CN106749752B - Preparation method of ultra-low viscosity alginate - Google Patents
Preparation method of ultra-low viscosity alginate Download PDFInfo
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- 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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Abstract
The invention discloses a preparation method of an alginate with ultralow viscosity, which comprises the steps of 1) taking brown algae as a raw material, and performing soaking, color fixation, washing, digestion, dilution, filtration, floating and fine filtration to obtain a glue solution; then, alginic acid is obtained by calcification or acidification, decalcification and dehydration, and then is crushed; 2) heating to degrade alginic acid, and discharging evaporated low boiling point substances; continuously stirring alginic acid in the heating process; 3) and (3) cooling the degraded alginic acid, adding alcohol, stirring uniformly, then adding alkali for neutralization, drying and crushing to obtain the ultra-low viscosity alginate. The invention solves the problems of poor product viscosity stability, oxidant odor residue and irradiation limitation existing in the prior technology of hydrogen peroxide degradation or irradiation degradation; the application effect of the product is improved, and the method is suitable for industrial production and application.
Description
Technical Field
The invention belongs to the technical field of alginate processing, and particularly relates to a preparation method of an ultra-low viscosity alginate.
Background
Sodium alginate is a natural polymer material extracted from brown algae plants, and is widely applied to the fields of medicine, food, chemical industry and agriculture. The ultra-low viscosity sodium alginate is generally prepared into commercial specification applications such as 10% mass concentration solution 100-. The sodium alginate has the characteristic of instant dissolution in water after ultralow viscosity, the viscosity of 1 percent solution is close to that of water, and the sodium alginate is generally dissolved into a high-concentration form to be applied to liquid stomach medicaments, beverages and film-forming materials, and the high-concentration solution has the requirements of light smell, good solution stability, low content of water insoluble substances and the like.
The process of extracting alginate generally comprises the steps of soaking brown algae in water, digesting with alkali, diluting with water, filtering to obtain a sodium alginate liquid, converting the sodium alginate into calcium alginate by using calcium chloride, converting the calcium alginate into alginic acid by using hydrochloric acid, dehydrating and neutralizing the alginic acid to obtain the alginate, and finally drying and crushing the alginate to obtain a product with uniform quality. The intermediate products of the process, namely the liquid state sodium alginate and the semi-dry state sodium alginate, have poor viscosity stability and are easy to degrade. However, if the liquid sodium alginate is degraded, subsequent calcification and acidification cannot be performed, and a large amount of colloid is lost; if the semi-dry alginic acid is degraded, the converted product of the alginic acid has the characteristic of quick dissolution, and the alginic acid is dissolved and sticky in a wet material state, so that the subsequent processing and recovery are difficult. For the reasons, the main technology for preparing the ultra-low viscosity alginate at present is to perform oxidative degradation or irradiation degradation on alginate particles, a large amount of hydrogen peroxide or high-dose irradiation is needed in the process, and oxidant residues in the alginate treated by the hydrogen peroxide cannot be thoroughly removed, so that the problems of pungent smell and poor viscosity stability are caused; in addition, high dose irradiation has certain limitations in food applications. The existing preparation technology of the alginate with ultra-low viscosity is mature, but has a plurality of defects.
The production process of alginate oligosaccharide disclosed in patent CN 1631905A is to oxidize and degrade solid sodium alginate with hydrogen peroxide and eliminate residual hydrogen peroxide in vacuum. The patent is suitable for industrialization, but the problems of residual oxidant smell and unstable viscosity of the sodium alginate caused by large hydrogen peroxide consumption in application exist. The low molecular weight alginate 1157415 is prepared through preparing water solution of alginic acid, physical, chemical or enzyme degradation, membrane filtering to obtain alginate with average molecular weight of 5000-. The patent discloses alginates with molecular weight requirements and ultra-low viscosity alginates with different quality requirements and uses. Patent publication 103351440B discloses a process for preparing pharmaceutical grade sodium alginate, which comprises dehydrating alginic acid extracted from brown algae, pulverizing, transferring into a high-pressure tank, treating at 120 deg.C and 10kPa for 30min, neutralizing with ethanol as medium, and centrifuging to obtain sodium alginate. The technical scheme of the thermal degradation in the patent is difficult to realize the accurate control of the ultralow viscosity value, and the problems of small production capacity and high cost exist in large-scale production. The patent CN105367684A discloses a preparation method of ultra-low viscosity sodium alginate, which comprises the steps of carrying out enzymolysis and digestion on brown algae, adding water to dilute and filter to obtain sodium alginate liquid, degrading the sodium alginate liquid under the condition of pH2-4, adding alkali to adjust the pH to be neutral, adding alcohol to precipitate, and finally carrying out centrifugal separation to obtain the sodium alginate. The sodium alginate prepared by the method has low purity, contains a large amount of water-soluble impurities and additional salt, has high separation cost by adding alcohol, and does not have large-scale production feasibility.
Disclosure of Invention
The invention relates to a preparation method of an alginate with ultralow viscosity, which can solve the problems of poor product viscosity stability, oxidant odor residue and irradiation limitation existing in the prior hydrogen peroxide degradation or irradiation degradation technology; the application effect of the product is improved, and the method is suitable for industrial production and application.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an ultra-low viscosity alginate comprises the following steps: 1) soaking brown algae as a raw material, fixing color, washing, digesting, diluting, filtering, floating and finely filtering to obtain a glue solution; then, alginic acid is obtained by calcification or acidification, decalcification and dehydration, and then is crushed; 2) heating to degrade alginic acid, and discharging evaporated low boiling point substances; continuously stirring alginic acid in the heating process; 3) and (3) cooling the degraded alginic acid, adding alcohol, stirring uniformly, then adding alkali for neutralization, drying and crushing to obtain the ultra-low viscosity alginate.
In order to obtain alginic acid with high purity, the transparency of the glue solution in the step 1) is more than 30 cm.
In order to prevent the ultra-low viscosity sodium alginate from being sticky in a wet material state, the water content of the alginic acid in the step 1) is controlled to be lower than 62%.
Further, fine filtration in the step 1) adopts diatomite assisted rate or a mesh with more than 350 meshes for fine filtration; the dehydration mode adopts organic solvent to assist dehydration, oil press dehydration or high-pressure screw dehydration.
The viscosity of alginic acid is reduced by adopting a thermal degradation mode, and alginic acid in the step 2) is heated to 60-80 ℃ for 1-5h until the water content of alginic acid is 40-50%.
Further, in the step 3), sodium carbonate, potassium carbonate, calcium carbonate or magnesium carbonate is used as the alkali.
Further, the alginic acid degraded in the step 3) is cooled to below 45 ℃.
Further, adding 60-80 DEG alcohol aqueous solution into the alginic acid after cooling in the step 3), wherein the mass ratio of the alcohol aqueous solution to the alginic acid is 1-3:1, and reacting the alginic acid with liquid alkali in a liquid environment.
In order to improve the yield of the ultra-low viscosity sodium alginate, adding pure alcohol into the alginic acid after cooling in the step 3) and uniformly mixing, wherein the adding amount of the pure alcohol is 1-15% of the mass of the alginic acid, keeping the alginic acid in a semi-dry state, and reacting the alginic acid in the semi-dry state with solid alkali under the stirring condition.
In order to promote the neutralization reaction of the contact between the semi-dry alginic acid and the solid base, the water content of the alginic acid in the step 1) is controlled to be 55-60%.
Compared with the prior art, the invention has the advantages and positive effects that:
the prior art mainly adopts a technical route for degrading sodium alginate by hydrogen peroxide or irradiation, and the patent discloses a technical route for preparing the ultra-low viscosity alginate by thermally degrading alginic acid. Compared with the technology of preparing the ultra-low viscosity alginate by alginic acid in the prior patent, the method has the advantages of production feasibility and production capacity which can meet the market demand (about 1000 tons/year).
Firstly, preparing alginic acid with high transparency (high purity) as a raw material for preparing the alginate with the ultralow viscosity; then, the alginic acid is degraded in a heating mode by utilizing the characteristic that the alginic acid is easier to be thermally degraded compared with sodium alginate, so that the viscosity of the alginic acid is degraded, and the moisture of the alginic acid is further reduced; and then, carrying out neutralization reaction to prepare the ultra-low viscosity sodium alginate, and adding alcohol into alginic acid to improve the material characteristics by utilizing the principle that the alcohol can reduce the solubility of the ultra-low viscosity sodium alginate, thereby effectively avoiding the problems of stickiness, caking, yellowing of material appearance and the like of the material during the neutralization reaction of the ultra-low viscosity alginic acid.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments.
The embodiment provides a preparation technology of 10% concentration aqueous solution 100-; thermally degrading alginic acid; alcohol treatment of alginic acid; alginic acid is neutralized with alkali and converted to alginate. The process is simple, and the industrial production of the alginate with ultra-low viscosity can be realized. The method comprises the following specific steps:
(1) soaking brown algae as raw material, fixing color, washing, digesting, diluting, filtering, floating and fine filtering to obtain glue solution with transparency of over 30 cm; then the alginic acid with high purity is obtained by calcification or acidification, decalcification and dehydration, and then is crushed. It is desirable to control the water content of the alginic acid to be less than 62%, and the lower the water content, the more beneficial it is to avoid the problem of stickiness of the alginate having an ultra-low viscosity.
The fine filtration adopts diatomite assisted rate or fine filtration with a screen of more than 350 meshes; the dehydration mode adopts organic solvent to assist dehydration, oil press dehydration or high-pressure screw dehydration machine dehydration, etc.
In the embodiment, firstly, alginic acid with high transparency (high purity) is prepared and used as a raw material for preparing the alginate with ultra-low viscosity, so that various problems caused by high content of water-insoluble substances when the alginate with ultra-low viscosity is applied in a form of high-concentration solution are solved.
(2) Heating alginic acid to 60-80 deg.C, discharging water and low boiling point substances such as hydrochloric acid, etc. evaporated from the heated alginic acid, and reducing water content to 40-50%. Alginic acid is continuously stirred in the heating process to keep the alginic acid in a loose state, so that the water vapor is convenient to circulate. The degradation time is adjusted according to the specification of the ultra-low viscosity alginate product, namely 10% mass concentration solution 100-.
In the embodiment, alginic acid is degraded by heating, which utilizes the characteristic that alginic acid is easily degraded by heat, so as to degrade the viscosity of alginic acid and further reduce the moisture of alginic acid. The viscosity of alginic acid is controlled by adjusting the heating temperature and time, when the heating temperature is lower than 60 ℃, the effects of thermal degradation and moisture reduction are poor, and when the heating temperature is higher than 80 ℃, the reaction conditions are severe and are not beneficial to controlling the viscosity and moisture, so that the problem of material deterioration is easy to occur.
In the embodiment, a thermal degradation mode is adopted, compared with a mode of degrading solid sodium alginate by hydrogen peroxide or irradiating, the product quality is improved, and the technical problems of poor viscosity stability of sodium alginate and oxidant odor residue caused by hydrogen peroxide residue are solved; the product without radiation residue has higher safety.
(3) Cooling the degraded alginic acid to below 45 ℃, adding alcohol, stirring uniformly, adding alkali for neutralization to obtain alginate, drying the alginate, and crushing to obtain the ultra-low viscosity alginate. The alkali is carbonate, such as sodium carbonate, potassium carbonate, calcium carbonate, magnesium carbonate, etc.
In the preparation method of the ultra-low viscosity alginate in the embodiment, the principle that alginic acid has poorer thermal stability than alginate is utilized, the alginic acid which is an intermediate product in the brown algae processing process is used as a raw material, thermal degradation is carried out on the alginic acid, and then neutralization reaction is carried out to prepare the ultra-low viscosity alginate. One of the key technologies is to control the water content of alginic acid to be below 62%. In the current industrial production of alginate, the water content of alginic acid is required to be 64-72%, and the alginic acid is not suitable for producing the alginate with ultra-low viscosity because the alginate with ultra-low viscosity has the characteristic of instant dissolution, and the water content of 64-72% can cause the alginate with ultra-low viscosity to be sticky in a wet material state. The second key technology is to utilize the principle that alcohol can reduce the solubility of the ultra-low viscosity alginate, add alcohol into alginic acid to improve the material characteristics, reduce the product loss, and avoid the problems of sticky materials, caking materials, yellowing material appearance and the like during the neutralization reaction of the ultra-low viscosity alginate.
In this example, alkali is added to alginic acid for neutralization in two ways:
the implementation mode is that alginic acid and liquid alkali are reacted in a liquid environment by taking an aqueous alcohol solution as a solvent, the mass ratio of the aqueous alcohol solution to the alginic acid is 1-3:1, and the volume concentration of alcohol in the aqueous alcohol solution is 60-80%.
And the second embodiment is that a small amount of pure alcohol is added into the cooled alginic acid and mixed evenly, the alginic acid is kept in a semi-dry state, and the semi-dry alginic acid reacts with solid alkali under the stirring condition to obtain the alginate. The addition amount of the pure alcohol is 1-15% of the mass of the alginic acid, when the addition amount is less than 1%, the effect of avoiding the stickiness of the materials is not obvious, and when the addition amount is more than 15%, the semi-dry state of the alginic acid is destroyed.
In order to increase the yield of the ultra-low viscosity sodium alginate, the second embodiment is preferably adopted. When the second embodiment is adopted, the alginic acid in the step 1) is required to have a water content of 55-60% because if the water content of the alginic acid is too low, that is, the alginic acid is too dry, the alginic acid in a semi-dry state is not beneficial to the neutralization reaction by contacting the alginic acid with solid alkali, and the inventor has proved through many experiments that when the alginic acid water content is controlled to 55-60%, the alginic acid does not affect the neutralization reaction, and the alginic acid prevents the material from being sticky under the action of alcohol.
Example 1
An ultra-low viscosity alginate was prepared as follows:
1. taking food-grade sodium alginate intermediate alginic acid, squeezing with a high-pressure screw dehydrator until the water content is 62%, and pulverizing;
2. pouring 400kg of alginic acid into a reactor, stirring and inducing air, heating the reaction tank to 65 ℃ after 20min, and keeping the temperature at 60-65 ℃ for 3h to reduce the water content of the alginic acid to 50%;
3. cooling the materials to below 40 ℃, adding 10kg of pure alcohol, and uniformly mixing;
4. adding 36kg of sodium carbonate solid, stirring and neutralizing for 20 min;
5. granulating and drying to obtain the sodium alginate with 10% mass concentration and 400mpa.s viscosity.
The product in example 1 was loss-free; the product is placed for 6 months at normal temperature, the viscosity is reduced by less than 5 percent, which shows that the viscosity stability of the product is good; the product quality is greatly improved, and the requirement of the medicinal market on the product stability is met, which is reflected in that the product is basically odorless (especially odorless with no oxidant residue); dissolving the mixture to a 10% solution, wherein the solution is stable (if a hydrogen peroxide degradation mode is adopted, the viscosity rapidly decreases in a short time due to the presence of hydrogen peroxide, and more precipitates exist); because of adopting high-purity alginic acid, the water insoluble substance in the glue solution is further reduced, thereby facilitating the filtration of the glue solution form application process of the product and preventing the filtration pores from being blocked.
Example 2
An ultra-low viscosity alginate was prepared as follows:
1. taking food-grade sodium alginate intermediate alginic acid, squeezing and dehydrating to water content of 62% by using a high-pressure screw dehydrator, and crushing;
2. pouring 400kg of alginic acid into a reactor, stirring, inducing air, adding 1L of hydrogen peroxide, heating to 65 ℃ in a reaction tank for 20min, keeping the temperature at 60-65 ℃ for 3h, and reducing the water content of the alginic acid to 49%;
3. cooling the material to below 40 ℃, and adding 8kg of pure alcohol for mixing;
4. adding 36kg sodium carbonate, stirring and neutralizing for 20 min;
5. granulating and drying to obtain the sodium alginate with 10% mass concentration and 400mpa.s viscosity.
The product in example 2 was loss-free; the whiteness of the appearance of the obtained sodium alginate is better than that of the sodium alginate in example 1, because the hydrogen peroxide plays a role in bleaching, and the hydrogen peroxide is completely removed through a thermal degradation process and a drying process due to the small consumption of the hydrogen peroxide, and the hydrogen peroxide residue is not detected.
Example 3
An ultra-low viscosity alginate was prepared as follows:
1. taking food-grade sodium alginate intermediate alginic acid, squeezing and dehydrating to water content of 62% by using a high-pressure screw dehydrator, and crushing;
2. pouring 400kg of alginic acid into a reactor, stirring and inducing air, heating the reaction tank to 65 ℃ after 20min, and keeping the temperature at 60-65 ℃ for 3h to reduce the water content of the alginic acid to 45%;
3. cooling the material to below 40 ℃;
4. preparing 70-degree alcohol water solution with the mass ratio of 1:1, adding liquid alkali to adjust the pH to be neutral, stirring for 10min, standing for 50min, and centrifuging;
5. granulating and drying to obtain the sodium alginate with 10% mass concentration and 400mpa.s viscosity.
The product yield was 90% of that of example 1, indicating that about 10% of the sodium alginate was dissolved in the alcohol solution and lost with the alcohol solution.
The above examples are only a few of the several preferred embodiments of the present invention, and it should be noted that the present invention is not limited to the above examples; for a person skilled in the art, modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (5)
1. A preparation method of an ultra-low viscosity alginate is characterized by comprising the following steps:
1) soaking brown algae as a raw material, fixing color, washing, digesting, diluting, filtering, floating and finely filtering to obtain a glue solution, wherein the transparency of the glue solution is more than 30 cm; then, the alginic acid is obtained through calcification or acidification, decalcification and dehydration, the water content of the alginic acid is controlled to be 55-60 percent, and then the alginic acid is crushed;
2) heating to degrade alginic acid, and discharging evaporated low boiling point substances; continuously stirring alginic acid in the heating process, heating the alginic acid to 60-80 ℃ for 1-5h until the water content of the alginic acid is 40-50%;
3) cooling the degraded alginic acid to below 45 ℃, adding alcohol, stirring uniformly, adding alkali for neutralization, drying and crushing to obtain the ultra-low viscosity alginate.
2. The method for preparing the alginate with ultra-low viscosity according to claim 1, wherein the fine filtration in step 1) is performed by diatomite-assisted filtration or fine filtration with a 350-mesh or higher net; the dehydration mode adopts organic solvent to assist dehydration, oil press dehydration or high-pressure screw dehydration.
3. The method for preparing the alginate with ultra-low viscosity according to claim 1, wherein the alkali used in step 3) is sodium carbonate, potassium carbonate, calcium carbonate or magnesium carbonate.
4. The method for preparing the alginate with the ultra-low viscosity according to any one of the claims 1 to 3, wherein the alginic acid after being cooled in the step 3) is added with 60 to 80 degrees of aqueous alcohol solution, the mass ratio of the aqueous alcohol solution to the alginic acid is 1 to 3:1, and the alginic acid and the liquid alkali are reacted in a liquid environment.
5. The method for preparing the alginate with the ultra-low viscosity according to any one of claims 1 to 3, wherein pure alcohol is added into the alginic acid after the temperature is reduced in the step 3) and is uniformly mixed, the adding amount of the pure alcohol is 1 to 15 percent of the mass of the alginic acid, the alginic acid is kept in a semi-dry state, and the alginic acid in the semi-dry state reacts with solid alkali under the stirring condition.
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| CN108191993B (en) * | 2017-12-26 | 2019-07-26 | 青岛明月海藻集团有限公司 | A kind of sodium alginate and its preparation method and application |
| CN108576404A (en) * | 2018-04-24 | 2018-09-28 | 扬州中微生物技术有限公司 | A kind of preparation method of low molecular weight feed alginic acid zinc |
| CN112442138A (en) * | 2020-11-26 | 2021-03-05 | 青岛聚大洋藻业集团有限公司 | Preparation method of high-purity sodium alginate and application of high-purity sodium alginate in biological 3D printing |
| CN112321746A (en) * | 2020-11-26 | 2021-02-05 | 青岛聚大洋藻业集团有限公司 | Extraction process of high-purity ultralow-viscosity sodium alginate |
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| CN1840548A (en) * | 2005-08-18 | 2006-10-04 | 山东寻山水产集团有限公司 | Process for preparing algin with fresh kelp as raw material |
| CN1927890A (en) * | 2006-09-28 | 2007-03-14 | 青岛明月海藻集团有限公司 | Production process of propylene glycol alginate special for beer |
| 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 by using giant kelp |
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| KR100198824B1 (en) * | 1996-09-13 | 1999-06-15 | 강병원 | Solution of alginnate sodium & its beverage |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1840548A (en) * | 2005-08-18 | 2006-10-04 | 山东寻山水产集团有限公司 | Process for preparing algin with fresh kelp as raw material |
| CN1927890A (en) * | 2006-09-28 | 2007-03-14 | 青岛明月海藻集团有限公司 | Production process of propylene glycol alginate special for beer |
| 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 by using giant kelp |
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