CN106343634B - Integral type mouth mask - Google Patents
Integral type mouth mask Download PDFInfo
- Publication number
- CN106343634B CN106343634B CN201610938593.5A CN201610938593A CN106343634B CN 106343634 B CN106343634 B CN 106343634B CN 201610938593 A CN201610938593 A CN 201610938593A CN 106343634 B CN106343634 B CN 106343634B
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- oil bath
- under
- mouth mask
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- 239000002808 molecular sieve Substances 0.000 claims abstract description 74
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical class [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 81
- 238000010438 heat treatment Methods 0.000 claims description 78
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 73
- 238000013019 agitation Methods 0.000 claims description 73
- 239000007788 liquid Substances 0.000 claims description 64
- 239000000701 coagulant Substances 0.000 claims description 63
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 62
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 62
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical class CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 48
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical class [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 48
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical class [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 48
- 239000003643 water by type Substances 0.000 claims description 46
- DBRMBYFUMAFZOB-UHFFFAOYSA-N molybdenum nitric acid Chemical compound [Mo].[N+](=O)(O)[O-] DBRMBYFUMAFZOB-UHFFFAOYSA-N 0.000 claims description 39
- 229910052750 molybdenum Inorganic materials 0.000 claims description 38
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 33
- 238000002425 crystallisation Methods 0.000 claims description 32
- 230000008025 crystallization Effects 0.000 claims description 32
- 230000010355 oscillation Effects 0.000 claims description 32
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 32
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 31
- 235000016768 molybdenum Nutrition 0.000 claims description 31
- -1 polytetrafluoroethylene Polymers 0.000 claims description 31
- 238000001291 vacuum drying Methods 0.000 claims description 31
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 30
- 229910052754 neon Inorganic materials 0.000 claims description 30
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims description 30
- 239000012535 impurity Substances 0.000 claims description 29
- 230000032683 aging Effects 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000002604 ultrasonography Methods 0.000 claims description 16
- 238000001802 infusion Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims 1
- 239000004744 fabric Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 56
- 230000000694 effects Effects 0.000 abstract description 9
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 239000004745 nonwoven fabric Substances 0.000 abstract description 3
- 241000269350 Anura Species 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 103
- 239000011733 molybdenum Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 10
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 101100269850 Caenorhabditis elegans mask-1 gene Proteins 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010033307 Overweight Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 235000020825 overweight Nutrition 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
A kind of integral type mouth mask, including mask body, described mask body both sides are provided with fixing band, and described mask body includes interior mouth mask and outer mouth mask, and described interior mouth mask and outer mouth mask are integrally formed, also there is filter space between interior mouth mask and outer mouth mask, filter space is equipped with purification of air filtrate, and described interior mouth mask and outer mouth mask are non-woven fabrics, and described filtrate is Mo, the molecular sieves of Ni SAPO 34/ZSM 12, for formaldehyde adsorption.The mask body of the present invention is additionally provided with filter space, and filter space is equipped with purification of air filtrate, can effectively filter haze, and formaldehyde adsorption effect is good.
Description
Technical field
The present invention relates to a kind of integral type mouth mask, belong to daily life field.
Background technology
Haze weather was increasingly severe in recent years, pm2.5 severe overweights, and its content of formaldehyde of place after finishing also often surpasses
Mark, mist bring great threat to the health of people, and current common mouth mask adsorbent is substantially based on activated carbon, still
Absorption and filter effect of the activated carbon to particulate pollutant are limited, and various Organic Waste Gas Pollution things also gradually increase in air, living
Property carbon adsorbent can not decompose remove these pollutants, even if being adsorbed onto on mouth mask, also have an impact to health, thus in order to
Ensure the health of people, it is necessary to be improved to mouth mask adsorbent.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of integral type mouth mask, filtering effect of formaldehyde is good.
To achieve these goals, the technical solution adopted by the present invention is：A kind of integral type mouth mask, including mask body,
Described mask body both sides are provided with fixing band, and described mask body includes interior mouth mask and outer mouth mask, described interior mouth mask and
Outer mouth mask is integrally formed, and also has filter space between interior mouth mask and outer mouth mask, and filter space is equipped with purification of air filtrate.
Described interior mouth mask and outer mouth mask are non-woven fabrics.
Described filtrate is Mo, Ni-SAPO-34/ZSM-12 molecular sieves, for formaldehyde adsorption.
The mask body of the present invention is additionally provided with filter space, and filter space is equipped with purification of air filtrate, can there is effectively mistake
Haze is filtered, formaldehyde adsorption effect is good.
Brief description of the drawings
Fig. 1 is the schematic diagram of the present invention.
1st, interior mouth mask, 2, outer mouth mask, 3, fixing band, 4, filtrate.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
A kind of integral type mouth mask, including mask body, described mask body both sides are provided with fixing band 3, described mouth mask
Body includes interior mouth mask 1 and outer mouth mask 2, and described interior mouth mask and outer mouth mask are integrally formed, also had between interior mouth mask and outer mouth mask
There is filter space, filter space is equipped with purification of air filtrate 4.
Described interior mouth mask and outer mouth mask are non-woven fabrics.
Described filtrate is using tetraethyl orthosilicate and aluminium isopropoxide as silicon source and silicon source, using tetraethyl ammonium hydroxide as mould
Plate agent, nickel nitrate are nickel source, and nitric acid molybdenum is molybdenum source, and ZSM-12 molecular sieves are carrier etc., modified by magnetization, ultrasonic oscillation etc.
The Mo that means are prepared, Ni-SAPO-34/ZSM-12 molecular sieve, for formaldehyde adsorption.
Its specific preparation method of Mo, Ni-SAPO-34/ZSM-12 molecular sieve is as follows：
Embodiment 1 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:1 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 10gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 10gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 2 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:2 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 20gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 20gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 3 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:3 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 30gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 30 as one kind gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 4 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:4 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 40gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 40gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 5 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:5 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 50gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 50gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 6 prepares nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:6 sample.Nitric acid molybdenum 10g, nickel nitrate 10g,
60gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml, its from
Sub- water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 60gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 7 prepares nitric acid molybdenum and adds nickel nitrate and ZSM-12 mass ratioes to be 1:5 sample, wherein nitric acid molybdenum:Nickel nitrate is
1：2.Nitric acid molybdenum 5g, nickel nitrate 10g, 75gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphoric acid
4ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 5g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 75gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 8 prepares nitric acid molybdenum and adds nickel nitrate and ZSM-12 mass ratioes to be 1:5 sample, wherein nitric acid molybdenum:Nickel nitrate is
1：3.Nitric acid molybdenum 5g, nickel nitrate 15g, 100gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphoric acid
4ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 5g nitric acid molybdenums, 15g nickel nitrates are in ultrasonic oscillation oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 100gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 9 prepares nitric acid molybdenum and adds nickel nitrate and ZSM-12 mass ratioes to be 1:5 sample, wherein nitric acid molybdenum:Nickel nitrate is
1：4.Nitric acid molybdenum 5g, nickel nitrate 20g, 125gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphoric acid
4ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 5g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 12 5gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Embodiment 10 prepares nitric acid molybdenum and adds nickel nitrate and ZSM-12 mass ratioes to be 1:5 sample, wherein nitric acid molybdenum:Nickel nitrate is
1：5.Nitric acid molybdenum 5g, nickel nitrate 25g, 150gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphoric acid
4ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 5g nitric acid molybdenums, 25g nickel nitrates are in ultrasonic oscillation oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 155gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Reference examples 1 prepare nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:5 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 50gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under common concussion are removed
It is miscellaneous;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in commonly concussion oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 50gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Reference examples 2 prepare nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:5 sample.Nitric acid molybdenum 10g, nickel nitrate
10g, 50gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml,
Its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and stir 70 DEG C of 3h of oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of oil bath heating is stirred simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in stirring 100 DEG C of 3h of oil bath heating；
Step 6, carrier 50gZSM-12 is added in above-mentioned coagulant liquid and stirs 70 DEG C of 3h of oil bath heating；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of oil bath heating are stirred in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Reference examples 3 prepare nitric acid molybdenum and add nickel nitrate and ZSM-12 mass ratioes to be 1:5 sample, wherein nitric acid molybdenum:Nickel nitrate is
1：3.Nitric acid molybdenum 5g, nickel nitrate 15g, 100gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphoric acid
4ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 5g nitric acid molybdenums, 15g nickel nitrates are in ultrasonic oscillation oil bath
70 DEG C of 2h removal of impurities;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 100gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Reference examples 4 prepare nitric acid molybdenum, and ZSM-12 mass ratioes are 1:5 sample.Nitric acid molybdenum 10g, 50gZSM-12 molecular sieve 10g,
Tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml, its ionized water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2,4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenum removed in 70 DEG C of 2h of ultrasonic oscillation oil bath
It is miscellaneous;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, gel is made being added dropwise while carrying out 100 DEG C of 2h of magnetic agitation oil bath heating
Liquid；
Step 5, carrier 50gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 6, by coagulant liquid aging 24h in atmosphere;
Step 7, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 8 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves.
Reference examples 5 prepare nitric acid molybdenum, nickel nitrate, and ZSM-12 mass ratioes are 1:1:4 sample.Nitric acid molybdenum 10g, nickel nitrate 10g,
40gZSM-12 molecular sieve 10g, tetraethyl orthosilicate 3ml, aluminium isopropoxide 20g, phosphatase 24 ml, tetraethyl ammonium hydroxide 5ml, its from
Sub- water 250ml.
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation
Removal of impurities;
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil
70 DEG C of 2h removal of impurities of bath;
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters are then added dropwise, with per minute 50 drop speed drops
Add, and 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously;
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is connecing
Dropwise addition phosphoric acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating is carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution,
Coagulant liquid is made in 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 6, carrier 40gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere;
Step 8, by coagulant liquid by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
Be put into autoclave 300 DEG C, under 200kpa under neon atmosphere crystallization 12h;
Step 9 and then the lower filtering under vavuum pump, remove moisture, 110 DEG C of vacuum drying chamber under vacuum rotary evaporator
Dry, finally calcine 8h under sufficient air atmosphere in Muffle furnace, obtain Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO- by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in 34/ZSM-12 molecular sieves simultaneously;
Step 11, during above-mentioned solution is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then incite somebody to action anti-
Answer kettle to be put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature is risen to 20 DEG C/min speed
300 DEG C, the crystallization 12h under neon atmosphere;
Step 12 and then the lower filtering under vavuum pump, remove moisture, vacuum drying chamber 110 under vacuum rotary evaporator
DEG C drying, finally calcines 8h under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
Adsorb methanol effect assessment
In 2m3In seal box, the formalin of 0.6ml volumes is measured, is put in surface plate, be placed in seal box 1 meter
Two pallets in place make formaldehyde volatilize naturally, stand 24 hours on one of them, are surveyed with formaldehyde speed and clever measure concentration of formaldehyde.24h
The Mo of the various ratios of preparation, Ni-SAPO-34/ZSM-12 molecular sieve mouth masks are placed in surface plate afterwards, are placed in two among sealing
On another of individual pallet at rice in pallet, Mo, Ni-SAPO-34/ZSM-12 molecular sieves mouth mask is exposed to the air containing formaldehyde
In, concentration of formaldehyde is measured after one week, 0.4ml formaldehyde is then measured and is added at 1m in surface plate.Do altogether 16 it is this
Device is tested together.One of which is that blank group does not have to Mo, Ni-SAPO-34/ZSM-12 molecular sieve mouth masks.
The Mo of the different proportion of table one, Ni-SAPO-34/ZSM-12 molecular sieve mouth mask formaldehyde adsorption compare
| Group | Formaldehyde amount (mg/m before absorption3) | Formaldehyde amount (mg/m after one week3) |
| Embodiment 1 | 2.25 | 0.77 |
| Embodiment 2 | 2.25 | 0.76 |
| Embodiment 3 | 2.25 | 0.71 |
| Embodiment 4 | 2.26 | 0.72 |
| Embodiment 5 | 2.25 | 0.05 |
| Embodiment 6 | 2.24 | 0.71 |
| Embodiment 7 | 2.25 | 0.72 |
| Embodiment 8 | 2.25 | 0.08 |
| Embodiment 9 | 2.23 | 0.76 |
| Embodiment 10 | 2.25 | 0.72 |
| Reference examples 1 | 2.25 | 0.81 |
| Reference examples 2 | 2.25 | 0.83 |
| Reference examples 3 | 2.26 | 0.78 |
| Reference examples 4 | 2.25 | 0.80 |
| Reference examples 5 | 2.25 | 0.86 |
| Blank group | 2.25 | 2.61 |
Test result indicates that Mo prepared by embodiment 5,8, Ni-SAPO-34/ZSM-12 molecular sieve mouth mask formaldehyde adsorption effects
Preferably, illustrate in manganese sulfate, Ludox, sodium aluminate mass ratio 1:1:5, also nitric acid molybdenum adds the nickel nitrate to be with ZM-12 mass ratioes
1:5, wherein nitric acid molybdenum:Nickel nitrate is 1：3 when when they between synergy it is best.It is made under other ratios
Mo, Ni-SAPO-34/ZSM-12 molecular sieves mouth mask also has certain adsorption capacity but effect is bad.Implementation column 5 is contrasted, it is right
As usual 1,2,4,5, it is found that single-element system is either added not under ultrasonic oscillation or only without magnetic agitation
The Mo, Ni-SAPO-34/ZSM-12, Ni-SAPO-34/ZSM-12 obtained, Mo-SAPO-34/ZSM-12 molecular sieves mouth mask absorption first
Aldehyde effect is bad.Implementation column 8 is contrasted with reference examples 3 and can found, Mo, Ni-SAPO-34/ made from crystallization not under neon atmosphere
ZSM-12 molecular sieve mouth mask formaldehyde adsorption effects are bad.
Claims (2)
1. a kind of integral type mouth mask, including mask body, described mask body both sides are provided with fixing band, described mask body
Including interior mouth mask and outer mouth mask, described interior mouth mask and outer mouth mask are integrally formed, and also have filtering between interior mouth mask and outer mouth mask
Space, filter space are equipped with purification of air filtrate, and described purification of air process of preparing filter material is as follows：
Step 1, first by 3ml tetraethyl orthosilicates, 20g aluminium isopropoxides 700 DEG C of oil bath ultrasound 3h under ultrasonic oscillation are removed
It is miscellaneous；
Step 2, by 4ml phosphoric acid, 5ml tetraethyl ammonium hydroxides, 10g nitric acid molybdenums, 10g nickel nitrates are in ultrasonic oscillation oil bath 70
DEG C 2h removal of impurities；
Step 3, aluminium isopropoxide is added drop-wise in flask, 100ml deionized waters is then added dropwise, be added dropwise with per minute 50 drop speed,
And 70 DEG C of 3h of magnetic agitation oil bath heating simultaneously；
Step 4, tetraethyl orthosilicate is added in above-mentioned solution, template tetraethyl ammonium hydroxide then is being added dropwise, is then dripping
Phosphorate acid, is added dropwise with per minute 20 drop speed, 100 DEG C of 2h of magnetic agitation oil bath heating are carried out simultaneously being added dropwise；
Step 5, nickel nitrate is dissolved in 50ml ionized waters, then nickel nitrate solution is added in above-mentioned solution, in magnetic
Coagulant liquid is made in power stirring 100 DEG C of 3h of oil bath heating；
Step 6, carrier 10gZSM-12 is added to 70 DEG C of 3h of magnetic agitation oil bath heating in above-mentioned coagulant liquid；
Step 7, by coagulant liquid aging 24h in atmosphere；
Step 8, during coagulant liquid is poured into the reactor that polytetrafluoroethylene (PTFE) is liner by flow diverter, then reactor is put into
300 DEG C in autoclave, under 200kpa under neon atmosphere crystallization 12h；
Step 9 and then the lower filtering under vavuum pump, remove moisture under vacuum rotary evaporator, and 110 DEG C of vacuum drying chamber is dry
It is dry, 8h finally is calcined under sufficient air atmosphere in Muffle furnace, obtains Ni-SAPO-34/ZSM-12 molecular sieves；
Step 10, nitric acid molybdenum is dissolved in 100ml ionized waters, molybdenum element is impregnated into by Ni-SAPO-34/ by infusion process
100 DEG C of 2h of magnetic agitation oil bath heating are carried out in ZSM-12 molecular sieves simultaneously；
Step 11, by above-mentioned solution by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then by reactor
It is put into microwave reactor and 400kpa is boosted to 25kap/min speed, temperature rises to 300 with 20 DEG C/min speed
DEG C, the crystallization 12h under neon atmosphere；
Step 12 and then the lower filtering under vavuum pump, remove moisture under vacuum rotary evaporator, and 110 DEG C of vacuum drying chamber is dry
It is dry, 8h finally is calcined under sufficient air atmosphere in Muffle furnace, obtains Mo, Ni-SAPO-34/ZSM-12 molecular sieves.
2. a kind of integral type mouth mask according to claim 1, it is characterised in that described interior mouth mask and outer mouth mask are nonwoven
Cloth.
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| CN201610938593.5A CN106343634B (en) | 2016-10-25 | 2016-10-25 | Integral type mouth mask |
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| CN201610938593.5A CN106343634B (en) | 2016-10-25 | 2016-10-25 | Integral type mouth mask |
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| CN106963000B (en) * | 2017-05-02 | 2018-10-23 | 长乐净能新材料科技有限公司 | A kind of combined filtration mask |
| KR102585442B1 (en) | 2017-11-13 | 2023-10-06 | 쓰리엠 이노베이티브 프로퍼티즈 캄파니 | Inner shell and mask including same |
| CN110227413B (en) * | 2019-07-19 | 2021-09-28 | 江苏理工学院 | Anti-haze composite adsorbent and application thereof |
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| US20070297975A1 (en) * | 2006-06-23 | 2007-12-27 | Janssen Marcel J | Metal loading of molecular sieves using organic carriers with limited water content |
| CN101362099B (en) * | 2008-09-19 | 2010-11-10 | 上海化工研究院 | Metal modified molecular screen and preparation method thereof |
| CN202697795U (en) * | 2012-04-09 | 2013-01-30 | 中央民族大学 | Mask with high filtering performance and high air permeability performance |
| CN104473351A (en) * | 2014-12-03 | 2015-04-01 | 常州市畅远无纺布制品有限公司 | Stereo mask |
| CN204653864U (en) * | 2015-05-06 | 2015-09-23 | 胡衍荣 | Respirator structure |
| CN205055245U (en) * | 2015-10-26 | 2016-03-02 | 杨宇坤 | Intelligence gauze mask |
| CN105999854A (en) * | 2016-06-15 | 2016-10-12 | 合肥凯特新能源科技有限公司 | Novel filtering material based on flexible substrate material and application in PM2.5 filtering mask |
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