CN105727628B - A kind of amination gelatin/nano silicon composite air filtering material and preparation method thereof - Google Patents
A kind of amination gelatin/nano silicon composite air filtering 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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- 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
- B01J20/26—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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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- 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 present invention provides a kind of amination gelatin/nano silicon composite air filtering material and preparation method thereof.This method first mixes amination gelatin solution and nano silicon 1 ~ 2 hour under the conditions of 40 DEG C, addition crosslinking agent and stirring 0.5 ~ 2 hour under the conditions of 40 DEG C, then prepare a kind of amination gelatin/nano silicon composite air filtering material using orientation freezing repeatedly afterwards.Amination gelatin/nano silicon composite air filtering material prepared by the present invention has multistage pore-size distribution on filtering direction, classified filtering is carried out to various sizes of solid particle in gas, with good filter efficiency；Amidized gelatin has good adsorption effect to the formaldehyde in air simultaneously；And raw material sources are extensively, environmentally degradable.Therefore, amination gelatin/nano silicon composite air filtering material that prepared by the present invention has good market application value and prospect.
Description
Technical field
The present invention relates to filtering material field, and in particular to a kind of amination gelatin/nano silicon composite air mistake
Filter material material and preparation method thereof.
Background technology
With the continuous propulsion of China's process of industrialization, problem of environmental pollution becomes increasingly conspicuous, especially air pollution problems inherent
Life and the health of people are badly influenced.Prominent environmental problem causes people to the consciousness of self-protection of air pollution increasingly
Strengthen, the application of air purifier and particulate matter protective mask is increasingly extensive, research and develop new and effective air filting material
The focus paid close attention to as scientific research.
Existing indoor air filtration material mainly has fibrofelt, filter membrane and porous ceramic film material in the market, its
It is mainly used in microorganism, particulate matter and pernicious gas for filtering, absorbing in room air etc..Wherein, by glass fiber and activated carbon
The compound fibrofelt filtering material prepared is because of its small volume, lightweight, filter efficiency is high is widely used.But this filtering material
In the presence of some insoluble problems：(1) because aperture is certain, it is therefore desirable to which the felt of multilayer different pore size is compound with realization pair
The barrier of different-grain diameter pollutant；(2) the materials'use glass fiber and the pernicious gas in activated carbon composite adsorption air, this
Inserted complex method reduces the specific surface area of activated carbon, reduces limited adsorption capacity；(3) reach service life and
The filtering material being replaced, which contains a large amount of pollutants, to be recycled, not degraded by environment after it is dropped, and cause environment
Secondary pollution.
Gelatin is the product of collagenous portion hydrolysis in animal tissue, and its wide material sources is environment-friendly degradable, and gelatin point
Son has a large amount of active groups, and the pernicious gas in air can be adsorbed to a certain extent, therefore by gelatin for preparing air
Filtering material has its distinctive advantage.But system of Himdu logic glue material bad mechanical strength, poor water resistance and it is difficult to form well-regulated hole
Road structure so that application of the gelatin in air filting material field is restricted.Research is found, uses cross-linking modified and nanoparticle
The son method such as filling-modified can significantly improve the mechanical performance of gelatin based material, block-water performance etc..Using the side of orientation freezing
There is gelatin based material prepared by method gradient to lead directly to pore structure, and one layer can be realized by changing freezing conditions adjustment aperture size
The classified filtering of material, it is to avoid hole is blocked in a short time, improves filter efficiency.
The present invention is prepared for a kind of amination gelatin/nanometer titanium dioxide using amination gelatin and nano silicon as raw material
Silicon composite air filtering material.Gelatin after will be amino modified is mixed with nano silica microsphere, adds a small amount of dialdehyde crosslinking
Agent, by orienting freezing method, cross-linking reaction is carried out while straight-through aperture is formed, and obtains having good filtering and adsorptivity
The air filting material of energy.One can be improved by preparing adsorbance of the gelatin used in material for formaldehyde after amination modified
More than times.The nano silica microsphere of addition is located at solid liquid interface in orientation refrigerating process, help to be formed perpendicular to
Two grades of unstable states in direction are solidified, the length of clear opening in porous material can be increased.In addition, the nanometer of embedded amination gelatin
Silica with the mechanical strength of reinforcing material, can improve the adsorption efficiency of material.
The content of the invention
It is of the invention by gelatin in order to prepare the gelatin-based nanometer air filting material with straight-through aperture and high adsorption efficiency
Amination obtains the amination gelatin with cationic property, improves pernicious gas and the air such as gelatin formaldehyde adsorption, methanol
The ability of middle microorganism, adds nano silica microsphere and improves mechanical strength, has by orienting the method for freezing and being made
Amination gelatin/nano silicon composite air filtering material of clear opening.
The present invention provides a kind of composite air filtering material, and its preparation method is as follows：
(1) it is the gelatin phosphate buffer solution that 5 mass concentrations are 1% ~ 5% to prepare 1 parts by volume pH value, adds gelatin dry weight 2
~ 5 times of amino supply reagent, then the pH value for adjusting above-mentioned cushioning liquid with 5mol/L hydrochloric acid solution is 5, then adds and accounts for bright
1- (3- the dimethyl aminopropyls) -3- ethyl carbodiimides salt of glue dry weight 30% ~ 50% is simultaneously determined using pH for 5 phosphate buffer solution
Hold to 2 parts by volume, after being reacted 4 ~ 48 hours under the conditions of 30 ~ 40 DEG C, mixed liquor is dialysed 3 ~ 5 days, freeze-drying obtains amino
Change gelatin；
(2) the amination aqueous gelatin solution that mass concentration is 1% ~ 10% is prepared, adds account for gelatin dry weight under fast stirring
10% ~ 50% nano silica microsphere, stirs under the conditions of 40 DEG C 1 ~ 2 hour, then adds the friendship for accounting for gelatin dry weight 1% ~ 10%
Join agent, continue to stir 0.5 ~ 2 hour under the conditions of 40 DEG C, mixed liquor is poured into stand 1 ~ 3 hour in mould at room temperature afterwards,
Obtain amination gelatin/nano silicon mixed solution；
(3) mold bottom that will be equipped with amination gelatin/nano silicon mixed solution is placed in orientation freezing in liquid nitrogen
2 ~ 10 minutes, the sample of freezing is placed 1 ~ 4 day under the conditions of -20 DEG C afterwards, mold bottom is then placed in 5 ~ 30 DEG C of water-baths
1 ~ 10 minute on pond, mold bottom is then placed in orientation freezing 2 ~ 10 minutes in liquid nitrogen again, afterwards under the conditions of -20 DEG C
Place 1 ~ 4 day, finally freeze-drying 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,
Any one in 2- ethylenediamines, diethylenetriamine, triethylene tetramine, 1,3- propane diamine, 1,6- hexamethylene diamines and spermine hydrochloride
Or several mixtures.
In amination gelatin/nano silicon composite air filtering material preparation process described in above-mentioned technology case
The crosslinking agent used is dialdehyde xanthans, dialdehyde starch, dialdehyde carboxymethyl cellulose, dialdehyde pulullan polysaccharide, dialdehyde alginic acid
Any one or a few mixing in sodium, dialdehyde Weilan gum, dialdehyde guar gum, glyoxal, glutaraldehyde and dialdehyde polyethylene glycol
Thing.
The ratio dry weight of nano silicon and gelatin described in above-mentioned technology case is 1:(2~10).
The present invention compared with the prior art, with many good effects and advantage, can inductive generalization it is as follows.
(1) present invention is provided a kind of amination gelatin/nano silicon composite air filtering material and its preparation side
Method, its base stock gelatin can be extracted by leather industry discarded object and obtained, it is cross-linking modified after gelatin materials have it is good
Mechanical strength, can form the porous material with micron order aperture, be a kind of environmentally friendly high-efficiency air filtering material.
(2) amination gelatin/nano silicon compound air that the present invention is prepared using the method for orientation freezing
Gas filtering material is a kind of material with gradient clear opening, it is possible to achieve the secondary filtration of layer of material, it is to avoid hole is short
It is blocked in time, improves filter efficiency.
(3) present invention is raw material using amidized gelatin, can not only strengthen air filting material formaldehyde adsorption etc.
The ability of pernicious gas, but also the ability that can promote air filting material that there is absorption microbes in air, with good
Market application value and prospect.
(4) method that the present invention is modified using cross-linking modified and nano-particles filled enhances gelatin base air filter material
The mechanical performance of material, meets the requirement of its market application, and the air filting material prepared is environment-friendly degradable.
Specific implementation method
Three embodiments of the present invention are given below, the present invention is specifically described by embodiment.It is necessary herein
, it is noted that embodiment is served only for that the present invention is further detailed, it is impossible to be interpreted as the limit to the scope of the present invention
System, the person skilled in the art in the field can make some nonessential modifications and adaptations according to the content of the invention described above.
Embodiment 1
It is the gelatin phosphate buffer solution that 5 mass concentrations are 1% to prepare 1 parts by volume pH value, adds the two of 3 times of gelatin dry weight
Ethene triamine, then the pH value for adjusting above-mentioned cushioning liquid with 5mol/L hydrochloric acid solution are 5, then add and account for gelatin dry weight 40%
1- (3- dimethyl aminopropyls) -3- ethyl carbodiimides salt and be settled to 2 parts by volume using pH for 5 phosphate buffer solution,
After being reacted 5 hours under the conditions of 30 DEG C, mixed liquor is dialysed 3 days, freeze-drying obtains amination gelatin.Preparing mass concentration is
1% amination aqueous gelatin solution, adds the nano silica microsphere for accounting for gelatin dry weight 12%, 40 DEG C of conditions under fast stirring
Lower stirring 1 hour, then adds the crosslinking agent for accounting for gelatin dry weight 3%, continues to stir under the conditions of 40 DEG C 2 hours, afterwards will mixing
Liquid is poured into stands 2 hours at room temperature in mould, obtain amination gelatin/nano silicon mixed solution；It will be equipped with amino
The mold bottom for changing gelatin/nano silicon mixed solution is placed in orientation freezing 9 minutes in liquid nitrogen, afterwards by the sample of freezing
Place 4 days, be then placed in mold bottom on 10 DEG C of sea water baths 5 minutes, then again by mold bottom under the conditions of -20 DEG C
Be placed in liquid nitrogen orientation freezing 3 minutes, placed afterwards under the conditions of -20 DEG C 3 days, finally freeze-drying obtain amination gelatin/
Nano silicon composite air filtering material.
Embodiment 2
It is the gelatin phosphate buffer solution that 5 mass concentrations are 4% to prepare 1 parts by volume pH value, adds the 1 of 2 times of gelatin dry weight,
2- ethylenediamines, then the pH value for adjusting above-mentioned cushioning liquid with 5mol/L hydrochloric acid solution are 5, then add and account for gelatin dry weight 30%
1- (3- dimethyl aminopropyls) -3- ethyl carbodiimides salt and be settled to 2 parts by volume using pH for 5 phosphate buffer solution,
After being reacted 36 hours under the conditions of 37 DEG C, mixed liquor is dialysed 5 days, freeze-drying obtains amination gelatin.Prepare mass concentration
For 5% amination aqueous gelatin solution, the nano silica microsphere for accounting for gelatin dry weight 50%, 40 DEG C of bars are added under fast stirring
Stirred under part 2 hours, then add the crosslinking agent for accounting for gelatin dry weight 2%, continue to stir under the conditions of 40 DEG C 1 hour, afterwards will be mixed
Conjunction liquid is poured into stands 3 hours at room temperature in mould, obtain amination gelatin/nano silicon mixed solution；It will be equipped with ammonia
The mold bottom of base gelatin/nano silicon mixed solution is placed in orientation freezing 3 minutes in liquid nitrogen, afterwards by the sample of freezing
Product are placed 3 days under the conditions of -20 DEG C, are then placed in mold bottom on 15 DEG C of sea water baths 2 minutes, then again by mould bottom
Portion is placed in orientation freezing 2 minutes in liquid nitrogen, is placed afterwards under the conditions of -20 DEG C 2 days, it is bright that finally freeze-drying obtains amination
Glue/nano silicon composite air filtering material.
Embodiment 3
It is the gelatin phosphate buffer solution that 5 mass concentrations are 2% to prepare 1 parts by volume pH value, adds the three of 4 times of gelatin dry weight
Ethene tetramine, then the pH value for adjusting above-mentioned cushioning liquid with 5mol/L hydrochloric acid solution are 5, then add and account for gelatin dry weight 50%
1- (3- dimethyl aminopropyls) -3- ethyl carbodiimides salt and be settled to 2 parts by volume using pH for 5 phosphate buffer solution,
After being reacted 24 hours under the conditions of 40 DEG C, mixed liquor is dialysed 4 days, freeze-drying obtains amination gelatin.Prepare mass concentration
For 3% amination aqueous gelatin solution, the nano silica microsphere for accounting for gelatin dry weight 45%, 40 DEG C of bars are added under fast stirring
Stirred under part 1 hour, then add the crosslinking agent for accounting for gelatin dry weight 1%, continued to stir under the conditions of 40 DEG C 1.5 hours, afterwards will
Mixed liquor is poured into stands 1 hour at room temperature in mould, obtain amination gelatin/nano silicon mixed solution；It will be equipped with
The mold bottom of amination gelatin/nano silicon mixed solution is placed in orientation freezing 8 minutes in liquid nitrogen, afterwards by freezing
Sample is placed 2 days under the conditions of -20 DEG C, is then placed in mold bottom on 20 DEG C of sea water baths 1 minute, then again by mould
Bottom is placed in orientation freezing 4 minutes in liquid nitrogen, is placed afterwards under the conditions of -20 DEG C 2 days, it is bright that finally freeze-drying obtains amination
Glue/nano silicon composite air filtering material.
Claims (3)
1. a kind of amination gelatin/nano silicon composite air filtering material, it is characterised in that first by amination gelatin
It is well mixed with nano silica microsphere, crosslinking agent is added afterwards, is then prepared using the method for orienting freezing repeatedly
Amination gelatin/nano silicon composite air filtering material, its specific preparation method is as follows：
(1) it is the gelatin phosphate buffer solution that 5 mass concentrations are 1% ~ 5% to prepare 1 parts by volume pH value, adds 2 ~ 5 times of gelatin dry weight
Amino supply reagent, then the pH value for adjusting above-mentioned cushioning liquid with 5mol/L hydrochloric acid solution is 5, then adds that to account for gelatin dry
Weigh 30% ~ 50% 1- (3- dimethyl aminopropyls) -3- ethyl carbodiimides salt and be settled to using pH for 5 phosphate buffer solution
2 parts by volume, after being reacted 4 ~ 48 hours under the conditions of 30 ~ 40 DEG C, mixed liquor are dialysed 3 ~ 5 days, it is bright that freeze-drying obtains amination
Glue；
(2) prepare mass concentration be 1% ~ 10% amination aqueous gelatin solution, under fast stirring add account for gelatin dry weight 10% ~
50% nano silica microsphere, stirs under the conditions of 40 DEG C 1 ~ 2 hour, then adds the crosslinking agent for accounting for gelatin dry weight 1% ~ 10%,
Continue to stir 0.5 ~ 2 hour under the conditions of 40 DEG C, mixed liquor is poured into stand 1 ~ 3 hour in mould at room temperature afterwards, obtained
Amination gelatin/nano silicon mixed solution；
(3) mold bottom that will be equipped with amination gelatin/nano silicon mixed solution is placed in orientation freezing 2 ~ 10 in liquid nitrogen
Minute, the sample of freezing is placed 1 ~ 4 day under the conditions of -20 DEG C afterwards, then mold bottom is placed in 1 on 5 ~ 30 DEG C of sea water baths
~ 10 minutes, mold bottom is then placed in orientation freezing 2 ~ 10 minutes in liquid nitrogen again, 1 is placed under the conditions of -20 DEG C afterwards
~ 4 days, finally freeze-drying obtained amination gelatin/nano silicon composite air filtering material.
2. amination gelatin/nano silicon composite air filtering material according to claim 1, it is characterised in that institute
It is 1,2- ethylenediamines, diethylenetriamine, triethylene tetramine, 1,3- propane diamine, 1,6- hexamethylene diamines and spermine to state amino supply reagent
Any one or a few mixture in hydrochloride.
3. amination gelatin/nano silicon composite air filtering material according to claim 1, it is characterised in that institute
Crosslinking agent is stated for dialdehyde xanthans, dialdehyde starch, dialdehyde carboxymethyl cellulose, dialdehyde pulullan polysaccharide, dialdehyde sodium alginate, double
Any one or a few mixture in aldehyde Weilan gum, dialdehyde melon bean gum, glyoxal, glutaraldehyde and dialdehyde polyethylene glycol.
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