CN105002587B - A kind of organic-inorganic nano fiber composite tow and its preparation method and application - Google Patents

A kind of organic-inorganic nano fiber composite tow and its preparation method and application Download PDF

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CN105002587B
CN105002587B CN201510469341.8A CN201510469341A CN105002587B CN 105002587 B CN105002587 B CN 105002587B CN 201510469341 A CN201510469341 A CN 201510469341A CN 105002587 B CN105002587 B CN 105002587B
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inorganic nano
nano fiber
fiber composite
tow
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CN105002587A (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 a kind of organic-inorganic nano fiber composite tow and its preparation method and application, wherein method is comprised the following steps:(1) acrylic copolymer, additives containing calcium and solvent are configured to into spinning liquid;Acrylic copolymer is obtained by organic monomer and acrylic acid copolymer, and the organic monomer is acrylonitrile, methyl methacrylate, styrene, poly(ethylene oxide), sodium p styrene sulfonate or acrylamide;(2) there is the pipe tobacco of carbanion as base material with surface attachment, electrostatic spinning is carried out to the spinning liquid obtained by step (1), obtain described organic-inorganic nano fiber composite tow.The present invention deposits organic-inorganic nano fiber on pipe tobacco using electrostatic spinning technique, using organic-inorganic nano fiber composite tow preparing for filter stick, and it is further prepared into sample cigarette, compared with same specification commercial cigarettes, in cigarette mainstream flue gas, HCN burst sizes reduce by 13 37%, ammonia burst size and reduce by 10 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, and in particular to a kind of organic-inorganic nano fiber composite tow and its preparation Methods and applications.
Background technology
Blausure (German) (HCN) in cigarette smoke is mainly derived from Nicotiana tabacum L. nitrate and nitrogen-containing compound during burning and sucking Oxidation Decomposition, its burst size be about 30-300 μ g/cig.HCN in flue gas quickly enters body Jing after respiratory tract absorption, right The healthy generation harm of people.With《The Framework Convention on Tobacco Control》Signing, research and development can effectively reduce cigarette main flue In gas, the new filter tip material of the burst size of HCN and ammonia has become the developing direction of international Medicated cigarette.Domestic and international researcher is more at present The HCN and ammonia in cigarette mainstream flue gas is removed using absorption method.
Inorganic component is introduced in organic matrix and constructs organic-inorganic nano fibrous membrane, can be with reference to organic component and nothing The advantage of machine component, strengthens mechanical strength, heat stability and the absorption property of nano fibrous membrane.In recent years, with high catalysis, suction The organic-inorganic nano fibrous membrane of attached, bio-compatible performance is of great interest.
For example, the patent of invention document of Publication No. CN 102352548A is using co-blend polypropylene nitrile solution and synthesis Silane copolymer, Jing electrostatic spinnings prepare precursor fibrous membrane, then Jing high temperature cabonizations, and silicon/carbon nanofiber membrane is obtained.The film Specific surface area is big, thermally-stabilised good, mechanical property and catalytic performance are excellent, in nano-wire devices, filtering material, composite reinforcing material Potential application prospect is suffered from field.
Additionally, the patent of invention document of Publication No. CN 102242464 is mutually multiple with ceramic material using polymeric material Close, by electrostatic spinning, prepare composite material nanometer fibrous membrane, the film can as the barrier film of lithium ion battery and microfiltration, The supporter of the filtering materials such as ultrafiltration, nanofiltration.
The nanofiber specific surface area prepared using method of electrostatic spinning is big, with good absorption property.Spun by changing The composition and spinning parameter of silk liquid, can prepare the nanofiber of different physical arrangements and chemical property.
At present, domestic tobacco business typically adopts cellulose acetate fibre tow or polypropylene fibre tow to make Medicated cigarette filter Rod, is modified to tow and has been also carried out research to improve lowering harm and decreasing coking performance.For example, Publication No. CN 103628253 send out The nanofibres deposit that method of electrostatic spinning is prepared by bright patent literature forms functionalization on the tow surface of continuous moving Tow, effectively reduces the burst size of coal-tar middle oil cigarette mainstream flue gas, nitrosamine and HCN, and does not affect smoking property of cigarette quality.
In prior art, the burst size for also not having can optionally to reduce HCN and ammonia in cigarette mainstream flue gas it is organic- The document report of the compound tow of inorganic nano-fiber, is not more available for the technology and technique of production application.
The content of the invention
The invention provides a kind of preparation method of organic-inorganic nano fiber composite tow, introduces in spinning liquid Mineralising calcium source, introduces mineralising carbonation source on tow is received so that the generation of nanofiber is carried out simultaneously with mineralising, is obtained CaCO3Particle equally distributed organic-inorganic nano fiber composite tow on nanofiber, the organic-inorganic nano fiber Compound tow can selectively adsorb HCN and ammonia.
A kind of preparation method of organic-inorganic nano fiber composite tow, comprises the following steps:
(1) acrylic copolymer, additives containing calcium and solvent are configured to into spinning liquid;
The acrylic copolymer is obtained by organic monomer and acrylic acid copolymer, and the organic monomer is acrylonitrile, first Base acrylic acid methyl ester., styrene, poly(ethylene oxide), sodium p styrene sulfonate or acrylamide;
(2) there is the pipe tobacco of carbanion as base material with surface attachment, the spinning liquid obtained by step (1) is carried out quiet Electrospun, obtains described organic-inorganic nano fiber composite tow.
The present invention introduces calcium source by additives containing calcium in spinning liquid, on pipe tobacco (receiving tow) introduces ore deposit Change carbonation source, realize nanofiber generation and mineralising while carry out, the calcium carbonate particle that mineralising is obtained is equal on nanofiber Even distribution.
Nanofibres deposit containing calcium carbonate particle on pipe tobacco surface, obtain with high-specific surface area it is organic- Inorganic nano-fiber is combined tow, the inorganic component in the organic-inorganic nano fiber composite tow can active adsorption HCN and Ammonia, during as cigarette filter, can effectively 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 so that spinning electrode iron wire table using carrier fluid groove Face coats a thin layer spinning liquid, and after applied voltage exceedes marginal value, the spinning liquid layer on spinning electrode iron wire surface is initially formed perhaps Many many taylor cones, are then drawn into very beam jet, then Jing whips are moved, and form nanofiber.
The preparation method of the organic-inorganic nano fiber composite tow that the present invention is provided, it is simple, it is adaptable to continuous raw Produce, ensure that the quality of production of cigarette filter rod, the needleless hair style electrostatic spinning technique production efficiency of employing is higher, it is not easy to produce The problem of raw blocking syringe needle, it is easy to maintenance;Enclosed mobile carrier fluid groove ensure that the constant of concentration of dope, can long-time Stably spinning, is conducive to large-scale continuous production.
The molecular weight of described polymer should be appropriate, to ensure that spinning liquid has suitable viscosity, it is ensured that spinning property, makees For preferred, the number-average molecular weight of the acrylic copolymer is 5 × 103~100 × 103g/mol.Further preferably, it is described poly- The number-average molecular weight of acrylic copolymer is 50 × 103~100 × 103g/mol。
Acrylic acid in acrylic copolymer can with the calcium ion in additives containing calcium reaction generate salt, beneficial to calcium from Dispersion of the son in spinning liquid, meanwhile, the content of acrylic acid structure unit to the dissolubility of acrylic copolymer, viscosity and Spinning properties have an impact, preferably, in the acrylic copolymer acrylic acid structure unit molar content be 10~ 90%.Further preferably, in the acrylic copolymer, the molar content of acrylic acid structure unit is 10~50%.
The solvent is advisable with dissolving acrylic copolymer, the solvent be water, DMF, N, N- dimethyl acetylamide, N-Methyl pyrrolidone or dimethyl sulfoxide.
Acrylic copolymer dissolves in a solvent, forms the solution of stable homogeneous, and additives containing calcium is scattered in the solution In, there is salt-forming reaction with acrylic acid, and in the presence of solution viscosity, be dispersed in spinning liquid.
The material that calcium ion can be provided in prior art can be used as additives containing calcium, it is preferable that the calcic adds Plus agent is CaCl2
The mass fraction of acrylic copolymer determines the viscosity of spinning liquid to a certain extent, affects nanofiber Size, and additives containing calcium then determines the quantity of the inorganic particulate introduced in nanofiber, it is final obtained in order to ensure Organic-inorganic nano fiber composite tow has high specific surface area, for HCN and ammonia have more preferable adsorption, to spinning In silk liquid, the mass fraction of acrylic copolymer and additives containing calcium is carried out preferably.
In the spinning liquid, the mass fraction of acrylic copolymer is 5~25%.I.e. in spinning liquid, polyacrylic acid is common Polymers quality is 5~25 with spinning liquid mass ratio:100.Further preferably, the mass fraction of acrylic copolymer be 15~ 25%.
In the spinning liquid, the mass fraction of additives containing calcium is 1~15%.I.e. in spinning liquid, additives containing calcium with spin Silk liquid mass ratio is 1~15:100.Further preferably, the mass fraction of additives containing calcium is 8~15%.
Before pipe tobacco enters electrostatic spinning chamber, carbanion is introduced on the surface of pipe tobacco, it is preferable that Pipe tobacco surface-coated Na2CO3Aqueous solution or (NH4)2CO3Aqueous solution, obtaining the surface attachment has the cigarette of carbanion Use tow.
Described Na2CO3The molar concentration of aqueous solution is 0.01~0.7M, described (NH4)2CO3Aqueous solution it is mole dense Spend for 0.01~0.7M.
Na2CO3Aqueous solution and (NH4)2CO3The molar concentration and consumption of aqueous solution are mutually fitted with the consumption of additives containing calcium Should, during coating operation, Na2CO3Aqueous solution or (NH4)2CO3Aqueous solution can not be adhering completely to the table of pipe tobacco Face, therefore, in actual mechanical process, Na2CO3Aqueous solution or (NH4)2CO3The consumption of aqueous solution is typically excessive, with most efficiently Generate calcium carbonate particle.
In order to the nanofiber of suitable dimension is deposited on the surface of pipe tobacco, it is preferable that in step (2), spinning voltage For 10~50kV, it is 5~25cm to receive distance, and the winding speed of pipe tobacco is 50~300m/min.
Further preferably, in step (2), spinning voltage is 30~50kV, and it is 15~25cm to receive distance, pipe tobacco Winding speed is 100~300m/min.
After completing electrostatic spinning, the nanofiber of gained compound tow is placed in into baking 1~60s, Ran Houjin under infrared lamp Row winding, obtains described organic-inorganic nano fiber composite tow.
Present invention also offers a kind of organic-inorganic nano fiber composite tow obtained using described preparation method, The organic-inorganic nano fiber composite tow includes pipe tobacco and is deposited on the nanofiber on pipe tobacco surface, institute State a diameter of 100~500nm of nanofiber.
Further preferably, a diameter of 100~300nm of nanofiber.
Pipe tobacco in the present invention adopts the cellulose acetate tow, the nanofiber with the mass ratio of pipe tobacco to be 0.0025~0.0125:1.
The nanofiber of appropriate consumption is deposited on pipe tobacco, to obtain the removal effect of optimal HCN and ammonia, as excellent Choosing, the nanofiber are 0.008~0.0125 with the mass ratio of pipe tobacco:1.
Present invention also offers a kind of cigarette filter rod, is prepared from by described organic-inorganic nano fiber composite tow.
The common vinegar fibre filter stick production sample cigarette in certain specification commercial cigarettes is substituted with obtained filter stick, using Cerulean SM450 type smoking machines (Cerulean, UK) carries out cigarette smoking experiment according to 3308 patterns of ISO, and with same specification commercial cigarettes For control, pumping volume is 35.0 milliliters, and suction time is 2 seconds, and puff interval is 58 seconds.
The present invention deposits organic-inorganic nano fiber on pipe tobacco using electrostatic spinning technique, obtains organic and inorganic Nanofiber is combined tow, is combined the nanofiber and inorganic component of high-specific surface area in tow to the HCN in cigarette smoke There is stronger adsorption with ammonia, using the commercially available volume of the sample cigarette and same specification of organic-inorganic nano fiber composite tow Cigarette is compared, and in cigarette mainstream flue gas, the burst size of HCN reduces 13%-37%, ammonia burst size and reduces 10%-40%.
Specific embodiment
The present invention is described in more detail by following examples, but the embodiment does not constitute the limit to the present invention System.
Embodiment 1
Select styrene and acrylic acid copolymerization that acrylic acid molar content is that 30%, number-average molecular weight is 10000g/mol Thing is polymer, dissolves the polymer in N,N-dimethylacetamide, is subsequently adding CaCl2, it is uniformly mixed, stands de- Bubble, it is 8%, CaCl that polymer quality fraction is obtained2Mass fraction is 3% spinning liquid (the i.e. quality of polymer and spinning liquid Than for 8:100, CaCl2Mass ratio with spinning liquid is 3:100).
It is 25cm to adjust the distance between spinning electrode iron wire and pipe tobacco (receiving distance), adjusts spinning voltage and is 50kV, is then placed in spinning liquid in the carrier fluid groove of needleless hair style electrostatic spinning machine, set the winding speed of pipe tobacco as 100m/min.Before pipe tobacco enters electrostatic spinning chamber, its surface spraying has the Na of 0.01M2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 450 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 60s, that is, organic-inorganic nano fiber composite is obtained The deposition of tow, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/250 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Pumping volume is set as 35mL in suction experiment, suction time is 2s, and puff interval is 58s, and following examples are such as Without specified otherwise, using identical experiment condition.
Embodiment 2
Select methyl methacrylate and propylene that acrylic acid molar content is that 10%, number-average molecular weight is 60000g/mol The copolymer of acid is polymer, dissolves the polymer in N,N-dimethylacetamide, is subsequently adding CaCl2, stirring mixing is It is even, standing and defoaming, it is 8%, CaCl that polymer quality fraction is obtained2Mass fraction is 3% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 32kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 100m/min.Cigarette silk Before beam enters electrostatic spinning chamber, its surface spraying has the Na of 0.1M2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 180 ± 15nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 5s, that is, organic-inorganic nano fiber composite silk is obtained The deposition of beam, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/120 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 3
Select acrylonitrile and acrylic acid copolymerization that acrylic acid molar content is that 90%, number-average molecular weight is 5000g/mol Thing is polymer, dissolves the polymer in DMF, is subsequently adding CaCl2, it is uniformly mixed, stands de- Bubble, it is 5%, CaCl that polymer quality fraction is obtained2Mass fraction is 1% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 35kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, sets the winding speed of pipe tobacco as 100m/min.Cigarette is used Before tow enters electrostatic spinning chamber, its surface spraying has the Na of 0.5M2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 150 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 5s, that is, organic-inorganic nano fiber composite silk is obtained The deposition of beam, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/280 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 4
Select styrene and acrylic acid copolymerization that acrylic acid molar content is that 50%, number-average molecular weight is 20000g/mol Thing is polymer, dissolves the polymer in dimethyl sulfoxide, is subsequently adding CaCl2, it is uniformly mixed, standing and defoaming, makes It is 10%, CaCl to obtain polymer quality fraction2Mass fraction is 5% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 35kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 100m/min.Cigarette silk Before beam enters electrostatic spinning chamber, its surface spraying has the (NH of 0.7M4)2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 130 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 5s, that is, organic-inorganic nano fiber composite silk is obtained The deposition of beam, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/55 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 5
Select acrylic acid molar content be 60%, number-average molecular weight be the poly(ethylene oxide) of 50000g/mol and acrylic acid Copolymer is polymer, is dissolved in N-Methyl pyrrolidone, is subsequently adding CaCl2, it is uniformly mixed, standing and defoaming, makes It is 16%, CaCl to obtain polymer quality fraction2Mass fraction is 7% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 35kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 100m/min.Cigarette silk Before beam enters electrostatic spinning chamber, its surface spraying has the (NH of 0.2M4)2CO3Aqueous solution.Power-on is to setting voltage, spinning liquid The nanofiber of a diameter of 120 ± 10nm is formed, and is deposited on the pipe tobacco surface for the continuous motion for receiving, Jing is infrared Wind after lamp drying 5s, that is, organic-inorganic nano fiber composite tow is obtained, wherein organic-inorganic nano fiber is in tow table The deposition in face for pipe tobacco quality 1/15.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 6
Select sodium p styrene sulfonate and propylene that acrylic acid molar content is that 20%, number-average molecular weight is 30000g/mol The copolymer of acid is polymer, dissolves the polymer in DMF, is subsequently adding CaCl2, stirring mixing is It is even, standing and defoaming, it is 20%, CaCl that polymer quality fraction is obtained2Mass fraction is 10% spinning liquid.
It is 5cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 10kV, then will be spun Silk liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 100m/min.Pipe tobacco Into before electrostatic spinning chamber, its surface spraying has the (NH of 0.3M4)2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 200 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 5s, that is, organic-inorganic nano fiber composite silk is obtained The deposition of beam, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/50 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 7
Select acrylic acid molar content be 30%, number-average molecular weight be the acrylamide of 70000g/mol and acrylic acid common Polymers is polymer, is dissolved in N,N-dimethylacetamide, is subsequently adding CaCl2, it is uniformly mixed, standing and defoaming, makes It is 20%, CaCl to obtain polymer quality fraction2Mass fraction is 15% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 40kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 50m/min.Pipe tobacco Into before electrostatic spinning chamber, its surface spraying has the Na of 0.6M2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 500 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 10s, that is, organic-inorganic nano fiber composite is obtained The deposition of tow, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/25 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Embodiment 8
Select acrylic acid molar content be 40%, number-average molecular weight be the acrylonitrile of 100000g/mol and acrylic acid common Polymers is polymer, is dissolved the polymer in N-Methyl pyrrolidone, adds CaCl2, it is uniformly mixed, standing and defoaming, Prepared polymer quality fraction is 20%, CaCl2Mass fraction is 10% spinning liquid.
It is 15cm to adjust the distance between spinning electrode iron wire and pipe tobacco, and regulation spinning voltage is 40kV, then will Spinning liquid is placed in the carrier fluid groove of needleless hair style electrostatic spinning machine, is set pipe tobacco and is wound speed as 300m/min.Cigarette silk Before beam enters electrostatic spinning chamber, its surface spraying has the Na of 0.3M2CO3Aqueous solution.
To setting voltage, spinning liquid forms the nanofiber of a diameter of 100 ± 10nm to power-on, and is deposited on for connecing The pipe tobacco surface of the continuous motion received, winds Jing after infrared lamp drying 5s, that is, organic-inorganic nano fiber composite silk is obtained The deposition of beam, wherein organic-inorganic nano fiber on pipe tobacco surface is the 1/10 of pipe tobacco quality.
Obtained organic-inorganic nano fiber composite tow is rolled into into cigarette filter rod on filter-stick forming device finally, and It is further prepared into sample cigarette.The sample cigarette for rolling is carried out according to ISO3308 patterns using CeruleanSM450 types smoking machine Cigarette smoking is tested, the burst size of HCN and ammonia in measure and calculation main flume.Using the commercial cigarettes of same specification as control volume Cigarette, the results are shown in Table 1.
Table 1
Sample name HCN burst sizes (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
Control Medicated cigarette 118.5 8.63
By drawing in table 1, using the standby cigarette filter rod of organic-inorganic nano fiber composite tow preparing for Medicated cigarette master HCN and ammonia in stream flue gas has good adsorption, and the burst size of HCN compares control Medicated cigarette can at most reduce by 43.4 μ g/ Cig, the burst size of ammonia compares control Medicated cigarette can at most reduce by 3.45 μ g/cig.

Claims (10)

1. a kind of preparation method of organic-inorganic nano fiber composite tow, it is characterised in that comprise the following steps:
(1) acrylic copolymer, additives containing calcium and solvent are configured to into spinning liquid;
The acrylic copolymer is obtained by organic monomer and acrylic acid copolymer, and the organic monomer is acrylonitrile, methyl-prop E pioic acid methyl ester, styrene, sodium p styrene sulfonate or acrylamide;
(2) there is the pipe tobacco of carbanion as base material with surface attachment, Static Spinning is carried out to the spinning liquid obtained by step (1) Silk, obtains 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 characterised in that the spinning In silk liquid, 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 characterised in that the spinning In silk liquid, 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, it is characterised in that use in cigarette Tow surface-coated Na2CO3Aqueous solution or (NH4)2CO3Aqueous solution, obtaining the surface attachment has the cigarette silk of carbanion Beam.
5. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterised in that described poly- The number-average molecular weight of acrylic copolymer is 5 × 103~100 × 103g/mol。
6. the preparation method of organic-inorganic nano fiber composite tow as claimed in claim 1, it is characterised in that described poly- In 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 characterised in that step (2) In, spinning voltage is 10~50kV, and it is 5~25cm to receive distance, and the winding speed of pipe tobacco is 50~300m/min.
8. the organic-inorganic nano fiber composite silk that a kind of preparation method using as described in claim 1~7 is arbitrary is obtained Beam, it is characterised in that the organic-inorganic nano fiber composite tow includes pipe tobacco and is deposited on pipe tobacco surface Nanofiber, the nanofiber it is a diameter of
100~500nm.
9. organic-inorganic nano fiber composite tow as claimed in claim 8, it is characterised in that the nanofiber and cigarette It is 0.0025~0.0125 with the mass ratio of tow:1.
10. a kind of cigarette filter rod, it is characterised in that by organic-inorganic nano fiber composite silk as claimed in claim 8 or 9 Beam is prepared from.
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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
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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