA, carry out a nanofiltration and remove macromolecular substance and must filtrate.
6. the method for from orange peel, shaddock skin, extracting pectin according to claim 1; It is characterized in that described nanofiltration II be with above-mentioned filtrating can elimination molecular weight be in the nanofiltration device of the following material of 100 dalton; Under the pressure of 0.01-0.15MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the pectin first product.
7. the method for from orange peel, shaddock skin, extracting pectin according to claim 1; It is characterized in that the described glue that stirs into is to place in the whisking appliance above-mentioned pectin first product and by weight 1: 1.5-2.5 adds 70-98% ethanol, stirs and promptly forms gel in 0.5-1 hour.
8. the method for from orange peel, shaddock skin, extracting pectin according to claim 1 is characterized in that described press filtration is that gel with pectin places the gelling thing that under the pressure of 0.2-0.3Mpa, makes pectin in the plate-and-frame filter press.
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