CN107556499A - A kind of preparation method of glucose crosslinking plural gel and the application in cigarette - Google Patents
A kind of preparation method of glucose crosslinking plural gel and the application in cigarette Download PDFInfo
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- CN107556499A CN107556499A CN201710624748.2A CN201710624748A CN107556499A CN 107556499 A CN107556499 A CN 107556499A CN 201710624748 A CN201710624748 A CN 201710624748A CN 107556499 A CN107556499 A CN 107556499A
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- crosslinking
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Abstract
The invention discloses a kind of glucose crosslinking nano SiO2The preparation method of chitosan composite aerogel and the application in cigarette filter.Chitosan is dissolved in acetum, glucose is added and makees crosslinking agent, support the three-dimensional framework of chitosan, then add Nano-meter SiO_22Powder, then NaHCO is added dropwise3Solution adjusts pH value, and the hydrosol is obtained after heating water bath.The hydrosol obtains glucose crosslinking nano SiO after deionized water is cleaned, is freeze-dried2Chitosan aerogel composite.By gained glucose crosslinking nano SiO2Chitosan aerogel composite is broken, sieving is prepared into the particles of 20 40 mesh, applied in cigarette filter, reducing harmful ingredients in flue gas burst size, and to Sensory Quality of Cigarette without negative effect.
Description
Technical field
The present invention relates to cigarette material preparing technical field, and in particular to a kind of glucose with flue gas harm reduction function is handed over
Join Nano-meter SiO_22The preparation method of-chitosan plural gel particle and the application in cigarette filter.
Background technology
In recent years, to reduce cigarette harmfulness, the health of smoking consumer is preferably protected, researcher is in cigarette
Harm reduction field expands extensive research.Wherein, nano material of the addition with harm reduction function is important research in filter tip
Direction, it can reduce cigarette consumption person suck the harmfulness of flue gas.But the characters powder of nano material, seriously constrain
Its application in cigarette.One side nano-powder material is difficult to be added in cigarette filter with industrialized mode, on the other hand
Dusty material is added to after cigarette filter easily enters smoking consumer oral cavity with flue gas, causes new potential safety hazard.It will receive
Scattered be anchored in three-dimensional porous structure material of ground rice powder material is then added in cigarette filter, can both utilize nano material
Harm reduction performance, solve the problems, such as the above-mentioned both sides of nano material again.Biogas gel rubber material is that a kind of novel three-dimensional is more
Pore structure material, mostly with it is safe and nontoxic the characteristics of, be adapted to cigarette application, be anchored on biology by nano-powder material is scattered
In the loose structure of matter aerogel material, cigarette filter is then applied to, is expected to form new flue gas harm reduction technology.《One kind tool
There are the aerogel particle preparation method of flue gas harm reduction function and the application in cigarette filter》(application number：
201610827775.5) a kind of porous agar aeroge prepared using agar as matrix is disclosed, and was prepared in agar gel
Nano-meter SiO_2 is added in journey2, form agar-Nano-meter SiO_22Composite aerogel, applied in cigarette filter, reduce harmful ingredients in flue gas
Burst size.But there is agar and Nano-meter SiO_2 in this method2With reference to firmness have the defects of to be strengthened.
Chitosan contains abundant hydroxyl, amino isopolarity functional group, is expected to and Nano-meter SiO_22Combine closely.Gather on shell
Sugared aeroge also has some reports.CN201610462306.8 discloses a kind of preparation method of chitosan aeroge, uses ethanol
Water dual solvent system, using chitosan, crosslinking agent in binary solvent solvability is different and caused minute yardstick activity
Grain, the fine skeleton of crosslinking can be formed during chemical gel, increase the gel probability of raw material, through CO 2 supercritical
Dry and the chitosan aeroge with high-specific surface area is made.But this method is using solidifying using crosslinking agents such as glutaraldehydes as being formed
The necessary condition of glue, preparation procedure is cumbersome, and Sensory Quality of Cigarette can be adversely affected applied to after cigarette filter.Together
When, use before supercritical drying the application that acetone and other organic solvent immersion is also it in cigarette to bury potential safety hazard.Chitosan-
Silicon dioxide composite aerogel also has been reported that (preparation, modification and its performance of the pretty chitosan-silicon dioxides composite aerogel of horse
Study master thesis, University Of Tianjin), but methods described is the preparation method based on aerosil, silica
For in-situ preparation, the particle diameter and pore structure of silica can not be selected.
Chitosan is dissolved in acetum by the present invention, adds glucose and stirring and dissolving, crosslinking agent is made using glucose,
The three-dimensional framework of chitosan is supported, then adds Nano-meter SiO_22Powder, then NaHCO is added dropwise3Solution adjusts pH value, through heating water bath
After obtain the hydrosol.The hydrosol obtains glucose crosslinking nano SiO after deionized water is cleaned, is freeze-dried2- chitosan is compound
Aerogel material；By gained glucose crosslinking nano SiO2- chitosan aerogel composite is prepared into the particle of 20-40 mesh,
Applied in cigarette filter, reducing harmful ingredients in flue gas burst size, and to Sensory Quality of Cigarette without negative effect.
The content of the invention
The purpose of the present invention is intended to fully porous with reference to the flue gas harm reduction performance and biogas gel three-dimensional of nano material
The carrier function of structure, there is provided a kind of suitable for cigarette filter addition, the glucose crosslinking nano with flue gas harm reduction function
SiO2The preparation method of-chitosan aerogel composite.
The present invention is realized by implementation below.
Unless otherwise indicated, percentage of the present invention is percetage by weight.
A kind of glucose crosslinking nano SiO2The preparation method of-chitosan composite aerogel, comprises the following steps：Prepare one
Determine the chitosan-acetic acid solution of concentration, add glucose and stirring and dissolving, make crosslinking agent using glucose, support the three of chitosan
Skeleton is tieed up, is proportionally added into Nano-meter SiO_22Powder, stir, then a certain amount of NaHCO is added dropwise3Solution, regulation reaction solution pH
Value, and stir, the hydrosol is obtained after heating water bath.The hydrosol soaks through deionized water, cleaned, and is obtained after freeze-drying
Glucose crosslinking nano SiO2- chitosan composite aerogel；Crush and sieve, obtain graininess gel rubber material.
The optimal technical scheme of preparation method of the present invention is：
(1) weigh 1 part of chitosan and be dissolved in the chitosan-acetic acid solution that 1wt% is made in 0.1M acetums；
(2) 0.1 part of glucose and stirring and dissolving are added, forms mixed solution；
(3) 0.2 part -0.8 part Nano-meter SiO_2 is weighed2Powder, it is added in the mixed solution of above-mentioned (2) formation, stirring is equal
It is even；
(4) 1mol/L NaHCO are added dropwise3Solution to pH be 6.4；
(5) liquid obtained by step (4) is put into insulation 1h in 45 DEG C of thermostat water baths and obtains hydrogel, water-setting calymma is existed
Soak, clean in deionized water；
(6) glucose crosslinking nano SiO is obtained by step (5) products obtained therefrom is freeze-dried2The compound airsetting of-chitosan
Glue；
(7) by step (6) the glucose crosslinking nano SiO2The broken sieving of-chitosan composite aerogel, obtains 20-40
Mesh gel particle.
Nano-meter SiO_22BET specific surface area be preferably specific surface area >=600m2/g。
The present invention also aims to provide above-mentioned glucose crosslinking nano SiO2- chitosan composite aerogel particle is being rolled up
Application in cigarette.
Invention also provides a kind of glucose crosslinking nano SiO2- chitosan composite aerogel is in cigarette filter
Using.100mg-120mg can be added into the cavity reserved between two-section vinegar fibre filter core, preferably during filter stick formation
100mg glucose crosslinking nano SiO2- chitosan composite aerogel particle, vinegar fibre filter stick-particle-vinegar fibre filter stick ternary is made
Composite filter.
Can also be by glucose crosslinking nano SiO2- chitosan composite aerogel particle dissipates the tow for being spread across cigarette filter rod
On, loading glucose crosslinking nano SiO is made2- chitosan composite aerogel particle vinegar fibre filter stick；Again will loading glucose crosslinking
Nano-meter SiO_22The vinegar fibre filter stick of-chitosan composite aerogel particle is connected with conventional vinegar fibre filter stick, and binary composite filter is made
Rod.By glucose crosslinking nano SiO2- chitosan composite aerogel particle is dissipated when being spread across on cigarette filter rod tow, preferably fine in vinegar
During filter stick formation, by the glucose crosslinking nano SiO2- chitosan composite aerogel particle presses 20~40mg/10mm silks
The addition of beam, which equably dissipates, to be sprinkled upon on filter stick tow.
Compared with prior art, the invention has the advantages that：
1st, gel preparation course without using glutaraldehyde etc. it is poisonous and harmful, influence Sensory Quality of Cigarette crosslinking agent, pass through Portugal
Grape sugar is cooked crosslinking agent, is supported the three-dimensional framework of chitosan, is added Nano-meter SiO_22The specific surface area of-chitosan gel rubber, tie hole
Structure is more flourishing.The present invention breaches the routine techniques of gel preparation, improves the security of chitosan gel rubber, it also avoid to
Sensory Quality of Cigarette is negatively affected；
2nd, chitosan forms three-dimensional net structure, Nano-meter SiO_22It is embedded on network, the two is tightly combined, and is both body phase material
Material, there is the performance of nano material again, adsorption rate and adsorption capacity can be increased.
3rd, the present invention adds glucose crosslinking nano SiO using binary, ternary composite rod as carrier2The compound gas of-chitosan
Gel particle, it can effectively reduce the content of the harmful components such as hydrogen cyanide in flue gas, crotonaldehyde.
Brief description of the drawings
Fig. 1 is glucose crosslinking nano SiO of the present invention2ESEM (SEM) photo of-chitosan composite aerogel；
Embodiment
Technical scheme is described further with reference to embodiments.Specific embodiment described herein is only
For explaining the present invention, and it should not be construed as limitation of the invention.
Embodiment 1
Weigh 50g chitosans and be dissolved in the chitosan-acetic acid solution that 1wt% is made in 0.1M acetums, add 5g glucose
And stirring and dissolving, add 10g Nano-meter SiO_2s2Powder, then ultrasonic disperse 5min is stirred until homogeneous scattered, then delay while stirring
It is slow that 1mol/L NaHCO are added dropwise3Solution to pH value is 6.4, high degree of agitation 5min again after dripping, is subsequently placed into 45 DEG C of thermostatted waters
1h is incubated in bath and obtains hydrogel, 12h in deionized water will be steeped after hydrogel stripping and slicing and a water was changed every 3 hours, most
It is freeze-dried 24h again afterwards and obtains glucose crosslinking nano SiO2- chitosan composite aerogel, gel white puff.The gel
Through broken, sieving, 20-40 mesh gel particles are obtained.
Embodiment 2
Weigh 50g chitosans and be dissolved in the chitosan-acetic acid solution that 1wt% is made in 0.1M acetums, add 5g glucose
And stirring and dissolving, add 20g Nano-meter SiO_2s2Powder, ultrasonic disperse 10min, be then stirred until homogeneous it is scattered, then while stirring
1mol/L NaHCO are slowly added dropwise3Solution to pH value is 6.4, high degree of agitation 5min again after dripping, is subsequently placed into 45 DEG C of constant temperature
1h is incubated in water-bath and obtains hydrogel, 12h in deionized water will be steeped after hydrogel stripping and slicing and a water was changed every 3 hours,
Finally being freeze-dried 24h again obtains glucose crosslinking nano SiO2- chitosan composite aerogel, gel white puff.It is described solidifying
Glue obtains 20-40 mesh gel particles through broken, sieving.
Embodiment 3
Weigh 50g chitosans and be dissolved in the chitosan-acetic acid solution that 1wt% is made in 0.1M acetums, add 5g glucose
And stirring and dissolving, add 40g Nano-meter SiO_2s2Powder, ultrasonic disperse 15min, be then stirred until homogeneous it is scattered, then while stirring
1mol/L NaHCO are slowly added dropwise3Solution to pH value is 6.4, high degree of agitation 5min again after dripping, is subsequently placed into 45 DEG C of constant temperature
1h is incubated in water-bath and obtains hydrogel, 12h in deionized water will be steeped after hydrogel stripping and slicing and a water was changed every 3 hours,
Finally being freeze-dried 24h again obtains glucose crosslinking nano SiO2- chitosan composite aerogel, gel white puff.It is described solidifying
Glue obtains 20-40 mesh gel particles through broken, sieving.
Meanwhile it is prepared for not adding glucose (glucose) Nano-meter SiO_2 using above-described embodiment method2- chitosan coagulates
Glue.BET specific surface area detection shows heretofore described glucose crosslinking nano SiO2The ratio surface of-chitosan three-dimensional aeroge
Product is significantly higher than the gel rubber material for being not added with glucose formation, see the table below 1.
The BET specific surface area contrast statistical form of the gel of table 1.
In addition, have detected the absorption property of both gel rubber materials using single column run device, by taking crotonaldehyde as an example, it is inhaled
Attached result see the table below 2, as a result show glucose crosslinking nano SiO of the present invention2The absorption property of-chitosan composite aerogel is remote
Higher than the gel rubber material for being not added with glucose formation.
The absorption property contrast statistical form of the gel of table 2.
Fig. 1 is glucose crosslinking nano SiO2ESEM (SEM) photo of-chitosan composite aerogel.
Application Example 1
Using the glucose crosslinking nano SiO of the present invention2- chitosan composite aerogel particle, passes through filter stick formation equipment
With particle feeding equipment, 100mg glucose crosslinking nanos are added in the 6mm cavitys reserved between every two-section vinegar fibre filter core
SiO2- chitosan composite aerogel particle, is prepared into vinegar fibre filter stick-particle-vinegar fibre filter stick Three-element composite filter core, filter stick all four
Roll cigarette, glucose crosslinking nano SiO in the ternary composite filter tip of every cigarette2- chitosan composite aerogel particle adds
Dosage is 100mg.Harmful ingredients in flue gas testing result shows, compared with conventional vinegar fibre filter stick, adds glucose crosslinking nano
SiO2The Three-element composite filter core of-chitosan composite aerogel particle, which can more significantly reduce hydrogen cyanide in flue gas, crotonaldehyde etc., to be had
Evil composition burst size.Sensory Quality of Cigarette smoking result shows glucose crosslinking nano SiO2- chitosan composite aerogel particle
To cigarette smoking quality without negative effect.
Application Example 2
Using the glucose crosslinking nano SiO of the present invention2- chitosan composite aerogel particle, utilizes filter stick formation process
In particle feeding equipment production loading glucose crosslinking nano SiO2The vinegar fibre filter stick of-chitosan composite aerogel particle, so
The filter stick and common vinegar fibre filter stick are mutually connected in by binary compound filter candle by filter stick equipment complex afterwards, filter stick all four roll cigarette
, glucose crosslinking nano SiO in the binary combined filter tip of every cigarette2The addition of-chitosan composite aerogel particle is
30mg.Harmful ingredients in flue gas testing result shows, compared with conventional vinegar fibre filter stick, adds glucose crosslinking nano SiO2- shell gathers
The binary compound filter candle of sugared composite aerogel particle can more effectively reduce the release of the harmful components such as hydrogen cyanide in flue gas, crotonaldehyde
Amount.Sensory Quality of Cigarette smoking result shows glucose crosslinking nano SiO2- chitosan composite aerogel particle is to cigarette smoking
Quality is without negative effect.
Claims (6)
- A kind of 1. glucose crosslinking nano SiO2- chitosan composite aerogel preparation method, it is characterised in that：Prepare finite concentration Chitosan-acetic acid solution, add glucose and stirring and dissolving, make crosslinking agent using glucose, support the three-dimensional bone of chitosan Frame, it is proportionally added into Nano-meter SiO_22Powder, stir, then a certain amount of NaHCO is added dropwise3Solution, reacting liquid pH value is adjusted, and Stir, the hydrosol is obtained after heating water bath.The hydrosol is soaked through deionized water, cleaned, and grape is obtained after freeze-drying Sugared crosslinking nano SiO2- chitosan composite aerogel；Crush and sieve, obtain graininess gel rubber material.
- 2. glucose crosslinking nano SiO according to claim 12The preparation method of-chitosan composite aerogel, its feature exist In comprising the steps：(1) weigh 1 part of chitosan and be dissolved in the chitosan-acetic acid solution that 1wt% is made in 0.1M acetums；(2) 0.1 part of glucose and stirring and dissolving are added, forms mixed solution；(3) 0.2 part -0.8 part Nano-meter SiO_2 is weighed2Powder, it is added in the mixed solution of above-mentioned (2) formation, stirs；(4) 1mol/L NaHCO are added dropwise3Solution to pH be 6.4；(5) liquid obtained by step (4) is put into 45 DEG C of thermostat water baths and is incubated 1h and obtains hydrogel, by water-setting calymma go from Soak, clean in sub- water；(6) glucose crosslinking nano SiO is obtained by step (5) products obtained therefrom is freeze-dried2- chitosan composite aerogel；(7) by step (6) the glucose crosslinking nano SiO2The broken sieving of-chitosan composite aerogel, obtains 20-40 mesh and coagulates Glue particle.
- A kind of 3. glucose crosslinking nano SiO according to claim 1 or 22- chitosan composite aerogel preparation method, its It is characterised by：Nano-meter SiO_22BET specific surface area >=600m2/g。
- A kind of 4. glucose crosslinking nano SiO2Application of-chitosan the composite aerogel in cigarette filter, it is characterised in that： During filter stick formation, 100mg-120mg glucose crosslinking nano is added into the cavity reserved between two-section vinegar fibre filter core SiO2- chitosan composite aerogel particle, vinegar fibre filter stick-particle-vinegar fibre filter stick Three-element composite filter core is made.
- A kind of 5. glucose crosslinking nano SiO2Application of-chitosan the composite aerogel in cigarette filter, it is characterised in that：Will Glucose crosslinking nano SiO2- chitosan composite aerogel particle, which dissipates, to be spread across on the tow of cigarette filter rod, and loading glucose is made Crosslinking nano SiO2- chitosan composite aerogel particle vinegar fibre filter stick；Again will loading glucose crosslinking nano SiO2- chitosan is multiple Close aerogel particle vinegar fibre filter stick with conventional vinegar fibre filter stick to be connected, binary compound filter candle is made.
- 6. glucose crosslinking nano SiO according to claim 52- chitosan composite aerogel answering in cigarette filter With, it is characterised in that：It is described by glucose crosslinking nano SiO2- chitosan composite aerogel particle dissipates the silk for being spread across cigarette filter rod Shu Shang, refer to during vinegar fibre filter stick formation, by the glucose crosslinking nano SiO2- chitosan composite aerogel particle is pressed The addition of 20~40mg/10mm tow, which equably dissipates, to be sprinkled upon on filter stick tow.
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| CN109225150A (en) * | 2018-10-10 | 2019-01-18 | 烟台工程职业技术学院 | A kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde |
| CN111285345A (en) * | 2020-02-25 | 2020-06-16 | 中国科学院化学研究所 | Method for preparing carbon aerogel from hydrogel precursor material through hydrothermal process |
| CN112316563A (en) * | 2020-10-23 | 2021-02-05 | 马鞍山中经悦怿生命科技有限公司 | Apparatus and method for producing filter particles in filter tip |
| CN112316562A (en) * | 2020-10-23 | 2021-02-05 | 马鞍山中经悦怿生命科技有限公司 | Production equipment and method of cigarette filter tip filtering material |
| CN112369671A (en) * | 2020-11-16 | 2021-02-19 | 安徽中烟工业有限责任公司 | Novel heating non-combustion cigarette filter tip rod and preparation method thereof |
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| CN112369671A (en) * | 2020-11-16 | 2021-02-19 | 安徽中烟工业有限责任公司 | Novel heating non-combustion cigarette filter tip rod and preparation method thereof |
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