CN107638737A - A kind of preparation method of efficient spider web type air filting material - Google Patents
A kind of preparation method of efficient spider web type air filting material Download PDFInfo
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- CN107638737A CN107638737A CN201710861986.5A CN201710861986A CN107638737A CN 107638737 A CN107638737 A CN 107638737A CN 201710861986 A CN201710861986 A CN 201710861986A CN 107638737 A CN107638737 A CN 107638737A
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Abstract
The invention discloses a kind of preparation method of efficient spider web type air filting material, (1) pre-processes to string, obtains pretreated string；(2) pretreated string is diluted with water, then adds the tert-butyl alcohol, while stirring makes it be uniformly dispersed, and obtains fibrous suspension；(3) fibrous suspension is put into shaping vessel and carries out freeze forming, obtain frozen samples；(4) frozen samples are subjected to freeze-drying process, obtain efficient spider web type air filting material.Filter material prepared by the present invention not only has the characteristics of biodegradable and secondary recovery utilizes, while notable to 300nm fine particle filter effects.Efficiently the preparation method technique simple possible of arachnoid filter material, production cost are relatively low by the present invention in addition, have good market development prospect.
Description
Technical field
The invention belongs to air filting material technical field, and in particular to a kind of efficient spider web type air filting material
Preparation method.
Background technology
In recent years due to the continuous aggravation of mankind's activity, quickening, Coal Energy Source such as industrialization and urbanization process it is big
Amount consumption, and in the air that is triggered of surge of vehicles number tiny particles content (PM) pollution problem, especially air
The dynamic fine particle (PM2.5) learned diameter and be less than 2.5 μm, has carried out great threat to mankind's health care belt.According to international cancer
Report that PM2.5 can induce the diseases such as coronary artery blockage, congestive heart failure and lung cancer, have a strong impact on the mankind in research center
Life security.Therefore, high performance air filting material is researched and developed out, to separate the PM2.5 in air, clean room
Interior air, all it is industrial quarters and academia's focus of attention all the time.At present, application and the relatively broad room air of research
Scavenging material mainly includes glass fiber material, active carbon fibre peacekeeping PTFE film material etc..But it is due to most
Belong to non-renewable oil radical derivative, while discarded filtering material can produce serious pollution to environment and bear, therefore
Need badly and find a kind of efficient and environment-friendly type air filting material.
Largely research all concentrates on polytetrafluoroethylene film, glass fibre or non-woven fabrics material to relevant air filting material
Expect to form composite with the material that some have adsorptivity.By by active carbon powder, pomelo peel powder, theanine and suction
Attached dose is laid in nonwoven layer, then compounds to form the air filting material with degerming functions with layers of nanofibers.Although its
Production cost is relatively low, yet with filter material is combined by multi-layer nonwoven fabrics, so technique is complex and filter efficiency is low
(application number： CN201520531709.4)；Using by glass fibre cotton layer, nylon-6 fiber layer and spunbond, melt-blown, terylene without
Spin layer of cloth and be combined into the higher filtering material of capturing efficiency, and antiseptic is coated on surface.Due to wherein glass fiber diameter compared with
It is small but the grade synthetic fibers of polyamide fibre 6 in filter material to be present so as to improve the filtering accuracy of filter material, discard filter material difficult degradation (application
Number：CN201520531742.7)；String is a kind of widely distributed reproducible biomass resource in nature, and
And there is biodegradable, lower-price characteristic, therefore it can prepare environmental protection as a kind of raw material of excellent performance
Type air filtering material.Material pore structure in itself can be kept furthermore with Freeze Drying Technique and avoids sample in drying process
Product shrink and cause hole to destroy, yet with filter material preparation process using water for freeze medium because its have it is larger
Surface tension, so as to cause fiber part wadding to gather, cause material distribution of pores uneven, the microstructure of filter material is presented in addition
Anisotropy, it is unfavorable for improving the filter efficiency (application number of filter material： CN201610859817.3).Above-mentioned listed patent and
Other same domain patents largely prepare high performance air filting material using glass fibre and synthetic fibers, but
Be present the problems such as complex manufacturing, difficult degradation in it, and prepared simultaneously using Freeze Drying Technique using string as raw material
Air filting material, although its is biodegradable, but the filter efficiency of filter material and filtering accuracy are relatively low.How to ensure
Degradable environment-friendly air filting material etc. is prepared on the premise of higher filter efficiency and precision at present not have
Correlative study.
The content of the invention
It is existing to overcome it is an object of the invention to provide a kind of preparation method of efficient spider web type air filting material
The problem of with the presence of technology, the present invention reduces the surface tension of fibrous suspension by adding the tert-butyl alcohol, so as to avoid fiber
Wadding gather, while cause material pore structure distribution it is more uniform, the addition of the another aspect tert-butyl alcohol serves controlled material
The effect of pore-size, and then cause the microstructure of filter material to be changed into isotropic spider from anisotropic layer structure
Network structure, be advantageous to catch more tiny particulate, finally prepare that efficient, pore structure enriches, biodegradable
Air filting material.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of preparation method of efficient spider web type air filting material, comprises the following steps：
(1) string is pre-processed, obtains pretreated string；
(2) pretreated string is diluted with water, then adds the tert-butyl alcohol, while stirring makes it be uniformly dispersed,
Obtain fibrous suspension；
(3) fibrous suspension is put into shaping vessel and carries out freeze forming, obtain frozen samples；
(4) frozen samples are subjected to freeze-drying process, obtain efficient spider web type air filting material.
Further, plant fiber pretreatment method is in step (1)：String pulpboard is first soaked 12 in water
~24h, recycle standard fluffer that fleeces agglomerate is discongested into 12000~15000r, the concentrated place again of the slurry after discongesting
Reason, equably it is laid down into grinding for 10% fibre stuff dough, then by fibre stuff dough so as to be configured to mass concentration
The inner side of pulp grinder, by 10000~50000r defibrination process, that is, obtain pretreated string.
Further, the tert-butyl alcohol described in step (2) is pure to analyze, and solid content is more than 99.99%.
Further, the mass ratio of the tert-butyl alcohol and water is (1 in fibrous suspension in step (2):9)~(4:6) it is, and fine
The mass concentration for tieing up string in suspension is 1.0~2.0%.
Further, it is stirred in step (2) using mechanical agitator, mixing speed is 500~1000r/min, is stirred
It is 15~30min to mix the time.
Further, the condition of freeze forming is in step (3)：Cryogenic temperature is -10~-196 DEG C；Cooling time is 2
~6h.
Further, freeze-drying condition is in step (4)：Drying temperature be -45~-56 DEG C, drying time be 48~
72h, the vacuum in drying process is 10~30Pa.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention uses medium of the tertiary butanol and water system for freeze-drying, so as to reduce the surface tension of solution, and then
Avoid and cause hole to collapse because the wadding of fiber is poly-.Be primarily due to add the tert-butyl alcohol after contribute to it is micro- in fibrillating fibre
Disperseing for fine fibre, prevents its reunion, to ensure to have sufficient microfibre to be formed the filament shape net in spider web frame
Network., can direct and surrounding microfibre shape when it is dispersed in water because a large amount of free hydroxyls are contained on microfibre surface
Hydrogen bond is formed into hydrogen bond action or logical overflow bridge and the fine fibre silk of surrounding, these filaments easily occur to reunite now after drying
As.And the hydroxyl in TBA molecular structures can form hydrogen bond with the hydroxyl on microfibre surface, inertia group (uncle is introduced in fiber
Butyl) the further formation of hydrogen bond is terminated, so as to reduce the probability that hydrogen bond is formed between microfibre, in addition with larger
The tert-butyl group of chemical steric hindrance can also increase the chemical steric hindrance between microfibre, hinder the formation of hydrogen bond, thus help to ensure that micro-
Fine fibre is in monofilament state.The tert-butyl alcohol can effectively prevent the growth of large ice crystals in refrigerating process in addition, so as to avoid with
Pure water for freezing medium when, the repulsion and squeezing action of the stratiform ice crystal of formation to the microfibre in fibrous suspension, so as to
So that the microstructure of the filtering material prepared is changed into isotropic web-like structure from anisotropic layer structure,
Compared to layer structure, web-like structure is more beneficial for improving the seizure of air filting material and intercepts the energy of fine particle
Power, it is final to obtain the air filting material with compared with filtration efficiency and filtering accuracy.
The present invention, as raw material, is on the one hand adsorbed using string because string belongs in itself with certain
The porous material of performance, while there are wide material sources again, the advantage such as biodegradable.And compare other drying modes such as baking oven
Dry etc., Freeze Drying Technique can maintain the original pore structure of material to greatest extent, so as to reduce the structure to material
Destroy.Therefore the air filting material that prepared by the present invention has higher filter efficiency and precision, biodegradable and green ring
The features such as guarantor.And a kind of efficient spider web type air filting material preparation method of the present invention is in the presence of operation is simple and feasible, nontoxic
The pollution-free, advantage such as production cost is low, has preferable application prospect.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention；
Fig. 2 be air filting material prepared by blank Example sample drawing and local SEM figures (wherein a is sample
Figure, b schemes for SEM, and b:×500)；
Fig. 3 is that (wherein c is sample for air filting material sample drawing prepared by the embodiment of the present invention 4 and local SEM figures
Figure, d schemes for SEM, and d:×500).
Embodiment
Embodiments of the present invention are described in further detail below in conjunction with the accompanying drawings：
Referring to Fig. 1, a kind of efficient spider web type air filting material preparation method, comprise the following steps：
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
12~24h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 12000~15000r, so that fiber fully moistens
It is swollen, be advantageous to the next step fibrillation processing of fiber.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, at 10000~50000r defibrination
Reason, finally obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while takes the tert-butyl alcohol (TBA) of certain mass, according to
The mass ratio of butanol/water is (1:9)~(4:6) tert-butyl alcohol is added, while using mechanical agitator with 500~1000r/min
Speed stir 15~30min it is uniformly dispersed, be finally configured to mass concentration be 1.0~2.0% fibrous suspension.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant can be freezer compartment of refrigerator (- 10~-26 DEG C), freeze drier (- 45~-56 DEG C) and liquid nitrogen frozen (-
196 DEG C) etc., make fibrous suspension cryogenic temperature be -10~-196 DEG C；Cooling time tentatively freezes under conditions of being 2~6h
Shaping.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 10~30Pa, and built-in temperature is -45~-56 DEG C, the sample drying time is 48~
72h, so as to obtain efficient arachnoid air filting material.
The present invention is described in further detail with reference to embodiment：
Blank Example
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
24h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 15000r, so that the abundant swollen of fiber, is advantageous to fibre
The next step fibrillation processing of dimension.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, by 50000r defibrination process, finally
Obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while using mechanical agitator with 1000r/min speed
Degree stirring 30min makes it be uniformly dispersed.Finally it is configured to the fibrous suspension that mass concentration is 2.0%.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant can be liquid nitrogen frozen, fibrous suspension is placed in the bar that cryogenic temperature is -196 DEG C, cooling time is 2h
Preliminary freeze forming under part.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 30Pa, and built-in temperature is -50 DEG C, and the sample drying time is 48h.So as to obtain layer
Shape air filting material.
Embodiment 1
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
12h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 12000r, so that the abundant swollen of fiber, is advantageous to fibre
The next step fibrillation processing of dimension.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, by 10000r defibrination process, finally
Obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while takes the tert-butyl alcohol (TBA) of certain volume, according to
The mass ratio of butanol/water is 1/9, i.e. tert-butyl alcohol addition mass concentration is 10%, is added in fibrous suspension, simultaneously
It is set to be uniformly dispersed with 500r/min speed stirring 15min using mechanical agitator.Finally being configured to mass concentration is
1.0% fibrous suspension.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant is freezer compartment of refrigerator, and cryogenic temperature is -10 DEG C, cooling time 6h so that the preliminary freeze forming of sample.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 10Pa, and built-in temperature is -45 DEG C, and the sample drying time is 72h.So as to obtain height
The arachnoid air filting material of effect.
Embodiment 2
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
16h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 13000r, so that the abundant swollen of fiber, is advantageous to fibre
The next step fibrillation processing of dimension.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, by 20000r defibrination process, finally
Obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while takes the tert-butyl alcohol (TBA) of certain volume, according to
The mass ratio of butanol/water is 2/8, i.e. tert-butyl alcohol addition mass concentration is 20%, is added in fibrous suspension, simultaneously
It is set to be uniformly dispersed with 700r/min speed stirring 20min using mechanical agitator.Finally being configured to mass concentration is
1.3% fibrous suspension.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant is freezer compartment of refrigerator, and cryogenic temperature is -26 DEG C, cooling time 5h so that the preliminary freeze forming of sample.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 15Pa, and built-in temperature is -50 DEG C, and the sample drying time is 56h.So as to obtain height
The arachnoid air filting material of effect.
Embodiment 3
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
20h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 14000r, so that the abundant swollen of fiber, is advantageous to fibre
The next step fibrillation processing of dimension.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, by 30000r defibrination process, finally
Obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while takes the tert-butyl alcohol (TBA) of certain volume, according to uncle
The mass ratio of butanol/water is 3/7, i.e. tert-butyl alcohol addition mass concentration is 30%, is added in fibrous suspension, while profit
It is set to be uniformly dispersed with 800r/min speed stirring 25min with mechanical agitator.Mass concentration is finally configured to as 1.6%
Fibrous suspension.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant can be freeze drier, and cryogenic temperature is -46 DEG C, cooling time 4h so that sample is tentatively frozen into
Type.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 32Pa, and built-in temperature is -56 DEG C, and the sample drying time is 58h.So as to obtain height
The arachnoid air filting material of effect.
Embodiment 4
Step 1：String pre-processes：The string pulpboard equivalent to oven-dry weight 15g is taken, tears up, add deionized water
24h is soaked, recycles standard fluffer that fleeces agglomerate is discongested into 15000r, so that the abundant swollen of fiber, is advantageous to fibre
The next step fibrillation processing of dimension.
Slurry after discongesting filters concentration through vavuum pump again, so as to be configured to the fiber pulp that mass concentration is 10%
Expect dough.Its fiber dough is equably laid down into the inner side of fiberizer again, by 50000r defibrination process, finally
Obtain the string of abundant wire-dividing broom purification.
Step 2：Fiber Jing Guo defibrination process is diluted with water, while takes the tert-butyl alcohol (TBA) of certain volume, according to
The mass ratio of butanol/water is 4/6, i.e. tert-butyl alcohol addition mass concentration is 40%, is added in fibrous suspension, simultaneously
It is set to be uniformly dispersed with 1000r/min speed stirring 30min using mechanical agitator.Finally being configured to mass concentration is
2.0% fibrous suspension.
Step 3：Fibrous suspension scattered in step 2 is poured into glass culture dish, is placed on certain freezing ring
In border：Refrigerating plant can be liquid nitrogen frozen, and cryogenic temperature is -196 DEG C, cooling time 2h so that sample is tentatively frozen into
Type.
Step 4：The complete sample for freezing reality is placed on low-temperature distillation in freeze drier again, removal ice crystal is freezed
Drying process.Freeze drier vacuum is 30Pa, and built-in temperature is -50 DEG C, and the sample drying time is 48h.So as to obtain height
The arachnoid air filting material of effect.
Fig. 1 is the process chart of the present invention.Fig. 2 and Fig. 3 is then the sample drawing of blank Example and embodiment 4 and micro-
See the contrast of shape appearance figure.It is substantially rough that the air filting material surface of blank is can be seen that from Fig. 2-a sample drawings, this master
If because the surface tension of pure aqueous solution is larger, so as to cause fiber part wadding poly-, cause material distribution of pores uneven
It is even；And from Fig. 3-c：Air filting material micropore exquisiteness, the densification of 40% tert-butyl alcohol are added, apparent form is more smooth.
This is due in refrigerating process, and tert-butyl alcohol molecule can form the less eutectic of size with water molecules, so as to limit body
The larger ice-crystal growth of product, and when ice crystal is removed by low-temperature distillation, the less pore structure of size is left, final sample
Show tiny, fine and close and smooth apparent form.Found simultaneously from Fig. 2-b, filter material microstructure prepared by blank Example
Obvious periodic layer structure is presented, this is the fibre concentration at ice crystal solidification end forward position under the promotion of ice crystal active force
Rise, cause solution supercooling, heat power freezing rate to reduce, plane ice crystal can be occurred by being close to turns to stratiform ice crystal
The limit freezing rate of change, cause the unstable of plane ice crystal solidification front, it is developed into the layer of periodic arrangement
Shape ice crystal structure.And the isotropic spider web structure of sample microscopic appearance presentation of the addition tert-butyl alcohol is found in Fig. 3-d, one
Aspect causes filament to be uniformly dispersed because the repulsion of the tert-butyl alcohol acts on, while the tert-butyl alcohol and hydrone shape in refrigerating process
Into eutectic, so as to reduce repulsion and squeezing action of the ice crystal to fiber, isotropic web-like structure is ultimately formed,
Be advantageous to improve seizure and interdiction capability of the air filting material to fine particle.
Influence of the content of the tert-butyl alcohol to the strainability of air filting material is as shown in table 1：
Influence of the content of the tert-butyl alcohol of table 1 to the strainability of air filting material
Note：Test particulate matter is DEHS aerosols, particle diameter 300nm.
From table 1, it is apparent that the strainability of air filting material can be obviously improved by adding the tert-butyl alcohol, and with
The content increase of the tert-butyl alcohol, filter efficiency improves constantly.Compared to blank Example, the air filtration material of the tert-butyl alcohol is added
Material forms the less eutectic of size in refrigerating process, and reduces squeezing action of the ice crystal to fiber, forms and catches
Catch the stronger web-like structure of fine particle ability.And with the increase of t butanol content, it is more abundant thin to form hole
Greasy web-like structure adds the collision of fine particle and air filting material so as to improve the specific surface area of filter material
Probability, and then improve the strainability of air filting material.
Claims (7)
1. a kind of preparation method of efficient spider web type air filting material, it is characterised in that comprise the following steps：
(1) string is pre-processed, obtains pretreated string；
(2) pretreated string is diluted with water, then adds the tert-butyl alcohol, while stirring makes it be uniformly dispersed, and obtains
Fibrous suspension；
(3) fibrous suspension is put into shaping vessel and carries out freeze forming, obtain frozen samples；
(4) frozen samples are subjected to freeze-drying process, obtain efficient spider web type air filting material.
A kind of 2. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly plant fiber pretreatment method is in (1)：String pulpboard is first soaked into 12~24h in water, recycling standard is discongested
Fleeces agglomerate is discongested 12000~15000r by machine, the concentrated processing again of the slurry after discongesting, is so as to be configured to mass concentration
10% fibre stuff dough, then fibre stuff dough is equably laid down into the inner side of fiberizer, by 10000~
50000r defibrination process, that is, obtain pretreated string.
A kind of 3. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly the tert-butyl alcohol described in (2) is pure to analyze, and solid content is more than 99.99%.
A kind of 4. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly the mass ratio of the tert-butyl alcohol and water is (1 in fibrous suspension in (2):9)~(4:6) string, and in fibrous suspension
Mass concentration is 1.0~2.0%.
A kind of 5. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly it is stirred in (2) using mechanical agitator, mixing speed is 500~1000r/min, and mixing time is 15~30min.
A kind of 6. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly the condition of freeze forming is in (3)：Cryogenic temperature is -10~-196 DEG C；Cooling time is 2~6h.
A kind of 7. preparation method of efficient spider web type air filting material according to claim 1, it is characterised in that step
Suddenly freeze-drying condition is in (4)：Drying temperature is -45~-56 DEG C, and drying time is 48~72h, the vacuum in drying process
Spend for 10~30Pa.
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| CN109126290A (en) * | 2018-09-20 | 2019-01-04 | 俞小峰 | A kind of high-strength anti-flaming air filting material and preparation method thereof |
| CN113509800A (en) * | 2020-04-10 | 2021-10-19 | 中国科学技术大学 | Multi-scale structure plant fiber air filtering material and preparation method and application thereof |
| WO2022095097A1 (en) * | 2020-11-09 | 2022-05-12 | 苏州纳昇源新材料科技有限公司 | Method for preparing fully biodegradable high-efficiency air composite filter material |
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| CN102531660A (en) * | 2010-12-31 | 2012-07-04 | 中国科学院金属研究所 | Method for preparing porous ceramic by using tertiary butanol-based freezing sublimation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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