CN106496630B - 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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- CN106496630B CN106496630B CN201610966783.8A CN201610966783A CN106496630B CN 106496630 B CN106496630 B CN 106496630B CN 201610966783 A CN201610966783 A CN 201610966783A CN 106496630 B CN106496630 B CN 106496630B
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- 238000006731 degradation reaction Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000015556 catabolic process Effects 0.000 title claims abstract description 25
- 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
- 150000000703 Cerium Chemical class 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
- 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
- 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
- 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
- 238000001035 drying Methods 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
- 238000001354 calcination Methods 0.000 claims description 3
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-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
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 25
- 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
- 239000000463 material Substances 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
- 238000005516 engineering process 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
- 239000003795 chemical substances by application Substances 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
- 230000007613 environmental effect 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
- 230000020477 pH reduction Effects 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
- 238000002791 soaking Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002195 synergetic effect Effects 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
- 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
-
- B01J35/39—
-
- 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
Abstract
The invention discloses a kind of methods of efficient light degradation polyester fiber, this method comprises: mixing polyester fiber, cetyl trimethylammonium bromide, catalyst and water in the presence of light source and carrying out degradation reaction；Wherein, the catalyst of catalyst the preparation method comprises the following steps: 1) conch meal and attapulgite are placed in acid solution are impregnated, filters to take filter cake so that activator is made；2) soluble cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator are placed in closed environment and carry out hydro-thermal reaction, filter off filter cake so that hydrothermal product is made；3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then dried, roast so that catalyst is made.The biodegrading process has the characteristics that degradation rate is high, environmentally protective and low energy consumption.
Description
Technical field
The present invention relates to high molecular light degradation, and in particular, to a kind of method of efficient light degradation polyester fiber belongs to
The preparation and application field of catalyst.
Background technique
Currently, with economic and science and technology fast development, polyester fiber using increasingly extensive, with apparel textile, non-
The polyester fiber waste that the forms such as woven cloths generate also increases year by year therewith.According to statistics, 2013, the annual textile fabric of China
Consumption is 38,000,000 tons, and the waste textile of generation is up to more than 2,350 ten thousand tons.However the main processing of waste textile at present
Mode is to bury or burn, and burial not only needs the even years up to a hundred decades that could thoroughly degrade, but also needs to waste big
The soil of amount；And it will cause serious atmosphere pollution for burning, therefore being recycled to waste and old polyester fiber is necessarily to become
Gesture.
Now, mainly there are two kinds of physiochemical mutagens, chemical recovery to the recovery and reuse technology of waste and old polyester fiber textile,
Physiochemical mutagens are simply processed i.e. by these waste polyester class clothings, are made into the secondary articles such as household mop class, this mode pole
The value of fibrous material is reduced greatly；Chemical method includes being chemically modified and chemical degradation, be chemically modified mainly change it is former just
There is ester structure；Chemical degradation is current research hotspot, and either neutral hydrolysis or both sexes hydrolysis in the method, there is all
Such as low efficiency pollutes the defects of big.
Summary of the invention
The object of the present invention is to provide a kind of method of efficient light degradation polyester fiber, which has degradation rate
It is high, environmentally protective and the characteristics of low energy consumption.
This method comprises:
In the presence of light source, polyester fiber, cetyl trimethylammonium bromide, catalyst and water are mixed and dropped
Solution reaction；The power of the light source is 300-1000W, degradation time 1-5h；Weight ratio are as follows: polyester fiber: cetyl three
Methyl bromide ammonium: catalyst: water=100:20-40:0.5-2:300-700；
The catalyst the preparation method comprises the following steps:
1) conch meal and attapulgite are placed in acid solution and are impregnated, filters to take filter cake so that activator is made；Weight ratio
Are as follows: conch meal: attapulgite: acid solution=100:42-56:200-300；
2) soluble 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, filters to take filter cake so that hydrothermal product is made；Weight ratio are as follows: soluble 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, reaction time 16-20h；
3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then dried, roast to be made described and urge
Agent；The molybdic acid saline solution is 150-200 parts by weight, and the concentration of molybdate is 30-40 weight in molybdic acid saline solution
Measure %；Dipping temperature is 70-85 DEG C, dip time 5-7h；Drying temperature is 100-120 DEG C, drying time 2-3h；Roasting
Temperature is 380-420 DEG C, calcining time 60-80min.
The light source is visible light source or infrared light sources.
Acid solution is selected from phosphoric acid solution, hydrochloric acid solution or sulfuric acid solution in the preparation method step 1) of the catalyst, and pH is
5-6.5；
The soluble cerium salt of the preparation method step 2) of the catalyst in cerous chloride, cerous nitrate and cerous sulfate one
Kind is a variety of.
Beneficial effect
Through the above technical solutions, catalyst provided by the invention by the synergistic effect of each raw material and each step so that
Catalyst obtained has excellent catalytic efficiency for the light degradation of polyester fiber；Meanwhile the biodegrading process has degradation rate
It is high, environmentally protective and the characteristics of low energy consumption.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides the present invention provides a kind of methods of efficient light degradation polyester fiber, this method comprises: in light
In the presence of source, polyester fiber, cetyl trimethylammonium bromide, catalyst and water are mixed and carry out degradation reaction；Wherein,
The catalyst of catalyst is impregnated the preparation method comprises the following steps: 1) conch meal and attapulgite are placed in acid solution, filters to take filter cake
Activator is made；2) soluble cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator are placed in closed ring
Hydro-thermal reaction is carried out in border, filters to take filter cake so that hydrothermal product is made；3) hydrothermal product is placed in molybdic acid saline solution and is carried out
Dipping is then dried, is roasted so that catalyst is made.
In above-mentioned light degradation method, the dosage of each material can select in a wide range, but in order to further mention
High photodegradation rate, it is preferable that relative to the polyester fiber of 100 parts by weight, the dosage of cetyl trimethylammonium bromide is 20-40
Parts by weight, the dosage of catalyst are 0.5-2 parts by weight, and the dosage of water is 300-700 parts by weight.
In above-mentioned light degradation method, the actual conditions of degradation reaction can select in a wide range, but in order into
One step improves photodegradation rate, it is preferable that degradation reaction at least meets the following conditions: the power of light source is 300-1000W, when degradation
Between be 1-5h.
In above-mentioned light degradation method, the specific type of light source can select in a wide range, but in order to further mention
High photodegradation rate and consider energy consumption and environmental protection, it is preferable that light source be visible light source or infrared light sources.
In above-mentioned steps 1) in, the dosage of each material can select in a wide range, but in order to further increase light
Degradation rate, it is preferable that in step 1), relative to the conch meal of 100 parts by weight, the dosage of attapulgite is 42-56 parts by weight,
The dosage of acid solution is 200-300 parts by weight.
Meanwhile in above-mentioned steps 1) in, the pH of acid solution can be selected in a wide range, but in order to further increase light
Degradation rate, it is preferable that the pH of acid solution is 5-6.5.
In the present invention, the specific type of acid solution can select in a wide range, but from the effect of acidification and at
Consider on this, it is preferable that acid solution is selected from phosphoric acid solution, hydrochloric acid solution or sulfuric acid solution.
In addition, the actual conditions of immersion can select in a wide range in step 1) of the invention, but in order into
One step improves photodegradation rate, it is preferable that in step 1), immersion at least meets the following conditions: soaking temperature is 45-60 DEG C, leaching
The bubble time is 40-60min.
In the step 2) of the preparation method of above-mentioned catalyst, the dosage of each material can select in a wide range, but
It is to further increase photodegradation rate, it is preferable that phosphoric relative to the soluble cerium salt of 100 parts by weight in step 2)
The dosage of tantalum is 30-45 parts by weight, and the dosage of graphene oxide is 8-10 parts by weight, and the dosage of hydrazine hydrate is 25-33 parts by weight,
The dosage of water is 300-500 parts by weight, and the dosage of activator is 60-85 parts by weight.
In the step 2) of the preparation method of above-mentioned catalyst, the specific type of soluble cerium salt can be selected in a wide range
It selects, but in order to further increase photodegradation rate, it is preferable that soluble cerium salt is in cerous chloride, cerous nitrate and cerous sulfate
It is one or more.
In the step 2) of the preparation method of above-mentioned catalyst, the actual conditions of hydro-thermal reaction can select in a wide range
It selects, but in order to further increase photodegradation rate, it is preferable that in step 2), hydro-thermal reaction at least meets the following conditions: reaction
Temperature is 140-160 DEG C, reaction time 16-20h.
In the step 3) of the preparation method of above-mentioned catalyst, the dosage of each material can select in a wide range, still
In order to further increase photodegradation rate, it is preferable that in step 3), in step 3), the hydro-thermal relative to 100 parts by weight is produced
Object, the dosage of molybdic acid saline solution are 150-200 parts by weight, and the concentration of molybdate is 30-40 weight in molybdic acid saline solution
Measure %；
In the step 3) of the preparation method of above-mentioned catalyst, the type of molybdic acid saline solution can be selected in a wide range
It selects, but in order to further increase photodegradation rate, it is preferable that it is water-soluble that molybdic acid saline solution is selected from molybdic acid aqueous solutions of potassium, sodium molybdate
One of liquid, molybdic acid beryllium aqueous solution and magnesium molybdate aqueous solution are a variety of.
In the step 3) of the preparation method of above-mentioned catalyst, the actual conditions of dipping can select in a wide range, but
It is to further increase photodegradation rate, it is preferable that in step 3), dipping at least meets the following conditions: dipping temperature 70-
85 DEG C, dip time 5-7h.
In the step 3) of the preparation method of above-mentioned catalyst, the actual conditions of drying can select in a wide range, but
Be to further increase photodegradation rate, it is preferable that drying at least meets the following conditions: drying temperature is 100-120 DEG C, drying
Time is 2-3h.
In the step 3) of the preparation method of above-mentioned catalyst, the actual conditions of roasting can select in a wide range, but
Be to further increase photodegradation rate, it is preferable that roasting at least meets the following conditions: maturing temperature is 380-420 DEG C, roasting
Time is 60-80min.
It below will the present invention will be described in detail by preparation example.
Preparation example 1
1) at 50 DEG C, conch meal and attapulgite is placed in the hydrochloric acid solution that pH is 5.5 and carry out immersion 50min (shellfish
Shell powder, attapulgite, acid solution weight ratio be 100:48:250), filter to take filter cake be made activator；
2) by cerous nitrate, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100:35:9:29:400:
75 weight ratio mixing is then placed in 150 DEG C of closed environment and carries out hydro-thermal reaction 18h, filters to take filter cake so that water is made
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 be 100:180) in carry out dipping 6h；Then 2.5h is dried at 110 DEG C, is roasted at 400 DEG C
70min is to be made catalyst A1.
Preparation example 2
1) at 45 DEG C, conch meal and attapulgite is placed in the phosphoric acid solution that pH is 5 and carry out immersion 40min (shell
Powder, attapulgite, acid solution weight ratio be 100:42:200), filter to take filter cake be made activator；
2) by cerous chloride, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100:30:8:25:
The weight ratio of 300:60 mixes, and is then placed in 140 DEG C of closed environment and carries out hydro-thermal reaction 16h, filters to take filter cake to make
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 be 100:150) in carry out dipping 5h；Then 2h is dried at 100 DEG C, roasts 60min at 380 DEG C
Catalyst A2 is made.
Preparation example 3
1) at 60 DEG C, conch meal and attapulgite is placed in the sulfuric acid solution that pH is 6.5 and carry out immersion 60min (shellfish
Shell powder, attapulgite, acid solution weight ratio be 100:56:300), filter to take filter cake be made activator；
2) by cerous sulfate, tantalic chloride, graphene oxide, hydrazine hydrate, water and activator according to 100:45:10:33:500:
85 weight ratio mixing is then placed in 160 DEG C of closed environment and carries out hydro-thermal reaction 20h, filters to take filter cake so that water is made
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 be 100:200) in carry out dipping 7h；Then 3h is dried at 120 DEG C, roasts 80min at 420 DEG C
Catalyst A3 is made.
Comparative example 1
Catalyst B1 is made according to the method for preparation example 1, the difference is that conch meal is not used in step 1).
Comparative example 2
Catalyst B2 is made according to the method for preparation example 1, the difference is that attapulgite is not used in step 1).
Comparative example 3
Catalyst B3 is made according to the method for preparation example 1, the difference is that graphene oxide and water are not used in step 2)
It closes hydrazine (graphene oxide can be reduced into graphene by hydrazine hydrate).
Comparative example 4
Catalyst B4 is made according to the method for preparation example 1, the difference is that cerous nitrate is not used in step 2).
Comparative example 5
Catalyst B5 is made according to the method for preparation example 1, the difference is that tantalic chloride is not used in step 2).
Comparative example 6
Catalyst B6 is made according to the method for preparation example 1, the difference is that not carrying out step 3).
Comparative example 7
Catalyst B7 is made according to the method for preparation example 1, the difference is that without calcining process in step 3).
Embodiment 1
In the presence of visible light or infrared ray, by polyester fiber, cetyl trimethylammonium bromide, above-mentioned catalyst
With water according to light degradation is carried out after certain weight ratio mixing, then catabolite is filtered, is then by mass fraction
10% sodium hydroxide solution washs the solid being obtained by filtration, and final solid is finally carried out weighing and calculates degradation rate, whereinSpecific degradation knot
Fruit and degradation condition are shown in Table 1.
Table 1
By above-mentioned preparation example, comparative example and embodiment it is found that catalyst provided by the invention for polyester fiber light
Degradation has excellent catalytic properties.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (4)
1. a kind of method of efficient light degradation polyester fiber, which is characterized in that this method comprises: will gather in the presence of light source
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 1-5h；Weight ratio are as follows: polyester fiber: cetyl trimethylammonium bromide: catalyst: water=100:
20-40:0.5-2:300-700；
The catalyst the preparation method comprises the following steps:
1) conch meal and attapulgite are placed in acid solution and are impregnated, filters to take filter cake so that activator is made；Weight ratio are as follows: shellfish
Shell powder: attapulgite: acid solution=100:42-56:200-300；
2) soluble cerium salt, tantalic chloride, graphene oxide, hydrazine hydrate, water and the activator are placed in closed environment
It carries out hydro-thermal reaction, filter to take filter cake so that hydrothermal product is made；Weight ratio are as follows: soluble 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,
Reaction time is 16-20h；
3) hydrothermal product is placed in molybdic acid saline solution and is impregnated, then dried, roast so that the catalyst is made；
The molybdic acid saline solution is 150-200 parts by weight, and the concentration of molybdate is 30-40 weight % in molybdic acid saline solution；Leaching
Stain temperature is 70-85 DEG C, dip time 5-7h；Drying temperature is 100-120 DEG C, drying time 2-3h；Maturing temperature is
380-420 DEG C, calcining time 60-80min.
2. the method as described in claim 1, which is characterized in that the light source is visible light source or infrared light sources.
3. the method as described in claim 1, which is characterized in that acid solution is selected from phosphorus in the preparation method step 1) of the catalyst
Acid solution, hydrochloric acid solution or sulfuric acid solution, pH 5-6.5.
4. the method as described in claim 1, which is characterized in that the soluble cerium salt choosing of the preparation method step 2) of the catalyst
From one of cerous chloride, cerous nitrate and cerous sulfate or a variety of.
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| CN103289122A (en) * | 2012-03-02 | 2013-09-11 | 江南大学 | Production method for depolymerizing waste polyester fibers through utilizing ethylene glycol method |
| CN102631913A (en) * | 2012-03-29 | 2012-08-15 | 吉林大学 | Preparation method of graphene supported cerium oxide nano cubit compound |
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