CN102304192A - Method for extracting low-ester pectin from sunflower heads and stems and ultrafiltration device - Google Patents
Method for extracting low-ester pectin from sunflower heads and stems and ultrafiltration device Download PDFInfo
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- CN102304192A CN102304192A CN201110098612A CN201110098612A CN102304192A CN 102304192 A CN102304192 A CN 102304192A CN 201110098612 A CN201110098612 A CN 201110098612A CN 201110098612 A CN201110098612 A CN 201110098612A CN 102304192 A CN102304192 A CN 102304192A
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Abstract
The invention discloses a method for extracting low-ester pectin from sunflower heads and stems and an ultrafiltration device, and relates to the technical field of biochemical pharmacy. The method for extracting low-ester pectin from the sunflower heads and stems is characterized by sequentially comprising the following steps of: crushing the sunflower heads and stems; boiling with hot water; washing with water and performing suction filtration; squeezing to remove water and taking residue; mixing and homogenizing; performing suction filtration; performing nanofiltration I; performing nanofiltration II; stirring to obtain gelatin; performing pressure filtration; distilling and recycling; performing spray drying; and crushing to obtain a pure product. Compared with the prior art, the method has the outstanding substantive characteristics and obvious progress of reducing the consumption of harmful organic solvents in the traditional extraction method, maintaining the original bioactivity in the extracting process, and ensuring that the extracting process is simple, environment-friendly, low in cost, and suitable for 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 ultra-filtration equipment technical field of from sunflower plate and bar, extracting low-ester 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 main component 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 pectin molecule of the pectin content that contained by them.Containing 30% pectin approximately in the pericarps such as oranges and tangerines, lemon, shaddock, is the abundantest source of pectin.By the composition of pectin two types of homogeneity polysaccharide and mixed polysaccharide can be arranged: homogeneity glycan pectin such as D-Polygalactan, L-arabinan 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 arabinan, 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.And low-methoxy pectin (also claiming low-ester pectin) is along with the develop rapidly of science and technology and the continuous expansion of Application Areas; More and more show the market requirement that it is powerful; And the technical indicator of existing low-ester pectin can not satisfy specific technical requirements, and its reason is because all there are tangible deficiency in material, the making method of existing production usefulness.Therefore, seeking a kind of novel material of producing low-ester pectin and novel method and special-purpose ultra-filtration equipment 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 new material and the usage quantity that can reduce traditional extraction process and harmful organic solvent be 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 and the ultra-filtration equipment that from sunflower plate and bar, extract low-ester 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 sunflower plate and bar, extracting low-ester pectin; Its special character is that described method comprises the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter; Be 1 with dry material in its weight ratio then: the ratio of 4-6 adds entry and the control water temperature of heating is to boil 1-2 hour in 70-100 ℃ the scope; Material after hot water boiled places in the suction filtration groove that is provided with filter cloth; Warm water with 40-60 ℃ washes 3-5 time repeatedly; Carry out suction filtration with negative-pressure gas simultaneously, squeezing is anhydrated and is got slag; Mix homogenate; Suction filtration; Ultrafiltration; Nanofiltration I; Nanofiltration II; Stir into glue; Press filtration; The 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 the squeezing 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 ultrafiltration be with above-mentioned homogenate through behind the suction filtration 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 low-ester pectin first product.
The above-mentioned described glue that stirs into is to place above-mentioned low-ester pectin first product in the agitator 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 low-ester pectin places the gelling thing that under the pressure of 0.2-0.3Mpa, makes low-ester pectin in the plate-and-frame filter press.
For further solving the problems of the technologies described above, following technical scheme is taked in ultrafiltration of the present invention:
A kind of special-purpose ultra-filtration equipment of method that from sunflower plate and bar, extracts low-ester pectin; Comprise at least one housing and the unit of the adapter of intracavity inter-connection with it; Its special character is that described housing inner chamber is provided with an airtight tubulose ultrafiltration body; The upper end of ultrafiltration body is provided with 2 adapters of inner chamber connection with it, and the tubular wall of ultrafiltration body is provided with can allow that medium gets into the ultra-filtration membrane of cavity between ultrafiltration body and the housing from its inner chamber.
One of above-mentioned described ultrafiltration body upper end is taken over and also is provided with a hold-up vessel and force (forcing) pump, and the input terminus of force (forcing) pump is connected with hold-up vessel, and its output terminal is connected with the ultrafiltration intracoelomic cavity.
Above-mentioned described housing bottom also is provided with water pipe and the valve that communicates with the housing inner chamber.
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 low-ester 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 low-ester pectin of the present invention keep original biological activity; Not only reach and improve low-ester pectin, and improved security, the reliability used in the range of application that is used for food, medicine, daily use chemicals and textile industry; It three is that the process for extracting of low-ester pectin of the present invention had both found the method for utilizing of renewable resource for depleted Sunflower Receptacle stalk; Take to use mechanical means to exercise the process of extracting low-ester pectin again, thereby make that the process for extracting of low-ester 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.
Description of drawings
Included accompanying drawing provides further understanding of the present invention, and it is incorporated into a part that constitutes this specification sheets in this specification sheets, and said accompanying drawing shows embodiments of the invention and is used to explain principle of the present invention with specification sheets.Identical in the accompanying drawings Reference numeral is represented identical parts.In the accompanying drawings:
Fig. 1 is the structural representation of a kind of ultra-filtration equipment of the embodiment of the invention 1.
Fig. 2 is the structural representation of a kind of ultra-filtration equipment of the embodiment of the invention 2.
Embodiment
Describe a kind of concrete implementation process and concrete CONSTRUCTED SPECIFICATION of ultra-filtration equipment of method of from sunflower plate and bar, extracting low-ester pectin of the present invention in detail below in conjunction with embodiment.
Embodiment 1:
A kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 1; Comprise the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter, carry out hot water then and boil, wash suction filtration, squeezing and anhydrate and get slag, mix homogenate, suction filtration, ultrafiltration, nanofiltration I, nanofiltration II, stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its practical implementation process is following:
1. get sunflower plate and bar is pulverized on pulverizer, its particle diameter is 1-2mm;
2. getting above-mentioned crushed material 10kg, is that 1: 4 ratio adds entry 40kg and heats in its weight ratio, and control water temperature is to boil 2 hours in 70-80 ℃ the scope;
3. the material after hot water being boiled places in the suction filtration groove that is provided with filter cloth, washes 3-4 time repeatedly with 40-50 ℃ warm water, carries out suction filtration with negative-pressure gas simultaneously, gets slag to reach to anhydrate;
4. above-mentioned material behind the washing suction filtration is placed on the squeezing machine and squeeze, with the moisture in the further removal material;
5. the material 10kg after will squeezing 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;
6. homogenate is placed in the suction filtration groove that is provided with filter cloth, wash 3-5 time repeatedly, carry out suction filtration with negative-pressure gas simultaneously, remove slag to reach receipts liquid with 50-60 ℃ warm water;
Ultrafiltration be with above-mentioned homogenate through liquid behind the suction 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;
8. 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 low-ester pectin first product;
10. stirring into glue is above-mentioned low-ester pectin first product to be placed in the agitator and by weight 1: 1.5 add 98% ethanol, stirs and promptly forms gel in 0.5 hour;
11. being the gel with low-ester pectin, press filtration places the gelling thing that under the pressure of 0.2Mpa, makes low-ester pectin in the plate-and-frame filter press;
12. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
13. above-mentioned gelling thing is carried out spraying drying, is prepared into the low-ester pectin dry product; Promptly got the low-ester pectin finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 1.
A kind of ultra-filtration equipment (referring to Fig. 1) of the embodiment of the invention 1; It is to be objective for implementation with the technical requirements of satisfying ultrafiltration operation in the present invention extracts low-ester pectin from sunflower plate and bar the method steps, with the ultrafiltration operation as a unit and designing independently.This ultrafiltration operation requires: with above-mentioned homogenate through liquid behind the suction filtration in can the rolling ultra-filtration equipment of the above material of molecular weight cut-off 10000 dalton, under the pressure of 0.01-0.02MPA, adopt cross flow filter to remove waste residue and get just and filtrate; Therefore the embodiment of the invention 1 described ultra-filtration equipment is by an airtight housing 2; Its two ends are the arcuate structure of evagination; Housing 2 lumen centers have in a tubular form a ultrafiltration body stem stem 3; Ultra-filtration membrane 5 in a tubular form of the outer surface suit of ultrafiltration body stem stem 3; Ultra-filtration membrane 5 is a tubular membrane; Each button of its two ends is stifled to have a ultrafiltration body plug 4,1 corresponding position in the upper end of housing 2 and input tube to establish a concentrated discharge conection 6 that communicates with ultrafiltration body stem stem 3 inner chambers.The bottom of housing 3 is provided with the drainage reuse tube stub 7 that communicates with cavity between the housing 2 with ultra-filtration membrane 5 outsides, the backwash tube joint constitutes the embodiment of the invention 1 described a kind of ultra-filtration equipment more than 8. structure respectively.
Embodiment 2:
A kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 2; Comprise the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter, carry out hot water then and boil, wash suction filtration, squeezing and anhydrate and get slag, mix homogenate, suction filtration, ultrafiltration, nanofiltration I, nanofiltration II, stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its practical implementation process is following:
1. get sunflower plate and bar is pulverized on pulverizer, its particle diameter is 1-2mm;
2. getting above-mentioned crushed material 10kg, is that 1: 4.5 ratio adds entry 45kg and heats in its weight ratio, and control water temperature is to boil 1.5 hours in 80-90 ℃ the scope;
3. the material after hot water being boiled places in the suction filtration groove that is provided with filter cloth, washes 4-5 time repeatedly with 50-60 ℃ warm water, carries out suction filtration with negative-pressure gas simultaneously, gets slag to reach to anhydrate;
4. above-mentioned material behind the washing suction filtration is placed on the squeezing machine and squeeze, with the moisture in the further removal material;
5. the material 10kg after will squeezing 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;
6. homogenate is placed in the suction filtration groove that is provided with filter cloth, wash 3-5 time repeatedly, carry out suction filtration with negative-pressure gas simultaneously, remove slag to reach receipts liquid with 50-60 ℃ warm water;
Ultrafiltration be with above-mentioned homogenate through liquid behind the suction 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;
8. 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 low-ester pectin first product;
10. stirring into glue is above-mentioned low-ester pectin first product to be placed in the agitator and by weight 1: 1.8 add 90% ethanol, stirs and promptly forms gel in 1 hour;
11. being the gel with low-ester pectin, press filtration places the gelling thing that under the pressure of 0.25Mpa, makes low-ester pectin in the plate-and-frame filter press;
12. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
13. above-mentioned gelling thing is carried out spraying drying, is prepared into the low-ester pectin dry product; Promptly got the low-ester pectin finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 2.
A kind of ultra-filtration equipment (referring to Fig. 2) of the embodiment of the invention 2; It is to be objective for implementation with the technical requirements of satisfying ultrafiltration operation in the present invention extracts low-ester pectin from sunflower plate and bar the method steps, with the ultrafiltration operation as a unit and designing independently.The ultrafiltration process requirements: the above homogenate after filtration through the liquid in the can MWCO 10,000 Daltons or more substances ultrafiltration device volumes in the 0.02-0.03MPA under the pressure of cross-flow filtration to remove residue was beginning of the filtrate ; Therefore, this embodiment of the ultrafiltration apparatus described in Example 2 is constituted by an ultrafiltration unit, the present invention is described in Example 2 of the ultrafiltration unit is a sealed housing 2, which both ends of the convex arcuate structure, the housing 2 has a tubular central cavity of the body of the stem 3 ultrafiltration, ultrafiltration outer body surface of the stem 3 is set a tubular membrane 5, the membrane 5 is a roll film, the ends of The buckle has an ultrafiltration body blocking plug 4, the upper end of the housing 2 with a corresponding input tube and ultrafiltration Office, located a body cavity core columns three interlinked concentrate output tube connector 6, also has an enrichment cycle storage tank 9, and a circulating pressurized concentrate pump 10, concentrate circulating pressurized input of the pump 10 circulating concentrate storage tank 9 through a pipe connected to the output terminal by concentration of the circulating pressurized inlet pipe 11 and the chamber body are connected through ultrafiltration .The bottom of housing 3 is provided with the reuse tube stub 7 that communicates with cavity between the housing 2 with ultra-filtration membrane 5 outsides, the backwash tube joint constitutes the embodiment of the invention 2 described a kind of ultra-filtration equipment more than 8. a structure respectively.
Embodiment 3:
A kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 3; Comprise the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter, carry out hot water then and boil, wash suction filtration, squeezing and anhydrate and get slag, mix homogenate, suction filtration, ultrafiltration, nanofiltration I, nanofiltration II, stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its practical implementation process is following:
1. get sunflower plate and bar is pulverized on pulverizer, its particle diameter is 1-2mm;
2. getting above-mentioned crushed material 10kg, is that 1: 5 ratio adds entry 50kg and heats in its weight ratio, and control water temperature is to boil 1 hour in 90-100 ℃ the scope;
3. the material after hot water being boiled places in the suction filtration groove that is provided with filter cloth, washes 3-4 time repeatedly with 45-55 ℃ warm water, carries out suction filtration with negative-pressure gas simultaneously, gets slag to reach to anhydrate;
4. above-mentioned material behind the washing suction filtration is placed on the squeezing machine and squeeze, with the moisture in the further removal material;
5. the material 10kg after will squeezing 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;
6. homogenate is placed in the suction filtration groove that is provided with filter cloth, wash 3-5 time repeatedly, carry out suction filtration with negative-pressure gas simultaneously, remove slag to reach receipts liquid with 50-60 ℃ warm water;
Ultrafiltration be with above-mentioned homogenate through liquid behind the suction 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;
8. 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 low-ester pectin first product;
10. stirring into glue is above-mentioned low-ester pectin first product to be placed in the agitator and by weight 1: 2 add 85% ethanol, stirs and promptly forms gel in 0.5 hour;
11. being the gel with low-ester pectin, press filtration places the gelling thing that under the pressure of 0.3Mpa, makes low-ester pectin in the plate-and-frame filter press;
12. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
13. above-mentioned gelling thing is carried out spraying drying, is prepared into the low-ester pectin dry product; Promptly got the low-ester pectin finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 3.
A kind of ultra-filtration equipment (referring to Fig. 2) of the embodiment of the invention 3; It is to be objective for implementation with the technical requirements of satisfying ultrafiltration operation in the present invention extracts low-ester pectin from sunflower plate and bar the method steps, with the ultrafiltration operation as a unit and designing independently.The ultrafiltration process requirements: the above homogenate after filtration through the liquid in the can MWCO 10,000 Daltons or more substances ultrafiltration device volumes in the 0.03-0.04MPA under the pressure of cross-flow filtration to remove residue was beginning of the filtrate ; Therefore, this embodiment of the ultrafiltration apparatus described in Example 3 is constituted by an ultrafiltration unit, the present invention is described in Example 3 of the ultrafiltration unit is a sealed housing 2, which both ends of the convex arcuate structure, the housing 2 has a tubular central cavity of the body of the stem 3 ultrafiltration, ultrafiltration outer body surface of the stem 3 is set a tubular membrane 5, the membrane 5 is a roll film, the ends of The buckle has an ultrafiltration body blocking plug 4, the upper end of the housing 2 with a corresponding input tube and ultrafiltration Office, located a body cavity core columns three interlinked concentrate output tube connector 6, also has an enrichment cycle storage tank 9, and a circulating pressurized concentrate pump 10, concentrate circulating pressurized input of the pump 10 circulating concentrate storage tank 9 through a pipe connected to the output terminal by concentration of the circulating pressurized inlet pipe 11 and the chamber body are connected through ultrafiltration .The bottom of housing 3 is provided with the reuse tube stub 7 that communicates with cavity between the housing 2 with ultra-filtration membrane 5 outsides, the backwash tube joint constitutes the embodiment of the invention 3 described a kind of ultra-filtration equipment more than 8. a structure respectively.
Embodiment 4:
A kind of method of from sunflower plate and bar, extracting low-ester pectin of wood inventive embodiments 4; Comprise the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter, carry out hot water then and boil, wash suction filtration, squeezing and anhydrate and get slag, mix homogenate, suction filtration, ultrafiltration, nanofiltration I, nanofiltration II, stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its practical implementation process is following:
1. get sunflower plate and bar is pulverized on pulverizer, its particle diameter is 1-2mm;
2. getting above-mentioned crushed material 10kg, is that 1: 5.5 ratio adds entry 55kg and heats in its weight ratio, and control water temperature is to boil 1.5 hours in 85-95 ℃ the scope;
3. the material after hot water being boiled places in the suction filtration groove that is provided with filter cloth, washes 4-5 time repeatedly with 40-50 ℃ warm water, carries out suction filtration with negative-pressure gas simultaneously, gets slag to reach to anhydrate;
4. above-mentioned material behind the washing suction filtration is placed on the squeezing machine and squeeze, with the moisture in the further removal material;
5. the material 10kg after will squeezing 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;
6. homogenate is placed in the suction filtration groove that is provided with filter cloth, wash 3-5 time repeatedly, carry out suction filtration with negative-pressure gas simultaneously, remove slag to reach receipts liquid with 50-60 ℃ warm water;
Ultrafiltration be with above-mentioned homogenate through liquid behind the suction 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;
8. 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 0.10.12MPA, 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 low-ester pectin first product;
10. stirring into glue is above-mentioned low-ester pectin first product to be placed in the agitator and by weight 1: 2.2 add 80% ethanol, stirs and promptly forms gel in 1 hour;
11. being the gel with low-ester pectin, press filtration places the gelling thing that under the pressure of 0.25Mpa, makes low-ester pectin in the plate-and-frame filter press;
12. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
13. above-mentioned gelling thing is carried out spraying drying, is prepared into the low-ester pectin dry product; Promptly got the low-ester pectin finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 4.
A kind of ultra-filtration equipment (referring to Fig. 2) of the embodiment of the invention 4; It is to be objective for implementation with the technical requirements of satisfying ultrafiltration operation in the present invention extracts low-ester pectin from sunflower plate and bar the method steps, with the ultrafiltration operation as a unit and designing independently.The ultrafiltration process requirements: the above homogenate after filtration through the liquid in the can MWCO 10,000 Daltons or more substances ultrafiltration device volumes in the 0.04-0.05MPA under the pressure of cross-flow filtration to remove residue was beginning of the filtrate ; Therefore, this embodiment of the ultrafiltration apparatus described in Example 4 is constituted by an ultrafiltration unit, the present invention is described in Example 4 of the ultrafiltration unit is a sealed housing 2, which both ends of the convex arcuate structure, the housing 2 has a tubular central cavity of the body of the stem 3 ultrafiltration, ultrafiltration outer body surface of the stem 3 is set a tubular membrane 5, the membrane 5 is a roll film, the ends of The buckle has an ultrafiltration body blocking plug 4, the upper end of the housing 2 with a corresponding input tube and ultrafiltration Office, located a body cavity core columns three interlinked concentrate output tube connector 6, also has an enrichment cycle storage tank 9, and a circulating pressurized concentrate pump 10, concentrate circulating pressurized input of the pump 10 circulating concentrate storage tank 9 through a pipe connected to the output terminal by concentration of the circulating pressurized inlet pipe 11 and the chamber body are connected through ultrafiltration .The bottom of housing 3 is provided with the reuse tube stub 7 that communicates with cavity between the housing 2 with ultra-filtration membrane 5 outsides, the backwash tube joint constitutes the embodiment of the invention 4 described a kind of ultra-filtration equipment more than 8. a structure respectively.
Embodiment 5:
A kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 5; Comprise the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter, carry out hot water then and boil, wash suction filtration, squeezing and anhydrate and get slag, mix homogenate, suction filtration, ultrafiltration, nanofiltration I, nanofiltration II, stir into glue, press filtration, distillation reuse, spraying drying and pulverizing and process pure article.Its practical implementation process is following:
1. get sunflower plate and bar is pulverized on pulverizer, its particle diameter is 1-2mm;
2. getting above-mentioned crushed material 10kg, is that 1: 6 ratio adds entry 60kg and heats in its weight ratio, and control water temperature is to boil 2 hours in 75-85 ℃ the scope;
3. the material after hot water being boiled places in the suction filtration groove that is provided with filter cloth, washes 4-5 time repeatedly with 50-60 ℃ warm water, carries out suction filtration with negative-pressure gas simultaneously, gets slag to reach to anhydrate;
4. above-mentioned material behind the washing suction filtration is placed on the squeezing machine and squeeze, with the moisture in the further removal material;
5. the material 10kg after will squeezing 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;
6. homogenate is placed in the suction filtration groove that is provided with filter cloth, wash 3-5 time repeatedly, carry out suction filtration with negative-pressure gas simultaneously, remove slag to reach receipts liquid with 50-60 ℃ warm water;
Ultrafiltration be with above-mentioned homogenate through liquid behind the suction 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;
8. 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, under the pressure of 0.14-0.15MPA, carry out the secondary nanofiltration and remove impurity, its trapped substance is the low-ester pectin first product;
10. stirring into glue is above-mentioned low-ester pectin first product to be placed in the agitator and by weight 1: 2.5 add 70% ethanol, stirs and promptly forms gel in 0.5 hour;
11. being the gel with low-ester pectin, press filtration places the gelling thing that under the pressure of 0.2Mpa, makes low-ester pectin in the plate-and-frame filter press;
12. the solution that above-mentioned press filtration is gone out distills, to reach recycling ethanol;
13. above-mentioned gelling thing is carried out spraying drying, is prepared into the low-ester pectin dry product; Promptly got the low-ester pectin finished product through pulverizing 80 mesh sieves.It more than is a kind of method of from sunflower plate and bar, extracting low-ester pectin of the embodiment of the invention 5.
A kind of ultra-filtration equipment (referring to Fig. 2) of the embodiment of the invention 5; It is to be objective for implementation with the technical requirements of satisfying ultrafiltration operation in the present invention extracts low-ester pectin from sunflower plate and bar the method steps, with the ultrafiltration operation as a unit and designing independently.The ultrafiltration process requirements: the above homogenate after filtration through the liquid in the can MWCO 10,000 Daltons or more substances ultrafiltration device volumes in the 0.03-0.04MPA under the pressure of cross-flow filtration to remove residue was beginning of the filtrate ; Therefore, this embodiment of the ultrafiltration apparatus described in Example 5 is constituted by an ultrafiltration unit, the present invention is described in Example 5 of the ultrafiltration apparatus is composed of a sealed housing 2, which both ends of the convex arcuate structure, the housing 2 has a tubular central cavity of the body of the stem 3 ultrafiltration, ultrafiltration outer body surface of the stem 3 is set a tubular membrane 5, the membrane 5 is a roll film, the ends of The buckle has an ultrafiltration body blocking plug 4, the upper end of the housing 2 with a corresponding input tube and ultrafiltration Office, located a body cavity core columns three interlinked concentrate output tube connector 6, also has an enrichment cycle storage tank 9, and a circulating pressurized concentrate pump 10, concentrate circulating pressurized input of the pump 10 circulating concentrate storage tank 9 through a pipe connected to the output terminal by concentration of the circulating pressurized inlet pipe 11 and the chamber body are connected through ultrafiltration .The bottom of housing 3 is provided with the reuse tube stub 7 that communicates with cavity between the housing 2 with ultra-filtration membrane 5 outsides, the backwash tube joint constitutes the embodiment of the invention 5 described a kind of ultra-filtration equipment more than 8. a structure respectively.
Claims (10)
1. method of from sunflower plate and bar, extracting low-ester pectin; It is characterized in that described method comprises the steps: that successively it is 1-2mm that sunflower plate and bar are crushed to particle diameter; Be 1 with dry material in its weight ratio then: the ratio of 4-6 adds entry and the control water temperature of heating is to boil 1-2 hour in 70-100 ℃ the scope; Material after hot water boiled places in the suction filtration groove that is provided with filter cloth; Warm water with 40-60 ℃ washes 3-5 time repeatedly; Carry out suction filtration with negative-pressure gas simultaneously, squeezing is anhydrated and is got slag; Mix homogenate; Suction filtration; Ultrafiltration; Nanofiltration I; Nanofiltration II; Stir into glue; Press filtration; The distillation reuse; Spraying drying and pulverizing and process pure article.
2. the method for from sunflower plate and bar, extracting low-ester pectin according to claim 1; It is characterized in that described mixing homogenate is that the material after the squeezing 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 sunflower plate and bar, extracting low-ester pectin according to claim 1 and 2; It is characterized in that described ultrafiltration be with above-mentioned homogenate through behind the suction filtration 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.
4. the method for from sunflower plate and bar, extracting low-ester 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.
5. the method for from sunflower plate and bar, extracting low-ester 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 low-ester pectin first product.
6. the method for from sunflower plate and bar, extracting low-ester pectin according to claim 1; It is characterized in that the described glue that stirs into is to place above-mentioned low-ester pectin first product in the agitator and by weight 1: 1.5-2.5 adds 70-98% ethanol, stirs and promptly forms gel in 0.5-1 hour.
7. the method for from sunflower plate and bar, extracting low-ester pectin according to claim 1 is characterized in that described press filtration is that gel with low-ester pectin places the gelling thing that under the pressure of 0.2-0.3Mpa, makes low-ester pectin in the plate-and-frame filter press.
8. the described special-purpose ultra-filtration equipment of method that from sunflower plate and bar, extracts low-ester pectin of a claim 1; Comprise at least one housing and the unit of the adapter of intracavity inter-connection with it; It is characterized in that described housing inner chamber is provided with an airtight tubulose ultrafiltration body; The upper end of ultrafiltration body is provided with 2 adapters of inner chamber connection with it, and the tubular wall of ultrafiltration body is provided with can allow that medium gets into the ultra-filtration membrane of cavity between ultrafiltration body and the housing from its inner chamber.
9. ultra-filtration equipment according to claim 8 is characterized in that an adapter of described ultrafiltration body upper end also is provided with a hold-up vessel and force (forcing) pump, and the input terminus of force (forcing) pump is connected with hold-up vessel, and its output terminal is connected with the ultrafiltration intracoelomic cavity.
10. according to Claim 8 or 9 described ultra-filtration equipment, it is characterized in that described housing bottom also is provided with water pipe and the valve that communicates with the housing inner chamber.
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| CN201110098612A CN102304192A (en) | 2011-04-09 | 2011-04-09 | Method for extracting low-ester pectin from sunflower heads and stems and ultrafiltration device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151445A (en) * | 2014-05-08 | 2014-11-19 | 江南大学 | Method for extracting natural low-ester pectin from sunflower heads |
| CN109125072A (en) * | 2018-07-27 | 2019-01-04 | 陈继珍 | A kind of medical instrument and its application method boiling drug |
| RU2706483C1 (en) * | 2019-03-22 | 2019-11-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный аграрный университет имени И.Т. Трубилина" | Method for production of pectin extract from sunflower clusters |
-
2011
- 2011-04-09 CN CN201110098612A patent/CN102304192A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151445A (en) * | 2014-05-08 | 2014-11-19 | 江南大学 | Method for extracting natural low-ester pectin from sunflower heads |
| CN104151445B (en) * | 2014-05-08 | 2016-08-24 | 江南大学 | A kind of method extracting natural low methoxyl pectin from sunflower plate |
| CN109125072A (en) * | 2018-07-27 | 2019-01-04 | 陈继珍 | A kind of medical instrument and its application method boiling drug |
| RU2706483C1 (en) * | 2019-03-22 | 2019-11-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный аграрный университет имени И.Т. Трубилина" | Method for production of pectin extract from sunflower clusters |
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Application publication date: 20120104 |