CN105002587A - Organic-inorganic nanofibers composite tow and preparation method and application thereof - Google Patents

Organic-inorganic nanofibers composite tow and preparation method and application thereof Download PDF

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CN105002587A
CN105002587A CN201510469341.8A CN201510469341A CN105002587A CN 105002587 A CN105002587 A CN 105002587A CN 201510469341 A CN201510469341 A CN 201510469341A CN 105002587 A CN105002587 A CN 105002587A
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organic
inorganic nano
nano fiber
fiber composite
composite tow
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CN105002587B (en
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储国海
朱强
徐志康
王韵
杨帅
万灵书
李海锋
徐建
刘建华
王高合
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China Tobacco Zhejiang Industrial Co Ltd
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China Tobacco Zhejiang Industrial Co Ltd
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Abstract

The invention discloses an organic-inorganic nanofibers composite tow and a preparation method and application thereof. The preparation method comprises the following steps that 1 acrylic copolymer, calcium-containing additive and solvent are prepared into spinning solution; the acrylic copolymer is obtained through copolymerization of organic monomer and crylic acid, and the organic monomer is acrylonitrile, methyl methacrylate, styrene, polyethylene oxide, sodium p-styrenesulfonate or acrylamide; 2 cigarette tow with carbonate ion adhering to the surface is used as a base material, electrostatic spinning is conducted on the spinning solution obtained in the step 1, and organic-inorganic nanofiber composite tow is obtained. According to the inorganic nanofibers composite tow and the preparation method and application thereof, organic-inorganic nanofiber is deposited on the cigarette tow through the electrostatic spinning technology, a filter rod is prepared through the organic-inorganic nanofiber composite tow, a sample cigarette is prepared further, compared with a market cigarette of the same standard, the release amount of HCN in main steam smoke of the cigarette is reduced by 13 to 37%, and the release amount of ammonia is reduced by 10 to 40%.

Description

A kind of organic-inorganic nano fiber composite tow and its preparation method and application
Technical field
The present invention relates to technical field of cigarettes, be specifically related to a kind of organic-inorganic nano fiber composite tow and its preparation method and application.
Background technology
Hydrogen cyanide (HCN) in cigarette smoke is mainly derived from nitrate and nitrogen-containing compound in tobacco and is burning and sucking the oxidation Decomposition in process, and its burst size is about 30-300 μ g/cig.HCN in flue gas enters body rapidly after respiratory tract absorbs, to the healthy generation harm of people.Along with the signing of " Framework Convention on Tobacco Control ", research and develop the developing direction that the novel filter tip material that effectively can reduce the burst size of HCN and ammonia in cigarette mainstream flue gas has become international cigarette.HCN at present in the cigarette mainstream flue gas of researcher's many employings absorption method removal both at home and abroad and ammonia.
In organic matrix, introduce inorganic component construct organic-inorganic nano tunica fibrosa, in conjunction with the advantage of organic component and inorganic component, the mechanical strength of nano fibrous membrane, heat endurance and absorption property can be strengthened.In recent years, have high catalysis, absorption, bio-compatible performance organic-inorganic nano tunica fibrosa receive and pay close attention to widely.
Such as, publication number is the patent of invention document employing co-blend polypropylene nitrile solution of CN 102352548A and the silane copolymer of synthesis, prepares precursor tunica fibrosa through electrostatic spinning, then through high temperature cabonization, and obtained silicon/carbon nanofiber membrane.Large, thermally-stabilised good, the mechanical property of this film specific area and catalytic performance excellent, have potential application prospect in fields such as nano-wire devices, filtering material, composite reinforcing materials.
In addition, publication number is that the patent of invention document of CN 102242464 adopts polymeric material and ceramic material phase compound, by electrostatic spinning, prepare composite material nanometer tunica fibrosa, this film can as the supporter of the filtering materials such as the barrier film of lithium ion battery and micro-filtration, ultrafiltration, nanofiltration.
The nanofiber specific area adopting method of electrostatic spinning to prepare is large, has good absorption property.By changing composition and the spinning parameter of spinning solution, the nanofiber of different physical arrangement and chemical property can be prepared.
At present, domestic tobacco business generally adopts cellulose acetate fibre tow or polypropylene fibre tow to make cigarette filter rod, carries out modification be also studied to improve lowering harm and decreasing coking performance tow.Such as, the publication number nanofibres deposit that to be the patent of invention bibliographical information of CN 103628253 prepare method of electrostatic spinning forms functionalization tow on the tow surface of continuous moving, the burst size of tar, nitrosamine and HCN in effective reduction cigarette mainstream flue gas, and do not affect smoking property of cigarette quality.
In prior art, also do not have the bibliographical information of the organic-inorganic nano fiber composite tow that optionally can reduce the burst size of HCN and ammonia in cigarette mainstream flue gas, more not having can for the technology of production application and technique.
Can provide the material of calcium ion all can as additives containing calcium in prior art, preferably, described additives containing calcium be CaCl 2.
The mass fraction of acrylic copolymer determines the viscosity of spinning solution to a certain extent, affect the size of nanofiber, additives containing calcium then determines the quantity of the inorganic particulate introduced in nanofiber, in order to ensure that final obtained organic-inorganic nano fiber composite tow has high specific area, for HCN and ammonia, there is better suction-operated, the mass fraction of acrylic copolymer in spinning solution and additives containing calcium is carried out preferably.
In described spinning solution, the mass fraction of acrylic copolymer is 5 ~ 25%.Namely, in spinning solution, acrylic copolymer quality and spinning solution mass ratio are 5 ~ 25:100.Further preferably, the mass fraction of acrylic copolymer is 15 ~ 25%.
In described spinning solution, the mass fraction of additives containing calcium is 1 ~ 15%.Namely, in spinning solution, additives containing calcium and spinning solution mass ratio are 1 ~ 15:100.Further preferably, the mass fraction of additives containing calcium is 8 ~ 15%.
Before pipe tobacco enters electrostatic spinning chamber, introduce carbanion on the surface of pipe tobacco, preferably, at pipe tobacco surface coating Na 2cO 3the aqueous solution or (NH 4) 2cO 3the aqueous solution, obtains the pipe tobacco that described surface attachment has carbanion.
Described Na 2cO 3the molar concentration of the aqueous solution is 0.01 ~ 0.7M, described (NH 4) 2cO 3the molar concentration of the aqueous solution is 0.01 ~ 0.7M.
Na 2cO 3the aqueous solution and (NH 4) 2cO 3the consumption of the molar concentration of the aqueous solution and consumption and additives containing calcium adapts, due in coating operating process, and Na 2cO 3the aqueous solution or (NH 4) 2cO 3the aqueous solution can not be attached to the surface of pipe tobacco completely, therefore, in actual mechanical process, and Na 2cO 3the aqueous solution or (NH 4) 2cO 3the consumption of the aqueous solution is generally excessive, most efficiently to generate calcium carbonate particle.
In order to the nanofiber of the surface deposition suitable dimension at pipe tobacco, preferably, in step (2), spinning voltage is 10 ~ 50kV, and receiving range is 5 ~ 25cm, and the winding speed of pipe tobacco is 50 ~ 300m/min.
Further preferably, in step (2), spinning voltage is 30 ~ 50kV, and receiving range is 15 ~ 25cm, and the winding speed of pipe tobacco is 100 ~ 300m/min.
After completing electrostatic spinning, toast 1 ~ 60s under the nanofiber compound tow of gained being placed in infrared lamp, then reel, obtain described organic-inorganic nano fiber composite tow.
Present invention also offers a kind of organic-inorganic nano fiber composite tow utilizing described preparation method to obtain, described organic-inorganic nano fiber composite tow comprises pipe tobacco and is deposited on the nanofiber on pipe tobacco surface, and the diameter of described nanofiber is 100 ~ 500nm.
Further preferably, the diameter of nanofiber is 100 ~ 300nm.
Pipe tobacco in the present invention adopts cellulose acetate tow, and the mass ratio of described nanofiber and pipe tobacco is 0.0025 ~ 0.0125:1.
Pipe tobacco deposits the nanofiber of suitable consumption, to obtain best HCN and the removal effect of ammonia, as preferably, the mass ratio of described nanofiber and pipe tobacco is 0.008 ~ 0.0125:1.
Present invention also offers a kind of cigarette filter rod, be prepared from by described organic-inorganic nano fiber composite tow.
The fine filter stick of the common vinegar substituted in certain specification commercial cigarettes with obtained filter stick produces sample cigarette, adopt Cerulean SM450 type smoking machine (Cerulean, UK) cigarette smoking experiment is carried out according to ISO 3308 pattern, and with same specification commercial cigarettes for contrast, pumping volume is 35.0 milliliters, suction time is 2 seconds, and puff interval is 58 seconds.
The present invention utilizes electrostatic spinning technique to deposit on pipe tobacco organic-inorganic nano-fiber, obtain organic-inorganic nano fiber composite tow, nanofiber and the inorganic component of the intrafascicular high-specific surface area of compound silk have stronger suction-operated to the HCN in cigarette smoke and ammonia, adopt the sample cigarette of organic-inorganic nano fiber composite tow compared with the commercial cigarettes of same specification, in cigarette mainstream flue gas, the burst size of HCN reduces 13%-37%, ammonia burst size reduces 10%-40%.
Summary of the invention
The invention provides a kind of preparation method of organic-inorganic nano fiber composite tow, in spinning solution, introduce mineralising calcium source, mineralising carbonic acid source introduced by reception tow, the generation of nanofiber and mineralising are carried out simultaneously, obtained CaCO 3particle is equally distributed organic-inorganic nano fiber composite tow on nanofiber, and this organic-inorganic nano fiber composite tow can optionally adsorb HCN and ammonia.
A preparation method for organic-inorganic nano fiber composite tow, comprises the following steps:
(1) acrylic copolymer, additives containing calcium and solvent are configured to spinning solution;
Described acrylic copolymer is obtained by organic monomer and acrylic acid copolymer, and described organic monomer is acrylonitrile, methyl methacrylate, styrene, poly(ethylene oxide), sodium p styrene sulfonate or acrylamide;
(2) there is the pipe tobacco of carbanion for base material with surface attachment, electrostatic spinning is carried out to the spinning solution of step (1) gained, obtain described organic-inorganic nano fiber composite tow.
The present invention introduces calcium source by additives containing calcium in spinning solution, in pipe tobacco (namely receiving tow) upper introducing mineralising carbonic acid source, the generation and the mineralising that realize nanofiber are carried out simultaneously, and the calcium carbonate particle that mineralising obtains is uniformly distributed on nanofiber.
Nanofibres deposit containing calcium carbonate particle is on pipe tobacco surface, obtain the organic-inorganic nano fiber composite tow with high-specific surface area, inorganic component in this organic-inorganic nano fiber composite tow can effectively adsorb HCN and ammonia, during as cigarette filter, effectively can reduce the burst size of HCN and ammonia in cigarette mainstream flue gas.
The present invention adopts needleless hair style electrostatic spinning technique, moving back and forth of carrier fluid groove is utilized to make spinning electrode iron wire surface coating skim spinning solution, after applying voltage exceedes critical value, the spinning liquid layer on spinning electrode iron wire surface first forms various taylor cones, then very beam jet is drawn into, move through whip again, form nanofiber.
The preparation method of organic-inorganic nano fiber composite tow provided by the invention, simple, be applicable to continuous seepage, the quality of production of cigarette filter rod can be ensured, the needleless hair style electrostatic spinning technique production efficiency adopted is higher, is not easy the problem producing blocking syringe needle, easy to maintenance; Enclosed mobile carrier fluid groove ensure that the constant of concentration of dope, can spinning long-term and stably, is conducive to large-scale continuous production.
The molecular weight of described polymer should be suitable, and to ensure that spinning solution has suitable viscosity, ensure spinning property, as preferably, the number-average molecular weight of described acrylic copolymer is 5 × 10 3~ 100 × 10 3g/mol.Further preferably, the number-average molecular weight of described acrylic copolymer is 50 × 10 3~ 100 × 10 3g/mol.
Acrylic acid in acrylic copolymer can react with the calcium ion in additives containing calcium and generate salt, be beneficial to the dispersion of calcium ion in spinning solution, simultaneously, the content of acrylic acid structure unit all has impact to the dissolubility of acrylic copolymer, viscosity and spinning properties, as preferably, in described acrylic copolymer, the molar content of acrylic acid structure unit is 10 ~ 90%.Further preferably, in described acrylic copolymer, the molar content of acrylic acid structure unit is 10 ~ 50%.
Described solvent is advisable can dissolve acrylic copolymer, and described solvent is water, DMF, DMA, 1-METHYLPYRROLIDONE or dimethyl sulfoxide (DMSO).
Acrylic copolymer dissolves in a solvent, and form the solution of stable homogeneous, additives containing calcium is scattered in this solution, with acrylic acid generation salt-forming reaction, and under the effect of solution viscosity, is dispersed in spinning solution.
Detailed description of the invention
By following examples, the present invention is described in more detail, but described embodiment is not construed as limiting the invention.
Embodiment 1
The styrene that selection acrylic acid molar content is 30%, number-average molecular weight is 10000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in DMA, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 8%, CaCl 2mass fraction be 3% spinning solution (namely the mass ratio of polymer and spinning solution is 8:100, CaCl 2be 3:100 with the mass ratio of spinning solution).
The distance (i.e. receiving range) between spinning electrode iron wire and pipe tobacco is regulated to be 25cm, adjustment spinning voltage is 50kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, the winding speed of setting pipe tobacco is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.01M 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 450 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 60s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/250 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Setting pumping volume in suction experiment is 35mL, and suction time is 2s, and puff interval is 58s, and following examples if no special instructions, all adopt identical experiment condition.
Embodiment 2
The methyl methacrylate that selection acrylic acid molar content is 10%, number-average molecular weight is 60000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in DMA, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 8%, CaCl 2mass fraction is the spinning solution of 3%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 32kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.1M 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 180 ± 15nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/120 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 3
The acrylonitrile that selection acrylic acid molar content is 90%, number-average molecular weight is 5000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in DMF, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 5%, CaCl 2mass fraction is the spinning solution of 1%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 35kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and the winding speed of setting pipe tobacco is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.5M 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 150 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/280 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 4
The styrene that selection acrylic acid molar content is 50%, number-average molecular weight is 20000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in dimethyl sulfoxide (DMSO), then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 10%, CaCl 2mass fraction is the spinning solution of 5%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 35kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the (NH of 0.7M 4) 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 130 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/55 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 5
The poly(ethylene oxide) that selection acrylic acid molar content is 60%, number-average molecular weight is 50000g/mol and acrylic acid copolymer are polymer, are dissolved in 1-METHYLPYRROLIDONE, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 16%, CaCl 2mass fraction is the spinning solution of 7%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 35kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the (NH of 0.2M 4) 2cO 3the aqueous solution.Power-on is to setting voltage, it is the nanofiber of 120 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on tow surface is 1/15 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 6
The sodium p styrene sulfonate that selection acrylic acid molar content is 20%, number-average molecular weight is 30000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in DMF, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 20%, CaCl 2mass fraction is the spinning solution of 10%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 5cm, adjustment spinning voltage is 10kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the (NH of 0.3M 4) 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 200 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/50 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 7
The acrylamide that selection acrylic acid molar content is 30%, number-average molecular weight is 70000g/mol and acrylic acid copolymer are polymer, are dissolved in DMA, then add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 20%, CaCl 2mass fraction is the spinning solution of 15%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 40kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 50m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.6M 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 500 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 10s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/25 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Embodiment 8
The acrylonitrile that selection acrylic acid molar content is 40%, number-average molecular weight is 100000g/mol and acrylic acid copolymer are polymer, by polymer dissolution in 1-METHYLPYRROLIDONE, add CaCl 2, be uniformly mixed, standing and defoaming, obtained polymer quality mark is 20%, CaCl 2mass fraction is the spinning solution of 10%.
Regulate the distance between spinning electrode iron wire and pipe tobacco to be 15cm, adjustment spinning voltage is 40kV, then spinning solution is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, and setting pipe tobacco winding speed is 300m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.3M 2cO 3the aqueous solution.
Power-on is to setting voltage, it is the nanofiber of 100 ± 10nm that spinning solution forms diameter, and be deposited on the pipe tobacco surface of the continuous motion for receiving, dry after 5s through infrared lamp and reel, i.e. obtained organic-inorganic nano fiber composite tow, wherein the deposition of organic-inorganic nano fiber on pipe tobacco surface is 1/10 of pipe tobacco quality.
Finally obtained organic-inorganic nano fiber composite tow is rolled into cigarette filter rod on filter-stick forming device, and be prepared into sample cigarette further.CeruleanSM450 type smoking machine is adopted by the sample cigarette rolled to carry out cigarette smoking experiment according to ISO3308 pattern, the burst size of HCN and ammonia in measure and calculation main flume.Adopt the commercial cigarettes cigarette in contrast of same specification, the results are shown in Table 1.
Table 1
Sample name HCN burst size (μ g/cig) Ammonia burst size (μ g/cig)
Embodiment 1 100.7 7.77
Embodiment 2 96.7 7.34
Embodiment 3 103.0 7.94
Embodiment 4 92.4 6.73
Embodiment 5 77.0 5.61
Embodiment 6 90.0 6.56
Embodiment 7 83.0 6.04
Embodiment 8 75.1 5.18
Contrast cigarette 118.5 8.63
Can draw by table 1, the standby cigarette filter rod of organic-inorganic nano fiber composite tow preparing is adopted to have good suction-operated for the HCN in cigarette mainstream flue gas and ammonia, the burst size of HCN compares and can reduce at most 43.4 μ g/cig according to cigarette, and the burst size of ammonia compares and can reduce at most 3.45 μ g/cig according to cigarette.

Claims (10)

1. a preparation method for organic-inorganic nano fiber composite tow, is characterized in that, comprises the following steps:
(1) acrylic copolymer, additives containing calcium and solvent are configured to spinning solution;
Described acrylic copolymer is obtained by organic monomer and acrylic acid copolymer, and described organic monomer is acrylonitrile, methyl methacrylate, styrene, poly(ethylene oxide), sodium p styrene sulfonate or acrylamide;
(2) there is the pipe tobacco of carbanion for base material with surface attachment, electrostatic spinning is carried out to the spinning solution of step (1) gained, obtain described organic-inorganic nano fiber composite tow.
2. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterized in that, in described spinning solution, the mass fraction of acrylic copolymer is 5 ~ 25%.
3. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterized in that, in described spinning solution, the mass fraction of additives containing calcium is 1 ~ 15%.
4. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, is characterized in that, at pipe tobacco surface coating Na 2cO 3the aqueous solution or (NH 4) 2cO 3the aqueous solution, obtains the pipe tobacco that described surface attachment has carbanion.
5. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterized in that, the number-average molecular weight of described acrylic copolymer is 5 × 10 3~ 100 × 10 3g/mol.
6. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterized in that, in described acrylic copolymer, the molar content of acrylic acid structure unit is 10 ~ 90%.
7. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterized in that, in step (2), spinning voltage is 10 ~ 50kV, and receiving range is 5 ~ 25cm, and the winding speed of pipe tobacco is 50 ~ 300m/min.
8. one kind utilize as arbitrary in claim 1 ~ 7 as described in the organic-inorganic nano fiber composite tow that obtains of preparation method, it is characterized in that, described organic-inorganic nano fiber composite tow comprises pipe tobacco and is deposited on the nanofiber on pipe tobacco surface, and the diameter of described nanofiber is 100 ~ 500nm.
9. organic-inorganic nano fiber composite tow as claimed in claim 8, it is characterized in that, the mass ratio of described nanofiber and pipe tobacco is 0.0025 ~ 0.0125:1.
10. a cigarette filter rod, is characterized in that, is prepared from by organic-inorganic nano fiber composite tow as claimed in claim 8 or 9.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109012213A (en) * 2018-07-09 2018-12-18 绍兴齐英膜科技有限公司 Preparation method, filter membrane and the membrane module of high-throughput Organic-inorganic composite filter membrane
CN117431652A (en) * 2023-12-14 2024-01-23 江苏康辉新材料科技有限公司 Method for preparing polyacrylic fiber through dry spinning

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08140653A (en) * 1994-11-15 1996-06-04 Kanebo Ltd Tobacco filter
CN1380019A (en) * 2001-04-17 2002-11-20 吴晨晓 High-effective tar-reducing filter rod
US20090293893A1 (en) * 2007-12-20 2009-12-03 Philip Morris Usa Inc. Hollow/porous fibers and applications thereof
CN101849709A (en) * 2009-04-03 2010-10-06 湖北中烟工业有限责任公司 Novel selective harm-reducing filter tip material and preparation method thereof
CN103628253A (en) * 2013-11-18 2014-03-12 湖南中烟工业有限责任公司 Preparation method of functionalized tobacco shred bundles for filter stick and application of preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08140653A (en) * 1994-11-15 1996-06-04 Kanebo Ltd Tobacco filter
CN1380019A (en) * 2001-04-17 2002-11-20 吴晨晓 High-effective tar-reducing filter rod
US20090293893A1 (en) * 2007-12-20 2009-12-03 Philip Morris Usa Inc. Hollow/porous fibers and applications thereof
CN101849709A (en) * 2009-04-03 2010-10-06 湖北中烟工业有限责任公司 Novel selective harm-reducing filter tip material and preparation method thereof
CN103628253A (en) * 2013-11-18 2014-03-12 湖南中烟工业有限责任公司 Preparation method of functionalized tobacco shred bundles for filter stick and application of preparation method

Cited By (3)

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CN109012213A (en) * 2018-07-09 2018-12-18 绍兴齐英膜科技有限公司 Preparation method, filter membrane and the membrane module of high-throughput Organic-inorganic composite filter membrane
CN117431652A (en) * 2023-12-14 2024-01-23 江苏康辉新材料科技有限公司 Method for preparing polyacrylic fiber through dry spinning
CN117431652B (en) * 2023-12-14 2024-03-22 江苏康辉新材料科技有限公司 Method for preparing polyacrylic fiber through dry spinning

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