CN109046190A - A kind of pectin dioxide composite silica aerogel and the preparation method and application thereof - Google Patents
A kind of pectin dioxide composite silica aerogel and the preparation method and application thereof Download PDFInfo
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- CN109046190A CN109046190A CN201811133309.2A CN201811133309A CN109046190A CN 109046190 A CN109046190 A CN 109046190A CN 201811133309 A CN201811133309 A CN 201811133309A CN 109046190 A CN109046190 A CN 109046190A
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- pectin
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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
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
Abstract
The invention particularly relates to a kind of pectin dioxide composite silica aerogels and the preparation method and application thereof.The invention discloses a kind of preparation methods of pectin dioxide composite silica aerogel, comprising the following steps: step 1: adjusting sodium silicate solution pH to 3-4, pectin and silica mixing is added, obtains mixture；Step 2: adjusting pH to 5-6 after mixture is mixed with calcium ions compound, obtain gel；Step 3: gel successively being passed through to aging, solvent displacement and freeze-drying, obtains pectin dioxide composite silica aerogel.In the preparation method, the pectin that calcium ion can very well in stable aeroge allows aeroge to keep mesoporous structure, destroy the network skeleton of aeroge will not by excessive surface tension, and reduce cost, easy to operate, is conducive to industrialized production.A large amount of hydrophobing agents need to be used by solving existing preparation method, to increase preparation cost, and the use of a large amount of hydrophobing agents is the technical issues of environment brings very big harm.
Description
Technical field
The present invention relates to aeroge technical field more particularly to a kind of pectin dioxide composite silica aerogel and its preparation sides
Method and application.
Background technique
Aeroge has low-density, and the aeroge of high surface area and low heat conductivity is novel high porous material, can be used for
Heat-insulated, Cherenkov detector, battery, supercapacitor and catalyst field.Wherein, organic polymer aeroge, such as isophthalic
Diphenol formaldehyde, to be derived from expensive and toxic material.Therefore, the cheap biomaterial aeroge based on biopolymer draws
Extensive concern is played.
As one of natural polysaccharide, pectin (PC) be considered as it is biodegradable, it is biocompatible, it is abundant, it is nontoxic
's.And in past several years, pectin aeroge has been developed that and is used for drug conveying and insulation field.However, making at present
Make pectin dioxide composite silica aerogel to need that hydrophobing agent is added, to reduce the brought surface tension that evaporates in hole, greatly
The use for measuring hydrophobing agent increases preparation cost, and the use of a large amount of hydrophobing agents is that environment brings very big harm.
Summary of the invention
The present invention provides a kind of pectin dioxide composite silica aerogels and the preparation method and application thereof, solve existing fruit
Glue dioxide composite silica aerogel preparation method need to use a large amount of hydrophobing agents, thus increase preparation cost, and a large amount of hydrophobing agents
The technical issues of using very big harm is brought for environment.
Its specific technical solution is as follows:
The present invention provides a kind of preparation methods of pectin dioxide composite silica aerogel, comprising the following steps:
Step 1: after adjusting sodium silicate solution pH to 3-4, pectin and silica mixing is added, obtains mixture；
Step 2: adjusting pH to 5-6 after the mixture is mixed with calcium ions compound, obtain gel；
Step 3: the gel successively being passed through into aging, solvent displacement and freeze-drying, obtains pectin composite silicon dioxide
Aeroge.
Preferably, in step 1, the concentration of sodium metasilicate is 12%~16%, more preferably 12% in sodium silicate solution；
It after adjusting pH to 3-4, is added before pectin, further includes: hydrochloric acid is added and carries out the first stirring；Wherein, the first stirring
Time is 0.5h~1h, and more preferably 0.5h, the first speed of agitator is 600rpm~800rpm, more preferably 600rpm；
After pectin and silica is added, being mixed by the second stirring, wherein the second mixing time is 1h~2h,
More preferably 1h, the second speed of agitator are 200rpm~400rpm, more preferably 300rpm.
Preferably, in step 2, pH to 5-6 is adjusted by ammonium hydroxide, wherein the concentration of ammonium hydroxide is 0.5mol/L~1mol/L,
More preferably 0.5mol/L；
After adjusting pH to 5-6, before obtaining gel, further includes: third stirring, until viscous pasty state；Wherein, third stirs
Time is 10min~30min, more preferably 15min.
Preferably, the calcium ions compound is calcium chloride, and reacting used is calcium chloride solution；
Preferably, after the aging, before the solvent displacement, further includes: washing and alcohol are washed, and are more preferably washed 3 times, alcohol
It washes 3 times.
Preferably, the sublimation drying is for 24 hours~48h, more preferably for 24 hours；
The temperature of the freeze-drying is -75 DEG C.
Because being difficult to dry pectin aerosil under normal pressure, and it is easily destroyed between aeroge more than 100 DEG C
Crosslinking, pectin can be agglomerated into one piece, and described use is freeze-dried.
Supercritical Drying Technology is expensive, it is difficult to mass production.
Preferably, the mass ratio of the pectin and the silica is 5:100~3:10, more preferably 3:10.
Preferably, the mass ratio of calcium ion and the pectin is 0.04:1~0.15:1 in the ionic calcium cpd, into
One step is preferably 0.04:1~0.08:1, more preferably 0.08:1.
Preferably, the time of the aging is 3h~12h, more preferably 3h；
The temperature of the aging is 60 DEG C~70 DEG C, more preferably 60 DEG C.
Preferably, the solvent displacement uses n-hexane.
Preferably, the solvent displacement number is 2~3 times, more preferably 2 times；
The solvent time swap is for 24 hours~48h, 12h~for 24 hours is divided between solvent displacement, it is highly preferred that when displacement
Between for for 24 hours, interval time 12h.
Preferably, after solvent displacement, before the freeze-drying, further includes: constant pressure and dry for 24 hours~48h, it is more excellent
It is selected as 24 hours.
It should be noted that constant pressure and dry herein is a small amount of solvent in dry surface in the embodiment of the present invention, still have
A large amount of solvent locks are inside aeroge.
The present invention also provides pectin dioxide composite silica aerogels made from above-mentioned preparation method.
The present invention also provides application of the above-mentioned pectin dioxide composite silica aerogel in absorption heavy metal.
Pectin is the chemical combination of the hydroxyl of a kind of polysaccharide matrix and/or the carboxyl (polysaccharide oxidation product) of galacturonic acid composition
The formation of object, this fruit onium compound can be carried out by ion exchange and complexing mechanism.And the functional group on pectin with
Heavy metal combines, and especially carboxyl has very big biological adsorption and heavy metals removal potentiality.
As can be seen from the above technical solutions, the invention has the following advantages that
In the preparation method of pectin dioxide composite silica aerogel provided by the invention, hydrophobic modification is replaced to try with calcium ion
Agent reduces the expense of reagent, and dosage is few, not can cause environmental pollution.Because calcium ion can very well in stable aeroge pectin,
It allows aeroge to keep mesoporous structure, break the network skeleton of aeroge will not by excessive surface tension
It is bad, it is advantageous to industrialized production, in addition, the pectin of suitable specific surface area can be made by regulation calcium ion concentration
Dioxide composite silica aerogel.It is easy natural degradation by the pectin dioxide composite silica aerogel that the above method is prepared,
It is very environmentally friendly.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is that the pectin dioxide composite silica aerogel nitrogen that the embodiment of the present invention one provides washes desorption curve and its aperture
(mass ratio of calcium ion and pectin is 0.08:1 to distribution map, 5%) mass ratio of pectin and silica is；
Fig. 2 is that the pectin dioxide composite silica aerogel nitrogen that the embodiment of the present invention one provides washes desorption curve and its aperture
(mass ratio of calcium ion and pectin is 0.08:1 to distribution map, 10%) mass ratio of pectin and silica is；
Fig. 3 is that pectin dioxide composite silica aerogel nitrogen provided by Embodiment 2 of the present invention washes desorption curve and its aperture
(mass ratio of calcium ion and pectin is 0.08:1 to distribution map, 30%) mass ratio of pectin and silica is；
The compound dioxy of pectin that Fig. 4 is prepared when being pectin provided in an embodiment of the present invention and silica different proportion
SiClx aeroge infrared spectrum comparison diagram (mass ratio of calcium ion and pectin is 0.08:1).
Specific embodiment
The embodiment of the invention provides a kind of pectin dioxide composite silica aerogels and the preparation method and application thereof, for solving
Certainly existing pectin dioxide composite silica aerogel preparation method higher cost, and using expensive critical dry technology, so that fruit
The technical issues of glue dioxide composite silica aerogel is difficult to mass production, brings very big harm for environment.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Raw material and examination used in pectin dioxide composite silica aerogel provided by the invention and the preparation method and application thereof
Agent is available on the market.
Below just a kind of pectin dioxide composite silica aerogel provided by the present invention and the preparation method and application thereof do into
One step explanation.
Embodiment one
It is sufficiently mixed to be diluted with water the hydrochloric acid that 7 times obtain with 1ml concentrated hydrochloric acid for the sodium silicate solution that 10ml mass fraction is 12%
Be bonded to ph be 3-4, stir half an hour (revolving speed 600rpm), be separately added into dissolve in advance with silica quality ratio be 5%,
10%, 20% and 30% pectin, after 1h is sufficiently stirred, the calcium chloride solution of 1ml is added, and (mass ratio of calcium ion and pectin is
80mg/g), after being sufficiently stirred, it is 5-6 that the ammonium hydroxide that 0.5mol/L is added, which adjusts pH, and 0.5h is sufficiently stirred, and (revolving speed is
300rpm), until viscous pasty state, takes out rotor, after waiting gel to finish, sealed beaker mouth is put into the baking that temperature is 60 DEG C
Case aging 3h, by washing, alcohol is washed respectively three times, and to remove the sodium and calcium ion inside gel, the n-hexane displacement of 10mL is added
Water in hole out, time swap be for 24 hours, it is primary every 12h replacement, constant pressure and dry for 24 hours after, freeze-drying for 24 hours, obtains pectin
Dioxide composite silica aerogel.
Embodiment two
The carry out infrared spectroscopy for the pectin dioxide composite silica aerogel that embodiment one to four is prepared, specific surface area
It is measured with meso-hole structure.
Fig. 1, Fig. 2, Fig. 3 and table 1 are please referred to, Fig. 1 to Fig. 3 shows apparent meso-hole structure, but specific surface area is low, may
Due to very few pectin cannot good cross-linked silica, only played ponding, when pectin content reaches 30%, two
It is crosslinked sufficiently between person, specific surface area is promoted significantly.With the addition of calcium ion, the pectin that the embodiment of the present invention is prepared is multiple
It closes aerosil specific surface area significantly to be risen, by 197m2/ g to 578m2/ g, pore capacities also become larger, and illustrate
Free carboxy anion in pectin molecule and calcium binding and the gel formed, while calcium ion also plays aeroge skeleton
It is acted on to certain consolidation, but the structure in hole is also changed, and can be seen that increasing with pectin from Fig. 1 and Fig. 2, this
Being that it is poroid to slowly become the slit-shaped formed to sheet-like particle for the significantly uniform column of H2 or black bottleneck shape structure
H3 structure, this illustrates that pectin gradually occupies the skeleton of aerosil, and generates accumulation on aeroge surface.
As shown in figure 4, remaining pectin dioxide composite silica aerogel has other than content pectin content is 0%
Apparent carboxylic group, there are also corresponding ester groups, all the peak Si-C all do not occur, illustrate the methoxy group hydrolysis of pectin, raw
At the silicone hydroxyl of hydroxyl and aerosil be mutually crosslinked.
Specific surface area and pore capacities value when the mass ratio of 1 calcium ion of table and pectin is 80mg/g
| Sample ID | Specific surface area (m2/g) | Pore capacities (cm3/g) |
| 5% pectin composite aerogel | 197 | 0.41 |
| 10% pectin composite aerogel | 191 | 0.23 |
| 30% pectin composite aerogel | 578 | 1.05 |
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of pectin dioxide composite silica aerogel, which comprises the following steps:
Step 1: after adjusting sodium silicate solution pH to 3-4, pectin and silica mixing is added, obtains mixture；
Step 2: adjusting pH to 5-6 after the mixture is mixed with calcium ions compound, obtain gel；
Step 3: the gel successively being passed through into aging, solvent displacement and freeze-drying, obtains pectin composite silicon dioxide airsetting
Glue.
2. preparation method according to claim 1, which is characterized in that the calcium ions compound is calcium chloride.
3. preparation method according to claim 1, which is characterized in that the sublimation drying is for 24 hours~48h；
The temperature of the freeze-drying is -75 DEG C.
4. preparation method according to claim 1, which is characterized in that the mass ratio of the pectin and the silica is
5:100~3:10.
5. preparation method according to claim 1, which is characterized in that calcium ion and the fruit in the ionic calcium cpd
The mass ratio of glue is 0.04:1~0.15:1.
6. preparation method according to claim 1, which is characterized in that the time of the aging is 3h~12h；
The temperature of the aging is 60 DEG C~70 DEG C.
7. preparation method according to claim 1, which is characterized in that the solvent displacement uses n-hexane.
8. preparation method according to claim 1, which is characterized in that described freeze-dried after the solvent displacement
Before, further includes: constant pressure and dry for 24 hours~48h.
9. pectin dioxide composite silica aerogel made from preparation method described in claim 1 to 8 any one.
10. application of the pectin dioxide composite silica aerogel as claimed in claim 9 in absorption heavy metal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023737A (en) * | 2021-03-08 | 2021-06-25 | 山西阳中新材有限责任公司 | Preparation method of aerogel not prone to powder falling |
| CN115124755A (en) * | 2022-07-12 | 2022-09-30 | 中国农业科学院农产品加工研究所 | Method for adjusting porous structure and texture of freeze-dried pectin aerogel |
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| CN115124755B (en) * | 2022-07-12 | 2023-06-20 | 中国农业科学院农产品加工研究所 | Method for regulating porous structure and texture of freeze-dried pectin aerogel |
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