CN106496630A - A kind of method of efficient light degradation polyester fiber - Google Patents
A kind of method of efficient light degradation polyester fiber Download PDFInfo
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- CN106496630A CN106496630A CN201610966783.8A CN201610966783A CN106496630A CN 106496630 A CN106496630 A CN 106496630A CN 201610966783 A CN201610966783 A CN 201610966783A CN 106496630 A CN106496630 A CN 106496630A
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- catalyst
- acid solution
- polyester fiber
- water
- activator
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 27
- 230000015556 catabolic process Effects 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 title claims abstract description 21
- 229920000728 polyester Polymers 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 43
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000012190 activator Substances 0.000 claims abstract description 17
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 229960000892 attapulgite Drugs 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 14
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000000703 Cerium Chemical class 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 10
- 235000012054 meals Nutrition 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 230000008030 elimination Effects 0.000 claims abstract description 7
- 238000003379 elimination reaction Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 5
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 4
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000015170 shellfish Nutrition 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 238000001782 photodegradation Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000007598 dipping method Methods 0.000 description 8
- 239000002699 waste material Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000007654 immersion Methods 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- MODMKKOKHKJFHJ-UHFFFAOYSA-N magnesium;dioxido(dioxo)molybdenum Chemical compound [Mg+2].[O-][Mo]([O-])(=O)=O MODMKKOKHKJFHJ-UHFFFAOYSA-N 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002144 chemical decomposition reaction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000003471 mutagenic agent Substances 0.000 description 2
- 231100000707 mutagenic chemical Toxicity 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000009933 burial Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of method of efficient light degradation polyester fiber, the method includes：In the presence of light source, polyester fiber, cetyl trimethylammonium bromide, catalyst and water are mixed and carries out degradation reaction；Wherein, the preparation method of the catalyst of catalyst is：1) conch meal and attapulgite are placed in acid solution carries out soaking, filters to take filter cake activator is obtained；2) solubility cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator are placed in closed environment carries out hydro-thermal reaction, crosses elimination filter cake hydrothermal product is obtained；3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then drying, roasting are with prepared catalyst.The characteristics of biodegrading process has high degradation rate, environmental protection and low energy consumption.
Description
Technical field
The present invention relates to high molecular light degradation, in particular it relates to a kind of method of efficient light degradation polyester fiber, belongs to
The preparation and application field of catalyst.
Background technology
Currently, with economic and science and technology fast development, the application of polyester fiber is increasingly extensive, with apparel textile, non-
The polyester fiber waste that the forms such as woven cloths are produced also increases therewith year by year.According to statistics, 2013, the annual textile fabric of China
Consumption is 38,000,000 tons, up to more than 2,350 ten thousand tons of the waste textile of generation.But the main process of waste textile at present
Mode for burial or is burned, and burying not only needs the even years up to a hundred decades thoroughly could degrade, and needs waste big
The soil of amount；And burn and can then cause serious atmospheric pollution, it is necessarily to become therefore to carry out recycling to waste and old polyester fiber
Gesture.
Now, mainly there is two kinds of physiochemical mutagens, chemical recovery to the recovery and reuse technology of waste and old polyester fiber textile,
Physiochemical mutagens will these waste polyester class medicated clothings, through simple processing, make the secondary articles for use such as domestic mop class, this mode pole
The value of fibrous material is reduced greatly；Chemical method includes being chemically modified and chemical degradation, is chemically modified and mainly just changes original
There is ester structure；Chemical degradation is current study hotspot, and in the method, either neutral hydrolysis or both sexes hydrolysis, exists all
Such as efficiency is low, pollute the defect such as big.
Content of the invention
It is an object of the invention to provide a kind of method of efficient light degradation polyester fiber, the biodegrading process has degradation rate
The characteristics of high, environmental protection and low energy consumption.
The method includes：
In the presence of light source, polyester fiber, cetyl trimethylammonium bromide, catalyst and water are mixed and is dropped
Solution reaction；The power of the light source is 300-1000W, and degradation time is 1-5h；Weight ratio is：Polyester fiber：Cetyl three
Methyl bromide ammonium：Catalyst：Water=100：20-40：0.5-2：300-700；
The preparation method of the catalyst is：
1) conch meal and attapulgite are placed in acid solution carries out soaking, filters to take filter cake activator is obtained；Weight ratio
For：Conch meal：Attapulgite：Acid solution=100：42-56：200-300；
2) solubility cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and the activator are placed in closed ring
Hydro-thermal reaction is carried out in border, cross elimination filter cake hydrothermal product is obtained；Weight ratio is：Solubility cerium salt：Tantalic chloride：Oxidation stone
Black alkene：Hydrazine hydrate：Water：Activator=100：30-45：8-10：25-33：300-500：60-85；Reaction temperature is 140-160
DEG C, the response time is 16-20h；
3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then dried, roasting to be being obtained described urging
Agent；It is 30-40 weights that the molybdic acid saline solution is the concentration of molybdate in 150-200 weight portions, and molybdic acid saline solution
Amount %；Dipping temperature is 70-85 DEG C, and dip time is 5-7h；Drying temperature is 100-120 DEG C, and drying time is 2-3h；Roasting
Temperature is 380-420 DEG C, and roasting time is 60-80min.
The light source is visible light source or infrared light sources.
The preparation method step 1 of the catalyst) in acid solution be selected from phosphoric acid solution, hydrochloric acid solution or sulfuric acid solution, pH is
5-6.5；
The preparation method step 2 of the catalyst) solubility cerium salt in cerous chloride, cerous nitrate and cerous sulfate one
Plant or multiple.
Beneficial effect
By above-mentioned technical proposal, the catalyst that the present invention is provided is caused by the synergism of each raw material and each step
Obtained catalyst has excellent catalytic efficiency for the light degradation of polyester fiber；Meanwhile, the biodegrading process has degradation rate
The characteristics of high, environmental protection and low energy consumption.
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides the invention provides a kind of method of efficient light degradation polyester fiber, the method includes：In light
In the presence of source, polyester fiber, cetyl trimethylammonium bromide, catalyst and water are mixed and carries out degradation reaction；Wherein,
The preparation method of the catalyst of catalyst is：1) conch meal and attapulgite are placed in acid solution carries out soaking, filters to take filter cake
So that activator is obtained；2) solubility cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator are placed in closed ring
Hydro-thermal reaction is carried out in border, cross elimination filter cake hydrothermal product is obtained；3) hydrothermal product is placed in molybdic acid saline solution is carried out
Dipping, then drying, roasting are with prepared catalyst.
In above-mentioned light degradation method, the consumption of each material can be selected in wide scope, but in order to further carry
High photodegradation rate, it is preferable that relative to the polyester fiber of 100 weight portions, the consumption of cetyl trimethylammonium bromide is 20-40
Weight portion, the consumption of catalyst is 0.5-2 weight portions, and the consumption of water is 300-700 weight portions.
In above-mentioned light degradation method, the actual conditions of degradation reaction can be selected in wide scope, but in order to enter
One step improves photodegradation rate, it is preferable that degradation reaction at least meets following condition：The power of light source is 300-1000W, during degraded
Between be 1-5h.
In above-mentioned light degradation method, the concrete species of light source can be selected in wide scope, but in order to further carry
High photodegradation rate and consider energy consumption and environmental protection, it is preferable that light source is visible light source or infrared light sources.
Above-mentioned steps 1) in, the consumption of each material can be selected in wide scope, but in order to further improve light
Degradation rate, it is preferable that in step 1) in, relative to the conch meal of 100 weight portions, the consumption of attapulgite is 42-56 weight portions,
The consumption of acid solution is 200-300 weight portions.
Meanwhile, above-mentioned steps 1) in, the pH of acid solution can be selected in wide scope, but in order to further improve light
Degradation rate, it is preferable that the pH of acid solution is 5-6.5.
In the present invention, the concrete species of acid solution can be selected in the wide scope, but from the effect of acidifying and into
Consider in sheet, it is preferable that acid solution is selected from phosphoric acid solution, hydrochloric acid solution or sulfuric acid solution.
Additionally, the step 1 in the present invention) in, the actual conditions of immersion can be selected in wide scope, but in order to enter
One step improves photodegradation rate, it is preferable that in step 1) in, immersion at least meets following condition：Soaking temperature is 45-60 DEG C, leaching
The bubble time is 40-60min.
The step of the preparation method of above-mentioned catalyst 2) in, the consumption of each material can be selected in wide scope, but
It is to further improve photodegradation rate, it is preferable that in step 2) in, relative to the solubility cerium salt of 100 weight portions, phosphoric
The consumption of tantalum is 30-45 weight portions, and the consumption of graphene oxide is 8-10 weight portions, and the consumption of hydrazine hydrate is 25-33 weight portions,
The consumption of water is 300-500 weight portions, and the consumption of activator is 60-85 weight portions.
The step of preparation method of above-mentioned catalyst 2) in, the concrete species of solubility cerium salt can be selected in wide scope
Select, but in order to further improve photodegradation rate, it is preferable that solubility cerium salt is in cerous chloride, cerous nitrate and cerous sulfate
One or more.
The step of preparation method of above-mentioned catalyst 2) in, the actual conditions of hydro-thermal reaction can be selected in wide scope
Select, but in order to further improve photodegradation rate, it is preferable that in step 2) in, hydro-thermal reaction at least meets following condition：Reaction
Temperature is 140-160 DEG C, and the response time is 16-20h.
The step of preparation method of above-mentioned catalyst 3) in, the consumption of each material can be selected in wide scope, but
In order to further improve photodegradation rate, it is preferable that in step 3) in, in step 3) in, the hydro-thermal relative to 100 weight portions is produced
Thing, the consumption of molybdic acid saline solution is 30-40 weights for the concentration of molybdate in 150-200 weight portions, and molybdic acid saline solution
Amount %；
The step of preparation method of above-mentioned catalyst 3) in, the species of molybdic acid saline solution can be selected in wide scope
Select, but in order to further improve photodegradation rate, it is preferable that molybdic acid saline solution is water-soluble selected from molybdic acid aqueous solutions of potassium, sodium molybdate
One or more in liquid, molybdic acid beryllium aqueous solution and magnesium molybdate aqueous solution.
The step of preparation method of above-mentioned catalyst 3) in, the actual conditions of dipping can be selected in wide scope, but
It is to further improve photodegradation rate, it is preferable that in step 3) in, dipping at least meets following condition：Dipping temperature is 70-
85 DEG C, dip time is 5-7h.
The step of preparation method of above-mentioned catalyst 3) in, the actual conditions of drying can be selected in wide scope, but
It is to further improve photodegradation rate, it is preferable that dry and at least meet following condition：Drying temperature is 100-120 DEG C, dries
Time is 2-3h.
The step of preparation method of above-mentioned catalyst 3) in, the actual conditions of roasting can be selected in wide scope, but
It is to further improve photodegradation rate, it is preferable that roasting at least meets following condition：Sintering temperature is 380-420 DEG C, roasting
Time is 60-80min.
Hereinafter will be described the present invention by preparation example.
Preparation example 1
1) at 50 DEG C, conch meal and attapulgite are placed in the hydrochloric acid solution that pH is 5.5 carries out immersion 50min (shellfishes
Shell powder, attapulgite, the weight ratio of acid solution are 100：48：250), filter to take filter cake activator is obtained；
2) by cerous nitrate, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100：35：9：29：400：
75 weight carries out hydro-thermal reaction 18h, crosses elimination filter cake water is obtained than mixing in the closed environment for being then placed in 150 DEG C
Hot；
3) at 78 DEG C, hydrothermal product is placed in sodium molybdate aqueous solution (hydrothermal product and the molybdic acid that concentration is 35 weight %
The weight ratio of saline solution is 100：180) dipping 6h is carried out in；Then 2.5h, in 400 DEG C at roasting are dried at 110 DEG C
70min is with prepared catalyst A1.
Preparation example 2
1) at 45 DEG C, conch meal and attapulgite are placed in the phosphoric acid solution that pH is 5 carries out immersion 40min (shells
Powder, attapulgite, the weight ratio of acid solution are 100：42：200), filter to take filter cake activator is obtained；
2) by cerous chloride, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100：30：8：25：
300：60 weight carries out hydro-thermal reaction 16h, crosses elimination filter cake to make than mixing in the closed environment for being then placed in 140 DEG C
Obtain hydrothermal product；
3) at 70 DEG C, hydrothermal product is placed in magnesium molybdate aqueous solution (hydrothermal product and the molybdic acid that concentration is 30 weight %
The weight ratio of saline solution is 100：150) dipping 5h is carried out in；Then at 100 DEG C dry 2h, at 380 DEG C roasting 60min
So that catalyst A2 is obtained.
Preparation example 3
1) at 60 DEG C, conch meal and attapulgite are placed in the sulfuric acid solution that pH is 6.5 carries out immersion 60min (shellfishes
Shell powder, attapulgite, the weight ratio of acid solution are 100：56：300), filter to take filter cake activator is obtained；
2) by cerous sulfate, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100：45：10：33：500：
85 weight carries out hydro-thermal reaction 20h, crosses elimination filter cake water is obtained than mixing in the closed environment for being then placed in 160 DEG C
Hot；
3) at 85 DEG C, hydrothermal product is placed in magnesium molybdate aqueous solution (hydrothermal product and the molybdic acid that concentration is 40 weight %
The weight ratio of saline solution is 100：200) dipping 7h is carried out in；Then at 120 DEG C dry 3h, at 420 DEG C roasting 80min
So that catalyst A3 is obtained.
Comparative example 1
Method according to preparation example 1 is obtained catalyst B1, except that, step 1) in conch meal is not used.
Comparative example 2
Method according to preparation example 1 is obtained catalyst B2, except that, step 1) in attapulgite is not used.
Comparative example 3
Method according to preparation example 1 is obtained catalyst B3, except that, step 2) in graphene oxide and water is not used
Close hydrazine (graphene oxide can be reduced into Graphene by hydrazine hydrate).
Comparative example 4
Method according to preparation example 1 is obtained catalyst B4, except that, step 2) in cerous nitrate is not used.
Comparative example 5
Method according to preparation example 1 is obtained catalyst B5, except that, step 2) in tantalic chloride is not used.
Comparative example 6
Method according to preparation example 1 is obtained catalyst B6, except that, do not carry out step 6).
Comparative example 7
Method according to preparation example 1 is obtained catalyst B7, except that, step 6) in without calcining process.
Embodiment 1
Visible ray or ultrared in the presence of, by polyester fiber, cetyl trimethylammonium bromide, above-mentioned catalyst
Then catabolite is filtered, then by mass fraction be than light degradation being carried out after mixing according to certain weight with water
Final solid is finally carried out calculating degradation rate of weighing by the solid that 10% sodium hydroxide solution washing and filtering is obtained, wherein,Specific degraded knot
Fruit and degradation condition are shown in Table 1.
Table 1
By above-mentioned preparation example, comparative example and embodiment, the catalyst that the present invention is provided is for the light of polyester fiber
Degraded has excellent catalytic performance.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, multiple simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy is no longer separately illustrated.
Additionally, combination in any can also be carried out between a variety of embodiments of the present invention, as long as which is without prejudice to this
The thought of invention, its should equally be considered as content disclosed in this invention.
Claims (4)
1. a kind of method of efficient light degradation polyester fiber, it is characterised in that the method includes：In the presence of light source, will be poly-
Ester fiber, cetyl trimethylammonium bromide, catalyst and water mix and carry out degradation reaction；The power of the light source is 300-
1000W, degradation time are 1-5h；Weight ratio is：Polyester fiber：Cetyl trimethylammonium bromide：Catalyst：Water=100：
20-40：0.5-2：300-700；
The preparation method of the catalyst is：
1) conch meal and attapulgite are placed in acid solution carries out soaking, filters to take filter cake activator is obtained；Weight ratio is：Shellfish
Shell powder：Attapulgite：Acid solution=100：42-56：200-300；
2) solubility cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and the activator are placed in closed environment
Carry out hydro-thermal reaction, cross elimination filter cake hydrothermal product is obtained；Weight ratio is：Solubility cerium salt：Tantalic chloride：Graphite oxide
Alkene：Hydrazine hydrate：Water：Activator=100：30-45：8-10：25-33：300-500：60-85；Reaction temperature is 140-160 DEG C,
Response time is 16-20h；
3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then drying, roasting are with the prepared catalyst；
It is 30-40 weight % that the molybdic acid saline solution is the concentration of molybdate in 150-200 weight portions, and molybdic acid saline solution；Leaching
Stain temperature is 70-85 DEG C, and dip time is 5-7h；Drying temperature is 100-120 DEG C, and drying time is 2-3h；Sintering temperature is
380-420 DEG C, roasting time is 60-80min.
2. the method for claim 1, it is characterised in that the light source is visible light source or infrared light sources.
3. the method for claim 1, it is characterised in that the preparation method step 1 of the catalyst) in acid solution be selected from phosphorus
Acid solution, hydrochloric acid solution or sulfuric acid solution, pH are 5-6.5.
4. the method for claim 1, it is characterised in that the preparation method step 2 of the catalyst) solubility cerium
One or more in cerous chloride, cerous nitrate and cerous sulfate of salt.
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| WO2023020293A1 (en) * | 2021-08-16 | 2023-02-23 | 苏州大学 | Method for photothermal degradation of polyester |
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