CN109046190B - Pectin composite silicon dioxide aerogel and preparation method and application thereof - Google Patents
Pectin composite silicon dioxide aerogel and preparation method and application thereof Download PDFInfo
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- CN109046190B CN109046190B CN201811133309.2A CN201811133309A CN109046190B CN 109046190 B CN109046190 B CN 109046190B CN 201811133309 A CN201811133309 A CN 201811133309A CN 109046190 B CN109046190 B CN 109046190B
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- 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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- 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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- 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 pectin composite silicon dioxide aerogel and a preparation method and application thereof. The invention discloses a preparation method of pectin composite silicon dioxide aerogel, which comprises the following steps: step 1: adjusting the pH value of the sodium silicate solution to 3-4, adding pectin and silicon dioxide, and mixing to obtain a mixture; step 2: mixing the mixture with calcium ion-containing compound, and adjusting pH to 5-6 to obtain gel; and step 3: and (3) sequentially carrying out aging, solvent replacement and freeze drying on the gel to obtain the pectin composite silicon dioxide aerogel. In the preparation method, the calcium ions can well stabilize the pectin in the aerogel, the aerogel keeps a mesoporous structure, the network framework of the aerogel cannot be damaged by overlarge surface tension in the drying process, the cost is reduced, the operation is simple, and the industrial production is facilitated. Solves the technical problems that the prior preparation method needs to use a large amount of hydrophobic agent, thereby increasing the preparation cost, and the use of a large amount of hydrophobic agent brings great harm to the environment.
Description
Technical Field
The invention relates to the technical field of aerogel, in particular to pectin composite silicon dioxide aerogel and a preparation method and application thereof.
Background
Aerogels having low density, high surface area and low thermal conductivity are novel highly porous materials that can be used in the fields of thermal insulation, Cherenkov detectors, batteries, supercapacitors and catalysts. Among these, organic polymer aerogels, such as resorcinol formaldehyde, are derived from expensive and toxic materials. Therefore, inexpensive biomaterial aerogels based on biopolymers have attracted a wide range of attention.
As one of the natural polysaccharides, Pectin (PC) is considered biodegradable, biocompatible, abundant, non-toxic. Also in the last few years pectin aerogels have been developed and used in the field of drug delivery and thermal insulation. However, the addition of a hydrophobic agent is required to reduce the surface tension caused by the volatilization of liquid in pores in the prior art, the use of a large amount of hydrophobic agent increases the preparation cost, and the use of a large amount of hydrophobic agent brings great harm to the environment.
Disclosure of Invention
The invention provides pectin composite silica aerogel and a preparation method and application thereof, and solves the technical problems that a large amount of hydrophobing agent is required in the existing preparation method of the pectin composite silica aerogel, so that the preparation cost is increased, and the use of a large amount of hydrophobing agent brings great harm to the environment.
The specific technical scheme is as follows:
the invention provides a preparation method of pectin composite silicon dioxide aerogel, which comprises the following steps:
step 1: adjusting the pH value of the sodium silicate solution to 3-4, adding pectin and silicon dioxide, and mixing to obtain a mixture;
step 2: mixing the mixture with a calcium ion-containing compound and adjusting the pH to 5-6 to obtain a gel;
and step 3: and (3) sequentially carrying out aging, solvent replacement and freeze drying on the gel to obtain the pectin composite silicon dioxide aerogel.
Preferably, in the step 1, the concentration of the sodium silicate in the sodium silicate solution is 12-16%, and more preferably 12%;
after the pH is adjusted to 3-4 and before the pectin is added, the method further comprises the following steps: adding hydrochloric acid for first stirring; wherein the first stirring time is 0.5 h-1 h, more preferably 0.5h, and the first stirring speed is 600 rpm-800 rpm, more preferably 600 rpm;
after the pectin and the silicon dioxide are added, mixing is carried out by second stirring, wherein the second stirring time is 1-2 h, more preferably 1h, and the second stirring speed is 200-400 rpm, more preferably 300 rpm.
Preferably, in the step 2, the pH is adjusted to 5-6 by ammonia water, wherein the concentration of the ammonia water is 0.5-1 mol/L, and more preferably 0.5 mol/L;
after the pH is adjusted to 5-6, before obtaining the gel, the method further comprises the following steps: thirdly, stirring until the mixture is viscous; wherein the third stirring time is 10min to 30min, and more preferably 15 min.
Preferably, the calcium ion-containing compound is calcium chloride, and a calcium chloride solution is used for reaction;
preferably, after the aging and before the solvent replacement, the method further comprises: water washing and alcohol washing, more preferably 3 times, alcohol washing 3 times.
Preferably, the freeze-drying time is 24h to 48h, more preferably 24 h;
the temperature of the freeze-drying was-75 ℃.
Freeze drying is used because it is difficult to dry pectin silica aerogels at atmospheric pressure and cross-linking between aerogels is easily broken beyond 100 ℃, and pectin agglomerates into a mass.
Supercritical drying techniques are expensive and difficult to mass-produce.
Preferably, the mass ratio of the pectin to the silicon dioxide is 5: 100-3: 10, more preferably 3: 10.
preferably, the mass ratio of calcium ions in the calcium ion compound to the pectin is 0.04: 1-0.15: 1, more preferably 0.04: 1-0.08: 1, more preferably 0.08: 1.
preferably, the aging time is 3 to 12 hours, more preferably 3 hours;
the temperature of the aging is 60 ℃ to 70 ℃, and more preferably 60 ℃.
Preferably, the solvent displacement employs n-hexane.
Preferably, the number of times of solvent replacement is 2-3 times, more preferably 2 times;
the solvent replacement time is 24 h-48 h, and the solvent replacement interval is 12 h-24 h, more preferably, the replacement time is 24h, and the interval time is 12 h.
Preferably, after the solvent replacement and before the freeze-drying, the method further comprises: drying for 24-48 h under normal pressure, and more preferably 24 h.
It should be noted that in the present embodiment, the drying under normal pressure is only to dry a small amount of solvent on the surface, and a large amount of solvent is still locked inside the aerogel.
The invention also provides the pectin composite silicon dioxide aerogel prepared by the preparation method.
The invention also provides application of the pectin composite silicon dioxide aerogel in heavy metal adsorption.
Pectins are compounds of the hydroxyl and/or carboxyl groups of galacturonic acid (polysaccharide oxidation products) of polysaccharide matrices, and the formation of such pectins can occur by ion exchange and complexation mechanisms. And the functional groups on the pectin are combined with heavy metals, particularly carboxyl groups have great biological adsorption and heavy metal removal potential.
According to the technical scheme, the invention has the following advantages:
in the preparation method of the pectin composite silicon dioxide aerogel provided by the invention, the hydrophobic modification reagent is replaced by calcium ions, so that the cost of the reagent is reduced, the dosage is low, and the environment is not polluted. Because of the pectin in the fine stable aerogel of calcium ion ability, let the aerogel keep the structure of mesopore, make the network skeleton of aerogel can not destroyed by too big surface tension in the drying process, very be favorable to industrial production, in addition, through regulation and control calcium ion concentration, can make the pectin composite silicon dioxide aerogel of suitable specific surface area. The pectin composite silicon dioxide aerogel prepared by the method is easy to naturally degrade and very environment-friendly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a nitrogen elution profile and a pore size distribution diagram of the pectin composite silica aerogel according to the first embodiment of the present invention (the mass ratio of calcium ions to pectin is 0.08: 1, and the mass ratio of pectin to silica is 5%);
fig. 2 is a nitrogen elution profile and a pore size distribution diagram of the pectin composite silica aerogel according to the first embodiment of the present invention (the mass ratio of calcium ions to pectin is 0.08: 1, and the mass ratio of pectin to silica is 10%);
fig. 3 is a nitrogen elution profile and a pore size distribution diagram of the pectin composite silica aerogel according to the second embodiment of the present invention (the mass ratio of calcium ions to pectin is 0.08: 1, and the mass ratio of pectin to silica is 30%);
fig. 4 is an infrared spectrum comparison graph of pectin composite silica aerogel prepared when pectin and silica are provided in different proportions in the embodiment of the present invention (mass ratio of calcium ion to pectin is 0.08: 1).
Detailed Description
The embodiment of the invention provides pectin composite silica aerogel and a preparation method and application thereof, and aims to solve the technical problems that the existing preparation method of the pectin composite silica aerogel is high in cost, and the pectin composite silica aerogel is difficult to produce in large quantities by using an expensive critical drying technology and brings great harm to the environment.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The pectin composite silicon dioxide aerogel provided by the invention, the preparation method thereof and the raw materials and reagents used in the application can be purchased from the market.
The pectin composite silica aerogel provided by the present invention, and the preparation method and application thereof are further described below.
Example one
10mL of sodium silicate solution with the mass fraction of 12 percent is fully mixed with 1mL of concentrated hydrochloric acid by adding water to dilute the solution by 7 times until the pH is 3-4, the mixture is stirred for half an hour (the rotating speed is 600rpm), pectin which is pre-dissolved and has the mass ratio of silicon dioxide of 5 percent, 10 percent, 20 percent and 30 percent is respectively added, after the mixture is fully stirred for 1 hour, 1mL of calcium chloride solution (the mass ratio of calcium ions to pectin is 80mg/g) is added, after the mixture is fully stirred, 0.5mol/L of ammonia water is added to adjust the pH to be 5-6, the mixture is fully stirred for 0.5 hour (the rotating speed is 300rpm) until the mixture is viscous, a rotor is taken out, after the gelation is finished, a beaker mouth is sealed, the beaker is placed into an oven with the temperature of 60 ℃ for aging for 3 hours, the mixture is washed by water and alcohol for three times respectively to remove sodium and calcium ions in the gel, 10mL of normal hexane is added to replace water in pores, the replacement time is 24h, the replacement is carried out every 12h, and after drying for 24h under normal pressure, the pectin composite silicon dioxide aerogel is obtained by freeze drying for 24 h.
Example two
And (4) performing infrared spectroscopy, specific surface area and mesoporous structure determination on the pectin composite silica aerogel prepared in the first to fourth embodiments.
Referring to fig. 1, fig. 2, fig. 3 and table 1, fig. 1 to fig. 3 show a clear mesoporous structure, but the specific surface area is low, and may be too little pectin cannot cross-link silica well, but plays a role in plugging, and when the pectin content reaches 30%, the cross-linking between the two is sufficient, and the specific surface area is greatly increased. With the addition of calcium ions, the specific surface area of the pectin composite silica aerogel prepared by the embodiment of the invention is obviously higherLiter, from 197m2G to 578m2The pore volume is also increased, which shows that the gel is formed by combining the free carboxyl anions in the pectin molecules with calcium ions, and the calcium ions also play a certain role in strengthening the aerogel skeleton, but the pore structure is also changed, and as can be seen from fig. 1 and 2, the uniform columnar or ink bottle neck-shaped structure which is originally obvious in H2 gradually changes into the slit-shaped pore H3 structure formed by the flaky particles with the increase of pectin, which shows that the pectin gradually occupies the skeleton of the silica aerogel and generates accumulation on the surface of the aerogel.
As shown in FIG. 4, except for the pectin content of 0%, the rest of the pectin-silica aerogel has obvious carboxyl groups and corresponding ester groups, and no Si-C peak appears, which indicates that the methoxyl groups of pectin are hydrolyzed, and the generated hydroxyl groups are crosslinked with the silicon hydroxyl groups of the silica aerogel.
TABLE 1 specific surface area and pore volume values at a mass ratio of calcium ions to pectin of 80mg/g
| Sample name | Specific surface area (m)2/g) | Pore volume (cm)3/g) |
| 5% pectin composite aerogel | 197 | 0.41 |
| 10% pectin composite aerogel | 191 | 0.23 |
| 30% pectin composite aerogel | 578 | 1.05 |
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the pectin composite silicon dioxide aerogel is characterized by comprising the following steps:
step 1: adjusting the pH value of the sodium silicate solution to 3-4, adding pectin and silicon dioxide, mixing, and stirring for 1-2 h to obtain a mixture;
step 2: mixing the mixture with a calcium ion-containing compound and adjusting the pH to 5-6 to obtain a gel;
and step 3: and (3) sequentially carrying out aging, solvent replacement and freeze drying on the gel to obtain the pectin composite silicon dioxide aerogel.
2. The method according to claim 1, wherein the calcium ion-containing compound is calcium chloride.
3. The method according to claim 1, wherein the freeze-drying time is 24 to 48 hours;
the temperature of the freeze-drying was-75 ℃.
4. The preparation method according to claim 1, wherein the mass ratio of the pectin to the silica is 5: 100-3: 10.
5. the method according to claim 1, wherein the mass ratio of calcium ions in the calcium ion compound to the pectin is 0.04: 1-0.15: 1.
6. the method according to claim 1, wherein the aging time is 3 to 12 hours;
the aging temperature is 60-70 ℃.
7. The method according to claim 1, wherein the solvent substitution is carried out using n-hexane.
8. The method of claim 1, further comprising, after the solvent displacement and before the freeze-drying: drying for 24-48 h under normal pressure.
9. Pectin composite silica aerogel produced by the production method according to any one of claims 1 to 8.
10. Use of the pectin composite silica aerogel of claim 9 for adsorbing heavy metals.
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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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