CN105295116A - Low-density gellan gum foam material and preparation method thereof - Google Patents
Low-density gellan gum foam material and preparation method thereof Download PDFInfo
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- CN105295116A CN105295116A CN201510755704.4A CN201510755704A CN105295116A CN 105295116 A CN105295116 A CN 105295116A CN 201510755704 A CN201510755704 A CN 201510755704A CN 105295116 A CN105295116 A CN 105295116A
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- gelling gum
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Abstract
The invention provides a low-density gellan gum foam material and a preparation method thereof. The low-density gellan gum foam material is made of high-acyl gellan gum or low-acyl gellan gum or the mixture of high-acyl gellan gum and low-acyl gellan gum and water or a mixed solvent formed by water and 1,4-dioxane. The preparation method of the low-density gellan gum foam material has the three steps of preparing a gellan gum solution, preparing gellan gum gel and preparing the low-density gellan gum foam material. The density of the low-density gellan gum foam material can approximate to 1 mg/cm<3>, and the low-density gellan gum foam material is of a three-dimensional network microhole structure, is good in foam uniformity and forming performance, and is expected to be applied in the field of food, biology, pharmaceuticals, chemical engineering, energy, environment, catalysis, optics and the like and the field of inertial confinement fusion (ICF) target materials. The preparation method of the low-density gellan gum foam material has the advantages that the process is simple, raw materials are easy to obtain, the preparation period is short, and environmental friendliness is achieved.
Description
Technical field
The invention belongs to foam materials field, be specifically related to a kind of low density gelling gum foam materials and preparation method thereof.
Background technology
Gelling gum is a kind of microorganism edible gum of Kelco company of the U.S. exploitation eighties in 20th century, it is by sphingomonas paucimobilis in neutral conditions, in the substratum formed for nitrogenous source and some inorganic salt for carbon source, ammonium nitrate with glucose, a kind of novel cell exocellular polysaccharide produced through aerobic fermentation.Gelling gum, according to the difference of acyl group content on molecular backbone chain, can be divided into high acyl gellan gum (HA, natural gelling gum) and low-acyl gellan gum (LA, deacylated gellan gum).After gelling gum is water-soluble, automatically can assemble between molecule and form double-spiral structure, stablize double-stranded reactive force mainly intermolecular hydrogen bonding, duplex is assembled further and can be formed tridimensional network, is convenient to trap water molecule and produces gelatin phenomenon.The gellifying property formed is remarkable, does not have toxicity, acid and alkali-resistance, not volatility, and temperature hysteresis is remarkable, and well, stability is desirable, has been widely used in the various fields such as pharmacy, food, chemical industry in recent years for histocompatibility and compatibility.At present, the investigation and application for gelling gum mainly concentrates on each gellike that gelling gum and gelling gum and other raw materials are formed jointly, and the investigation and application for gelling gum foam is few.In view of the performance of gelling gum gel uniqueness, by the low density gelling gum foam materials with vesicular structure that it is prepared by certain method, be expected to there is important application prospect in fields such as food, biology, medicine, chemical industry, environment, the energy, catalysis, optics and inertial confinement fusion (ICF) target materials.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of low density gelling gum foam materials, and another technical problem that the present invention will solve is to provide a kind of preparation method of low density gelling gum foam materials.
The main flow of low density gelling gum foam materials of the present invention and preparation method thereof in a heated state gelling gum is dissolved in solvent, make gelling gum solution, gelling gum solution forms gelling gum gel after cooling down, gelling gum gel directly can carry out vacuum lyophilization, or carries out CO after solvent exchange
2supercritical drying, obtained low density gelling gum foam materials.
Low density gelling gum foam materials of the present invention, is characterized in, described low density gelling gum foam materials comprises gelling gum and solvent; The mass percentage of gelling gum is 0.5% ~ 10%, and the mass percentage of solvent is 90% ~ 99.5%; Described gelling gum is high acyl gellan gum, low-acyl gellan gum or the mixture of the two; Described solvent is the mixed solvent of water or water and Isosorbide-5-Nitrae-dioxane.
The preparation method of low density gelling gum foam materials of the present invention, is characterized in, comprises the following steps:
A. prepare gelling gum solution, gelling gum is added in the solvent of 70 DEG C ~ 90 DEG C, under condensing reflux state, keep the temperature of 70 DEG C ~ 90 DEG C to be stirred to gelling gum and dissolve completely, obtain the gelling gum solution that achromaticity and clarification is transparent;
B. prepare gelling gum gel, the gelling gum solution obtained by step a injects mould, leaves standstill and cooling down to 0 ~ 40 DEG C, place more than 12 hours, obtain the gelling gum gel of clear homogeneous after sealing;
C. prepare low density gelling gum foam materials, drying treatment is carried out to the gelling gum gel that step b obtains, obtains the low density gelling gum foam materials of mould institute figuration shape.
Drying method described in step c is vacuum freeze-drying method or CO
2supercritical drying drying method.
Vacuum freeze-drying method is that then in vacuum-freeze-dry machine, carry out vacuum lyophilization, removal solvent, obtains the low density gelling gum foam materials of mould institute figuration shape by gelling gum gel quick freezing to solidifying.
CO
2supercritical drying drying method be first by gelling gum soak in replacement solvent, to displace in gel contained solvent by replacement solvent, then in supercritical drying instrument, carry out CO
2supercritical drying removing replacement solvent, obtains the low density gelling gum foam materials of mould institute figuration shape.
Replacement solvent is acetone or dehydrated alcohol.
Because solvent exists certain crystallization in freezing dry process, have certain destruction to the structure of gel, and in process of vacuum drying, the sublimation process of solvent exists certain surface tension, the gelling gum foam contraction therefore obtained is comparatively large, and pore structure is alligatoring comparatively; And adopt CO
2supercritical drying, solution is by the CO of supercritical state
2completely after displacement, then at slow releasing CO
2, in drying process, there is not the impact of solvent crystallization, surface tension has not existed yet, and therefore makes to adopt CO
2the low density gelling gum foam materials that supercritical drying obtains shrinks less, and pore structure is fine uniform more.Therefore, CO is adopted
2it is the preferred technical solution of the present invention that supercritical drying drying method carries out drying treatment.
Low density gelling gum foam materials of the present invention, density is minimum can close to 1mg/cm
3, there is three-dimensional netted microvoid structure.Low density gelling gum foam densities of the present invention is low, good uniformity, good moldability, is expected to be applied in the fields such as food, biology, medicine, chemical industry, the energy, environment, catalysis, optics and inertial confinement fusion (ICF) target material field; Low density gelling gum preparation method of the present invention has that technique is simple, raw material is easy to get, preparation cycle is short, eco-friendly feature.
Embodiment
By the following examples the present invention is further elaborated.But the present invention is not limited thereto, person skilled in art can do some nonessential transformation and adjustment to the present invention by foregoing according to the present invention, can by realizing the present invention with following specific embodiment diverse ways.
The experimental technique used in following embodiment if no special instructions, is the ordinary method of chemical and field of material preparation.
The material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1
Water purified for 100ml is added in flask, is heated to 90 DEG C, under whipped state, add high acyl gellan gum 0.1g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 3 hours.By the solution casting of this gelling gum in mould, Temperature fall to 20 DEG C, leaves standstill 24 hours, obtains gelling gum gel.With liquid nitrogen vapor by gelling gum gel quick freezing, the demoulding after vacuum lyophilization, obtains gelling gum foam, and sample rate is 1.89mg/cm
3.
Embodiment 2
Isosorbide-5-Nitrae-the dioxane of water purified for 80ml and 20ml is joined in flask, mixes and be heated to 70 DEG C, under whipped state, adding high acyl gellan gum 0.05g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 4 hours.By this gelling gum solution casting in mould, Temperature fall to 20 DEG C, leaves standstill 36 hours, obtains gelling gum gel.With liquid nitrogen vapor by gel quick freezing, the demoulding after vacuum lyophilization, obtains gelling gum foam, and sample rate is 1.65mg/cm
3.
Embodiment 3
Isosorbide-5-Nitrae-the dioxane of water purified for 80ml and 20ml is joined in flask, mixes and be heated to 70 DEG C, under whipped state, adding low-acyl gellan gum 0.1g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 5 hours.By this gelling gum solution casting in mould, Temperature fall to 30 DEG C, leaves standstill 24 hours, obtains gelling gum gel.With liquid nitrogen by gelling gum gel quick freezing, the demoulding after vacuum lyophilization, obtains gelling gum foam, and sample rate is 13.15mg/cm
3.
Embodiment 4
Isosorbide-5-Nitrae-the dioxane of water purified for 60ml and 40ml is joined in flask, mixes and be heated to 70 DEG C, under whipped state, adding low-acyl gellan gum 10g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 5 hours.By this gelling gum solution casting in mould, Temperature fall to 40 DEG C, leaves standstill 12 hours, obtains gelling gum gel.With the mixed solution of liquid nitrogen and acetone by gelling gum gel quick freezing, the demoulding after vacuum lyophilization, obtains gelling gum foam, and sample rate is 103.50mg/cm
3.
Embodiment 5
Water purified for 100ml is added in flask, is heated to 90 DEG C, under whipped state, add high acyl gellan gum 0.05g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 3 hours.By this gelling gum solution casting in mould, Temperature fall to 20 DEG C, leaves standstill 48 hours, obtains gelling gum gel.Gelling gum soak is carried out solvent exchange in acetone, within every 24 hours, changes an acetone, replace 4 times altogether.Then gelling gum gel is carried out CO
2the demoulding after supercritical drying, obtains gelling gum foam, and sample rate is 1.07mg/cm
3.
Embodiment 6
Isosorbide-5-Nitrae-the dioxane of water purified for 60ml and 40ml is joined in flask, mixes and be heated to 70 DEG C.Under whipped state, add low-acyl gellan gum 1g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 5 hours.By this gelling gum solution casting in mould, put into refrigerator and be cooled to 0 DEG C, leave standstill 24 hours, obtain gelling gum gel.Gelling gum soak is carried out solvent exchange in dehydrated alcohol, within every 24 hours, changes a dehydrated alcohol, replace 5 times altogether.Then gelling gum gel is carried out CO
2the demoulding after supercritical drying, obtains gelling gum foam, and sample rate is 11.26mg/cm
3.
Embodiment 7
Isosorbide-5-Nitrae-the dioxane of water purified for 50ml and 50ml is joined in flask, mixes and be heated to 70 DEG C.Under whipped state, add low-acyl gellan gum 0.5g, high acyl gellan gum 0.5g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 5 hours.By this gelling gum solution casting in mould, naturally cooling is cooled to 20 DEG C, leaves standstill 24 hours, obtains gelling gum gel.Soak is carried out solvent exchange in acetone, within every 24 hours, changes an acetone, replace 5 times altogether.Then gelling gum gel is carried out CO
2the demoulding after supercritical drying, obtains gelling gum foam, and sample rate is 10.87mg/cm
3.
Embodiment 8
Isosorbide-5-Nitrae-the dioxane of water purified for 80ml and 20ml is joined in flask, mixes and be heated to 80 DEG C.Under whipped state, add low-acyl gellan gum 6g, high acyl gellan gum 4g, continue the gelling gum solution that heated and stirred condensing reflux obtain clear for 5 hours.By this gelling gum solution casting in mould, naturally cooling is cooled to 20 DEG C, leaves standstill 24 hours, obtains gelling gum gel.Gelling gum soak is carried out solvent exchange in acetone, within every 24 hours, changes an acetone, replace 5 times altogether.Then gelling gum gel is carried out CO
2the demoulding after supercritical drying, obtains gelling gum foam, and sample rate is 101.57mg/cm
3.
Specific embodiment parameter is as shown in table 1.
Table 1
Claims (6)
1. a low density gelling gum foam materials, is characterized in that, described low density gelling gum foam materials comprises gelling gum and solvent; The mass percentage of gelling gum is 0.5% ~ 10%, and the mass percentage of solvent is 90% ~ 99.5%; Described gelling gum is high acyl gellan gum, low-acyl gellan gum or the mixture of the two; Described solvent is the mixed solvent of water or water and Isosorbide-5-Nitrae-dioxane.
2. a preparation method for low density gelling gum foam materials according to claim 1, is characterized in that, comprise the following steps:
A. prepare gelling gum solution, gelling gum is added in the solvent of 70 DEG C ~ 90 DEG C, under condensing reflux state, keep the temperature of 70 DEG C ~ 90 DEG C to be stirred to gelling gum and dissolve completely, obtain the gelling gum solution that achromaticity and clarification is transparent;
B. prepare gelling gum gel, the gelling gum solution obtained by step a injects mould, leaves standstill and cooling down to 0 ~ 40 DEG C, place more than 12 hours, obtain the gelling gum gel of clear homogeneous after sealing;
C. prepare low density gelling gum foam materials, drying treatment is carried out to the gelling gum gel that step b obtains, obtains the low density gelling gum foam materials of mould institute figuration shape.
3. low density gelling gum foam materials preparation method according to claim 2, is characterized in that: the drying method described in step c is vacuum freeze-drying method or CO
2supercritical drying drying method.
4. low density gelling gum foam materials preparation method according to claim 3, it is characterized in that: described vacuum freeze-drying method is to solidifying by gelling gum gel quick freezing, then in vacuum-freeze-dry machine, vacuum lyophilization is carried out, remove solvent, obtain the low density gelling gum foam materials of mould institute figuration shape.
5. low density gelling gum foam materials preparation method according to claim 3, is characterized in that: described CO
2supercritical drying drying method be first by gelling gum soak in replacement solvent, to displace in gel contained solvent by replacement solvent, then in supercritical drying instrument, carry out CO
2supercritical drying removing replacement solvent, obtains the low density gelling gum foam materials of mould institute figuration shape.
6. low density gelling gum foam materials preparation method according to claim 5, is characterized in that: described replacement solvent is acetone or dehydrated alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109007196A (en) * | 2018-08-10 | 2018-12-18 | 米盈食品科技(苏州)有限公司 | Collagent casing for sausages fruit juice jelly and preparation method containing the luxuriant isapgol husk of circle |
| CN111315811A (en) * | 2017-04-10 | 2020-06-19 | 时威尔生物科学 | Hydrogels for cell culture and biomedical applications |
| CN117384418A (en) * | 2023-10-24 | 2024-01-12 | 湘潭大学 | A kind of bio-based airgel thermal insulation material and its preparation method and application |
Citations (4)
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|---|---|---|---|---|
| US5382285A (en) * | 1993-04-06 | 1995-01-17 | Regents Of The University Of California | Biofoam |
| CN1275335A (en) * | 1999-03-31 | 2000-12-06 | 麦克内尔-Ppc股份有限公司 | Stable foam composition |
| CN102417606A (en) * | 2011-08-03 | 2012-04-18 | 武汉大学 | Preparation method of chitin aerogel |
| PT107200A (en) * | 2013-09-30 | 2015-03-30 | Faculdade De Ci Ncias E Tecnologia Da Universidade Nova De Lisboa | PROCESS FOR OBTAINING AEROGELS BASED ON ALFARROBA GUM |
-
2015
- 2015-11-10 CN CN201510755704.4A patent/CN105295116A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5382285A (en) * | 1993-04-06 | 1995-01-17 | Regents Of The University Of California | Biofoam |
| CN1275335A (en) * | 1999-03-31 | 2000-12-06 | 麦克内尔-Ppc股份有限公司 | Stable foam composition |
| CN102417606A (en) * | 2011-08-03 | 2012-04-18 | 武汉大学 | Preparation method of chitin aerogel |
| PT107200A (en) * | 2013-09-30 | 2015-03-30 | Faculdade De Ci Ncias E Tecnologia Da Universidade Nova De Lisboa | PROCESS FOR OBTAINING AEROGELS BASED ON ALFARROBA GUM |
Non-Patent Citations (1)
| Title |
|---|
| 宋健等: "《微胶囊化技术及应用》", 30 September 2001, 化学工业出版社 精细化工出版中心 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111315811A (en) * | 2017-04-10 | 2020-06-19 | 时威尔生物科学 | Hydrogels for cell culture and biomedical applications |
| CN109007196A (en) * | 2018-08-10 | 2018-12-18 | 米盈食品科技(苏州)有限公司 | Collagent casing for sausages fruit juice jelly and preparation method containing the luxuriant isapgol husk of circle |
| CN117384418A (en) * | 2023-10-24 | 2024-01-12 | 湘潭大学 | A kind of bio-based airgel thermal insulation material and its preparation method and application |
| CN117384418B (en) * | 2023-10-24 | 2024-09-06 | 湘潭大学 | A bio-based aerogel thermal insulation material and its preparation method and application |
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