CN102718884B - A kind of method adopting fresh Sargassum fusiforme to extract algin - Google Patents
A kind of method adopting fresh Sargassum fusiforme to extract algin Download PDFInfo
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Abstract
The present invention relates to a kind of method adopting fresh Sargassum fusiforme to extract algin.The method step is fixation, washing, fragmentation, enzymolysis, conversion, coarse filtration, dilution, floating, the smart filter of foaming, acid out bleaching, dehydration, solid phase transformation, granulation, whole grain, oven dry.Beneficial effect of the present invention is: (1) present invention process have employed enzymolysis process, solve the problem that Sargassum fusiforme is difficult to extract algin, adopt fresh Sargassum fusiforme to be raw material production low viscosity and ultra-low viscosity algin, expand the raw material range of algin processing; (2) the calcification technology adopting acid out technical substitution traditional, improves that traditional algin calcium content is high, the shortcoming of poorly water-soluble, insoluble object height; (3) adopt and drip NaClO solution at acid out simultaneously and bleach, change traditional employing adds bleaching by chlorine gas after essence filter technique in glue, make bleaching effect better, technological operation is safer.
Description
Technical field
The present invention relates to the extracting method of algin, particularly relate to a kind of method adopting fresh Sargassum fusiforme to extract algin.
Background technology
Hizikia is in phaeophyta Sargassaceae plant, and be the economical alga resource of China's abundant, frond is tawny, and time dry, blackout, is mainly distributed in the coastlands such as Guangdong, Shandong, Fujian, Zhejiang in China, and exports to the states such as Japan.
Algin is the phaeophyta such as sea-tangle, Sargassum fusiforme, through adding the water-soluble high viscosity colloid of one that alkaline extraction goes out, comprise water-soluble alignic ammonium, sodium, sylvite, and water-fast alginic acid and calcium, iron etc. two metallic salt more than valency thereof, in general algin mainly refers to sodium alginate.In China, main use sea-tangle extracts algin as raw material, and output is about about 30,000 tons, most of as printing paste, for the dyeing and printing auxiliary of textile industry.
In prior art, most employing sea-tangle is as raw material production algin, because Sargassum fusiforme is relative to sea-tangle, cell walls is thicker, be difficult to extract algin, if extract the method that algin uses traditional laminaria production algin from Sargassum fusiforme, yield is low, Sargassum fusiforme, as a kind of marine algae resource of rich reserves, does not obtain rationalizing use.
Extract from sea-tangle in the production process of algin in prior art, adopt calcification technology, the algin produced has that calcium content is high, the shortcoming of poorly water-soluble, insoluble object height, the calcium content of algin is an important indicator, when it is as dyeing and printing auxiliary, if calcium content is high, gel can be formed, poor fluidity, be difficult to after mixing with dyestuff by dyeing filter screen, Color is poor.
Summary of the invention
In order to solve the problem, the invention provides one and utilizing Sargassum fusiforme for raw material, the method for the extraction adopting acid out technology the to replace calcification technology not algin of calcic.
Technical scheme of the present invention is:
Adopt fresh Sargassum fusiforme to extract a method for algin, the steps include:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 35-40%, formaldehyde add-on is the 10-20% of fresh Sargassum fusiforme quality, then adds fresh Sargassum fusiforme quality 1-3 tap water doubly, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, after fixation 20-24 hour, washing, the formaldehyde of removing impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 230-340u/g, and enzymolysis 6-8h at 45-55 DEG C of temperature, is then warming up to 90 DEG C, keeps 20-30min at this temperature, make enzyme deactivation;
(4) transform
Control between 60-90 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 4-7 times of hot water, add soda ash, add-on is the 4%-7% of fresh Sargassum fusiforme quality, and digestion 5-8 hour, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 30-100 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
In diluent, add flocculant solution, the quality adding flocculant solution is the 0.05-0.1 ‰ of Sargassum fusiforme quality, foams;
B. floating
Glue after foaming is left standstill 2.5-4 hour, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 200 order or 260 object screen filtrations, obtain smart filtrate;
(8) acid out bleaching
The dilute hydrochloric acid that concentration is 5-10% is slowly added in smart filtrate, the NaCIO solution simultaneously dripping available chlorine content 6%-10% is bleached, until start have throw out to produce, then 2-5h is left standstill, 5-10% dilute hydrochloric acid is slowly added toward leaving standstill in liquid, adjustment pH is 1-2, namely obtains alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 80%-85%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 65-72%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is the 8-10% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 6-8, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin.
Preferably, the compound method of described flocculant solution is:
(1) weigh flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, then add flocculation agent, fully dissolve;
(2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution.
Beneficial effect of the present invention is:
(1) present invention process have employed enzymolysis process, solves the problem that Sargassum fusiforme is difficult to extract algin, adopts fresh Sargassum fusiforme to be raw material production low viscosity and ultra-low viscosity algin, expand the raw material range of algin processing;
(2) the calcification technology adopting acid out technical substitution traditional, improves that traditional algin calcium content is high, the shortcoming of poorly water-soluble, insoluble object height;
(3) adopt and drip NaCIO solution at acid out simultaneously and bleach, change traditional employing adds bleaching by chlorine gas after essence filter technique in glue, make bleaching effect better, technological operation is safer.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
Embodiment
The present invention is described in further detail below, and a kind of method adopting fresh Sargassum fusiforme to extract algin, the steps include:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 35-40%, formaldehyde add-on is the 10-20% of fresh Sargassum fusiforme quality, then adds fresh Sargassum fusiforme quality 1-3 tap water doubly, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, after fixation 20-24 hour, washing, the formaldehyde of removing impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 230-340u/g, and enzymolysis 6-8h at 45-55 DEG C of temperature, is then warming up to 90 DEG C, keeps 20-30min at this temperature, make enzyme deactivation;
(4) transform
Control between 60-90 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 4-7 times of hot water, add soda ash, add-on is the 4%-7% of fresh Sargassum fusiforme quality, and digestion 5-8 hour, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 30-100 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
Flocculant solution is added in diluent, the quality adding flocculant solution is the 0.05-0.1 ‰ of Sargassum fusiforme quality, foam, the compound method of flocculant solution is: (1) weighs flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, add flocculation agent again, fully dissolve; (2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution;
B. floating
Glue after foaming is left standstill 2.5-4 hour, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 200 order or 260 object screen filtrations, obtain smart filtrate;
(8) acid out bleaching
The dilute hydrochloric acid that concentration is 5-10% is slowly added in smart filtrate, the NaClO solution simultaneously dripping available chlorine content 6%-10% is bleached, until start have throw out to produce, then 2-5h is left standstill, 5-10% dilute hydrochloric acid is slowly added toward leaving standstill in liquid, adjustment pH is 1-2, namely obtains alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 80%-85%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 65-72%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is the 8-10% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 6-8, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin.
Embodiment 1:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 40%, formaldehyde add-on is 20% of fresh Sargassum fusiforme quality, then adds the tap water of fresh Sargassum fusiforme quality 3 times, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, fixation is after 24 hours, and washing, removes the formaldehyde of impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 340u/g, and enzymolysis 8h at 55 DEG C of temperature, is then warming up to 90 DEG C, keeps 30min at this temperature, make enzyme deactivation;
(4) transform
Control between 90 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 7 times of hot water, add soda ash, add-on is 7% of fresh Sargassum fusiforme quality, digests 8 hours, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 100 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
Flocculant solution is added in diluent, the quality adding flocculant solution is 0.1 ‰ of Sargassum fusiforme quality, foam, the compound method of flocculant solution is: (1) weighs flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, add flocculation agent again, fully dissolve; (2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution;
B. floating
Glue after foaming is left standstill 4 hours, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 260 object screen filtration, obtains smart filtrate;
(8) acid out bleaching
In smart filtrate, slowly add the dilute hydrochloric acid that concentration is 10%, the NaClO solution simultaneously dripping available chlorine content 10% is bleached, until start have throw out to produce, then 5h is left standstill, slowly adding 10% dilute hydrochloric acid toward leaving standstill in liquid, regulating pH to be 2, namely obtaining alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 85%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 72%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is 10% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 8, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin.
Embodiment 2:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 35%, formaldehyde add-on is 10% of fresh Sargassum fusiforme quality, then adds the tap water of fresh Sargassum fusiforme quality 1 times, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, fixation is after 20 hours, and washing, removes the formaldehyde of impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 230u/g, and enzymolysis 6h at 45 DEG C of temperature, is then warming up to 90 DEG C, keeps 20min at this temperature, make enzyme deactivation;
(4) transform
Control between 60 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 4 times of hot water, add soda ash, add-on is 4%% of fresh Sargassum fusiforme quality, digests 5 hours, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 30 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
Flocculant solution is added in diluent, the quality adding flocculant solution is 0.05 ‰ of Sargassum fusiforme quality, foam, the compound method of flocculant solution is: (1) weighs flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, add flocculation agent again, fully dissolve; (2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution;
B. floating
Glue after foaming is left standstill 2.5 hours, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 200 object screen filtration, obtains smart filtrate;
(8) acid out bleaching
In smart filtrate, slowly add the dilute hydrochloric acid that concentration is 5%, the NaClO solution simultaneously dripping available chlorine content 6% is bleached, until start have throw out to produce, then 2h is left standstill, slowly adding 5% dilute hydrochloric acid toward leaving standstill in liquid, regulating pH to be 1, namely obtaining alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 80%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 65%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is 8% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 6, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin.
Embodiment 3:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 38%, formaldehyde add-on is 15% of fresh Sargassum fusiforme quality, then adds the tap water of fresh Sargassum fusiforme quality 2 times, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, fixation is after 22 hours, and washing, removes the formaldehyde of impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 300u/g, and enzymolysis 7h at 50 DEG C of temperature, is then warming up to 90 DEG C, keeps 25min at this temperature, make enzyme deactivation;
(4) transform
Control between 70 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 6 times of hot water, add soda ash, add-on is 6% of fresh Sargassum fusiforme quality, digests 7 hours, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 50 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
Flocculant solution is added in diluent, the quality adding flocculant solution is 0.08 ‰ of Sargassum fusiforme quality, foam, the compound method of flocculant solution is: (1) weighs flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, add flocculation agent again, fully dissolve; (2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution;
B. floating
Glue after foaming is left standstill 3 hours, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 260 object screen filtration, obtains smart filtrate;
(8) acid out bleaching
In smart filtrate, slowly add the dilute hydrochloric acid that concentration is 8%, the NaClO solution simultaneously dripping available chlorine content 8% is bleached, until start have throw out to produce, then 4h is left standstill, slowly adding 8% dilute hydrochloric acid toward leaving standstill in liquid, regulating pH to be 2, namely obtaining alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 82%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 70%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is 9% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 7, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin.
Claims (1)
1. adopt fresh Sargassum fusiforme to extract a method for algin, the steps include:
(1) fixation, washing
In fixation pond, add the formaldehyde that concentration is 35-40%, formaldehyde add-on is the 10-20% of fresh Sargassum fusiforme quality, then adds fresh Sargassum fusiforme quality 1-3 tap water doubly, then fresh Sargassum fusiforme is thrown uniformly in fixation pond, after fixation 20-24 hour, washing, the formaldehyde of removing impurity and surplus;
(2) broken
Sargassum fusiforme after washing is carried out fragmentation;
(3) enzymolysis
Fresh Sargassum fusiforme after fragmentation adds the citric acid solution of 1mol/L, and make soak solution pH be 4.8, cellulase consumption is 230-340u/g, and enzymolysis 6-8h at 45-55 DEG C of temperature, is then warming up to 90 DEG C, keeps 20-30min at this temperature, make enzyme deactivation;
(4) transform
Control between 60-90 DEG C by the Sargassum fusiforme temperature after enzymolysis, complement to 4-7 times of hot water, add soda ash, add-on is the 4%-7% of fresh Sargassum fusiforme quality, and digestion 5-8 hour, obtains glue;
(5) coarse filtration, dilution
Glue, through 40 order coarse filtration, dilutes filtrate, and the solution quality after dilution is 30-100 times of Sargassum fusiforme quality;
(6) foam floating
A. foam
In diluent, add flocculant solution, the quality adding flocculant solution is the 0.05-0.1 ‰ of Sargassum fusiforme quality, foams;
B. floating
Glue after foaming is left standstill 2.5-4 hour, after glue clarification, obtains clear liquid;
(7) essence filter
Clear glue solution after floating is passed through upper strata 120 order successively, and lower floor 200 order or 260 object screen filtrations, obtain smart filtrate;
(8) acid out bleaching
The dilute hydrochloric acid that concentration is 5-10% is slowly added in smart filtrate, the NaClO solution simultaneously dripping available chlorine content 6%-10% is bleached, until start have throw out to produce, then 2-5h is left standstill, 5-10% dilute hydrochloric acid is slowly added toward leaving standstill in liquid, adjustment pH is 1-2, namely obtains alginic acid throw out;
(9) dewater
Dewatered by alginic acid throw out, the moisture content that first time controls alginic acid throw out is 80%-85%, and then carry out second dehydration, the moisture content of second dehydration alginic acid throw out is 65-72%;
(10) solid phase transformation
Alginic acid throw out and soda ash are neutralized, soda ash consumption is the 8-10% of alginic acid throw out weight, with 5 minutes in stirring, in N-process, regulates caustic dosage, makes material pH value be 6-8, obtain algin;
(11) granulation, whole grain
(12) dry
Dried by algin after granulation, whole grain, moisture is no more than 15%, obtains algin;
The compound method of described flocculant solution is:
(1) weigh flocculation agent, add the water that quality is flocculation agent quality 100 times, then add the glacial acetic acid with flocculation agent equal in quality, stir, then add flocculation agent, fully dissolve;
(2) flocculation agent dissolved is filtered in diluting tank by 18 order mesh bags, adds 10 times of water and rush rare, obtain flocculant solution.
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| CN103172761B (en) * | 2013-04-22 | 2015-03-18 | 青岛贝尔特生物科技有限公司 | Energy-saving and emission-reducing production method of high-quality sodium alginate |
| CN103360509B (en) * | 2013-07-16 | 2016-08-10 | 山东洁晶集团股份有限公司 | Alginic acid and the method for alginic acid salt is prepared for raw material with fresh sargassum |
| CN105504086B (en) * | 2015-12-09 | 2018-07-20 | 江苏明月海洋生物科技有限公司 | A kind of preparation method of food-grade calcium alginate |
| CN110590970B (en) * | 2019-09-23 | 2021-10-15 | 青岛明月海藻集团有限公司 | Preparation method and application of brown algae polysaccharide rich in fucoidin and sodium alginate |
| CN110922501A (en) * | 2019-10-24 | 2020-03-27 | 浙江工业大学 | Process for extracting sodium alginate by using ultrasonic-assisted complex enzyme |
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| CN1252954A (en) * | 1998-11-06 | 2000-05-17 | 荣成市神通海洋生物公司 | Process for preparing liquid extract of kelp |
| CN101585890A (en) * | 2008-06-20 | 2009-11-25 | 青岛聚大洋海藻工业有限公司 | Method for preparing sodium alginate from kelp |
| CN101983974A (en) * | 2010-10-08 | 2011-03-09 | 青岛聚大洋海藻工业有限公司 | Extracting and processing technology of food additive G-type alginate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1252954A (en) * | 1998-11-06 | 2000-05-17 | 荣成市神通海洋生物公司 | Process for preparing liquid extract of kelp |
| CN101585890A (en) * | 2008-06-20 | 2009-11-25 | 青岛聚大洋海藻工业有限公司 | Method for preparing sodium alginate from kelp |
| CN101983974A (en) * | 2010-10-08 | 2011-03-09 | 青岛聚大洋海藻工业有限公司 | Extracting and processing technology of food additive G-type alginate |
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Address after: 266400 Shandong Province, Qingdao city Huangdao District Feiyu Road No. 118 Applicant after: QINGDAO JUDAYANG ALGAE INDUSTRY GROUP CO., LTD. Address before: 266000, No. two, 17 West Road, Jiaonan, Shandong, Shanghai, Qingdao Applicant before: Qingdao Gather Great Ocean Seaweed Industry Co., Ltd. |
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