CN102585025A - Preparation method for low-sulfate-group low-viscosity carrageenan - Google Patents
Preparation method for low-sulfate-group low-viscosity carrageenan Download PDFInfo
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- CN102585025A CN102585025A CN2012100244280A CN201210024428A CN102585025A CN 102585025 A CN102585025 A CN 102585025A CN 2012100244280 A CN2012100244280 A CN 2012100244280A CN 201210024428 A CN201210024428 A CN 201210024428A CN 102585025 A CN102585025 A CN 102585025A
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Abstract
The invention relates to a preparation method for low-sulfate-group low-viscosity carrageenan. The preparation method comprises the following steps of: weighing eucheuma and adding the eucheuma into 7-40 percent potassium hydroxide alkali solution in an amount which is 4-8 times the weight of the eucheuma; heating to 20-90 DEG C and treating for 2-168 hours; separating the eucheuma from the alkali solution and washing the eucheuma with clear water until the eucheuma is neutral; then adding water in an amount which is 5-10 times the weight of the eucheuma; heating to 100 DEG C and boiling gel for 1.5-2.5 hours; immediately filtering solution through diatomite; and gelating the filtrate and dehydrating and drying to prepare the low-sulfate-group low-viscosity carrageenan. According to the preparation method for the low-sulfate-group low-viscosity carrageenan, the alkaline treatment method in which conventional NaOH and KCI are substituted by KOH is adopted, so that the capacity of removing sulfate groups at sites 3 and 6 of galactose in the eucheuma is greatly improved; the content of the sulfate group in the carrageenan and the viscosity are reduced; the gel strength and the yield of the carrageenan are improved; the potassium hydroxide can be recycled unlimitedly; the production cost of enterprises is reduced; and the aims of low carbon, energy conservation and emission reduction are fulfilled.
Description
Technical field
The invention belongs to the Sargassum polysaccharides preparing technical field, be specifically related to a kind of preparation method of low sulfate low-viscosity carrageenin.
Background technology
Carrageenin mainly is present in the cell walls of Eucheuma (prominent Eucheuma muricatum (Gmel.) Web of ear and agar), Chondrus, China fir Lepidium and husky Lepidium etc. in the Rhodophyceae, and it is main needing only with Eucheuma muricatum (Gmel.) Web at present.Carrageenin is by 1,3-β-D-galactopyranose and 1, and 4-α-D-galactopyranose is as basic framework; The linear sulfate polysaccharide that alternately is formed by connecting according to the link position of sulfate, can be divided into kappa-carrageenan; Lambda-carrageenan, μ-carrageenin, ν-carrageenin; ι-carrageenin, ξ-carrageenin, 7 kinds of main types such as θ-carrageenin.
The production of carrageenin is that 20th century are inchoate, and the U.S. produces 4500 tons per year at present, and Denmark produces 3000 tons per year; 2800 tons in France; China produces 1.5 ten thousand tons, is mainly used in jelly production, senior soft sweets, food-drink thickening material, meat binder etc., about 6000 tons/year of home sale; After in the world's three big seaweed gels, coming algin, occupy second.The most important quality index of carrageenin is the size of gel-strength, sulfate content and viscosity, and gel-strength, viscosity and sulfate have very confidential relation, and sulfate content is high, and gel-strength is little, and viscosity is big; Sulfate content is low, and gel-strength is big, and viscosity is little.Traditional method is the method that the raw material (at present mainly be Eucheuma muricatum (Gmel.) Web) higher to sulfate content adopts the high temperature diluted alkaline to handle, that is: 90 ± 2 ℃, and 5-10%NaOH, 5%KCI handled 4 hours.The NaOH alkaline purification can remove the sulfate on 3,6 of the semi-lactosis in the Eucheuma muricatum (Gmel.) Web, makes these units become 3, and 6-inner ether semi-lactosi has reduced the sulfate content and the viscosity of carrageenin, also improves the gel-strength of carrageenin; When the effect of KCI was pyroprocessing, micromolecular carrageenin dissolved in the alkaline purification liquid in the prevention Eucheuma muricatum (Gmel.) Web, but still there are many defectives in this method:
(1) the sulfate content of carrageenin is too up to arriving 15-40%.
(2) viscosity of carrageenin is high, and 1.5% concentration is measured the result greater than 10mpa.s at 75 ℃.
(3) ash content is high, because sulfate content is up to 15-40% in the carrageenin, water-insoluble reaches about 1.0%.
(4) sodium hydroxide and Repone K treatment solution can not unlimitedly recycle, because potassium ion can not stop small molecules carrageenin stripping in the Eucheuma muricatum (Gmel.) Web fully in the Repone K; The a collection of Eucheuma muricatum (Gmel.) Web of every processing always has a spot of OK a karaoke club peptization in alkali lye; Polluted alkali lye, handle 20 batches of Eucheuma muricatum (Gmel.) Webs after, just again can not use; Not only increase the carrageenin cost, also environment has been produced huge pollution.
(5) greatest problem that carrageenin is produced in highly energy-consuming, high pollution, conventional art be early stage water consumption and alkali charge big, 1 ton of carrageenin of every production; Need more than 1000 ton of water; Consume chemical bases more than 1 ton, and produce about 500～700 tons and contain alkali waste water, need carry out large amount of sewage and handle.Owing to above-mentioned technical defective, had a strong impact on the quality of carrageenin, restricted the application of carrageenin in the high-end field.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of low sulfate low-viscosity carrageenin; It can not only remedy the above-mentioned deficiency of prior art; But also can improve the yield of carrageenin, handling alkali lye can unlimitedly recycle, and reaches the purpose that low-carbon energy-saving reduces discharging.
Method of the present invention is to come from Eucheuma muricatum (Gmel.) Web, to prepare carrageenin with Pottasium Hydroxide replace sodium hydroxide and Repone K.
The preparation method of low sulfate low-viscosity carrageenin of the present invention is characterized in that at first taking by weighing the 7-40% Pottasium Hydroxide alkaline solution that Eucheuma muricatum (Gmel.) Web adds 4-8 times of Eucheuma muricatum (Gmel.) Web weight, is warming up to 20-90 ℃ and handles 2-168 hour; Again with Eucheuma muricatum (Gmel.) Web and alkali solution separation, and with clear water Eucheuma muricatum (Gmel.) Web is washed till neutrality; Add the heavy water of 5-10 times of Eucheuma muricatum (Gmel.) Web then, be warming up to 100 ℃ and boiled glue 1.5-2.5 hour, immediately solution is passed through diatomite filtration, filtered liq is through gel, and low sulfate low-viscosity carrageenin is processed in dehydration after the oven dry.
Described Eucheuma muricatum (Gmel.) Web is prominent Eucheuma muricatum (Gmel.) Web of ear or agar, and the prominent Eucheuma muricatum (Gmel.) Web of ear contains the kappa-carrageenan height, and it is high that the thorn kylin just contains ι-carrageenin.
Above-mentioned Pottasium Hydroxide alkaline solution be recycled after Eucheuma muricatum (Gmel.) Web separates.
The preparation method of low sulfate low-viscosity carrageenin of the present invention is the alkali treatment method that adopts the alternative traditional NaOH+KCI of KOH, has greatly improved to remove semi-lactosi 3 in the Eucheuma muricatum (Gmel.) Web; 6 abilities that go up sulfate; Reduced sulfate content and viscosity in the carrageenin, improve the gel-strength and the yield of carrageenin, and Pottasium Hydroxide can unlimitedly recycle; Reduce the enterprise production cost; Reach the purpose that low-carbon energy-saving reduces discharging, opened restriction China high-end carrageenin technology of preparing bottleneck, widened carrageenin intensive processing Application Areas.
Embodiment
The preparation method of low sulfate low-viscosity carrageenin of the present invention, it is characterized in that taking by weighing the mass percent that Eucheuma muricatum (Gmel.) Web adds 4-8 times of Eucheuma muricatum (Gmel.) Web weight is the Pottasium Hydroxide alkaline solution of 7-40%, is warming up to 20-90 ℃; Alkaline purification 2-168 hour, Eucheuma muricatum (Gmel.) Web is separated with alkali lye, and Eucheuma muricatum (Gmel.) Web is washed till neutrality with clear water; Add the heavy water of 5-10 times of Eucheuma muricatum (Gmel.) Web then, be warming up to 100 ℃ and boiled glue 1.5-2.5 hour, while hot diatomite filtration; Filtered liq is through gel, and dehydration is dried; Pulverize, packing obtains low sulfate low-viscosity carrageenin of the present invention.
The mass percent of described Pottasium Hydroxide is 7-40%; If the mass percent of Pottasium Hydroxide is less than 7%; Then greatly weakened the ability that removes sulfate in the Eucheuma muricatum (Gmel.) Web, but, then can increase washing times and the water consumption of Eucheuma muricatum (Gmel.) Web along with the increase gradually of the mass percent of Pottasium Hydroxide; Increase production cost, corresponding pollution also can strengthen.
Embodiment 1:
Take by weighing the 100Kg Eucheuma muricatum (Gmel.) Web, the adding mass percent is 10% potassium hydroxide solution 500Kg, 90 ± 2 ℃; Alkaline purification 3 hours, the potassium ion in the Pottasium Hydroxide can stop micromolecular carrageenin stripping in the Eucheuma muricatum (Gmel.) Web fully, make the potassium hydroxide solution can unlimited recycle and reuse; Reduce cost, energy-saving and emission-reduction 30-40%, but also can more imitate in the Eucheuma muricatum (Gmel.) Web polysaccharide 3 with having; Sulfate on 6 is removed; Sulfate content is reduced to below 5% from 15-40% by the carrageenin that traditional method makes, and viscosity is from reducing to less than 1mpa.s greater than 10mpa.s, and gel-strength is from 1000g/cm
2About be increased to greater than 1200g/cm
2, improved the quality of carrageenin, widened the application of carrageenin at medicine, protective foods and cosmetic field.The Eucheuma muricatum (Gmel.) Web that alkaline purification is good separates with potassium hydroxide solution, and Eucheuma muricatum (Gmel.) Web, joins then and boils the glue jar to neutral with the tap water flushing, and adds the 600Kg tap water; Be warming up to 100 ℃, boiled glue 2 hours, while hot diatomite filtration; Filtered liq is through cooling gel, and press dewatering is dried; Pulverize, packing obtains the low sulfate low-viscosity carrageenin 21.2Kg of the present invention.The viscosity of carrageenin is 0.78mpa.s, sulfate content 4.12%, ash content 8.4%, gel-strength 1220g/cm
2
Embodiment 2
Take by weighing the 100Kg Eucheuma muricatum (Gmel.) Web, the adding mass percent is 18% potassium hydroxide solution 500Kg, 60 ± 2 ℃, and alkaline purification 8 hours, the Eucheuma muricatum (Gmel.) Web that alkaline purification is good separates with potassium hydroxide solution; Eucheuma muricatum (Gmel.) Web, joins then and boils the glue jar to neutral with the tap water flushing, and adds the 600Kg tap water, is warming up to 100 ℃; Boiled glue 2 hours, diatomite filtration while hot, filtered liq be through cooling gel, press dewatering; Oven dry is pulverized, and packing obtains the low sulfate low-viscosity carrageenin 23.5Kg of the present invention.The viscosity of carrageenin is 0.56mpa.s, sulfate content 3.1%, ash content 6.4%, gel-strength 1280g/cm
2
Embodiment 3
Take by weighing the 100Kg Eucheuma muricatum (Gmel.) Web, the adding mass percent is 38% potassium hydroxide solution 500Kg, 20 ± 2 ℃, and alkaline purification 72 hours, the Eucheuma muricatum (Gmel.) Web that alkaline purification is good separates with potassium hydroxide solution; Eucheuma muricatum (Gmel.) Web, joins then and boils the glue jar to neutral with the tap water flushing, and adds the 600Kg tap water, is warming up to 100 ℃; Boiled glue 2 hours, diatomite filtration while hot, filtered liq be through cooling gel, press dewatering; Oven dry is pulverized, and packing obtains the low sulfate low-viscosity carrageenin 24.7Kg of the present invention.The viscosity of carrageenin is 0.14mpa.s, sulfate content 1.8%, ash content 4.1%, gel-strength 1340g/cm
2
Along with the increase of Pottasium Hydroxide mass percent, the corresponding reduction of the temperature of alkaline purification, also corresponding prolongation of treatment time; Production cost also increases; But the sulfate of carrageenin, viscosity and ash oontent but significantly reduce, and gel-strength improves constantly, and the quality product of carrageenin improves constantly.
Claims (5)
1. the preparation method of one kind low sulfate low-viscosity carrageenin is characterized in that, is to come from Eucheuma muricatum (Gmel.) Web, to prepare carrageenin with Pottasium Hydroxide replace sodium hydroxide and Repone K.
2. preparation method as claimed in claim 1, its concrete steps are following: at first take by weighing the 7-40% Pottasium Hydroxide alkaline solution that Eucheuma muricatum (Gmel.) Web adds 4-8 times of Eucheuma muricatum (Gmel.) Web weight, be warming up to 20-90 ℃ and handled 2-168 hour; Again with Eucheuma muricatum (Gmel.) Web and alkali solution separation, and with clear water Eucheuma muricatum (Gmel.) Web is washed till neutrality; Add the heavy water of 5-10 times of Eucheuma muricatum (Gmel.) Web then, be warming up to 100 ℃ and boiled glue 1.5-2.5 hour, immediately solution is passed through diatomite filtration, filtered liq is through gel, and low sulfate low-viscosity carrageenin is processed in dehydration after the oven dry.
3. preparation method as claimed in claim 1 is characterized in that described Eucheuma muricatum (Gmel.) Web is prominent Eucheuma muricatum (Gmel.) Web of ear or agar.
4. preparation method as claimed in claim 2 can unlimitedly be recycled after it is characterized in that described Pottasium Hydroxide alkaline solution and Eucheuma muricatum (Gmel.) Web separating.
5. a carrageenin is prepared by the described method of claim 1.
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| CN2012100244280A CN102585025B (en) | 2012-02-05 | 2012-02-05 | Preparation method for low-sulfate-group low-viscosity carrageenan |
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| CN2012100244280A CN102585025B (en) | 2012-02-05 | 2012-02-05 | Preparation method for low-sulfate-group low-viscosity carrageenan |
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| CN102585025B CN102585025B (en) | 2013-12-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105104923A (en) * | 2015-09-15 | 2015-12-02 | 常州市鼎日环保科技有限公司 | Preparation method for preparing high-elasticity kappa-type carrageenan |
| CN107118284A (en) * | 2017-06-02 | 2017-09-01 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN110724208A (en) * | 2019-10-30 | 2020-01-24 | 临沂艾德森生物科技有限公司 | Anti-freezing carrageenan oligosaccharide and preparation method and application thereof |
| CN111700266A (en) * | 2020-06-09 | 2020-09-25 | 邱涛 | Refined carrageenan and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307111A (en) * | 2008-07-04 | 2008-11-19 | 深圳市宝志得实业有限公司 | Process for manufacturing IOTA type carrageenin |
| CN102180988A (en) * | 2011-04-15 | 2011-09-14 | 江南大学 | Method for preparing k-carrageenan with high gel strength from eucheuma |
-
2012
- 2012-02-05 CN CN2012100244280A patent/CN102585025B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307111A (en) * | 2008-07-04 | 2008-11-19 | 深圳市宝志得实业有限公司 | Process for manufacturing IOTA type carrageenin |
| CN102180988A (en) * | 2011-04-15 | 2011-09-14 | 江南大学 | Method for preparing k-carrageenan with high gel strength from eucheuma |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105104923A (en) * | 2015-09-15 | 2015-12-02 | 常州市鼎日环保科技有限公司 | Preparation method for preparing high-elasticity kappa-type carrageenan |
| CN107118284A (en) * | 2017-06-02 | 2017-09-01 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN107118284B (en) * | 2017-06-02 | 2019-05-03 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN110724208A (en) * | 2019-10-30 | 2020-01-24 | 临沂艾德森生物科技有限公司 | Anti-freezing carrageenan oligosaccharide and preparation method and application thereof |
| CN111700266A (en) * | 2020-06-09 | 2020-09-25 | 邱涛 | Refined carrageenan and preparation method and application thereof |
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| CN102585025B (en) | 2013-12-04 |
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Address after: 266003 Shandong Province, Qingdao city Laoshan District Songling Road No. 238 Patentee after: Ocean University of China Patentee after: Fujian sea biological Polytron Technologies Inc Address before: 266003 Shandong Province, Qingdao city Laoshan District Songling Road No. 238 Patentee before: Ocean University of China Patentee before: Fujian Global Ocean Biotechnology Co., Ltd. |
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