CN108250321A - A kind of preparation method and applications of oxidized konjac glucomannan - Google Patents
A kind of preparation method and applications of oxidized konjac glucomannan Download PDFInfo
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- CN108250321A CN108250321A CN201611230947.7A CN201611230947A CN108250321A CN 108250321 A CN108250321 A CN 108250321A CN 201611230947 A CN201611230947 A CN 201611230947A CN 108250321 A CN108250321 A CN 108250321A
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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
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/009—Konjac gum or konjac mannan, i.e. beta-D-glucose and beta-D-mannose units linked by 1,4 bonds, e.g. from Amorphophallus species; Derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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Abstract
A kind of preparation method and applications of oxidized konjac glucomannan, it is characterised in that：Oxidized konjac glucomannan is prepared at a certain temperature through microwave ozone direct oxidation by konjaku glucomannan.This method carries out the ozone oxidation of konjaku glucomannan using microwave reaction, and the reaction time greatly shortens；The oxidability of ozone is strong, and catalyst and other chemical oxidation reagents need not be added in reaction process；Due to ozone, there is no residue problems, and also the residue problem without chemical reagent, the oxidized konjac glucomannan of gained can be used to the capsule material preparation of plant hollow capsule without further refinement treatment compared with the prior art, and production efficiency greatly improves.The oxidized konjac glucomannan impurity that is produced using this method is few, purity is high, the labor intensity of production is low, low in the pollution of the environment, at low cost, and production process has higher economic benefit and social benefit without waste discharge.
Description
Technical field
The present invention relates to a kind of preparation method and applications of oxidized konjac glucomannan, specifically direct using microwave ozone
Oxidized konjac glucomannan is made in oxidized konjac glucomannan, without being further processed, you can directly as production Amorphophallus rivieri glucomannan
The capsule material raw material of glycan Capsules, production efficiency greatly improve.
Background technology
Konjaku glucomannan（KGM）It is the main component of Araeceae Amorphophallus perennial herb tuberous plant konjaku, is
By D-Glucose and D-MANNOSE in 1: 1.6 ratio with the heteroglycan of β-Isosorbide-5-Nitrae glucosides key connection, KGM is after starch and fiber
Another, with excellent thickening property and unique gelling, in food, changes compared with the renewable resource of horn of plenty after element
The industries such as work, weaving, medicine have important purposes.KGM water imbibitions are strong, and large viscosity, swellbility in water is high, bulk solution
Up to 80~100 times；Since its colloidal sol viscosity is excessive and unstable, limits it and widely apply.
To improve KGM collosol stabilities and film forming, it is necessary to KGM is modified, reduce its viscosity.The modification side of KGM
Method has Physical, bioanalysis, chemical method.Physical is ground using colloid mill, cleanliness without any pollution, suitable for industrial production, but to carrying
The ability of high film build energy is limited.Bioanalysis uses enzymatic isolation method degradation konjaku powder, but since the specificity of enzyme is strong, the production cycle
It is long, it is of high cost, it easily loses activity not easy to maintain, these shortcomings all cause the method at present can not also extensive use.Chemical modification
Colloidal sol viscosity can be reduced, improves colloidal sol solid content, is method of modifying ideal at present.Part of hydroxyl on KGM strands
After being oxidized to carboxyl or being replaced by carboxymethyl, product oxidation Glucomannan（O-KGM）Or Carboxyl Methyl Glucomannan（CM-
KGM）Be highly soluble in water, aqueous solution is transparent, fine and smooth, good fluidity, and tool is a bit sticky, and be not easy by temperature, pH value, when
Between influence, stability, filming performance greatly improve, and expands its application field.
Patent CN 200510019212.5, CN201310396514.9 are reacted using KGM with hydrogen peroxide prepares O-KGM, specially
Sharp document CN201510062092.0 prepares O-KGM using KGM and sodium hypochlorite reaction, needs to add in sodium sulfite after reaction
Restore unreacted oxidant, then through ethanol precipitation, be filtered, washed and remove remaining sodium sulphate and sodium sulfite, again through drying
Multi step strategies is waited to obtain O-KGM.Patent document CN 201210132662.5, is obtained by the reaction using KGM and monoxone and potassium iodide
CM-KGM is also required to after reaction by acetone precipitation reactant, and washing precipitate is multiple repeatedly, then passes through for 50% and 80% ethyl alcohol
Soaked in absolute ethyl alcohol 10 hours to remove unreacted monoxone and potassium iodide, then could be obtained finally through 60 DEG C of freeze-day with constant temperature
The CM-KGM prepared available for Capsules.Common problem existing for the technique of existing chemical method modification Glucomannan is technique
Step is more and time-consuming, and multiple precipitation, carrying out washing treatment cause product yield low.
Microwave is a kind of frequency range in the GHz of 300 MHz~300, electricity of the respective wavelength in the range of the mm of 100 cm~1
Magnetic wave.Microwave carries out energy as a kind of electromagnetic wave, the propagation of reflection, transmission, refraction, diffraction and ghost with electromagnetic wave
The characteristics such as transmission.For polarizable medium（Such as water, polar organic matter）Microwave can be absorbed, and is converted into thermal energy, makes itself
Temperature increases.And microwave heating be different from traditional mode of heating, traditional heating mainly using heat transfer and thermal convection current come
It realizes, body surface is initially heated, and then heat from outward appearance to inner essence passes to inside again.Therefore within the initial stage of heating, object
Temperature distribution is non-uniform in portion, and after only reaching thermal balance, internal and external temperature just can be consistent.And during microwave heating, microwave is extremely strong to be worn
Saturating power can enter inside material, so as to realize the heating to object inside and outside entirety to a certain extent.In addition to thermal effect
It is not as caused by temperature " non-thermal effect " that outer microwave reaction is answered, which to also have one kind,.Microwave exacerbates the movement between material molecule, carries
The high average energy of molecule, reduces the activation energy of reaction, considerably increases the collision frequency of material molecule, make to be swift in response
It completes.The chemical modification reaction of KGM is both needed to carry out in the liquid phase, therefore microwave technology fully can be applied and be greatly speeded up
Chemical reaction velocity.
Ozone（O3）Also known as super oxygen is oxygen（O2）Allotrope.It is water-soluble, and solubility in water compared with
Oxygen is big, and the solubility of ozone in water is about 13 times higher than oxygen under room temperature normality normal pressure, 25 times higher than air, and it is anti-to be suitable for liquid phase
It should.The oxidability of ozone is extremely strong, and oxidation-reduction potential in water is 2.07 eV, is only second to fluorine（2.5 eV）, it is better than double
Oxygen water（1.28 eV）.Ozone molecule structure is very unstable, and half-life period is only 30~60 min.It is in water than in air
In be easier voluntarily to be decomposed into oxygen, therefore do not generate residual contamination, and conventional hydrogen peroxide oxidation needs pair after reaction
Unreacted hydrogen peroxide carries out electronation, further refines and removes chemical reducing agent, and processing step is troublesome and reduces production
The yield of product.In the present invention mainly using ozone strong oxidizing and the characteristic of noresidue.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of quick, easy and without chemical agent residue O-KGM, adopt
With microwave ozone direct oxidation KGM, pass through controlling reaction temperature（Microwave intensity）, ozone the ginsengs such as intake, time, pH value
Number, obtain a kind of low-viscosity, solubility property it is good, can gel O-KGM, and since ozone is there is no chemical residual, can divide naturally
Solution, the prior art compares prepared O-KGM, without being further processed, you can capsule material and vegetable protein as Capsules
Compound is formed, production cost is reduced, improves production efficiency.
A kind of method for preparing O-KGM with microwave ozone direct oxidation KGM of the present invention, this method is by the water of KGM
Solution microwave heating controls temperature at 10~80 DEG C, and it is small to be passed through the ozone contact reaction 0.2~4 generated by ozonization device
When, generate O-KGM；After reaction, product O-KGM directly forms compound with vegetable protein, through colloidal sol, keeps the temperature, dips in glue, dry
Plant hollow capsule is prepared after dry, demoulding, cutting, fitting.
Solvent is water.
The mass percentage concentration of ozone is 0~100 mg/L.
It is characteristic of the invention that preparing O-KGM using microwave ozone direct oxidation KGM, oxidant is ozone；Solvent is water.
Compared with the prior art the present invention, has the characteristics that following：（1）Oxidation is carried out to KGM using microwave ozone and prepares O-KGM,
Without other chemical reagent other than aqueous solvent in reaction process；（2）The time of oxidation reaction greatly shortens, by original 2~4
Hour shortens to 0.5~1 hour, i.e., sends out 2 times or more faster than conventional hydrogen peroxide oxidation reaction speed using microwave ozone；（3）Instead
After answering, do not need to be post-processed, the yield of product O-KGM can be based on 100%（Conventional hydrogen peroxide oxidation technique, reaction knot
It needs to carry out electronation after beam, multiple alcohol precipitation is filtered, washed post-processing operation, and yield is only 60%）；（4）Ozone reaction
After be converted into oxygen, noresidue, therefore be a kind of free from environmental pollution, technique cleaning compared with hydrogen peroxide is the method for oxidant,
It is environmental-friendly, meet energy conservation and environmental protection, the development trend of green chemical industry；（5）Prepared O-KGM solution is without dry, you can adds
Enter vegetable protein and form compound, be used to prepare the capsule material of Capsules, simplify the preparation process of Capsules, reduce life
Cost is produced, improves production efficiency.
Specific embodiment
Embodiment 1
1st, raw material selects：Purity is the KGM of 90 more than %；
2nd, reaction process：0.1 kg KGM are mixed with 10 kg water, the rotating speed stirring swelling of 100 r/min adds in microwave and carries
It takes in tank, opens air compressor and ozone generator, the ozone gas of 40 mg/L are passed into microwave extraction tank with 60 L/min
In reaction solution in, reaction temperature by certain microwave power control at 70 DEG C, 30 min of microwave radiation processing to get
OKGM aqueous solutions.
3rd, the detection method of OKGM carboxyls degree of substitution：
Precision measurement OKGM solution is appropriate, is diluted to 0.5 % concentration, precision adds in 0.1mol/L NaOH titrating solution 25mL, while stirring
Side heating water bath is mixed, being titrated to solution pink with the titration with hydrochloric acid liquid of 0.1mol/L while hot as indicator using phenolphthalein takes off, 30s
Do not become terminal, the volume of the consumed titration with hydrochloric acid liquid of record.Calculate the degree of substitution of OKGM（DS）.
DS=0.162A/ (1- 0.044A), A=(CNaOHVNaOH-CHClVHCl)/m；
In formula, A is neutralizes the amounts of NaOH that are consumed of OKGM, mmol/g；VNaOHFor the volume of NaOH titrating solutions, mL；CNaOHFor
The concentration of NaOH titrating solutions, mol/L；VHClFor the volume of titration with hydrochloric acid liquid, mL；CHClFor the concentration of titration with hydrochloric acid liquid, mol/L；m
For the quality of OKGM, g；The 0.162 mM quality for Glucomannan structural unit, g/mmol；0.044 is mM of carboxyl
Quality, g/mmol.
4th, product quality：The carboxyl degree of substitution that oxidized konjac glucomannan is detected by acid-base titration is 0.4812.
Embodiment 2
1st, raw material selects：Purity is the KGM of 85 more than %；
2nd, reaction process：0.2 kg KGM are mixed with 10 kg water, the rotating speed stirring swelling of 250 r/min, with 1% NaOH tune
The pH to 8.0 of reaction solution is saved, is added in microwave extraction tank, opens air compressor and ozone generator, the ozone gas of 60 mg/L
Body is passed into 60 L/min in the reaction solution in microwave extraction tank, and reaction temperature is controlled by certain microwave power at 60 DEG C
Under, 50 min of microwave radiation processing is to get OKGM aqueous solutions.
3rd, the detection method of OKGM carboxyls degree of substitution（With embodiment one）
4th, product quality：The carboxyl degree of substitution that OKGM is detected by acid-base titration is 0.4624.
Embodiment 3
1st, raw material selects：Purity is the KGM of 80 more than %；
2nd, reaction process：0.3 kg KGM are mixed with 10 kg water, the rotating speed stirring swelling of 100 r/min, with 1% HC1 tune
The pH to 6.0 of reaction solution is saved, is added in microwave extraction tank, opens air compressor and ozone generator, the ozone gas of 60 mg/L
Body is passed into 60 L/min in the reaction solution in microwave extraction tank, and reaction temperature is controlled by certain microwave power at 50 DEG C
Under, 60 min of microwave radiation processing is to get OKGM aqueous solutions.
3rd, the detection method of OKGM carboxyls degree of substitution（With embodiment one）
4th, product quality：The carboxyl degree of substitution that OKGM is detected by acid-base titration is 0.4528.
Embodiment 4
1st, raw material selects：Purity is the KGM of 95 more than %；
2nd, reaction process：0.3 kg KGM are mixed with 100 kg water, the rotating speed stirring swelling of 100 r/min adds in microwave and carries
It takes in tank, opens air compressor and ozone generator, the ozone gas of 80 mg/L are passed into microwave extraction tank with 60 L/min
In reaction solution in, reaction temperature by certain microwave power control at 60 DEG C, 60 min of microwave radiation processing to get
OKGM aqueous solutions.
3rd, the detection method of OKGM carboxyls degree of substitution（With embodiment one）
4th, product quality：The carboxyl degree of substitution that OKGM is detected by acid-base titration is 0.5383.
Embodiment 5
1st, raw material selects：Purity is the KGM of 95 more than %；
2nd, reaction process：0.3 kg KGM are mixed with 10 kg water, the rotating speed stirring swelling of 100 r/min adds in microwave and carries
It takes in tank, opens air compressor and ozone generator, the ozone gas of 100 mg/L are passed into Microwave Extraction with 60 L/min
In reaction solution in tank, reaction temperature by certain microwave power control at 60 DEG C, 60 min of microwave radiation processing to get
OKGM aqueous solutions.
3rd, the detection method of OKGM carboxyls degree of substitution（With embodiment one）
4th, product quality：The carboxyl degree of substitution that OKGM is detected by acid-base titration is 0.5439.
Embodiment 6 prepares Capsules
Colloidal sol：1000 mL of OKGM solution prepared by Example 3~5 adds in 15 g of soybean protein isolate, crosslinking agent trimerization
Sodium phosphate 1.8 g, 60 DEG C of reaction 2h.It adds in 12 g carragheens and is warming up to 80 DEG C, 30 min of insulated and stirred.Add in dodecyl
Sodium sulfonate 0.1g, 0.01 g of ethyl hydroxy benzoate, at 60 DEG C or so, insulated and stirred, vacuum outgas measures viscosity and reaches for temperature control
Colloidal sol is completed after it is required that.
Heat preservation：2 hours are kept the temperature after filtering for 50 ± 1 DEG C.
Dip in glue：Room temperature control is at 20~25 DEG C, 50 ± 1 DEG C of glue temperature, and the tringle of mold immerses glue to carrying at 4/5
Go out liquid level, stirring makes glue cool down gelatinization.
It is dry：In temperature 60 C, humidity 20~45%, dry reached to water content provides to require.
Demoulding cutting：Through de- evil spirit, pull out shell, konjaku glucomannan hollow capsule cap is made in cutting, fitting.
OKGM produced by the present invention has excellent film forming, therefore in the sol-process for preparing Capsules, does not need to
Add in the plasticisers such as glycerine.Prepared Capsules press 2015 editions four gelatin hollow capsule items of Chinese Pharmacopoeia under elasticity,
The compound standards of pharmacopoeia of the capsules such as friability, disintegration time, loss on drying Indexs measure.
Claims (8)
1. a kind of preparation method of oxidized konjac glucomannan, it is characterised in that：It is through microwave ozone oxygen by konjaku glucomannan
Change is directly prepared, the specific steps are：
The aqueous solution of konjaku glucomannan is added in microwave reactor, ozone is passed through, is reacted, after reaction, obtained
Oxidized konjac glucomannan, due to there is no a chemical residual, prepared oxidized konjac glucomannan need not move through alcohol precipitation, washing,
The last handling processes such as dry, you can used as the raw material for preparing konjaku glucomannan capsule；Wherein, the konjaku glucomannan
It is the konjaku flour of more than 85% Glucomannan or the konjakus purified product such as konjaku powder or konjac glucomannan from purity.
2. a kind of preparation method of oxidized konjac glucomannan according to claim 1, it is characterised in that：The konjaku
The mass concentration of the aqueous solution of Glucomannan is 0.1~10 %.
3. a kind of preparation method of oxidized konjac glucomannan according to claim 2, it is characterised in that：The konjaku
The aqueous solution mass concentration of Glucomannan is 1~3 %.
4. a kind of preparation method of oxidized konjac glucomannan according to claim 1, it is characterised in that：The ozone
It is to be made by corona discharge or ultra violet lamp air or oxygen.
5. a kind of preparation method of oxidized konjac glucomannan according to claim 1, it is characterised in that：With 0~60
Ozone is passed through in the microwave reactor by the speed of Lmin, and is stirred by the rotating speed using rotating speed as 50~250 r/min
Come into full contact with the aqueous solution of the ozone and the konjaku glucomannan；Wherein, the ozone concentration of the ozone is 0~100
mg/L。
6. a kind of preparation method of oxidized konjac glucomannan according to any one of claims 1 to 5, it is characterised in that：
The process conditions reacted are as follows：For control ph between 4~10, the pH value is by 1% HC1 or 1% NaOH
It adjusts；Reaction temperature is between 10~80 DEG C；Reaction time is between 0.2~4 hour.
7. a kind of preparation method of oxidized konjac glucomannan according to claim 6, it is characterised in that：Control ph exists
Between 6~8；Reaction temperature is between 50~70 DEG C.
8. a kind of preparation method of oxidized konjac glucomannan according to claim 6, it is characterised in that：Reaction time exists
Between 0.5~1 hour.
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| CN201611230947.7A CN108250321A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method and applications of oxidized konjac glucomannan |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380927A (en) * | 2022-02-28 | 2022-04-22 | 西南大学 | Modified glucomannan and preparation method thereof |
| CN116676812A (en) * | 2023-06-01 | 2023-09-01 | 华邦古楼新材料有限公司 | Chlorine-free reinforced food packaging paper |
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| CN101585889A (en) * | 2009-06-23 | 2009-11-25 | 西南大学 | Prepartion method of carboxymethyl konjac glucomannan (KGM) |
| CN103800576A (en) * | 2012-11-11 | 2014-05-21 | 龙再兴 | Konjac capsule |
| CN105985450A (en) * | 2015-02-05 | 2016-10-05 | 北京化工大学 | Modified konjac glucomannan and preparation method and application thereof |
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2016
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| CN101585889A (en) * | 2009-06-23 | 2009-11-25 | 西南大学 | Prepartion method of carboxymethyl konjac glucomannan (KGM) |
| CN103800576A (en) * | 2012-11-11 | 2014-05-21 | 龙再兴 | Konjac capsule |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380927A (en) * | 2022-02-28 | 2022-04-22 | 西南大学 | Modified glucomannan and preparation method thereof |
| CN116676812A (en) * | 2023-06-01 | 2023-09-01 | 华邦古楼新材料有限公司 | Chlorine-free reinforced food packaging paper |
| CN116676812B (en) * | 2023-06-01 | 2024-03-22 | 华邦古楼新材料有限公司 | Chlorine-free reinforced food packaging paper |
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Application publication date: 20180706 |