CN108272133A - A kind of additive and the preparation method and application thereof - Google Patents
A kind of additive and the preparation method and application thereof Download PDFInfo
- Publication number
- CN108272133A CN108272133A CN201810004581.4A CN201810004581A CN108272133A CN 108272133 A CN108272133 A CN 108272133A CN 201810004581 A CN201810004581 A CN 201810004581A CN 108272133 A CN108272133 A CN 108272133A
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- Prior art keywords
- mgapo
- additive
- preparation
- added
- boehmite
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- 239000000654 additive Substances 0.000 title claims abstract description 28
- 230000000996 additive effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 63
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 36
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 31
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 27
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 13
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000003517 fume Substances 0.000 claims abstract description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000725 suspension Substances 0.000 claims description 16
- -1 boehmite2O3 Chemical compound 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000002808 molecular sieve Substances 0.000 abstract description 9
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 230000000391 smoking effect Effects 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000000779 smoke Substances 0.000 description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- 239000003546 flue gas Substances 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 108010033040 Histones Proteins 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 210000000577 adipose tissue Anatomy 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003683 cardiac damage Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002010 green coke Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000006749 inflammatory damage Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000862 numbness Toxicity 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0204—Preliminary operations before the filter rod forming process, e.g. crimping, blooming
- A24D3/0212—Applying additives to filter materials
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
Abstract
The present invention disclose it is a kind of can in selectivity reducing cigarette fume ammonia level additive and the preparation method and application thereof.Using triethylamine as template, boehmite is silicon source, and phosphoric acid is phosphorus source, and magnesium nitrate is function monomer, using 5 molecular sieves of hydro-thermal method poromerics MgAPO.By the additive application in cigarette filter, additive amount can be adjusted arbitrarily as needed.It only adds additive 20mg and can selectively reduce ammonia content and be up to 50.38%, selectivity reduces the effect of ammonia clearly, can be used in production of cigarettes.
Description
Technical field
The present invention relates to a kind of additives and the preparation method and application thereof, and in particular to a kind of energy selectivity reducing cigarette cigarette
The additive and the preparation method and application thereof of ammonia level, belongs to cigarette material preparing technical field in gas.
Background technology
Nitrogenous compound of the ammonia in tobacco and other auxiliary materials in cigarette smoke, suitable nitrogenous compound
Content can keep flue gas physiological strength appropriate and concentration, but excessively high nitrogenous compound content not only makes flue gas coarse, production
Green coke burning, and will produce a large amount of harmful components.During the smoking process, these nitrogenous compounds can different degrees of real estate
Ammonifying.Ammonia not only influences the jealous of cigarette, also has certain toxicity.Low concentration ammonia has stimulation, high strength ammonia to mucous membrane
The tissue solubilities such as histone denaturation, adipose tissue saponification can be caused downright bad（That is saponification）.The higher ammonia warp of concentration
Respiratory tract sucks alveolar, and most of absorbed into serum makes ammonia concentration increase, and causes central nervous system damage, numb after first excited
Numbness；Ammonia can also cause fatty degeneration of liver, kidney interstitial inflammation and cardiac damage.
So control reduction ammonia level is extremely important in a certain range.Certainly, the research of ammonia in cigarette is reduced at present
Also have very much, a such as patent CN201210001070, but the absorption do not have selectivity in flue gas beneficial to pernicious gas all
There is absorption.In addition 30% or more can be reached to ammonia gas absorption in patent CN201410134481, but the material in the patent adds
Amount is 40mg or more.If the material amount too conference added in filter tip influences draw resistance, it is unfavorable for smoking.
Invention content
The purpose of the present invention is to solve the shortcomings of the prior art ammonia in a kind of energy selectivity reducing cigarette fume of offer
Additive of content and the preparation method and application thereof.Additive prepared by the present invention is MgAPO-5, which is that a kind of magnesium changes
Property phosphate molecule sieve, specific surface area is larger, and hydro-thermal is good, with stronger B acid position can be directed to flue gas in ammonia have choosing
Selecting property chemisorption can effectively reduce the ammonia level in cigarette smoke.
The object of the invention is achieved through the following technical solutions：
It is a kind of can in selectivity reducing cigarette fume the additive of ammonia level preparation method, include the following steps：
（1）The preparation of MgAPO-5 Primogels：Suspension is made with water in boehmite, later by magnesium nitrate water dissolution
Afterwards, it is added in boehmite suspension, is stirred in suspension；Later, it under stirring, is added dropwise
The phosphoric acid that volumetric concentration is 80~85%, after continuing 0.9~1.1h of stirring after adding, is added dropwise three second in the state of stirring
Amine continues 1.9~2.1h of stirring after adding, obtain MgAPO-5 Primogels；
Wherein, the Al in magnesium nitrate, boehmite2O3、H3PO4, triethylamine and water total dosage molar ratio be n:(1-n):
1:0.74~0.76:M, wherein n=0.03~0.09, m=1.00~1.22；Total dosage of the water is institute in boehmite
The amount of the crystallization water contained, the amount that boehmite is made to water used in suspension with by the amount of magnesium nitrate dissolving water used it
With.
（2）Crystallization, drying and roasting：By step（1）The MgAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
In the reaction kettle of liner, at 180~200 DEG C after 24~48h of crystallization, taking-up is rapidly cooled to room temperature, washes 2 ~ 5 later
It is secondary, be placed in 118~122 DEG C of baking ovens dry 7.5~8.5h, take out, wear into fine powder to 100 mesh, finally by fine powder 450~
650 DEG C of Muffle 4~6h of kiln roasting, obtains MgAPO-5, i.e., the described additive.
The present invention also provides the additive MgAPO-5 made from the preparation method.
The present invention also provides the additive MgAPO-5 made from the preparation method as answering in cigarette additive
With.
Preferably, MgAPO-5 is added in cigarette filter.
XRD tests are done to MgAPO-5 obtained, test spectrogram is as shown in Figure 2.The XRD of MgAPO-5 as can be seen from Figure 2
There is characteristic peak and corresponds to crystal face in 2 θ=100 °, 20 °, 34 °, 56 °, 59 °, 69 °, 36 ° and 23 ° in spectrogram（100）、（211）、
（002）、（200）、（110）、（220）、（311）、（400）It is completely the same with the characteristic peak of APO-5, illustrate metal heteroatom crystalline substance
It is in AFI topological structures not destroy original phosphate aluminium molecular sieve skeleton after aluminium on lattice substitution skeleton.Table 1 is to pass through cell parameter
The data being calculated, it can be seen that the unit cell volume of APO-5 increases compared with the unit cell volume of MgAPO-5, and in figure
There is no the appearance of the peak of metal and metal oxide, and this illustrates metals to be successfully doped in skeleton.
Table 1
Metal state in framework of molecular sieve is measured to MgAPO-5 molecular sieves XPS, curve obtained is as shown in figure 3, can from Fig. 3
To find that stronger peak occurs at 1304.6eV in the sample, correspond to the Mg1s of divalent magnesium, it was demonstrated that have Mg2+Presence.And
Al3+By Mg2+Electronics pair can be received by having extra active sites after substitution and vacating, and produce acid centre, and ammonia molecule has a pair
Lone electron pair can be coordinated with unoccupied orbital, so MgAPO-5 molecular screen materials are to NH3There are a large amount of absorption.
Nitrogen adsorption-desorption test to MgAPO-5 molecular sieves, Fig. 4 is nitrogen adsorption-desorption of MgAPO-5 molecular sieves
Curve and graph of pore diameter distribution, it is seen that adsorption desorption balanced line is 0.3<P/P0<Standard is presented in 0.9 pressure limit
IV type hysteresis loop, illustrate that two kinds of materials are the uniform mesoporous material in aperture；Absorption when relative pressure is relatively low is by hole wall
It caused by monolayer adsorption, is hereafter adsorbed for multilayer under medium relative pressure, is capillary condensation under higher relative pressure, is allowed to
There is hysteresis loop.It is as shown in table 2 through BJH method result of calculations.The aperture of the purer APO-5 of MgAPO-5 is more as can be seen from Table 2
Greatly, specific surface area is smaller, after illustrating that Mg elements enter APO-5 skeletons instead of part Al elements and part P element, causes
The structure of MgAPO-5 is regular not as good as APO-5, destroys the order in duct so that total specific surface area reduces, and part pore structure
Caving in causes average pore size slightly to increase.By BET data it can be seen that the channel that the presence of MgAPO-5 meso-hole structures provides allows to have
Evil ingredient ammonia enters, it is possible to a large amount of ammonias of physical absorption.
Table 2
Compared with prior art, the present invention has the following advantages：
1, the present invention prepares MgAPO-5 molecular sieves compound materials using the method that hydrothermal synthesis and chemical preparation are modified, and prepares item
Part is mild, favorable reproducibility；
2, MgAPO-5 additive amounts prepared by the present invention are 10 ~ 20mg/ branch, and the ammonia amount that can significantly effectively reduce in flue gas is high
Up to 27.08 ~ 50.38%, the reduced rate of ammonia in cigarette smoke compared with the prior art can be greatly improved；
3, smoking experiment after, by infrared detection, do not find the material on cambridge filter, illustrate the material will not with smoking and
In suction body, so the material is safe and reliable.
Description of the drawings
Fig. 1 is the scanning electron microscope of MgAPO-5 prepared by embodiment 3（SEM）Figure；
The XRD spectra for the MgAPO-5 sieve samples that Fig. 2 is APO-5 and prepared by embodiment 3；
Fig. 3 is the XPS spectrum figure of MgAPO-5 prepared by embodiment 3；
Fig. 4 is physical absorption-desorption curve of MgAPO-5 prepared by embodiment 3.
Specific implementation mode
Embodiment is the further description to the present invention below, but embodiment is not to technical scheme of the present invention
It limits.
Embodiment 1
It is a kind of can in selectivity reducing cigarette fume the additive of ammonia level preparation method, include the following steps：
（1）The preparation of MgAPO-5 Primogels：Suspension is made with water in boehmite, later by magnesium nitrate water dissolution
Afterwards, it is added in boehmite suspension, is stirred in suspension；Later, it under stirring, is added dropwise
The phosphoric acid that volumetric concentration is 80% continues after stirring 0.9h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 1.9h, obtains MgAPO-5 Primogels；
Wherein, the Al in magnesium nitrate, boehmite2O3、H3PO4, triethylamine and water total dosage molar ratio be 0.03:
0.97:1:0.74:1.00；
（2）Crystallization, drying and roasting：By step（1）The MgAPO-5 Primogels prepared are added using polytetrafluoroethylene (PTFE) as liner
Reaction kettle in, at 180 DEG C after crystallization 36h, taking-up used ice water to be rapidly cooled to room temperature, later use deionized water
Washing 2 times is placed in 118 DEG C of baking ovens dry 7.5h, takes out, wear into fine powder to 100 mesh using agate mortar, finally fine powder exists
450 DEG C of Muffle kiln roasting 6h, obtains MgAPO-5, i.e., the described additive.
MgAPO-5 molecular screen materials made from the present embodiment are first passed through and are ground up, sieved to 40 ~ 60 mesh, made by comminutor
Grain, is added to normal activated carbon adding method in filter tip.Addition is every 20mg, and cigarette finished product is made.It is taken out in standard
Smoking experiment is carried out under the conditions of suction, the blank cigarette of MgAPO-5 molecular sieves not to be added as a contrast, each sample test 6
Cigarette, and one group of Duplicate Samples is set, collect smoke components with the trap of built-in cambridge filter.Need before experiment by all samples and
Cambridge filter is in temperature（20±2）DEG C, humidity（60±2）48h is placed in the constant temperature and humidity tandem-driving bogie of %, utilizes Britain Si Rulin
The linear smoking machine of CERULEANSM450 types is measured respectively according to method as defined in GB/T19609-2004 by being rolled up after filter tip
The content of cigarette ammonia in flue gas, result reduce ammonia 27.08% in cigarette smoke, and total granules reduced rate is 8.99%, is shown in Table 3.
Table 3
。
Embodiment 2
It is a kind of can in selectivity reducing cigarette fume the additive of ammonia level preparation method, include the following steps：
（1）The preparation of MgAPO-5 Primogels：Suspension is made with water in boehmite, later by magnesium nitrate water dissolution
Afterwards, it is added in boehmite suspension, is stirred in suspension；Later, it under stirring, is added dropwise
The phosphoric acid that volumetric concentration is 85% continues after stirring 1h after adding, triethylamine is added dropwise in the state of stirring, adds subsequent
Continuous stirring 2h, obtains MgAPO-5 Primogels；
Wherein, the Al in magnesium nitrate, boehmite2O3、H3PO4, triethylamine and water total dosage molar ratio be 0.06:
0.94:1:0.75:1.10；
（2）Crystallization, drying and roasting：By step（1）The MgAPO-5 Primogels prepared are added using polytetrafluoroethylene (PTFE) as liner
Reaction kettle in, at 190 DEG C after crystallization 48h, taking-up used ice water to be rapidly cooled to room temperature, later use deionized water
Washing 3 times is placed in 120 DEG C of baking ovens dry 8h, takes out, wear into fine powder to 100 mesh using agate mortar, finally fine powder exists
550 DEG C of Muffle kiln roasting 5h, obtains MgAPO-5, i.e., the described additive.
MgAPO-5 molecular screen materials made from the present embodiment are first passed through and are ground up, sieved to 40 ~ 60 mesh, made by comminutor
Grain, is added to normal activated carbon adding method in filter tip.Addition is every 20mg, and cigarette finished product is made.It is taken out in standard
Smoking experiment is carried out under the conditions of suction, the blank cigarette of MgAPO-5 molecular sieves not to be added as a contrast, each sample test 6
Cigarette, and one group of Duplicate Samples is set, collect smoke components with the trap of built-in cambridge filter.Need before experiment by all samples and
Cambridge filter is in temperature（20±2）DEG C, humidity（60±2）48h is placed in the constant temperature and humidity tandem-driving bogie of %, utilizes Britain Si Rulin
The linear smoking machine of CERULEANSM450 types is measured respectively according to method as defined in GB/T19609-2004 by being rolled up after filter tip
The content of cigarette ammonia in flue gas.Its result reduces ammonia 50.38% in cigarette smoke, and total granules reduced rate is 12.81%, is shown in Table 4.
Table 4
。
Embodiment 3
It is a kind of can in selectivity reducing cigarette fume the additive of ammonia level preparation method, include the following steps：
（1）The preparation of MgAPO-5 Primogels：Suspension is made with water in boehmite, later by magnesium nitrate water dissolution
Afterwards, it is added in boehmite suspension, is stirred in suspension；Later, it under stirring, is added dropwise
The phosphoric acid that volumetric concentration is 83% continues after stirring 1.1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 2.1h, obtains MgAPO-5 Primogels；
Wherein, the Al in magnesium nitrate, boehmite2O3、H3PO4, triethylamine and water total dosage molar ratio be 0.09:
0.91:1:0.76:1.22；
（2）Crystallization, drying and roasting：By step（1）The MgAPO-5 Primogels prepared are added using polytetrafluoroethylene (PTFE) as liner
Reaction kettle in, at 200 DEG C crystallization for 24 hours after, taking-up used ice water to be rapidly cooled to room temperature, later use deionized water
Washing 5 times is placed in 122 DEG C of baking ovens dry 8.5h, takes out, wear into fine powder to 100 mesh using agate mortar, finally fine powder exists
650 DEG C of Muffle kiln roasting 4h, obtains MgAPO-5, i.e., the described additive.
The scanning electron microscope of MgAPO-5 obtained（SEM）Figure is as shown in Figure 1, with the XRD spectra of APO-5 as shown in Fig. 2, XPS
Spectrogram is as shown in figure 3, physical absorption-desorption curve is as shown in Figure 4.
MgAPO-5 molecular screen materials made from the present embodiment are first passed through and are ground up, sieved to 40 ~ 60 mesh, made by comminutor
Grain, is added to normal activated carbon adding method in filter tip.Addition is every 20mg, and cigarette finished product is made.It is taken out in standard
Smoking experiment is carried out under the conditions of suction, the blank cigarette of MgAPO-5 molecular sieves not to be added as a contrast, each sample test 6
Cigarette, and one group of Duplicate Samples is set, collect smoke components with the trap of built-in cambridge filter.Need before experiment by all samples and
Cambridge filter is in temperature（20±2）DEG C, humidity（60±2）48h is placed in the constant temperature and humidity tandem-driving bogie of %, utilizes Britain Si Rulin
The linear smoking machine of CERULEANSM450 types is measured respectively according to method as defined in GB/T19609-2004 by being rolled up after filter tip
The content of cigarette ammonia in flue gas.Its result reduces ammonia 33.71% in cigarette smoke, and total granules reduced rate is 11.81%, is shown in Table 5；
Table 5
。
Claims (6)
1. the preparation method of the additive of ammonia level, includes the following steps in a kind of energy selectivity reducing cigarette fume：
（1）The preparation of MgAPO-5 Primogels：Suspension is made with water in boehmite, later by magnesium nitrate water dissolution
Afterwards, it is added in boehmite suspension, is stirred in suspension；Later, it under stirring, is added dropwise
The phosphoric acid that volumetric concentration is 80~85%, after continuing 0.9~1.1h of stirring after adding, is added dropwise three second in the state of stirring
Amine continues 1.9~2.1h of stirring after adding, obtain MgAPO-5 Primogels；
（2）Crystallization, drying and roasting：By step（1）The MgAPO-5 Primogels that prepare are added in reaction kettle, 180~
At 200 DEG C after 24~48h of crystallization, taking-up is rapidly cooled to room temperature, is washed 2 ~ 5 times later, in 118~122 DEG C dry 7.5
~8.5h takes out, wears into fine powder to 100 mesh, fine powder is finally roasted to 4~6h at 450~650 DEG C, obtains MgAPO-5, i.e. institute
State additive.
2. preparation method according to claim 1, which is characterized in that the Al in magnesium nitrate, boehmite2O3、H3PO4、
The molar ratio of total dosage of triethylamine and water is n:(1-n):1:0.74~0.76:M, wherein n=0.03~0.09, m=1.00~
1.22。
3. preparation method according to claim 1, which is characterized in that step（2）It is cooled in ice after middle crystallization
It is quenched in water.
4. additive MgAPO-5 made from preparation method described in claim 1.
5. the additive described in claim 4 is as the application in cigarette filter-tip additive agent.
6. application according to claim 5, which is characterized in that the additive MgAPO-5 to be added in cigarette filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810004581.4A CN108272133A (en) | 2018-01-03 | 2018-01-03 | A kind of additive and the preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810004581.4A CN108272133A (en) | 2018-01-03 | 2018-01-03 | A kind of additive and the preparation method and application thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5888921A (en) * | 1995-10-25 | 1999-03-30 | Abb Lummus Global Inc. | Binary molecular sieves having a core and shell of different structures and compositions |
| US20050133053A1 (en) * | 2003-12-22 | 2005-06-23 | Philip Morris Usa Inc. | Smoking articles comprising copper-exchanged molecular sieves |
| CN102205975A (en) * | 2011-05-28 | 2011-10-05 | 山西昆明烟草有限责任公司 | Modified aluminium phosphate molecular sieve additive capable of reducing aldehyde and ketone compound contents in cigarette smoke as well as preparation and application thereof |
| CN107252672A (en) * | 2017-07-21 | 2017-10-17 | 云南中烟工业有限责任公司 | A kind of modified phosphate aluminium molecular sieve filter tip adsorption material and preparation method and application |
| CN107416857A (en) * | 2017-07-21 | 2017-12-01 | 云南中烟工业有限责任公司 | A kind of modified phosphate aluminum molecular screen flue gas sorbing material containing cobalt and preparation method and application |
| CN107433179A (en) * | 2017-07-25 | 2017-12-05 | 滁州卷烟材料厂 | A kind of filter tip for being used to adsorb pernicious gas material in cigarette smoke |
-
2018
- 2018-01-03 CN CN201810004581.4A patent/CN108272133A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5888921A (en) * | 1995-10-25 | 1999-03-30 | Abb Lummus Global Inc. | Binary molecular sieves having a core and shell of different structures and compositions |
| US20050133053A1 (en) * | 2003-12-22 | 2005-06-23 | Philip Morris Usa Inc. | Smoking articles comprising copper-exchanged molecular sieves |
| CN102205975A (en) * | 2011-05-28 | 2011-10-05 | 山西昆明烟草有限责任公司 | Modified aluminium phosphate molecular sieve additive capable of reducing aldehyde and ketone compound contents in cigarette smoke as well as preparation and application thereof |
| CN107252672A (en) * | 2017-07-21 | 2017-10-17 | 云南中烟工业有限责任公司 | A kind of modified phosphate aluminium molecular sieve filter tip adsorption material and preparation method and application |
| CN107416857A (en) * | 2017-07-21 | 2017-12-01 | 云南中烟工业有限责任公司 | A kind of modified phosphate aluminum molecular screen flue gas sorbing material containing cobalt and preparation method and application |
| CN107433179A (en) * | 2017-07-25 | 2017-12-05 | 滁州卷烟材料厂 | A kind of filter tip for being used to adsorb pernicious gas material in cigarette smoke |
Non-Patent Citations (3)
| Title |
|---|
| SHYAMAL KUMAR SAHA,SURESH B. WAGHMODE,HIROYOSHI MAEKAWA等: "Synthesis of aluminophosphate molecular sieves with AFI topology substituted by alkaline earth metal and their application to solid acid catalysis", 《MICROPOROUS AND MESOPOROUS MATERIALS》 * |
| 冯利利，朱岳麟，齐兴义，李征，朱立群: "MgAPO-5分子筛的合成与表征", 《石油化工》 * |
| 杨晨，王亚明，蒋丽红: "磷铝分子筛的制备与应用研究进展", 《石油学报（石油加工）》 * |
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