CN105727628A - Aminated gelatin and nano-silicon dioxide composite air filtration material and preparation method thereof - Google Patents
Aminated gelatin and nano-silicon dioxide composite air filtration material and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/02—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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention provides an aminated gelatin and nano-silicon dioxide composite air filtration material and a preparation method thereof.The method comprises the steps that an aminated gelatin solution and nano-silicon dioxide are mixed and stirred for 1-2 h under the condition of 40 DEG C, a crosslinking agent is added, the materials are stirred for 0.5-2 h under the condition of 40 DEG C, and then the aminated gelatin and nano-silicon dioxide composite air filtration material is obtained through a repeated directional freezing method.The prepared aminated gelatin and nano-silicon dioxide composite air filtration material has multistage pore diameter distribution in the filtration direction and conducts classifying filtration on solid particles with different sizes in air, and good filtration efficiency is achieved; meanwhile, aminated gelatin has a good adsorption effect on formaldehyde in the air; the raw materials are wide in source and environmentally degradable.Therefore, the prepared aminated gelatin and nano-silicon dioxide composite air filtration material has good market application value and prospects.
Description
Technical field
The present invention relates to filtering material field, be specifically related to a kind of amination gelatin/nano silicon composite air filtering material and preparation method thereof.
Background technology
Along with the continuous propelling of China's process of industrialization, problem of environmental pollution becomes increasingly conspicuous, and especially air pollution problems inherent has badly influenced life and the health of people.Prominent environmental problem makes people that air-polluting consciousness of self-protection day by day be strengthened, and the application of air purifier and particulate matter protective mask is increasingly extensive, and researching and developing new and effective air filting material becomes the focus that scientific research is paid close attention to.
Existing indoor air filtration material mainly has fiber felt, filter membrane and porous ceramic film material in the market, and it is mainly used in microorganism, particulate matter and the harmful gas etc. that filter, absorb in room air.Wherein, glass fiber and activated carbon compound the fiber felt filtering material prepared is widely used because its volume is little, lightweight, filter efficiency is high.But there are some insoluble problems in this filtering material: (1) is certain due to aperture, it is therefore desirable to the felt compound of multilamellar different pore size is to realize the obstruct to different-grain diameter pollutant；(2) this materials'use glass fiber and the harmful gas in activated carbon composite adsorption air, this inserted complex method reduces the specific surface area of activated carbon, reduces limited adsorption capacity；(3) filtering material reaching service life and be replaced contains a large amount of pollutant cannot be recycled, its not degraded by environment after being dropped, and causes the secondary pollution of environment.
Gelatin is the product of collagenous portion hydrolysis in animal tissue, its wide material sources, environmental friendliness degradable, and gelatin molecule have a large amount of active group, can the harmful gas in absorbed air to a certain extent, therefore gelatin being used for prepares air filting material there is its distinctive advantage.But because of gelatin materials bad mechanical strength, poor water resistance and be difficult to form well-regulated pore passage structure so that the gelatin application in air filting material field is restricted.Research finds, method can significantly improve the mechanical performance of gelatin based material, block-water performance etc. to use cross-linking modified and nano-particles filled modified etc..Adopt gelatin based material prepared by directed freezing method to have gradient clear opening structure, the classified filtering of layer of material can be realized by changing freezing conditions adjustment aperture size, it is to avoid hole is blocked at short notice, improves filter efficiency.
The present invention is prepared for a kind of amination gelatin/nano silicon composite air filtering material with amination gelatin and nano silicon for raw material.Gelatin after amino modified is mixed with nano silica microsphere, adds a small amount of dialdehyde cross-linking agent, by directed freezing method, while forming straight-through aperture, carry out cross-linking reaction, obtain the air filting material with good filtration and absorption property.Prepare the gelatin used in material can be enhanced about more than once for the adsorbance of formaldehyde after amination modified.The nano silica microsphere added is positioned at solid liquid interface place in directed refrigerating process, contributes to forming the two grades of unstable states being perpendicular to solidification direction, it is possible to increase the length of clear opening in porous material.Additionally, the mechanical strength of all right reinforcing material of nano silicon embedding amination gelatin, improve the adsorption efficiency of material.
Summary of the invention
In order to prepare the gelatin-based nanometer air filting material with straight-through aperture and high adsorption efficiency, gelatin amination is obtained the amination gelatin with cationic property by the present invention, improve the ability of the harmful gass such as gelatin formaldehyde adsorption, methanol and microbes in air, add nano silica microsphere and improve mechanical strength, be made for the amination gelatin/nano silicon composite air filtering material with clear opening by directed freezing method.
The present invention provides a kind of composite air filtering material, and its preparation method is as follows:
(1) 1 parts by volume pH value is prepared to be 5 mass concentrations is the gelatin phosphate buffer solution of 1% ~ 5%, add the amino supply reagent of gelatin dry weight 2 ~ 5 times, pH value with the hydrochloric acid solution above-mentioned buffer solution of adjustment of 5mol/L is 5 again, it is subsequently adding 1-(3-the dimethyl aminopropyl)-3-ethyl carbodiimide salt accounting for gelatin dry weight 30% ~ 50% and the phosphate buffer solution using pH to be 5 is settled to 2 parts by volume, after reacting 4 ~ 48 hours under 30 ~ 40 DEG C of conditions, being dialysed 3 ~ 5 days by mixed liquor, lyophilization obtains amination gelatin；
(2) preparation mass concentration is the amination aqueous gelatin solution of 1% ~ 10%, add the nano silica microsphere accounting for gelatin dry weight 10% ~ 50% under fast stirring, stir 1 ~ 2 hour under 40 DEG C of conditions, it is subsequently adding the cross-linking agent accounting for gelatin dry weight 1% ~ 10%, continue to stir 0.5 ~ 2 hour under 40 DEG C of conditions, mixed liquor is poured in mould afterwards and at room temperature stand 1 ~ 3 hour, obtain amination gelatin/nano silicon mixed solution；
(3) will be equipped with the mold bottom of amination gelatin/nano silicon mixed solution and be placed in liquid nitrogen directed freezing 2 ~ 10 minutes, afterwards freezing sample is placed 1 ~ 4 day under-20 DEG C of conditions, then mold bottom is placed on 5 ~ 30 DEG C of sea water baths 1 ~ 10 minute, then again mold bottom is placed in liquid nitrogen directed freezing 2 ~ 10 minutes, placing 1 ~ 4 day under-20 DEG C of conditions afterwards, last lyophilization obtains amination gelatin/nano silicon composite air filtering material.
The amino supply reagent used in amination modified gelatin preparation process described in above-mentioned technology case is 1,2-ethylenediamine, diethylenetriamine, triethylene tetramine, 1, any one or a few mixture in 3-propane diamine, 1,6-hexamethylene diamine and spermine hydrochlorate.
The cross-linking agent used in amination gelatin described in above-mentioned technology case/nano silicon composite air filtering material preparation process is any one or a few the mixture in dialdehyde xanthan gum, dialdehyde starch, dialdehyde carboxymethyl cellulose, dialdehyde pulullan polysaccharide, dialdehyde sodium alginate, dialdehyde Weilan gum, dialdehyde guar gum, Biformyl, carbodiimide, vanillin, glutaraldehyde and dialdehyde Polyethylene Glycol.
The ratio dry weight of the nano silicon described in above-mentioned technology case and gelatin is 1:(2 ~ 10).
Compared with the prior art the present invention, has many-sided good effect and advantage, can inductive generalization as follows.
(1) a kind of amination gelatin/nano silicon composite air filtering material provided by the invention and preparation method thereof, its base stock gelatin can be extracted by leather industry garbage and obtain, gelatin materials after cross-linking modified has good mechanical strength, the porous material with micron order aperture can be formed, be a kind of environmentally friendly high-efficiency air filtering material.
(2) present invention uses amination gelatin/nano silicon composite air filtering material that directed freezing method prepares to be a kind of material with gradient clear opening, the cascade filtration of layer of material can be realized, avoid hole blocked at short notice, improve filter efficiency.
(3) present invention uses amidized gelatin to be raw material, the ability of the harmful gass such as air filting material formaldehyde adsorption can not only be strengthened, but also air filting material can be promoted to have the ability of microorganism in absorbed air, there is good market using value and prospect.
(4) present invention adopts cross-linking modified and that nano-particles filled is modified method to enhance the mechanical performance of gelatin-based air filting material, meets the requirement of its market application and the air filting material environmental friendliness degradable of preparation.
Specific implementation method
Three embodiments of the present invention are given below, by embodiment, the present invention are specifically described.Be necessary it is pointed out here that, embodiment is served only for the present invention is further detailed, it is impossible to be interpreted as limiting the scope of the invention, and the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Prepare 1 parts by volume pH value to be 5 mass concentrations be the gelatin phosphate buffer solution of 1%, add the diethylenetriamine of gelatin dry weight 3 times, pH value with the hydrochloric acid solution above-mentioned buffer solution of adjustment of 5mol/L is 5 again, it is subsequently adding 1-(3-the dimethyl aminopropyl)-3-ethyl carbodiimide salt accounting for gelatin dry weight 40% and the phosphate buffer solution using pH to be 5 is settled to 2 parts by volume, after reacting 5 hours under 30 DEG C of conditions, being dialysed 3 days by mixed liquor, lyophilization obtains amination gelatin.Preparation mass concentration is the amination aqueous gelatin solution of 1%, add the nano silica microsphere accounting for gelatin dry weight 12% under fast stirring, stir 1 hour under 40 DEG C of conditions, it is subsequently adding the cross-linking agent accounting for gelatin dry weight 3%, continue to stir 2 hours under 40 DEG C of conditions, mixed liquor is poured in mould afterwards and at room temperature stand 2 hours, obtain amination gelatin/nano silicon mixed solution；Will be equipped with the mold bottom of amination gelatin/nano silicon mixed solution and be placed in liquid nitrogen directed freezing 9 minutes, afterwards freezing sample is placed 4 days under-20 DEG C of conditions, then mold bottom is placed in 10 DEG C of sea water bath upper 5 minutes, then again mold bottom is placed in liquid nitrogen directed freezing 3 minutes, placing 3 days under-20 DEG C of conditions afterwards, last lyophilization obtains amination gelatin/nano silicon composite air filtering material.
Embodiment 2
Prepare 1 parts by volume pH value to be 5 mass concentrations be the gelatin phosphate buffer solution of 4%, add the 1 of gelatin dry weight 2 times, 2-ethylenediamine, pH value with the hydrochloric acid solution above-mentioned buffer solution of adjustment of 5mol/L is 5 again, it is subsequently adding 1-(3-the dimethyl aminopropyl)-3-ethyl carbodiimide salt accounting for gelatin dry weight 30% and the phosphate buffer solution using pH to be 5 is settled to 2 parts by volume, after reacting 36 hours under 37 DEG C of conditions, being dialysed 5 days by mixed liquor, lyophilization obtains amination gelatin.Preparation mass concentration is the amination aqueous gelatin solution of 5%, add the nano silica microsphere accounting for gelatin dry weight 50% under fast stirring, stir 2 hours under 40 DEG C of conditions, it is subsequently adding the cross-linking agent accounting for gelatin dry weight 2%, continue to stir 1 hour under 40 DEG C of conditions, mixed liquor is poured in mould afterwards and at room temperature stand 3 hours, obtain amination gelatin/nano silicon mixed solution；Will be equipped with the mold bottom of amination gelatin/nano silicon mixed solution and be placed in liquid nitrogen directed freezing 3 minutes, afterwards freezing sample is placed 3 days under-20 DEG C of conditions, then mold bottom is placed in 15 DEG C of sea water bath upper 2 minutes, then again mold bottom is placed in liquid nitrogen directed freezing 2 minutes, placing 2 days under-20 DEG C of conditions afterwards, last lyophilization obtains amination gelatin/nano silicon composite air filtering material.
Embodiment 3
Prepare 1 parts by volume pH value to be 5 mass concentrations be the gelatin phosphate buffer solution of 2%, add the triethylene tetramine of gelatin dry weight 4 times, pH value with the hydrochloric acid solution above-mentioned buffer solution of adjustment of 5mol/L is 5 again, it is subsequently adding 1-(3-the dimethyl aminopropyl)-3-ethyl carbodiimide salt accounting for gelatin dry weight 50% and the phosphate buffer solution using pH to be 5 is settled to 2 parts by volume, after reacting 24 hours under 40 DEG C of conditions, being dialysed 4 days by mixed liquor, lyophilization obtains amination gelatin.Preparation mass concentration is the amination aqueous gelatin solution of 3%, add the nano silica microsphere accounting for gelatin dry weight 45% under fast stirring, stir 1 hour under 40 DEG C of conditions, it is subsequently adding the cross-linking agent accounting for gelatin dry weight 1%, continue to stir 1.5 hours under 40 DEG C of conditions, mixed liquor is poured in mould afterwards and at room temperature stand 1 hour, obtain amination gelatin/nano silicon mixed solution；Will be equipped with the mold bottom of amination gelatin/nano silicon mixed solution and be placed in liquid nitrogen directed freezing 8 minutes, afterwards freezing sample is placed 2 days under-20 DEG C of conditions, then mold bottom is placed in 20 DEG C of sea water bath upper 1 minutes, then again mold bottom is placed in liquid nitrogen directed freezing 4 minutes, placing 2 days under-20 DEG C of conditions afterwards, last lyophilization obtains amination gelatin/nano silicon composite air filtering material.
Claims (3)
1. amination gelatin/nano silicon composite air filtering material, it is characterized in that first being mixed homogeneously with nano silica microsphere by amination gelatin, add cross-linking agent afterwards, then adopting repeatedly directed freezing method to prepare amination gelatin/nano silicon composite air filtering material, its concrete preparation method is as follows:
(1) 1 parts by volume pH value is prepared to be 5 mass concentrations is the gelatin phosphate buffer solution of 1% ~ 5%, add the amino supply reagent of gelatin dry weight 2 ~ 5 times, pH value with the hydrochloric acid solution above-mentioned buffer solution of adjustment of 5mol/L is 5 again, it is subsequently adding 1-(3-the dimethyl aminopropyl)-3-ethyl carbodiimide salt accounting for gelatin dry weight 30% ~ 50% and the phosphate buffer solution using pH to be 5 is settled to 2 parts by volume, after reacting 4 ~ 48 hours under 30 ~ 40 DEG C of conditions, being dialysed 3 ~ 5 days by mixed liquor, lyophilization obtains amination gelatin；
(2) preparation mass concentration is the amination aqueous gelatin solution of 1% ~ 10%, add the nano silica microsphere accounting for gelatin dry weight 10% ~ 50% under fast stirring, stir 1 ~ 2 hour under 40 DEG C of conditions, it is subsequently adding the cross-linking agent accounting for gelatin dry weight 1% ~ 10%, continue to stir 0.5 ~ 2 hour under 40 DEG C of conditions, mixed liquor is poured in mould afterwards and at room temperature stand 1 ~ 3 hour, obtain amination gelatin/nano silicon mixed solution；
(3) will be equipped with the mold bottom of amination gelatin/nano silicon mixed solution and be placed in liquid nitrogen directed freezing 2 ~ 10 minutes, afterwards freezing sample is placed 1 ~ 4 day under-20 DEG C of conditions, then mold bottom is placed on 5 ~ 30 DEG C of sea water baths 1 ~ 10 minute, then again mold bottom is placed in liquid nitrogen directed freezing 2 ~ 10 minutes, placing 1 ~ 4 day under-20 DEG C of conditions afterwards, last lyophilization obtains amination gelatin/nano silicon composite air filtering material.
2. amination gelatin/nano silicon composite air filtering material according to claim 1, it is characterized in that described amino supply reagent is 1,2-ethylenediamine, diethylenetriamine, triethylene tetramine, 1, any one or a few mixture in 3-propane diamine, 1,6-hexamethylene diamine and spermine hydrochlorate.
3. amination gelatin/nano silicon composite air filtering material according to claim 1, it is characterised in that described cross-linking agent is any one or a few the mixture in dialdehyde xanthan gum, dialdehyde starch, dialdehyde carboxymethyl cellulose, dialdehyde pulullan polysaccharide, dialdehyde sodium alginate, dialdehyde Weilan gum, dialdehyde guar gum, Biformyl, carbodiimide, vanillin, glutaraldehyde and dialdehyde Polyethylene Glycol.
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| CN108940225A (en) * | 2018-08-10 | 2018-12-07 | 南华大学 | Sodium alginate/amino mesoporous silica gel ball preparation method and application for low concentration uranium-bearing wastewater processing |
| CN111375357A (en) * | 2020-04-07 | 2020-07-07 | 华东理工大学 | Preparation method of multifunctional nano aerogel with amphipathy |
| CN111793995A (en) * | 2020-08-20 | 2020-10-20 | 江苏阳光股份有限公司 | Improved wool fabric dyeing method |
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| CN111793995B (en) * | 2020-08-20 | 2022-12-13 | 江苏阳光股份有限公司 | Improved wool fabric dyeing method |
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