CN105504086A - Preparation method of food-grade calcium alginate - Google Patents
Preparation method of food-grade calcium alginate Download PDFInfo
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- CN105504086A CN105504086A CN201510906222.4A CN201510906222A CN105504086A CN 105504086 A CN105504086 A CN 105504086A CN 201510906222 A CN201510906222 A CN 201510906222A CN 105504086 A CN105504086 A CN 105504086A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a preparation method of food-grade calcium alginate. The preparation method comprises the following steps: embathing brown alga, and adding sodium carbonate for digesting the brown alga to extract alginic acid; diluting and filtering the product; carrying out air air floatation separation; carrying out fine filtration; introducing chlorine gas for bleaching; adding calcium chloride solution to enable water-soluble sodium alginate to be converted into water-insoluble calcium alginate; washing; carrying out dehydration; drying; grinding. According to the preparation method, kieselguhr is added for fine filtration, so that harmful substances such as pigment, heavy metal and the like are removed; the produced calcium alginate meets the food grade requirements and is widely used in the industries such as medicines, food and daily use chemical.
Description
Technical field
The invention belongs to the technical field preparing alginate calcium, particularly a kind of preparation method of food grade alginate calcium.
Background technology
Alginates is a kind of natural polysaccharide extracted from the brown algas such as sea-tangle, sargassun, bulk kelp, bladder wrack, conventional alginates is the water miscible seaweed gel such as sodium alginate, potassium alginate, and alginate calcium is a kind of water-insoluble alginates, there is good edible safety, can be used as gelling thickener, calsium supplement etc., it has been put into foodstuff additive in countries such as Japan, Russia, European Union, the U.S., within 2016, rises domesticly to be applied as foodstuff additive by permission alginate calcium.Utilize alginate calcium to meet water-dispersion, add the characteristic that alkali or salt dissolves and be widely used in the industries such as medicine, food, chemical industry, play the function such as suspending, thick stabilization, emulsification, film forming, slowly-releasing of aqueous colloidal.
Domestic using the intermediate product of calcification technique as alginate calcium product at present, product heavy metal, inorganic salt are residual high, can only be used for industry; The alginate manufacturing enterprise being abroad representative with Japanese FMC adopts Lalgine in acidization technique to prepare alginate calcium, and product purity is high, but technique is more loaded down with trivial details and produce the waste liquids such as sour water.
The people such as Chen Hong disclose a kind of production method of high-quality calcium alginate in patent (CN103333271A).This production method is that " sodium alginate prepared by brown alga produces Lalgine through acidifying; Lalgine adopts the complex cleaning and washing agent of ethanol, propyl alcohol, ethyl acetate and water composition to clean 2-4 time; Lalgine after cleaning is that medium and calcium source neutralization reaction occurs are made alginate calcium with water ".This preparation method is similar to the acidization abroad adopted, and introduce other organic solvents in the reaction, make finished product reach food quality requirement, but technique is loaded down with trivial details, cost is high.
The people such as Liu Junxia disclose a kind of preparation method of alginate calcium in patent (CN102977224A).This preparation method for " brown alga is embathed, add soda ash digestion, add calcium preparation calcification, acidifying after extract Lalgine; Wash and dewater; Granulation; Freezing and pulverizing; Add calcium preparation calcification; Dehydration; Dry; Pulverize ".The method is at the sodium alginate will extracted from brown alga, and after adding calcium preparation calcification, Lalgine is extracted in acidifying, and again add calcium preparation calcification, dehydration, drying after then granulation, freezing and pulverizing, technique is more complicated, cost is higher.
Summary of the invention
The present invention, by adding diatomite adsorption drainage in the sodium alginate soln after dissolved air flotation, removes the objectionable impurities such as pigment, heavy metal; In sodium alginate and calcium chloride solution mixing process, pass into a certain amount of chlorine, not only technique is simple, and production cost is low, effectively can suppress the molecule crosslinked structure cooperating microorganisms of alginate calcium and improve product color simultaneously, reaching the requirement of food safety.
For achieving the above object, the present invention adopts following technical proposals to be achieved: a kind of preparation method of food grade alginate calcium, it is characterized in that, step is: 1) sodium alginate preparation: brown alga is embathed, add that sodium carbonate carries out digestion reaction, thin up, filtration obtain clarifying sodium alginate soln; 2) sodium alginate purifying: add diatomite adsorption drainage in sodium alginate soln; 3) filter: sodium alginate and diatomaceous mixed solution essence are filtered and obtains clarifying glue; 4) glue bleaching: pass into chlorine, bleaching glue; 5) alginate calcium preparation: add calcium chloride solution in above-mentioned clarification glue, makes water miscible sodium alginate change water-insoluble calcium alginate gel into and concentrates precipitation; 6) post-processed: washing, dehydration, dry, pulverizing, obtain food grade alginate calcium.
Further, described step 1) in brown alga be one or more in sea-tangle, bulk kelp, bladder wrack, sargassun.
Further, described step 1) in digestion reaction temperature be 40-60 DEG C, reaction times 4-8h.
Further, described step 1) in sodium carbonate add-on be brown alga quality 20-30%.
Further, described step 2) in diatomaceously add the 1-5 ‰ that quality is sodium alginate soln quality.
Further, described step 3) the middle smart filter type filtering employing press filtration or vacuum filtration.
Further, described step 4) in the amount of chlorine that passes into be 1-4m
3/ h.
Further, described step 5) in the mass concentration of calcium chloride solution be 10-15%, the amount adding calcium chloride solution is the 2-4% of glue volume.
Further, described step 6) in, dewater to Han Shui Liang≤70%, be dried to Han Shui Liang≤15%.
Compared with prior art, advantage of the present invention and positively effect are:
1, the present invention is by adding diatomite, has adsorbed the impurity such as the pigment in alginate solution, heavy metal, improves the quality of finished product alginate calcium.Sodium alginate after diatomite purifying, can directly adopt calcification technique, be converted into alginate calcium, shorten technical process, reduces production cost, reduces the discharge of waste liquid.
2, the present invention passes into chlorine in sodium alginate soln, reduces alginate calcium and causes because of microbiological deterioration shape of product to change, and ensure that in finished product, microbiological indicator meets food grade requirement.Simultaneously due to the bleaching action of chlorine, obviously can improve the color and luster of finished product, improve product quality.
Embodiment
The invention provides a kind of preparation method of food grade alginate calcium, step is as follows:
1) sodium alginate is prepared: add the water logging being equivalent to dry brown alga weight 6-10 times and wash brown alga; Add the sodium carbonate of dry brown alga quality 20-30%, carry out digestion reaction 4-8h at 40-60 DEG C, obtain sodium alginate; With being equivalent to dry brown alga quality 80-120 water dilution glue doubly; Dissolved air flotation obtains clarifying sodium alginate soln; Wherein said brown alga is one or more in sea-tangle, bulk kelp, bladder wrack, sargassun.
2) sodium alginate purifying: add diatomite adsorption drainage in above-mentioned clarification sodium alginate soln; Describedly diatomaceously add the 1-5 ‰ that quality is sodium alginate soln quality, diatomite order number is 50-200 order (model is preferably emerging brightness SY-RS600).Add diatomite and can adsorb the impurity such as pigment, heavy metal in alginate solution, improve the quality of finished product alginate calcium, meet food grade standard.
3) filter: sodium alginate and diatomaceous mixed solution are carried out essence and filter, remove and adsorbed the diatomite of impurity, obtain clarifying glue; Adopt the mode such as press filtration or vacuum filtration to carry out essence to filter.
4) glue bleaching: pass into 1-4m in above-mentioned clarification glue
3/ h chlorine; Glue is bleached, for improving the color and luster of finished product, reducing alginate calcium and causing because of microbiological deterioration shape of product to change, and ensure that in finished product, microbiological indicator meets food grade requirement.
5) alginate calcium preparation: add calcium chloride solution in the glue after above-mentioned bleaching, make water miscible sodium alginate change water-insoluble calcium alginate gel into and concentrate precipitation, the amount adding calcium chloride solution is the 2-4% of glue volume, and the mass concentration of calcium chloride solution is 10-15%.
6) post-processed: add water washing calcium alginate gel, dehydration, to containing water amount≤70%, is dried to containing water amount≤15%, and be crushed to granularity 100% and cross 100 mesh sieves, 70% crosses 200 mesh sieves.Obtain end product food grade alginate calcium.
Raw material used in method of the present invention and auxiliary agent all adopt food grade standard.
End product alginate calcium prepared by the present invention is creamy white, lead content≤4mg/kg, arsenic content≤2mg/kg, cl content≤0.1mg/kg, microbial count≤1000cfu/g, CaO content 12.0-13.0%, meets food grade standard, can be used for the high-grade products productions such as medicine, food, daily use chemicals, improve added value of product.
Embodiment 1
The preparation method of alginate calcium of the present invention comprises the following steps:
1, sea-tangle is embathed and digests: 12h is washed in sea-tangle water logging, then adds the sodium carbonate of dry sea-tangle quality 20%, after 40 DEG C of insulation digestion 5h, is smashed by sea-tangle by mechanical stirring; Add the water dilution glue being equivalent to dry sea-tangle raw material weight 100 times, after dissolved air flotation, obtain the sodium alginate soln clarified;
2, sodium alginate purifying: the diatomite adding solution quality 1.3 ‰ in sodium alginate soln, diatomite order number is 100 orders (model is emerging brightness SY-RS600);
3, filter: what be separated with diatomaceous mixed solution by sodium alginate by Plate Filtration arrives clarification glue;
4, bleach: in glue, pass into 1m
3/ h chlorine, bleaching glue.
5, alginate calcium preparation: add the calcium chloride solution that mass concentration is 13% in the glue after above-mentioned bleaching, the amount of calcium chloride solution is 2.3% of glue volume, and water miscible Lalgine solution is become water-insoluble calcium alginate gel;
6, post-processed: add water washing calcium alginate gel, and use expeller device to dewater to water content < 70%;
7, adopt boiling-bed drying to dry alginate calcium to Han Shui Liang≤15%, be crushed to granularity 100% and cross 100 orders, 70% crosses 200 orders, obtains alginate calcium product.
The experimental result of gained alginate calcium product: moisture content 11.2%, total plate count≤1000cfu/g, mould, yeast sum≤100cfu/g, lead content 3.8mg/kg, arsenic 1.9mg/kg, cl content 0.09mg/kg, CaO content 12.1%.
Embodiment 2
1, sea-tangle is embathed and digests: 12h is washed in sea-tangle water logging, then adds the sodium carbonate of dry sea-tangle quality 23%, after 50 DEG C of insulation digestion 4h, is smashed by sea-tangle by mechanical stirring; Add the water dilution glue being equivalent to dry sea-tangle raw material weight 100 times, after dissolved air flotation, obtain the sodium alginate soln clarified.
2, sodium alginate purifying: the diatomite adding glue quality 2.0 ‰ in sodium alginate soln, diatomite order number is 100 orders (model is emerging brightness SY-RS600).
3, filter: by vacuum filtration sodium alginate is separated with diatomaceous mixed solution and obtains clarification glue.
4, bleach: glue is bleached: pass into 1.2m
3/ h chlorine, bleaching glue.
5, alginate calcium preparation: add the calcium chloride solution that mass concentration is 14% in glue, the amount of calcium chloride solution is 2.1% of glue volume, and water miscible Lalgine solution is become water-insoluble calcium alginate gel.
6, post-processed: add water washing calcium alginate gel, and use expeller device to dewater to water content < 70%.
7, adopt boiling-bed drying to dry alginate calcium to Han Shui Liang≤15%, be crushed to granularity 100% and cross 100 orders, 70% crosses 200 orders, obtains alginate calcium product.
The experimental result of gained alginate calcium: moisture content 10.0%, total plate count≤1000cfu/g, mould, yeast sum≤100cfu/g, lead content 3.6mg/kg, arsenic 1.7mg/kg, cl content 0.08mg/kg, CaO content 12.3%
Embodiment 3
1, bulk kelp is embathed and digests: 24h is washed in bulk kelp water logging, then adds the sodium carbonate of bulk kelp quality 26%, after 55 DEG C of insulation digestion 8h, is smashed by bulk kelp by mechanical stirring; Add the water dilution glue being equivalent to dry sea-tangle raw material weight 100 times, after dissolved air flotation, obtain the sodium alginate soln clarified.
2, sodium alginate purifying: the diatomite adding glue quality 2.2 ‰ in sodium alginate soln, diatomite order number is 100 orders (model is emerging brightness SY-RS600)
3, filter: by vacuum filtration sodium alginate is separated with diatomaceous mixed solution and obtains clarification glue.
4, bleach: glue is bleached: pass into 2.1m
3/ h chlorine, bleaching glue.
5, alginate calcium preparation: add the calcium chloride solution that mass concentration is 15% in glue, the amount of calcium chloride solution is 2.5% of glue volume, and water miscible Lalgine solution is become water-insoluble calcium alginate gel.
6, post-processed: add water washing calcium alginate gel, and use expeller device to dewater to water content < 70%.
7, adopt boiling-bed drying to dry alginate calcium to Han Shui Liang≤15%, be crushed to granularity 100% and cross 100 orders, 70% crosses 200 orders, obtains alginate calcium product.
The experimental result of gained alginate calcium: moisture content 12.0%, total plate count≤1000cfu/g, mould, yeast sum≤100cfu/g, lead content 2.5mg/kg, arsenic 1.6mg/kg, cl content 0.09mg/kg, CaO content 12.0%.
Above embodiment only in order to technical scheme of the present invention to be described, but not is limited; Although with reference to previous embodiment to invention has been detailed description, for the person of ordinary skill of the art, still can modify to the technical scheme described in previous embodiment, or equivalent replacement is carried out to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of the present invention's technical scheme required for protection.
Claims (9)
1. a preparation method for food grade alginate calcium, is characterized in that, step is:
1) sodium alginate preparation: brown alga is embathed, add that sodium carbonate carries out digestion reaction, thin up, filtration obtain clarifying sodium alginate soln;
2) sodium alginate purifying: add diatomite adsorption drainage in sodium alginate soln;
3) filter: sodium alginate and diatomaceous mixed solution essence are filtered and obtains clarifying glue;
4) glue bleaching: pass into chlorine, bleaching glue;
5) alginate calcium preparation: add calcium chloride solution in above-mentioned clarification glue, makes water miscible sodium alginate change water-insoluble calcium alginate gel into and concentrates precipitation;
6) post-processed: washing, dehydration, dry, pulverizing, obtain food grade alginate calcium.
2. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, the brown alga in described step 1) is one or more in sea-tangle, bulk kelp, bladder wrack, sargassun.
3. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, in described step 1), digestion reaction temperature is 40-60 DEG C, reaction times 4-8h.
4. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, in described step 1), sodium carbonate add-on is brown alga quality 20-30%.
5. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, described step 2) in diatomaceously add the 1-5 ‰ that quality is sodium alginate soln quality.
6. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, in described step 3), essence filters the filter type adopting press filtration or vacuum filtration.
7. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, the amount of chlorine passed in described step 4) is 1-4m3/h.
8. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, in described step 5), the mass concentration of calcium chloride solution is 10-15%, and the amount adding calcium chloride solution is the 2-4% of glue volume.
9. the preparation method of a kind of food grade alginate calcium according to claim 1, is characterized in that, in described step 6), dewaters to Han Shui Liang≤70%, is dried to Han Shui Liang≤15%.
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| CN106674373A (en) * | 2016-12-14 | 2017-05-17 | 青岛明月海藻集团有限公司 | Method for extracting alginate and method for recycling waste calcium water |
| CN108210978A (en) * | 2017-11-21 | 2018-06-29 | 青岛明月海藻集团有限公司 | A kind of calcium alginate non-woven fabrics and preparation method thereof |
| CN108659143A (en) * | 2018-06-14 | 2018-10-16 | 青岛海之林生物科技开发有限公司 | A kind of green extraction and purification process of algin |
| CN110862561A (en) * | 2019-11-19 | 2020-03-06 | 青岛明月藻酸盐组织工程材料有限公司 | Preparation method of water-insoluble alginate for in vivo implantation |
| CN114532463A (en) * | 2022-03-08 | 2022-05-27 | 渤海水产股份有限公司 | Seaweed compound, preparation method and application thereof, and fish culture feed |
| CN114700046A (en) * | 2022-03-31 | 2022-07-05 | 华南理工大学 | Crystal violet dye adsorption hydrogel microspheres and preparation method and application thereof |
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| CN110862561A (en) * | 2019-11-19 | 2020-03-06 | 青岛明月藻酸盐组织工程材料有限公司 | Preparation method of water-insoluble alginate for in vivo implantation |
| CN114532463A (en) * | 2022-03-08 | 2022-05-27 | 渤海水产股份有限公司 | Seaweed compound, preparation method and application thereof, and fish culture feed |
| CN114532463B (en) * | 2022-03-08 | 2023-12-22 | 渤海水产股份有限公司 | Seaweed compound, preparation method and application thereof, and fish-farming feed |
| CN114700046A (en) * | 2022-03-31 | 2022-07-05 | 华南理工大学 | Crystal violet dye adsorption hydrogel microspheres and preparation method and application thereof |
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