CN107252672A - A kind of modified phosphate aluminium molecular sieve filter tip adsorption material and preparation method and application - Google Patents
A kind of modified phosphate aluminium molecular sieve filter tip adsorption material and preparation method and application Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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- 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
- A24D3/16—Use of materials for tobacco smoke filters of inorganic materials
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The present invention relates to a kind of modified phosphate aluminium molecular sieve filter tip adsorption material and preparation method and application, belong to technical field of cigarettes.The sorbing material belongs to a kind of metal Fe and is modified the molecular sieves of APO 5, specific preparation process includes the steps such as preparation, crystallization, drying, the roasting of the Primogels of FeAPO 5, the sorbing material of preparation is the homogeneous molecular sieves of mesoporous APO 5 in aperture, Fe atoms are entered by lattice substitution changes its electronegativity and generation B Suan Wei centers after the skeletons of APO 5, use it for preparing after composite filter tip in cigarette filter, the burst size of phenol in cigarette mainstream flue gas, HCN and crotonaldehyde can be effectively reduced, thus with preferable application value.
Description
Technical field
The invention belongs to technical field of cigarettes, and in particular to a kind of modified phosphate aluminium molecular sieve filter tip adsorption material and its preparation
Method and application.
Background technology
With the continuous improvement of people's living standards, concern of the mankind to health and environment is generally strengthened, and smoking is brought
Health and ambient influnence attracted increasing attention.World tobacco tissue to the reducing tar and reducing harm of cigarette for a long time always
All pay much attention to, each national capital active response, and cigarette industry, as one of pillar industry of Chinese Economy Development, market is to cigarette
Requirement more and more higher.On the premise of consumer sensory's comfort level is not influenceed, the harmful components in cigarette smoke are reduced, this
It is directly the focus of tobacco research.It is a kind of effective method that sorbing material is added in cigarette filter.
Phenol, hydrogen cyanide and crotonaldehyde, which are belonged to, in flue gas negatively affects larger harmful components, all the time all by
The attention of scientific workers.But phenol in the reduction cigarette smoke carried out both at home and abroad, HCN and crotons aldehyde are ground at present
Work is studied carefully, for that can adsorb the material of three kinds of gas simultaneously and the few of reduction content requirement can be reached.Patent
CN 104941606A are used to reduce containing for crotonaldehyde and HCN in cigarette mainstream flue gas using molecular sieve-Polyethersulfone Composites
Amount, the reduced rate of crotonaldehyde is up to 22.03%-32.48%, and HCN reduced rate is up to 21.58%-34.20%；Patent
CN106263024A is prepared for a kind of cigarette additive, can reduce phenol 28.34% in flue gas；There is preparation in above-mentioned patent
The problem of technique is complex, or be difficult to while the problem of removing multiple harmful substances.How phenol, HCN, crotonaldehyde are reduced
Burst size, reduces bitting midges, is significant.
The content of the invention
Can be while reducing benzene in cigarette smoke there is provided one kind the invention aims to solve the deficiencies in the prior art
The sorbing material of phenol, hydrogen cyanide and crotonaldehyde release amount.The sorbing material is a kind of molecular sieve, uses it for preparing cigarette and is combined
Filter tip, so as to reduce the phenol in cigarette smoke, hydrogen cyanide and crotonaldehyde release amount；Invention also provides the sorbing material
Preparation method, the sorbing material is prepared from using hydrothermal synthesis method, and APO-5 molecular sieves are modified using lattice method of substitution,
Add FeAPO-5 after Fe and change electronegativity, material of the present invention is used for preparation in cigarette filter compound by generation B Suan Wei centers
After filter tip, the burst size of phenol in cigarette mainstream flue gas, HCN and crotonaldehyde can be effectively reduced, highest can reduce its burst size：
58%th, 55%, 54%, thus with preferable application value.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80%~85% phosphoric acid, continues to stir after 0.9~1.1h after adding, three are added dropwise in the state of stirring
Ethamine, continues to stir 1.9~2.1h after adding, obtains FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be n：（1-n）：
1：0.74~0.76：M, wherein n=0.03~0.09, m=1.00~1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
In the reactor of liner, after crystallization 24h~48h at a temperature of 180 DEG C~200 DEG C, to take out its rapid cooling room temperature, it
Wash 2 ~ 5 times afterwards, be placed in 118~122 DEG C of baking ovens and dry 7.5~8.5h, take out, wear into fine powder to minus 100 mesh, finally will be thin
Powder obtains FeAPO-5 in 450 DEG C~650 DEG C of Muffle kiln roasting 4h~6h hours, that is, is modified the absorption of phosphate aluminium molecular sieve filter tip
Material.
It is further preferred that step（1）In, by the water used in boehmite and by used in nitric acid dissolved ferric iron
Water is distilled water.
It is further preferred that step（2）In, after crystallization, taking-up is used frozen water to cool down, and makes its rapid cooling chamber
Temperature.
It is further preferred that step（2）In, step（2）During middle washing, adopt and be washed with deionized.
Washing in the present invention is not specifically limited to the consumption of water, is according to ordinary skill in the art means
Can.
It is further preferred that step（2）In, when wearing into fine powder, using agate mortar.
The present invention also provides modified phosphorus aluminium point made from the preparation method of above-mentioned modified phosphate aluminium molecular sieve filter tip adsorption material
Son sieve filter tip adsorption material.
Present invention simultaneously provides modified phosphorus aluminium made from the preparation method of above-mentioned modified phosphate aluminium molecular sieve filter tip adsorption material
Molecular sieve filter tip adsorption material as cigarette additive application.
It is further preferred that modified phosphate aluminium molecular sieve filter tip adsorption material is added in cigarette filter.
It is further preferred that addition is 20mg/ branch.
The amount of the crystallization water contained in boehmite in the present invention, boehmite is made to water used in suspension
Measure and be not specifically limited the amount of the water used in nitric acid dissolved ferric iron, as long as total amount is in the framework of the present definition.
Compared with prior art, its advantage is the present invention：
（1）The addition granulation that the present invention is propped up the FeAPO-5 of preparation by 20mg/ is made an addition in the middle part of cigarette filter, with preferable
Reduction cigarette smoke in phenol, HCN and crotonaldehyde release amount effect, and after infrared test is adsorbed Cambridge filter
Piece, sieve component is not found, illustrates that the material has good security.
（2）The invention provides a kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, the preparation of the material
Method belongs to hydrothermal synthesis method, and the sorbing material of preparation is the homogeneous mesoporous APO-5 molecular sieves in aperture, and Fe atoms enter APO-5
The iron load of skeleton replaces load for lattice, i.e., the coordination tetrahedron substitution bone of generating portion ferrous metal and oxygen in framework of molecular sieve
Aluminum-oxygen tetrahedron in frame.
（3）The present invention is modified APO-5 molecular sieves using lattice method of substitution, and FeAPO-5 changes electronegativity after Fe is added,
B Suan Wei centers are generated, material of the present invention is used to prepare after composite filter tip in cigarette filter, cigarette mainstream flue gas can be effectively reduced
In phenol, the burst size of HCN and crotonaldehyde, highest can reduce its burst size：58%th, 55%, 54%, thus with preferably pushing away
Wide application value.
Brief description of the drawings
Fig. 1 is the modified phosphate aluminum molecular screen of the preparation of present example nine in 20 μm of lower ESEMs（SEM）Figure；
Fig. 2 is the modified phosphate aluminum molecular screen of the preparation of present example nine in 10 μm of lower ESEMs（SEM）Figure.
Embodiment
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright scope.In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, are that can be obtained by buying
Conventional products.
Embodiment 1
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80% phosphoric acid, continues to stir after 0.9h after adding, triethylamine is added dropwise in the state of stirring, adds
Continue to stir 1.9h afterwards, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.03：
0.97：1：0.75：1.00；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 36h at a temperature of 200 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 2 times, is placed in 118 DEG C of baking ovens and dries 7.5h, takes out, fine powder is worn into minus 100 mesh using agate mortar,
Fine powder is finally obtained into FeAPO-5 in 550 DEG C of Muffle kiln roasting 6h hours, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material
Material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 2
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 85% phosphoric acid, continues to stir after 1.1h after adding, triethylamine is added dropwise in the state of stirring, adds
Continue to stir 2.1h afterwards, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.03：
0.97：1：0.75：1.11；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 24h at a temperature of 180 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 5 times, is placed in 122 DEG C of baking ovens and dries 8.5h, takes out, fine powder is worn into minus 100 mesh using agate mortar,
Fine powder is finally obtained into FeAPO-5 in 450 DEG C of Muffle kiln roasting 5h hours, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material
Material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 3
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80% phosphoric acid, continues to stir after 1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 2h, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.03：
0.97：1：0.75：1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 48h at a temperature of 190 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 2 times, is placed in 120 DEG C of baking ovens and dries 8h, take out, fine powder is worn into minus 100 mesh using agate mortar, most
Fine powder is obtained into FeAPO-5 in 650 DEG C of Muffle kiln roasting 4h hours afterwards, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 4
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80% phosphoric acid, continues to stir after 0.9h after adding, triethylamine is added dropwise in the state of stirring, adds
Continue to stir 2.1h afterwards, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.06：
0.94：1：0.75：1.00；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 48h at a temperature of 180 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 4 times, is placed in 119 DEG C of baking ovens and dries 7.6h, takes out, fine powder is worn into minus 100 mesh using agate mortar,
Fine powder is finally obtained into FeAPO-5 in 450 DEG C of Muffle kiln roasting 6h hours, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material
Material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 5
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 83% phosphoric acid, continues to stir after 1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 1.95h, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.06：
0.94：1：0.76：1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 24h at a temperature of 200 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 3 times, is placed in 121 DEG C of baking ovens and dries 8h, take out, fine powder is worn into minus 100 mesh using agate mortar, most
Fine powder is obtained into FeAPO-5 in 550 DEG C of Muffle kiln roasting 4h hours afterwards, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 6
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80% phosphoric acid, continues to stir after 1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 2h, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.06：
0.94：1：0.74：1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 36h at a temperature of 190 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 3 times, is placed in 120 DEG C of baking ovens and dries 8h, take out, fine powder is worn into minus 100 mesh using agate mortar, most
Fine powder is obtained into FeAPO-5 in 450 DEG C of Muffle kiln roasting 6h hours afterwards, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 7
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 85% phosphoric acid, continues to stir after 1.05h after adding, triethylamine is added dropwise in the state of stirring, adds
Continue to stir 2.05h afterwards, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.09：
0.91：1：0.75：1.00；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 24h at a temperature of 190 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 4 times, is placed in 121 DEG C of baking ovens and dries 8.2h, takes out, fine powder is worn into minus 100 mesh using agate mortar,
Fine powder is finally obtained into FeAPO-5 in 450 DEG C of Muffle kiln roasting 4h hours, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material
Material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 8
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 85% phosphoric acid, continues to stir after 1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 2h, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.09：
0.91：1：0.75：1.11；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 48h at a temperature of 200 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 3 times, is placed in 120 DEG C of baking ovens and dries 8h, take out, fine powder is worn into minus 100 mesh using agate mortar, most
Fine powder is obtained into FeAPO-5 in 650 DEG C of Muffle kiln roasting 6h hours afterwards, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Embodiment 9
A kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, comprises the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 85% phosphoric acid, continues to stir after 1h after adding, triethylamine is added dropwise in the state of stirring, after adding
Continue to stir 2h, obtain FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be 0.09：
0.91：1：0.75：1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
For in the reactor of liner, after crystallization 36h at a temperature of 180 DEG C, taking-up is used frozen water to cool down room temperature rapidly, is adopted afterwards
It is washed with deionized 3 times, is placed in 120 DEG C of baking ovens and dries 8h, take out, fine powder is worn into minus 100 mesh using agate mortar, most
Fine powder is obtained into FeAPO-5 in 550 DEG C of Muffle kiln roasting 5h hours afterwards, that is, is modified phosphate aluminium molecular sieve filter tip adsorption material,
Its scanning electron microscope (SEM) photograph is as depicted in figs. 1 and 2.
Step（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
Application process
The acetate fiber filter tip of cigarette is cut from middle part, the sorbing material prepared in embodiment 1-9 is added thereto, before addition
Sorbing material need to be controlled in 40-60 mesh by the granulation of common comminutor, granular size, and with normal activity charcoal mouth rod adding method
Add in cigarette filter, addition is 20mg/ branch, and to be cut but be added without FeAPO-5 blank cigarette in the middle part of filter tip
As control, each 6 cigarette of sample test, and one group of Duplicate Samples is set, collect flue gas with the trap of built-in cambridge filter
Composition.Needed all samples and cambridge filter before experiment in temperature（20±2）DEG C, humidity（60±2）% constant temperature and humidity tandem-driving bogie
Middle placement 48h, using the linear smoking machine of Britain Si Rulin CERULEANSM450 types, according to as defined in GB/T19609-2004
Method determines the content by phenol, HCN and crotonaldehyde in cigarette smoke after filter tip respectively, the results are shown in Table 1.
The testing result that the cigarette smoke of table 1 passes through middle phenol, HCN, crotons aldehyde after filter tip
It is can be seen that from upper table testing result after the sorbing material added in cigarette filter prepared by the present invention, can be preferably
Reduction flue gas in phenol, HCN and crotonaldehyde burst size.When preparation condition is：Metal molar ratio（Fe：Al）0.09th, crystallization
When time 36h, 180 DEG C of crystallization temperature, demoulding time 5h, 550 DEG C of calcining temperature when, prepared Fe-APO5 molecular sieves are reachable
To optimal adsorption effect, the reduced rate of phenol, HCN and crotonaldehyde is respectively up to 58%, 55%, 54% in flue gas.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material, it is characterised in that comprise the following steps：
Step（1）, the preparation of FeAPO-5 Primogels：Suspension is made of water for boehmite, afterwards by ferric nitrate water
After dissolving, it is added in boehmite suspension, stirring is mixed in suspension；Afterwards, under stirring, dropwise
Addition volumetric concentration is 80%~85% phosphoric acid, continues to stir after 0.9~1.1h after adding, three are added dropwise in the state of stirring
Ethamine, continues to stir 1.9~2.1h after adding, obtains FeAPO-5 Primogels；
Wherein, the Al in ferric nitrate, boehmite2O3、H3PO4, triethylamine and water the mol ratio of total consumption be n：（1-n）：
1：0.74~0.76：M, wherein n=0.03~0.09, m=1.00~1.22；
Total consumption of described water is made used in suspension for the amount of the crystallization water contained in boehmite, by boehmite
Water amount and the amount sum by the water used in nitric acid dissolved ferric iron；
Step（2）, crystallization, drying and roasting：By step（1）The FeAPO-5 Primogels prepared are added with polytetrafluoroethylene (PTFE)
In the reactor of liner, after crystallization 24h~48h at a temperature of 180 DEG C~200 DEG C, to take out its rapid cooling room temperature, it
Wash 2 ~ 5 times afterwards, be placed in 118~122 DEG C of baking ovens and dry 7.5~8.5h, take out, wear into fine powder to minus 100 mesh, finally will be thin
Powder obtains FeAPO-5 in 450 DEG C~650 DEG C of Muffle kiln roasting 4h~6h hours, that is, is modified the absorption of phosphate aluminium molecular sieve filter tip
Material.
2. the preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 1, it is characterised in that step
（1）In, it is distilled water by the water used in boehmite and by the water used in nitric acid dissolved ferric iron.
3. the preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 1, it is characterised in that step
（2）In, after crystallization, taking-up is used frozen water to cool down, and it is rapidly decreased to room temperature.
4. the preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 1, it is characterised in that step
（2）In, step（2）During middle washing, adopt and be washed with deionized.
5. the preparation method of modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 1, it is characterised in that step
（2）In, when wearing into fine powder, using agate mortar.
6. change made from the preparation method of the modification phosphate aluminium molecular sieve filter tip adsorption material in claim 1-5 described in any one
Property phosphate aluminium molecular sieve filter tip adsorption material.
7. change made from the preparation method of the modification phosphate aluminium molecular sieve filter tip adsorption material in claim 1-5 described in any one
Property phosphate aluminium molecular sieve filter tip adsorption material as cigarette additive application.
8. modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 7 is as the application of cigarette additive, it is special
Levy and be, modified phosphate aluminium molecular sieve filter tip adsorption material is added in cigarette filter.
9. modified phosphate aluminium molecular sieve filter tip adsorption material according to claim 8 is as the application of cigarette additive, it is special
Levy and be, addition is 20mg/ branch.
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| CN108246247A (en) * | 2018-01-03 | 2018-07-06 | 昆明理工大学 | A kind of modified phosphate aluminum molecular screen flue gas sorbing material and preparation method and application |
| CN108272133A (en) * | 2018-01-03 | 2018-07-13 | 昆明理工大学 | A kind of additive and the preparation method and application thereof |
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