CN109796540A - A kind of refining methd of pharmaceutical grade xanthan gum - Google Patents
A kind of refining methd of pharmaceutical grade xanthan gum Download PDFInfo
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Abstract
The invention discloses a kind of refining methds of pharmaceutical grade xanthan gum.After it includes the following steps: that S1 calcium alginate crosslinking microsphere of zeolite forms gel precipitation in industrial grade xanthan gum aqueous solution, filtering obtains sediment A;Sediment A is dissolved in aqueous solution of alcohol by S2, is filtered to get filtrate;Filtrate is formed sediment B by S3 in alcoholic solvent;Alcoholic solvent is the alcohol in step S2 aqueous solution of alcohol;Sediment B in step S3 is washed, is drying to obtain by S4.Refining methd of the invention is crosslinked microsphere of zeolite precipitation and separation xanthan gum using calcium alginate, resulting xanthan gum product can reach medicinal grade standard, meet the quality standard of 2015 editions the 4th pharmaceutical grade xanthan gum using industrial grade xanthan gum as raw material.
Description
Technical field
The present invention relates to a kind of refining methds of pharmaceutical grade xanthan gum.
Background technique
Xanthan gum (xanthan gum) alias yellow glue, xanthan gum, also known as Xanthan Gum.U.S.'s agriculture the 1950s
North research department, industry portion finds this neutral water soluble polysaccharide from xanthomonas campestris NRRLB-1459.It is with carbohydrate at present
For primary raw material, a kind of outer heteroglycan of extracellular microbial of fermented production, relative molecular mass 2 × 106~2 × 107.Xanthan gum
Preparation include fermentation, purify and be made finished product three parts.Its fermentation liquid has the characteristics that high viscosity, high impurity and content are low,
Difficulty is caused to purifying, purifying cost is made to occupy very big ratio in total preparation cost.Its finished product division of labor industry crude product grade, industry
Grade, food-grade and 4 kinds of pharmaceutic adjuvant grade, wherein food-grade and pharmaceutic adjuvant grade be because of quality requirement height, thus purifying difficulty and at
This height.
Currently, the process of medicinal rank xanthan gum product separation and Extraction mainly has direct drying method, Ultra filtration membrane
Method, organic solvent precipitation method and salt precipitation method etc., but applying the upper restriction all by respective condition.Direct drying method is to adopt
It is simple process, easy to operate, low in cost with the dry fermentation liquid of the methods of roller drying or spray drying, but cannot go
Depigmentation and the impurity such as organic matter therein and inorganic matter.Ultra filtration membrane method is to be carried out using ultrafiltration to xanthan gum fermentation broth
Concentration, can be greatly decreased alcohol dosage, the quality of xanthan gum increases, but it is relatively difficult to establish large-scale industrialization device
(such as a set of ultrafiltration apparatus cost is in million to ten million ranks).Organic solvent precipitation method is most one of industrial application at present
Kind extracts the maturation method of xanthan gum, but the method needs to consume big energy, while alcohol during recycling alcohol using a large amount of alcohol
Loss it is inevitable, on the one hand pollute environment, on the other hand increase xanthan gum production cost.Salt precipitation method is analysed in alcohol
During inorganic salts are added, to reduce the dosage of alcohol during alcohol analysis, but the method will cause a large amount of brine waste, and
The brine waste of xanthan gum is current most intractable waste water.Those problems demands solve.
Summary of the invention
In order to solve the defect of above-mentioned pharmaceutical grade xanthan gum separating-purifying process, the invention proposes a kind of pharmaceutical grade xanthan
The refining methd of glue.Refining methd of the invention, it is heavy using calcium alginate crosslinking microsphere of zeolite using industrial grade xanthan gum as raw material
Form sediment separation xanthan gum, and resulting xanthan gum product can reach medicinal grade standard, meet 2015 editions the 4th pharmaceutical grade xanthan gum
Quality standard.
The present invention is realized by following Technology Ways:
A kind of refining methd of pharmaceutical grade xanthan gum comprising following step:
After S1 calcium alginate crosslinking microsphere of zeolite forms gel precipitation in industrial grade xanthan gum aqueous solution, filtering, it is heavy to obtain
Starch A;
The sediment A is dissolved in aqueous solution of alcohol by S2, and filtering obtains filtrate;
The filtrate is formed sediment B by S3 in alcoholic solvent;Wherein, the alcoholic solvent is alcohol-containing water described in step S2
Alcohol in solution;
The xanthan gum of pharmaceutical grade is washed, is drying to obtain to sediment B in step S3 by S4.
In step S1, the calcium alginate crosslinking microsphere of zeolite can preferably lead to be made by conventional method in that art
Cross following step acquisition: 1) by zeolite powder and sodium alginate aqueous solution, insulated and stirred obtains mixed liquor;Wherein, the zeolite powder is
Pass through the acid heat of 200 meshes treated zeolite;2) mixed liquor is added dropwise in calcium chloride solution, after stirring, is filtered, it will
Obtained solid is drying to obtain.The diameter of the calcium alginate crosslinking microsphere of zeolite is preferably 2.00 ± 0.05mm.
In step 1), the zeolite powder can be made by conventional method in that art, be obtained preferably by following step: i)
Zeolite after 0.5~1.5h of stirring in water bath, is removed and placed in Muffle furnace and is heated in the hydrochloric acid solution of 0.8~1.2mol/L
500~600 DEG C of 1.5~2.5h of heat preservation obtain acid heat treated zeolite;Ii) by the acid heat, treated that zeolite is ground to powder
Shape crosses 200 meshes;Obtain more preferably by following step: i) by 8g zeolite, water-bath is stirred in the hydrochloric acid solution of 1.0mol/L
It after mixing 1h, is removed and placed in Muffle furnace and is heated to 550 DEG C of heat preservation 2h, obtain acid heat treated zeolite;It ii) will be at the acid heat
Zeolite after reason is ground to powdery and crosses 200 meshes.Wherein, acid is carried out after the zeolite is generally first cleaned with deionized water again
Heat treatment.The operation of the grinding carries out generally in mortar.
In step 1), in the sodium alginate aqueous solution, the concentration of sodium alginate can be conventional for this field, and generally 1.0
~2.0%, preferably 1.5%.
In step 1), mass volume ratio 1:(9~11 of the zeolite powder and the sodium alginate aqueous solution) g/mL, more preferably
Ground is 1:10g/mL.
In step 1), the operation of the insulated and stirred and condition can be conventional for this field.The temperature one of the insulated and stirred
As be 30~50 DEG C, preferably 40 DEG C.The time of the insulated and stirred is generally 0.5~1.5h, preferably 1h.
In step 2), the operation of the dropwise addition and condition can be conventional for this field, are generally added dropwise using needle tubing.The chlorination
The concentration of calcium solution can be conventional for this field, generally 0.08~0.12mol/L, preferably 0.1mol/L.The stirring
Operation and condition can be conventional for this field, generally 9~11h of stirring, such as 10h.The operation of the filtering and condition can be this
Field is conventional, is generally filtered using filter paper.The operation of the drying and condition can be conventional for this field, generally at 60~70 DEG C
Dry 4~6h, such as the dry 5h at 65 DEG C.
In step S1, the industrial grade xanthan gum aqueous solution can be made by conventional method in that art, generally by technical grade
Xanthan gum is dissolved in purified water.According to common sense in the field it is found that the water used in the industrial grade xanthan gum aqueous solution
For purified water.The industrial grade xanthan gum can be commercially available any industrial grade xanthan gum.In the industrial grade xanthan gum, generally contain
Nitrogen quantity >=2.0%, acetone acid content≤1.0%, content of ashes≤20.0%, content of beary metal > 200ppm.
In step S1, in the industrial grade xanthan gum aqueous solution, the mass ratio of purified water and industrial grade xanthan gum can be this
Field is conventional, preferably (3-10): 1, be more preferably (4~9): 1, such as 5:1,6:1 or 8:1.
In step S1, the mass ratio of the calcium alginate crosslinking microsphere of zeolite and the industrial grade xanthan gum can be this field
It is conventional, preferably (0.01-0.1): 1, be more preferably (0.02-0.09): 1 such as 0.03:1,0.05:1,0.06:1 or
0.07:1。
In step S1, the temperature for forming gel precipitation can be conventional for this field, generally room temperature.The formation gel
The time of precipitating can be conventional for this field, preferably 30-200min, for example, 30min, 90min, 120min, 180min or
200min。
In step S1, the operation of the filtering and condition can be the operation and condition of this field routine, generally use filter cloth
Or filter paper filtering means dehydration.
In step S1, calcium salt and xanthan gum in solution form complex compound, change the hydrogen bond environment inside xanthan gum, into
And form gel.
In step S2, according to common sense in the field it is found that the aqueous solvent in the aqueous solution of alcohol is generally purified water.
The mass volume ratio of water in aqueous solution of alcohol described in sediment A described in step S1 and step S2 can be ability
Domain is conventional, preferably 1:(3-5) g/mL, such as 1:4g/mL.
The mass volume ratio of alcohol in aqueous solution of alcohol described in sediment A described in step S1 and step S2 can be ability
Domain is conventional, preferably 1:(0.5-2.5) g/mL, such as 1:1g/mL, 1:1.5g/mL or 1:2g/mL.
In step S2, the alcohol in the aqueous solution of alcohol can be the C of this field routine1~C3Alcohol, preferably methanol,
One of ethyl alcohol and isopropanol are a variety of.
In step S2, the operation of the filtering and condition can be the operation and condition of this field routine, generally use filter cloth
It is filtered.The mesh number of the filter cloth can routinely remove the mesh number that calcium alginate is crosslinked microsphere of zeolite for this field, generally
For 200~800 mesh, such as 200 mesh, 400 mesh or 800 mesh.
In step S2, xanthan gum is higher in the solubility of the alcoholic solution of low content, in the alcoholic solution of high-content solubility compared with
It is low, it can be precipitated.The purpose that water and alcoholic solvent are added in step S2 is to be soluble in xanthan gum in solution, and then filter seaweed
Sour calcium is crosslinked microsphere of zeolite.If being added without alcoholic solvent in step S2, it may occur that the phenomenon similar with step S1, xanthan gum are also shape
At gel.
In step S3, the alcoholic solvent can be the C of this field routine1~C3Alcohol, preferably methanol, ethyl alcohol and isopropyl
One of alcohol is a variety of.
The mass volume ratio of alcoholic solvent described in sediment A described in step S1 and step S3 can be conventional for this field, compared with
Goodly it is 1:(2~8) g/mL, such as 1:4g/mL, 1:5g/mL, 1:6g/mL, 1:7g/mL or 1:8g/mL.
The alcoholic solvent used in step S3 must be as the alcoholic solvent in S2, if the alcoholic solvent type in S2 and S3 is not
Together, the microenvironment in solution can be changed, and then influence the dissolution of xanthan gum.
In step S4, the operation of the washing and condition can be conventional for this field, generally use alcoholic solvent.The alcohol of washing
Solvent can be the C of this field routine1~C3Alcohol, preferably one of methanol, ethyl alcohol and isopropanol or a variety of.Step S1
Described in the mass volume ratio of alcoholic solvent of sediment A and washing can be conventional for this field, preferably 1:(0.01-0.05)
G/mL, such as 1:0.02g/mL, 1:0.03g/mL or 1:0.04g/mL.
In step S4, the operation of the drying and parameter can be conventional for this field.The temperature of the drying is preferably 60-
80 DEG C, such as 70 DEG C.The time of the drying is preferably 5-10h, such as 6h, 7h, 8h or 9h.
It is being original with industrial grade xanthan gum that the present invention also provides a kind of calcium alginate crosslinking microsphere of zeolite as adsorbent
Expect the application in purification medicinal grade xanthan gum.
In the present invention, calcium alginate is crosslinked microsphere of zeolite can be to be made by conventional method in that art, and specific method is as before
It is described.The diameter of the calcium alginate crosslinking microsphere of zeolite is preferably 2.00 ± 0.05mm.
In the present invention, the calcium alginate crosslinking microsphere of zeolite can preferably lead to be made by conventional method in that art
It is obtained to spend aforementioned the step of referring to.
In the present invention, the sediment A, the sediment B have no particular meaning, only indicate different sediment inhomogeneities
Type.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that:
The method that the present invention is crosslinked microsphere of zeolite absorption by calcium alginate, can be made medicinal by the xanthan gum of technical grade
Grade xanthan gum, meets the quality standard of 2015 editions the 4th pharmaceutical grade xanthan gum.Operating method of the invention is simple, at low cost
It is honest and clean, it can satisfy industrialized production.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
In following embodiments, calcium alginate is crosslinked microsphere of zeolite and can be made by conventional method in that art, such as its preparation
Method may include following step:
8g zeolite is taken, uses 1moL after being cleaned with deionized water-1Hydrochloric acid stirring in water bath 1h, take out and rinse and be put into Muffle
550 DEG C of heat preservation 2h are heated in furnace;Acid heat treated zeolite is taken out, powdery is worn into mortar and is sieved by the sieve of 200 mesh
It is spare;1.5% sodium alginate 150mL solution is mixed in stirring in water bath device with 15g zeolite powder, keeps 40 DEG C of temperature stirrings
Then 0.1molL is slowly added dropwise by needle tubing in 1h-1Calcium chloride solution continue stir 10h after, filter paper filtering, gained is consolidated
Body dry 5h at 65 DEG C again, obtains calcium alginate crosslinking microsphere of zeolite, diameter is in 2.00 ± 0.05mm.
Embodiment 1
S1 takes 100g industrial grade xanthan gum, is added in beaker, and 400mL purified water is added, and stirring and dissolving obtains technical grade Huang
Virgin rubber aqueous solution;Then 5g calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 120min, using filter cloth or
Person's filter paper is filtered, and obtains sediment A, about 100g;
400mL purified water, 100mL ethyl alcohol is added in S2 in sediment A, and stirring dissolves solid.With 200 mesh filter-cloth filterings
Calcium alginate is crosslinked microsphere of zeolite, obtains filtrate;
400mL ethyl alcohol is added in S3 in filtrate, forms sediment B;
S4 3g ethanol washing sediment B, 70 DEG C of dry 6h to get pharmaceutical grade xanthan gum product.
Embodiment 2
S1 takes 100g industrial grade xanthan gum, is added in beaker, and 300mL purified water is added, and stirring and dissolving obtains technical grade Huang
Virgin rubber aqueous solution;Then 1g calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 200min, using filter cloth or
Person's filter paper is filtered, and obtains sediment A, about 100g;
300mL purified water, 250mL methanol is added in S2 in sediment A, and stirring dissolves solid.With 400 mesh filter-cloth filterings
Calcium alginate is crosslinked microsphere of zeolite, obtains filtrate;
600mL methanol is added in S3 in filtrate, forms sediment B;
S4 1g methanol washing precipitate B, 60 DEG C of dry 10h are to get pharmaceutical grade xanthan gum product.
Embodiment 3
S1 takes 100g industrial grade xanthan gum, is added in beaker, and 1000mL purified water is added, and stirring and dissolving obtains technical grade
Xanthan gum solution;Then 10g calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 30min, using filter cloth
Or filter paper is filtered, and obtains sediment A, about 100g;
500mL purified water, 50mL isopropanol is added in S2 in sediment A, and stirring dissolves solid.With 800 mesh filter cloth mistakes
It filters calcium alginate and is crosslinked microsphere of zeolite, obtain filtrate;
800mL isopropanol is added in S3 in filtrate, forms sediment B;
S4 5g isopropanol washing precipitate B, 80 DEG C of dry 5h are to get pharmaceutical grade xanthan gum product.
Embodiment 4
S1 takes 10kg industrial grade xanthan gum, is added in beaker, and 50kg purified water is added, and stirring and dissolving obtains technical grade Huang
Virgin rubber aqueous solution;Then 0.6kg calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 150min, using filter cloth
Or filter paper is filtered, and obtains sediment A, about 10kg;
40kg purified water, 20kg ethyl alcohol is added in S2 in sediment A, and stirring dissolves solid.With 400 mesh filter-cloth filtering seas
Calcium alginate is crosslinked microsphere of zeolite, obtains filtrate;
40kg ethyl alcohol is added in S3 in filtrate, forms sediment B;
S4 0.2kg ethanol washing sediment B, 80 DEG C of dry 7h are to get pharmaceutical grade xanthan gum.
Embodiment 5
S1 takes 1000kg industrial grade xanthan gum, is added in beaker, and 6000kg purified water is added, and stirring and dissolving obtains industrial
Grade xanthan gum solution;Then 70k calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 90min, using filter
Cloth or filter paper are filtered, and obtain sediment A, about 1000kg;
3000kg purified water, 1500kg methanol is added in S2 in sediment A, and stirring dissolves solid.With 800 mesh filter cloth mistakes
It filters calcium alginate and is crosslinked microsphere of zeolite, obtain filtrate;
5000kg methanol is added in S3 in filtrate, forms sediment B;
S4 30kg methanol washing precipitate B, 60 DEG C of dry 9h are to get pharmaceutical grade xanthan gum.
Embodiment 6
S1 takes 1000kg industrial grade xanthan gum, is added in beaker, and 8000kg purified water is added, and stirring and dissolving obtains industrial
Grade xanthan gum solution;Then 30k calcium alginate is added and is crosslinked microsphere of zeolite, at room temperature, stirring and adsorbing 180min, using filter
Cloth or filter paper are filtered, and obtain sediment A, about 1000kg;
4000kg purified water, 2000kg isopropanol is added in S2 in sediment A, and stirring dissolves solid.With 200 mesh filter clothes
It filters calcium alginate and is crosslinked microsphere of zeolite, obtain filtrate;
7000kg isopropanol is added in S3 in filtrate, forms sediment B;
S4 40kg isopropanol washing precipitate B, 70 DEG C of dry 8h are to get pharmaceutical grade xanthan gum.
Comparative example 1
100g industrial grade xanthan gum is taken, is added in beaker, 400mL purified water, 400mL ethyl alcohol is added, stirring makes xanthan
Peptization solution.It filters, 400mL ethyl alcohol is added in filtrate, form precipitating.Solid is collected by filtration, sufficiently washs solid with 3g ethyl alcohol, 70
DEG C dry 6h, obtains xanthan gum.
Effect example
Table 1 be Examples 1 to 6, comparative example 1, nitrogen content in technical grade also virgin rubber and medicinal grade standard, pyruvic acid,
Ash content and heavy metal data.Wherein, nitrogen content, pyruvic acid, ash content and heavy metal are according to 2015 editions Chinese Pharmacopoeia xanthan gum
Item detection.
Table 1
Note: industrial grade xanthan gum, xanthan gum prepared by embodiment 1-6 and comparative example 1 other physical and chemical indexes (such as
Viscosity, loss on drying, arsenic, microbial limit) it is all satisfied 2015 editions standards of pharmacopoeia requirements.Comparative example 1 uses and 4 phase of embodiment
Same alcohol and identical alcohol dosage.The xanthan gum heavy metal that comparative example 1 produces does not meet pharmaceutical grade requirement, in ash content, acetone
It is not so good as quality of the invention on acid, content of beary metal.
Claims (10)
1. a kind of refining methd of pharmaceutical grade xanthan gum, which is characterized in that it includes the following steps:
After S1 calcium alginate crosslinking microsphere of zeolite forms gel precipitation in industrial grade xanthan gum aqueous solution, filtering obtains sediment
A;
The sediment A is dissolved in aqueous solution of alcohol by S2, and filtering obtains filtrate;
The filtrate is formed sediment B by S3 in alcoholic solvent;Wherein, the alcoholic solvent is aqueous solution of alcohol described in step S2
In alcohol;
The xanthan gum of pharmaceutical grade is washed, is drying to obtain to sediment B in step S3 by S4.
2. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that in step S1, the alginic acid
The diameter that calcium is crosslinked microsphere of zeolite is 2.00 ± 0.05mm;
And/or in step S1, the industrial grade xanthan gum aqueous solution is that industrial grade xanthan gum is dissolved in purified water to obtain;
In industrial grade xanthan gum, general nitrogen content >=2.0%, acetone acid content≤1.0%, content of ashes≤20.0%, heavy metal contains
Measure > 200ppm.
3. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that in step S1, the technical grade
In xanthan gum solution, the mass ratio of purified water and industrial grade xanthan gum is (3-10): 1, preferably (4-9): 1, such as 5:
1,6:1 or 8:1;
And/or in step S1, the mass ratio of the calcium alginate crosslinking microsphere of zeolite and industrial grade xanthan gum is (0.01-
0.1): 1, preferably (0.02-0.09): 1, such as 0.03:1,0.05:1,0.06:1 or 0.07:1;
And/or in step S1, it is described formed gel precipitation time be 30-200min, such as 90min, 120min or
180min。
4. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that sediment A described in step S1
Mass volume ratio with the water in aqueous solution of alcohol described in step S2 is 1:(3-5) g/mL, such as 1:4g/mL;
And/or the mass volume ratio of the alcohol in aqueous solution of alcohol described in sediment A described in step S1 and step S2 is 1:
(0.5-2.5) g/mL, such as 1:1g/mL, 1:1.5g/mL or 1:2g/mL;
And/or in step S2, the alcohol in the aqueous solution of alcohol is C1~C3Alcohol, preferably methanol, ethyl alcohol and isopropanol
One of or it is a variety of;
It is described to be filtered into filter-cloth filtering and/or in step S2.
5. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that in step S3, the alcoholic solvent
For C1~C3Alcohol, preferably one of methanol, ethyl alcohol and isopropanol or a variety of;
And/or the mass volume ratio of alcoholic solvent described in sediment A described in step S1 and step S3 is 1:(2~8) g/mL,
Such as 1:4g/mL, 1:5g/mL, 1:6g/mL or 1:7g/mL.
6. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that in step S4, the washing
Operation uses alcoholic solvent;The alcoholic solvent of washing is C1~C3Alcohol, preferably one of methanol, ethyl alcohol and isopropanol or
It is a variety of;The mass volume ratio of sediment A described in step S1 and the alcoholic solvent of washing is preferably 1:(0.01-0.05) g/
ML, such as 1:0.02g/mL, 1:0.03g/mL or 1:0.04g/mL;
And/or in step S4, the temperature of the drying is 60-80 DEG C, such as 70 DEG C;
And/or in step S4, the time of the drying is 5-10h, such as 6h, 7h, 8h or 9h.
7. the refining methd of pharmaceutical grade xanthan gum as described in claim 1, which is characterized in that in step S1, the alginic acid
Calcium is crosslinked microsphere of zeolite and is obtained by following step: 1) by zeolite powder and sodium alginate aqueous solution, insulated and stirred obtains mixed liquor;
Wherein, the zeolite powder is by the acid heats of 200 meshes treated zeolite;2) mixed liquor is added dropwise to calcium chloride solution
In, after stirring, obtained solid is drying to obtain by filtering.
8. such as the refining methd for the pharmaceutical grade xanthan gum that claim 7 is stated, which is characterized in that in step 1), the zeolite powder is logical
It crosses following step acquisition: i) after 0.5~1.5h of stirring in water bath, taking out zeolite simultaneously in the hydrochloric acid solution of 0.8~1.2mol/L
It is put into Muffle furnace and is heated to 500~600 DEG C of 1.5~2.5h of heat preservation, obtain acid heat treated zeolite;It ii) will be at the acid heat
Zeolite after reason is ground to powdery and crosses 200 meshes;It is obtained preferably by following step: i) by 8g zeolite in 1.0mol/L
Hydrochloric acid solution in after stirring in water bath 1h, be removed and placed in Muffle furnace and be heated to 550 DEG C of heat preservation 2h, obtain acid heat treated boiling
Stone;Ii) by the acid heat, treated that zeolite is ground to powdery crosses 200 meshes.
9. such as the refining methd for the pharmaceutical grade xanthan gum that claim 7 is stated, which is characterized in that in step 1), the sodium alginate
In aqueous solution, the concentration of sodium alginate is 1.0~2.0%, such as 1.5%;
And/or in step 1), mass volume ratio 1:(9~11 of the zeolite powder and the sodium alginate aqueous solution) g/mL, example
Such as 1:10g/mL;
And/or in step 1), the temperature of the insulated and stirred is 30~50 DEG C, such as 40 DEG C;
And/or in step 1), the time of the insulated and stirred is 0.5~1.5h, such as 1h;
And/or in step 2), the concentration of the calcium chloride solution is 0.08~0.12mol/L, such as 0.1mol/L.
10. a kind of calcium alginate crosslinking microsphere of zeolite is as adsorbent using industrial grade xanthan gum as feed purification pharmaceutical grade xanthan
Application in glue.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1046758A (en) * | 1989-04-29 | 1990-11-07 | 化工部天津化工研究院 | Extract the processing method of xanthan gum |
CN101210054A (en) * | 2007-12-24 | 2008-07-02 | 山东阜丰生物科技开发有限公司 | Method for extracting high transparent xanthan gum |
CN102659954A (en) * | 2011-12-16 | 2012-09-12 | 四川金稞生物科技有限公司 | Separation and purification technology of xanthan gum |
CN102671641A (en) * | 2012-05-24 | 2012-09-19 | 上海交通大学 | Preparation and application for nanometer SiO2 strengthened calcium alginate-xanthan gum composite absorbent |
CN103894121A (en) * | 2014-03-12 | 2014-07-02 | 上海交通大学 | Preparation and application of nano zeolite reinforced xanthan gum composite hydrogel functional microspheres |
JP5746834B2 (en) * | 2010-06-18 | 2015-07-08 | Dsp五協フード&ケミカル株式会社 | Cation-modified xanthan gum with excellent storage stability |
CN105646731A (en) * | 2016-04-05 | 2016-06-08 | 浙江立恩生物科技有限公司 | Method for preparing high-quality biological polysaccharide |
-
2019
- 2019-02-26 CN CN201910142596.1A patent/CN109796540A/en not_active Withdrawn
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1046758A (en) * | 1989-04-29 | 1990-11-07 | 化工部天津化工研究院 | Extract the processing method of xanthan gum |
CN101210054A (en) * | 2007-12-24 | 2008-07-02 | 山东阜丰生物科技开发有限公司 | Method for extracting high transparent xanthan gum |
JP5746834B2 (en) * | 2010-06-18 | 2015-07-08 | Dsp五協フード&ケミカル株式会社 | Cation-modified xanthan gum with excellent storage stability |
CN102659954A (en) * | 2011-12-16 | 2012-09-12 | 四川金稞生物科技有限公司 | Separation and purification technology of xanthan gum |
CN102671641A (en) * | 2012-05-24 | 2012-09-19 | 上海交通大学 | Preparation and application for nanometer SiO2 strengthened calcium alginate-xanthan gum composite absorbent |
CN103894121A (en) * | 2014-03-12 | 2014-07-02 | 上海交通大学 | Preparation and application of nano zeolite reinforced xanthan gum composite hydrogel functional microspheres |
CN105646731A (en) * | 2016-04-05 | 2016-06-08 | 浙江立恩生物科技有限公司 | Method for preparing high-quality biological polysaccharide |
Non-Patent Citations (9)
Title |
---|
中国农业出版社: "《现代食品生物技术》", 31 August 2002 * |
姚毅: "海藻酸钙交联沸石微球对污泥中重金属除去的模拟应用研究", 《中国优秀硕士学位全文数据库工程科技I辑》 * |
张帆 等: "钙离子诱导的海藻酸钠/黄原胶凝胶化临界行为研究", 《高分子学报》 * |
张泾生等: "《矿用药剂》", 30 November 2008, 冶金工业出版社 * |
易绍金 等: "《石油与环境微生物技术》", 31 July 2002 * |
李仲民 等: "海藻酸钙微球对亚甲基蓝的吸附行为", 《广西大学学报(自然科学版)》 * |
王向东 等: "《食品生物技术》", 30 September 2007, 东南大学出版社 * |
赵丹华 等: "CaC2O4/AR138-海藻酸钙复合微球的制备及吸附性能研究》", 《化学与生物工程》 * |
韩冠英 等: "黄原胶纯化工艺研究进展", 《中国生化药物杂质》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115703640A (en) * | 2021-08-13 | 2023-02-17 | 同济大学 | Molecular sieve microsphere material, preparation method and loudspeaker |
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