CN109700072A - A kind of Biodegradable composite filter tip material of controllable cigarette filter temperature and preparation method thereof - Google Patents
A kind of Biodegradable composite filter tip material of controllable cigarette filter temperature and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Biodegradable composite filter tip materials of a kind of controllable cigarette filter temperature and preparation method thereof, wherein Biodegradable composite filter tip material, it is using the excellent high molecular material of biological degradability as substrate, by the nanoparticle processing acquisition for adding high thermal conductivity coefficient；The high molecular material is the excellent high molecular material PVA of biological degradability；The nanoparticle is one of BN, AlN, GO.A kind of cheap, safe and harmless, and the polymer-based composite suitable for cigarette filter with excellent heat-transfer capability can be prepared in the method for the present invention.It is used as the problem of cigarette filter tip can effectively reduce cigarette mainstream flue gas, and has the characteristics that few additive, cooling effect are obvious, substantially reduce flue gas harmful substance.
Description
Technical field
The present invention relates to Biodegradable composite filter tip material of a kind of controllable cigarette filter temperature and preparation method thereof,
Belong to technical field of cigarettes.
Background technique
As the bridge between smoker and flue gas, cigarette filter is the important medium of reducing tar and reducing harm.Cigarette burning process
The aerosol particle of middle release is filtered in filter tip by directly retaining, after the physical actions such as inertial collision and diffusional deposition,
To reduce intake of the human body to harmful substance.Studies have shown that flue-gas temperature is to intercepted aerosol particle speed, small size
The cohesion again of particle, the short grained condensation deposition of flue gas substance etc. have important influence.In addition, it was discovered by researchers that
Close in the preceding 2-3 mouthfuls of suctions terminated, the flue-gas temperature at filter tip position may be up to 70-80 DEG C for suction, and in depth suction mode
Under, the temperature of filter end even can achieve 100 DEG C or more.Excessively high filter tip temperature is not only to filter tip to flue gas aerosol particle
Rejection effect of the object in filter tip generates large effect, while can also reduce consumer to the degree of recognition of flue gas aesthetic quality.
Therefore, the flue-gas temperature of Effective Regulation cigarette filter plays a significant role raising retention efficiency and product quality.
For a long time, consumer gets used to generally directly being discarded in environment smoked stub is taken out as garbage disposal
In the middle.And common cellulose acetate and polypropylene-base filter tip material are difficult to be dropped by biology in the natural environment currently on the market
Solution, be easy to cause environmental pollution.In addition, acetate filter is the chemical products obtained using high-quality timber as raw material, it is not easy
Regeneration, and polypropylene filter tip is then using petroleum as raw material, consumption is non-renewable resources.Therefore, either from improvement environment
Pollution, or from scarcity of resources angle, it is good to develop novel, sustainable regeneration, safety and environmental protection and biological degradability
Filter tip material be that entire cigarette production industry needs the problem of paying attention to and addressing.
Polyvinyl alcohol (PVA) is the high molecular material that biodegradability is excellent always, is generally acknowledged 100% complete in the world
Biodegradable plastic.It is from a wealth of sources, it can both be obtained by petroleum path, and can also be obtained by coal, natural gas route, be
Mature, stable, transparent primary industry system has apparent price advantage compared with other biological degradative plastics.In addition,
PVA has good grease and gas barrier property, can obstruct in addition to vapor and ammonia most of gas and a variety of
Lipoid material and chemical solvent, therefore barriering effect especially can be played as packaging material.Meanwhile PVA also has height
Intensity, high transparency, it is antistatic the advantages that.Currently, yet there are no with PVA base degradable macromolecule to prepare cigarette filter material
Report.
In general, high molecular material itself has lower thermal coefficient.Therefore, single polymer-based material makes
With the temperature of cigarette filter section can not be reduced well, harmful substances from flue gases is cut to be difficult to further to promote filter tip
Stay effect.It is a large amount of both at home and abroad studies have shown that by adding the two-dimensional slice nanoparticle with high thermal conductivity coefficient into matrix,
Continuous heat transfer network is formed, the heat-transfer capability of polymer base material can be also significantly improved.Evenly dispersed nanoparticle is certainly
The physical barriers network that body is formed also has barrier action to the diffusion for the harmful substance that result of combustion of tobacco generates, and then reduces human body
Intake to harmful substance.The nanoparticle of suitable high thermal conductivity coefficient is added into base filter, to construct continuous equal
Even heat transfer network.It is of great advantage to improve harmful substance retention efficiency to cigarette smoke temperature is reduced for this.Currently, such design
Have not yet to see report.
Summary of the invention
For existing cigarette filter because biological degradability difference easily causes environmental pollution and cigarette smoking in the process because excessively high
Flue-gas temperature caused by filter tip rejection effect is bad and the outstanding problems such as Sensory Quality of Cigarette difference, the present invention provides one kind can
Regulate and control the Biodegradable composite filter tip material and preparation method thereof of cigarette filter temperature.
The Biodegradable composite filter tip material of the controllable cigarette filter temperature of the present invention, is excellent with biological degradability
As substrate, the nanoparticle by adding high thermal conductivity coefficient is processed to be obtained high molecular material.
The high molecular material is the excellent high molecular material PVA of biological degradability, preferably
One of or it is a variety of.
The nanoparticle is one of BN, AlN, GO.
The quality of nanoparticle is the 5-50wt% of high molecular material quality.
The preparation method of the Biodegradable composite filter tip material of the controllable cigarette filter temperature of the present invention, including walk as follows
It is rapid:
Step 1: high molecular material PVA being dissolved in deionized water at 65-85 DEG C, preparing and obtaining concentration is 15-
The Polymer Solution of 25wt%；
Step 2: in order to improve the dispersion effect of the nanoparticle of high thermal conductivity coefficient in the substrate, avoiding its formation serious
Reunite, nanoparticle is modified, obtains modified Nano particle；Modifying process is as follows:
For BN, since there are few reactive group (such as hydroxyls) on the surface BN, therefore the method for taking non-covalent bond modified,
Specifically comprise the following steps: that a certain amount of BN powder is taken to be dispersed in 500mL water, it is ultrasonic in CQX25-06 ultrasonic cleaner
8-10h is handled, later addition PEI class modifying agent, the mass ratio of BN and PEI class modifying agent is 1:2-4, continues to be ultrasonically treated 4h；
After reaction, centrifugation removes the unstripped BN opened, and gained filtrate is filtered, is dried to obtain modified BN.The PEI class modifying agent
For the mixing of one or more of PEI600, PEI1800, PEI10000, PEI70000.There are Louis between BN and PEI
Acid-base function.
For AlN, using surfactant-modified method, specifically comprise the following steps: that suitable AlN powder is taken to be dispersed in
In 200mL water, it being ultrasonically treated 8-10h, is added surfactant later, the mass ratio of AlN and surfactant is 1:4-6, after
Continuous ultrasonic treatment 5h；After reaction, centrifugation removes the unstripped AlN opened, and gained filtrate is filtered, is dried to obtain Modification on Al N.
The surfactant is cetyl trimethylammonium bromide, neopelex, lauryl sodium sulfate, myristyl
The mixing of one or more of trimethyl ammonium chloride.
GO contains on surface more hydroxyl reactive group, therefore takes silane coupling agent graft-modification method, specifically includes
Following steps: taking suitable GO, is dispersed in 200mL ethyl alcohol, is ultrasonically treated 8-10h, silane coupling agent, GO and silicon are added later
The mass ratio of alkane coupling agent is 1:3-5, continues ultrasonic reaction 5h；It is centrifuged, is successively washed with ethyl alcohol, deionization after reaction
It washs, is dried to obtain modified GO.The silane coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane, ethylene
The mixing of one or more of base three (beta-methoxy ethyoxyl) silane, gamma-aminopropyl-triethoxy-silane.
Step 3: by modified Nano particle ultrasonic disperse in deionized water, obtaining uniform dispersion liquid；Gained is dispersed
Liquid is added in the Polymer Solution that step 1 is prepared, and continues to be stirred by ultrasonic, and mixes two kinds of particles being added with basis material
It is even, obtain composite solution；
Step 4: being processed, prepared by the composite solution that electrostatic spinning or twin-screw extrusion molding obtain step 3
Obtain the filter tip material of high porosity.
The electrostatic spinning is to carry out Static Spinning in the sample injector for take the composite solution addition electrostatic spinning machine of step 3 acquisition
Silk, spinning voltage 16-22kV, the distance of spray head to receiver board are 9-15cm, and injecting speed is 0.01-0.1mm/min.
The twin-screw extrusion molding includes the following steps: the composite solution forced air drying for obtaining step 3, obtains bulk
Composite material adds twin-screw extrude after high-temperature fusion, filter tip material is obtained after extrusion molding.In order to increase filter tip and cigarette
The contact area of gas, using honeycomb die, obtains the filter tip material with special cellular structure when twin-screw extrusion forms；
Double screw extruder parameter are as follows: diameter D=35mm, draw ratio L/D=36, axle speed in the same direction is variable, temperature range: 120-250 DEG C,
Extruded velocity is 200r/min.
The filter tip material that the present invention prepares can be used directly as cigarette filter tip material.
Compared with prior art, the beneficial effects of the present invention are embodied in:
The high polymer filter substrate that the present invention uses has excellent biological degradability, and the filter tip after discarding can be in enzyme, micro-
The substances such as carbon dioxide and water are degraded under the conditions of biology etc., not will cause environmental pollution；The present invention is for the first time by high thermal conductivity coefficient
Nanoparticle be added in base filter, be capable of forming continuous heat conduction network in the substrate with nanoparticle；The present invention adopts
The cigarette filter of high-specific surface area and porosity can be obtained with electrostatic spinning and extrusion molding processing technology；It is of the invention first
Secondary to be prepared for a kind of polymer-based cigarette filter of Biodegradable, which can effectively control cigarette mainstream flue gas temperature
At 40 DEG C or so.
Specific embodiment
Following embodiment is further intended to illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses.
Embodiment 1:
1, modified BN preparation: 0.5g BN is taken, is dispersed in 200mL water, 8-10h is ultrasonically treated.1.5gPEI- is added later
10000, continue ultrasound 5h.After reaction, 3500rpm centrifugation removes the unstripped BN opened.Filtrate is filtered, is dried to obtain most
Final product.
2, prepared by composite high-molecular solution: taking appropriate modified BN to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 75 DEG C, concentration 15wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 5wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 18kV, the distance of spray head to receiver board are 13cm, and injecting speed is 0.1mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 125 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Embodiment 2:
1, modified BN preparation: 0.5g BN is taken, is dispersed in 200mL water, 8-10h is ultrasonically treated.2.0gPEI- is added later
12000, continue ultrasound 5h.After reaction, 3500rpm centrifugation removes the unstripped BN opened.Filtrate is filtered, is dried to obtain most
Final product.
2, prepared by composite high-molecular solution: taking appropriate modified BN to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 75 DEG C, concentration 18wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 10wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 19kV, the distance of spray head to receiver board are 12cm, and injecting speed is 0.08mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 125 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Embodiment 3:
1, prepared by Modification on Al N: taking 0.5g AlN, is dispersed in 200mL water, is ultrasonically treated 8-10h.2.5g ten is added later
Six alkyl trimethyl ammonium bromides continue ultrasound 5h.After reaction, 3500rpm centrifugation removes the unstripped AlN opened.By filtrate
It filters, is dried to obtain final product.
2, prepared by composite high-molecular solution: taking appropriate Modification on Al N to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 65 DEG C, concentration 15wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 5wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 17kV, the distance of spray head to receiver board are 15cm, and injecting speed is 0.1mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 185 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Embodiment 4:
1, prepared by Modification on Al N: taking 0.5g AlN, is dispersed in 200mL water, is ultrasonically treated 8-10h.2.0g ten is added later
Sodium dialkyl sulfate continues ultrasound 5h.After reaction, 3500rpm centrifugation removes the unstripped AlN opened.Filtrate is filtered, is done
It is dry to obtain final product.
2, prepared by composite high-molecular solution: taking appropriate Modification on Al N to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 65 DEG C, concentration 18wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 10wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 18kV, the distance of spray head to receiver board are 16cm, and injecting speed is 0.12mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 185 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Embodiment 5:
1, modified GO preparation: 0.5g GO is taken, is dispersed in 200mL ethyl alcohol, 8-10h is ultrasonically treated.2.0g second is added later
Alkenyl triethoxysilane continues ultrasound 5h.After reaction, 3500rpm is centrifuged, and ethyl alcohol, deionized water washing are dried to obtain
Final product.
2, prepared by composite high-molecular solution: taking appropriate modified GO to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 85 DEG C, concentration 15wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 5wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 18kV, the distance of spray head to receiver board are 15cm, and injecting speed is 0.1mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 150 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Embodiment 6:
1, modified GO preparation: 0.5g GO is taken, is dispersed in 200mL ethyl alcohol, 8-10h is ultrasonically treated.2.5g is added later
Gamma-aminopropyl-triethoxy-silane continues ultrasound 5h.After reaction, 3500rpm is centrifuged, and ethyl alcohol, deionized water washing are done
It is dry to obtain final product.
2, prepared by composite high-molecular solution: taking appropriate modified GO to be added in 100mL water, continual ultrasonic 6-8h is divided
Dispersion liquid A.It weighs a certain amount of PVA master batch to be dissolved completely in 100mL water, heating temperature is 85 DEG C, concentration 18wt%, ultrasound
It stirs evenly, obtains solution B.B solution is added in solution A, and continues ultrasound 4h, mixes two kinds of particles being added with matrix
Uniformly.It is 10wt% that the dosage of modified Nano particle, which accounts for macromolecule dosage,.
3, composite filter tip material forms
1. prepared by cigarette filter material electrostatic spinning: above-mentioned composite solution 10mL being taken to be added in the sample injector of electrostatic spinning machine
Carry out electrostatic spinning.Spinning voltage 19kV, the distance of spray head to receiver board are 16cm, and injecting speed is 0.12mm/min.
2. prepared by the filter tip material with special cellular structure: by above-mentioned composite solution in 70 DEG C of dryings, obtaining blocky multiple
Condensation material.The block that 150 DEG C of high-temperature fusions obtain, and using double screw extruder and the mold of honeycomb coaly, squeeze out cooling
It obtains with composite filter tip material.
Compared with Example 1, the filter tip material that embodiment 2 obtains shows the effect for preferably reducing flue-gas temperature, this
It is because more thermally conductive BN particles, which are added, is conducive to the network that conducts heat with forming continuous effective in the base, thus well will be hot
Amount evacuation.Continuous BN network can also provide more effective barrier action, be conducive to the retention to flue gas harmful substance.Equally
Ground, by comparing embodiment 3,4 and 5,6, it can be found that the composite filter tip material of high particle additive amount is all shown preferably
The effect of cooling and retention harmful substance.By comparing embodiment 2,4,6, it can be found that containing oxidation stone under identical additive amount
The filter tip material of black nanoparticle has best cooling effect, this may be because graphite oxide itself is with higher thermally conductive
Coefficient.In addition, the filter tip material containing graphite oxide also shows optimal harmful substance crown_interception, this may be due to it
With biggish lamella size and surface functional group abundant.
Claims (8)
1. a kind of Biodegradable composite filter tip material of controllable cigarette filter temperature, it is characterised in that:
It is to be obtained using the excellent high molecular material of biological degradability as substrate by the nanoparticle processing of addition high thermal conductivity coefficient
?；
The high molecular material is the excellent high molecular material PVA of biological degradability；
The nanoparticle is one of BN, AlN, GO.
2. Biodegradable composite filter tip material according to claim 1, it is characterised in that:
The high molecular material isPVA-210、PVA-105、PVA-224、
PVA-203、PVA-117、One of PVA-103 or a variety of.
3. Biodegradable composite filter tip material according to claim 1 or 2, it is characterised in that:
The quality of nanoparticle is the 5-50wt% of high molecular material quality.
4. the preparation method of Biodegradable composite filter tip material described in claim 1,2 or 3, it is characterised in that including as follows
Step:
Step 1: high molecular material PVA being dissolved in deionized water at 65-85 DEG C, preparing and obtaining concentration is 15-25wt%
Polymer Solution；
Step 2: in order to improve the dispersion effect of the nanoparticle of high thermal conductivity coefficient in the substrate, it being avoided to form serious group
It is poly-, nanoparticle is modified, modified Nano particle is obtained；
Step 3: by modified Nano particle ultrasonic disperse in deionized water, obtaining uniform dispersion liquid；Gained dispersion liquid is added
In the Polymer Solution for entering step 1 preparation, continue to be stirred by ultrasonic, is uniformly mixed two kinds of particles being added with basis material, obtains
Obtain composite solution；
Step 4: being processed, be prepared by the composite solution that electrostatic spinning or twin-screw extrusion molding obtain step 3
The filter tip material of high porosity.
5. the preparation method according to claim 4, it is characterised in that:
The electrostatic spinning is to carry out electrostatic spinning in the sample injector for take the composite solution addition electrostatic spinning machine of step 3 acquisition,
Spinning voltage 16-22kV, the distance of spray head to receiver board are 9-15cm, and injecting speed is 0.01-0.1mm/min.
6. the preparation method according to claim 4, it is characterised in that:
The twin-screw extrusion molding includes the following steps: the composite solution forced air drying for obtaining step 3, obtains blocky compound
Material adds twin-screw extrude after high-temperature fusion, filter tip material is obtained after extrusion molding.
7. preparation method according to claim 6, it is characterised in that:
When twin-screw extrusion forms, using honeycomb die.
8. preparation method according to claim 6 or 7, it is characterised in that:
Double screw extruder parameter are as follows: diameter D=35mm, draw ratio L/D=36, axle speed in the same direction is variable, temperature range: 120-
250 DEG C, extruded velocity 200r/min.
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| CN201811611032.XA CN109700072B (en) | 2018-12-24 | 2018-12-24 | Biodegradable composite filter tip material capable of regulating and controlling temperature of cigarette filter tip and preparation method thereof |
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| CN201811611032.XA CN109700072B (en) | 2018-12-24 | 2018-12-24 | Biodegradable composite filter tip material capable of regulating and controlling temperature of cigarette filter tip and preparation method thereof |
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| CN111304765A (en) * | 2020-03-30 | 2020-06-19 | 安徽中烟工业有限责任公司 | Carbon/phase-change material composite membrane for reducing mainstream smoke temperature of cigarette filter and preparation method thereof |
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| CN111304765A (en) * | 2020-03-30 | 2020-06-19 | 安徽中烟工业有限责任公司 | Carbon/phase-change material composite membrane for reducing mainstream smoke temperature of cigarette filter and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN109700072B (en) | 2020-08-28 |
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