CN103936382B - A kind of semi-hydrated gypsum and application with photocatalytic activity - Google Patents
A kind of semi-hydrated gypsum and application with photocatalytic activity Download PDFInfo
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- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 125
- 239000010440 gypsum Substances 0.000 title claims abstract description 125
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 111
- 229910052742 iron Inorganic materials 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910001868 water Inorganic materials 0.000 claims abstract description 44
- 238000007146 photocatalysis Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 29
- 238000012423 maintenance Methods 0.000 claims description 28
- 238000001354 calcination Methods 0.000 claims description 18
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 16
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 16
- 238000005056 compaction Methods 0.000 claims description 14
- -1 polyoxyethylene Polymers 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000011268 mixed slurry Substances 0.000 claims description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical group CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 10
- 229920001661 Chitosan Polymers 0.000 claims description 9
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 8
- HVAMZGADVCBITI-UHFFFAOYSA-M pent-4-enoate Chemical compound [O-]C(=O)CCC=C HVAMZGADVCBITI-UHFFFAOYSA-M 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000011028 pyrite Substances 0.000 claims description 8
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 8
- 229910052683 pyrite Inorganic materials 0.000 claims description 8
- 229920002101 Chitin Polymers 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000004408 titanium dioxide Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 40
- 238000010298 pulverizing process Methods 0.000 description 20
- 238000012360 testing method Methods 0.000 description 20
- 230000015556 catabolic process Effects 0.000 description 19
- 238000006731 degradation reaction Methods 0.000 description 19
- 230000006835 compression Effects 0.000 description 15
- 238000007906 compression Methods 0.000 description 15
- 239000000203 mixture Substances 0.000 description 13
- 206010013786 Dry skin Diseases 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- 238000000227 grinding Methods 0.000 description 10
- 238000009775 high-speed stirring Methods 0.000 description 10
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 10
- 229910052753 mercury Inorganic materials 0.000 description 10
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 238000003556 assay Methods 0.000 description 5
- 239000004568 cement Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002826 coolant Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011505 plaster Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229960001860 salicylate Drugs 0.000 description 3
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000011507 gypsum plaster Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910021646 siderite Inorganic materials 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
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- Catalysts (AREA)
- Building Environments (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to a kind of gypsum product and the application thereof with photocatalysis performance, utilize titanium powder plant sulfuric acid process output titanium white gypsum as raw material, titanium white gypsum is converted into semi-hydrated gypsum, increases its intensity; By adding water-resisting agent, retardant and whipping agent, obtained qualified building block or the sheet material with water resistance, adds whipping agent and obtains insulating layer of external wall.Utilize the catalyzed oxidation ability of titanium dioxide in titanium white gypsum and ferric oxide, after adding virgin iron ore, strengthen its catalytic activity, can to degrade under sunlight or visible ray toxic organic pollutant for buildings material.
Description
Technical field
The present invention relates to a kind of semi-hydrated gypsum product and application thereof, particularly there is the semi-hydrated gypsum of photocatalytic activity, can to degrade under sunlight or visible ray toxic organic pollutant for buildings material.
Background technology
Gypsum raw material is divided into the plaster of paris and chemical gypsum.Plaster of paris main component is CaSO
42H
2o, is also called plaster stone, through calcining, levigately obtains semi-hydrated gypsum (CaSO
41/2H
2o).It is a kind of air hardening cementitious materials, and have α and β two kinds of forms, all assume diamond in shape crystallization, but physicals is different.Alpha semi-hydrated gypsum well-crystallized, solid; Beta-type semi-hydrated gypsum is sheet and has the crystal of crackle, and crystallization is very thin, and specific surface area is more much bigger than alpha semi-hydrated gypsum.Chemical gypsum can be divided into phosphogypsum, desulfurated plaster, titanium white gypsum and fluorgypsum etc. according to the difference of composition.Titanium white gypsum be adopt Titanium White Production By Sulfuric Acid Process time, be administer acid waste water, add the waste residue that lime (or carbide slag) produces to neutralize a large amount of acid waste water, its moisture many (45-60%) and contain Fe
2o
3, TiO
2, Al
2o
3, MgO, Cr
2o
3, Na
2o and SiO
2deng impurity.In humid conditions, Fe (OH) wherein
3precipitation exists with the form of colloid, and therefore titanium gypsum has viscosity greatly, is placed in air and easily becomes the features such as redness.
End 2010, China's titanium white powder production capacity, more than 2,000,000 t, becomes the country that global titanium dioxide production capacity is maximum.Often produce 1t titanium dioxide and just produce 5 ~ 6t gypsum tailings, China about produces 1,000 ten thousand t titanium white gypsum every year.Titanium white gypsum is the chemical industry by-product gypsum that utilization ratio is minimum, and only have on a small quantity for the preparation of composite cementitious materials, admixture as cement, gypsum block and plasterboard, a large amount of titanium white gypsum is not used effectively.Because titanium white gypsum resource utilising efficiency is low, adopt concentrates stacking more, not only takies a large amount of soil, contaminate environment, the destruction eubiosis, and causes huge economical load to titanium dioxide enterprise.Therefore explore one without new waste, to produce without new pollution and by producing the waste ' s reclamation of titanium dioxide, to make the key subjects being full of ski-jump flow undoubtedly.Ultraviolet radiation in sunlight is lower, only account for the 4-5% of total solar radiation, if by the semiconductor catalyst modification of ultraviolet excitation, make the extended spectral response of catalyzer to visible ray, thus realize degraded titanium white gypsum and virgin iron ore being applied to organic pollutant in air under solar light irradiation, there is great economic implications and social benefit.
Summary of the invention
The object of the present invention is to provide a kind of semi-hydrated gypsum goods and the application thereof with photocatalysis performance, this plastering can degradable organic pollutant under sunlight or visible ray.
A kind of semi-hydrated gypsum with photocatalytic activity, based on titanium white gypsum, raw material obtains semi-hydrated gypsum, then adds iron ore in semi-hydrated gypsum, water-resisting agent, retardant, the obtained semi-hydrated gypsum with photocatalysis performance after whipping agent, by weight, 100 parts, titanium white gypsum, iron ore 4-25 part, water-resisting agent 0.6-5.8 part, retardant 0.5-2.8 part, whipping agent 0.1-1.3 part.
The solid waste that described titanium white gypsum produces for Titanium White Production By Sulfuric Acid Process, its composition comprises calcium sulfate, water, iron ion, titanium ion, aluminum ion, magnesium ion and silicon-dioxide; Described virgin iron ore is magnetite, rhombohedral iron ore, pyrite, limonite, one or more in spathic iron ore; Described water-resisting agent is butyl acrylate and/or allyl acetate; Described retardant be in chitin, chitosan, glucose one or more; Described whipping agent is alkylphenol-polyethenoxy.
There is a preparation method for the semi-hydrated gypsum of photocatalytic activity, comprise the following steps:
(1) by titanium white gypsum calcination 1-2h at 300-700 DEG C, pulverize after cooling, vibration screening to granularity is 5-100 micron, is placed in autoclave, passes into saturation steam by this titanium white gypsum particle, under the vapour pressure of 110-135 DEG C and 1.2-3.5 KPa, insulation 1-5h, ball milling after cooling, dry 1-2h at 130-135 DEG C, ball milling vibration screening to granularity is 0.5-50 micron again, and obtained semi-hydrated gypsum is stand-by;
(2) by magnetite, rhombohedral iron ore, pyrite, limonite, one or more mixed ores in spathic iron ore pulverize and sieve calcines 1-3 h after granularity is 5-100 micron at 300-600 DEG C, and being milled to iron ore particle degree after cooling is 5-20 micron, and obtained iron ore is stand-by;
(3) water-resisting agent is added water mixing after, drip Sodium dodecylbenzene sulfonate, and be warming up to 75-85 DEG C after stirring 40 min with the speed of 120-200r/min, be incubated 1 h, be down to room temperature and regulate pH to 7.5, filter, obtained water-resisting agent filtrate is stand-by, and wherein the weight ratio of water-resisting agent, water, Sodium dodecylbenzene sulfonate is 10:80:0.1 ~ 1;
(4) water-resisting agent in the iron ore in step (2), step (3), retardant are added to the water, 40 ~ 60min is stirred with the speed of 80 ~ 100r/min, obtained mixed slurry, wherein the weight ratio of iron ore, water-resisting agent, retardant, water is 4-25:0.6-5.8:0.5-2.8:50-70;
(5) add the mixed slurry in step (4) toward semi-hydrated gypsum, be poured in mould after stirring 2-5 min, vibratory compaction, is placed in climatic chamber, at 25 ± 3 DEG C through maintenance 2-3 days, and maintenance after the demoulding, obtained plastering;
(6) or in the mixed slurry of step (4) add whipping agent alkylphenol polyoxyethylene, stir, wherein mixed slurry is 100:0.1-1.0 with the weight ratio of alkylphenol polyoxyethylene;
(7) in semi-hydrated gypsum, add the mixed slurry in step (6), stir 2-5min after-pouring in mould, vibratory compaction, is placed in climatic chamber, at 25 ± 3 DEG C of maintenance 2-3 days, and maintenance after the demoulding, obtained plastering.
Adopt technical scheme of the present invention, have the following advantages:
1. the present invention is by titanium dioxide residual in modification titanium white gypsum and ferric oxide, makes it have catalytic performance, and improves catalytic performance by additional iron ore, toxic pollutant in catalyzed degradation air under sunlight or visible ray.
2. the present invention is by adding water-resisting agent and whipping agent, not only can improve waterproof effect, and with other material of construction, the building block quality of unit volume of the present invention is light, and thermal conductivity is little, and intensity is high, can as the insulating layer of external wall of building.
3. present invention process is simple, mild condition, efficent use of resources.
Embodiment
Titanium white gypsum in experiment has an area of titanium white factory by Qianjiang, Hubei to be provided, and its chemical constitution is as shown in table 1.Magnetic iron ore, hematite, yellow iron, limonite ore and siderite are provided by Central-South Institute of Metallurgical Technology of Ministry of Metallurgical Industry, and its iron level is respectively: 39.01 %, 38.50%, 26.18%, 21.62% and 20.73%.
Table 1 titanium white gypsum main component
| Index | Ca | Fe | Al | Ti | Si | Mg |
| Main component | 28.76% | 7.34% | 1.25% | 2.58% | 0.98% | 0.52% |
embodiment 1
100 titanium white gypsum calcinations to 450 DEG C, pulverize, vibration screening, makes it at 40 microns.Be placed in autoclave, pass into saturation steam, after 125 DEG C and 2.8 kPa vapour pressures are incubated 3 hours, pearl is ground, 140 DEG C of dryings, and grinding and pulverizing, vibration screening to 10 micron obtained semi-hydrated gypsum.Pulverized by 12.5g pyrite, vibration screening, makes it at 16 microns.Organic waterproof agent butyl acrylate 2.8 kg is added water after mixing, add 0.2 kg Sodium dodecylbenzene sulfonate, be warming up to 70 DEG C and be incubated 1h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent filtrate successively, in the iron ore after pulverizing and 0.5 kg chitosan, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 3 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, the obtained plastering with photocatalytic activity.Get 1 g semi-hydrated gypsum respectively; The semi-hydrated gypsum that 1g has a photocatalytic activity joins 50 mL and contains 4 × 10
-5in rhodamine B (RhB) solution of concentration, adjust ph, after dark reaction 4h, to degrade 4 h at 400 W Metal-halogen lamps, carries out blank assay simultaneously.Experimental result: do not add semi-hydrated gypsum RhB after 4 hours degradation efficiency be 8.3%, add semi-hydrated gypsum RhB 4 hours degradation efficiencies 21.4%, add semi-hydrated gypsum mixture RhB 4 hours degradation efficiencies 26.1% with photocatalytic activity.
embodiment 2
Preparation process is as embodiment 1, and only the following step is different:
The calcination to 550 DEG C of titanium white gypsum, pulverizes, makes it at 65 microns, be placed in autoclave, pass into saturation steam, 132 DEG C of dryings after 135 DEG C and 2.1 kPa vapour pressures are incubated 3.5 hours, and grinding and pulverizing, vibration screening, makes it at 2 microns of semi-hydrated gypsums; Pulverized by rhombohedral iron ore, vibration screening, makes it at 12 microns, then at 480 DEG C of calcining 3 h, grinding and pulverizing, vibration screening to 8 micron.Allyl acetate 0.8 kg is added water after mixing, add 0.3 kg Sodium dodecylbenzene sulfonate, be warming up to 80 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, in the iron ore after pulverizing and 0.2 kg chitin, 0.6 kg glucose solution, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 4 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, obtained plastering.Get semi-hydrated gypsum that semi-hydrated gypsum 1.0 g and 1g have a photocatalytic activity respectively to join 50 mL and contain in certain density salicylic acid solution, adjust ph, after dark reaction 4h, at 400 W Metal-halogen lamps degraded 6h, carries out blank assay simultaneously.Experimental result: control group after 6 hours salicylate degradation efficiency be 9.3%, add semi-hydrated gypsum salicylate degradation efficiency 25.9% after 6 hours, add after there is the semi-hydrated gypsum of photocatalytic activity, salicylate degradation efficiency 33.5% after 6 hours.
embodiment 3
Preparation process is as embodiment 1, and only the following step is different:
The calcination to 600 DEG C of titanium white gypsum, pulverize, vibration screening, makes it at 85 microns, is placed in autoclave, passes into saturation steam, 132 DEG C of dryings after 135 DEG C and 2.1 kPa vapour pressures are incubated 3.5 hours, grinding and pulverizing, the semi-hydrated gypsum of vibration screening to 10 micron.Magnetite 20 g and rhombohedral iron ore 130 g is pulverized and mixed, vibration screening, makes it at 22 microns, then at 350 DEG C of calcining 1 h, be milled to 10 microns.Organic waterproof agent butyl acrylate 2.8 kg is added water after mixing, add 0.2 kg Sodium dodecylbenzene sulfonate, be warming up to 70 DEG C and be incubated 1h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, in the iron ore after pulverizing and 0.5 kg chitosan, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 3 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, the obtained plastering with photocatalytic activity.Get semi-hydrated gypsum that semi-hydrated gypsum 1.0 g and 1g have a photocatalytic activity respectively to join 100 mL and contain certain density 2, in 4-chlorophenol solution, adjust ph, after dark reaction 4h, carry out degradation experiment at 9 in morning mid-August at 3 in afternoon, carry out blank assay simultaneously.Experimental result: control group after 6 hours 2,4-chlorophenol degradation efficiencies be 6.6%, add semi-hydrated gypsum, degradation efficiency 18.4 % of 2,4-chlorophenols after 6 hours, add and there is degradation efficiency 27.8 % of semi-hydrated gypsum 2,4-chlorophenols after 6 hours of photocatalytic activity.
embodiment 4
Preparation process is as embodiment 1, and only the following step is different:
The calcination to 400 DEG C of titanium white gypsum, pulverize, vibration screening, makes it at 35 microns, is placed in autoclave, passes into saturation steam, 130 DEG C of dryings after 130 DEG C and 2.8 kPa vapour pressures are incubated 3 hours, grinding and pulverizing, the semi-hydrated gypsum of vibration screening to 20 micron.Limonite 80 g and spathic iron ore 60 g is pulverized and mixed, vibration screening, makes it at 30 microns, then at 350 DEG C of calcining 2 h, be milled to 10 microns.Organic waterproof agent butyl acrylate 0.6 kg, allyl acetate 0.8 kg are added water after mixing, add 0.4 kg Sodium dodecylbenzene sulfonate, be warming up to 55 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, stir in the iron ore after pulverizing, 0.75 kg alkylphenol polyoxyethylene and chitin 0.6 kg, chitosan 0.1 kg solution, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 2 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 2-3 days, obtain through the maintenance demoulding semi-hydrated gypsum goods that expansion type has photocatalytic activity.Get semi-hydrated gypsum goods that semi-hydrated gypsum 1.0 g and 1g have a photocatalytic activity respectively to join 100 mL and contain in certain density RhB solution, adjust ph, after dark reaction 4h, carry out degradation experiment at 9 in morning mid-August at 3 in afternoon, carry out blank assay simultaneously.Experimental result: do not add semi-hydrated gypsum, after 6 hours, the degradation efficiency of polychlorobiphenyl is 3.5%, adds semi-hydrated gypsum, the degradation efficiency 11.9% of polychlorobiphenyl after 6 hours, add the semi-hydrated gypsum with photocatalytic activity, the degradation efficiency 18.1% of polychlorobiphenyl after 6 hours.
embodiment 5
Preparation process is as embodiment 1, and only the following step is different:
The calcination to 700 DEG C of titanium white gypsum, pulverize, vibration screening, makes it at 35 microns, is placed in autoclave, passes into saturation steam, 132 DEG C of dryings after 135 DEG C and 2.1 kPa vapour pressures are incubated 3.5 hours, grinding and pulverizing, vibration screening to 1 micron semi-hydrated gypsum.Magnetite 20 g and rhombohedral iron ore 130 g is pulverized and mixed, vibration screening, makes it at 26 microns, then at 350 DEG C of calcining 1 h, be milled to 5 microns.Organic waterproof agent butyl acrylate 2.7 kg, allyl acetate 1.2 kg are added water after mixing, add 0.3 kg Sodium dodecylbenzene sulfonate, be warming up to 66 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, the iron ore after pulverizing, in 1.0 kg alkylphenol polyoxyethylene and chitosan 0.3kg, glucose 0.5kg solution, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 2 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 2-3 days, obtain through the maintenance demoulding plastering that expansion type has photocatalytic activity.Get semi-hydrated gypsum that semi-hydrated gypsum 1.0 g and 1.0g have a photocatalytic activity respectively to join 100 mL and contain in certain density formaldehyde solution, adjust ph, after dark reaction 4h, carry out degradation experiment at 9 in morning mid-August at 3 in afternoon, carry out blank assay simultaneously.Experimental result: control group after 6 hours Degradation Formaldehyde efficiency be 8.6%, add the degradation efficiency 23.0% of semi-hydrated gypsum formaldehyde after 6 hours, add degradation efficiency 39.8 % with formaldehyde behind 6 hours of photocatalytic activity.
embodiment 6
100 kg titanium white gypsum calcinations to 700 DEG C, pulverize, vibration screening, makes it at 30 microns, is placed in autoclave, passes into saturation steam, and after 115 DEG C and 1.6 kPa vapour pressures are incubated 1.5 hours, pearl is ground, 135 DEG C of dryings, ball milling vibration screening to 5 micron.Pyrite 2 kg, rhombohedral iron ore 13 kg are pulverized, vibration screening, make it at 12 microns.Organic waterproof agent butyl acrylate 2.8 kg is added water after mixing, add 0.4 kg Sodium dodecylbenzene sulfonate, be warming up to 60 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.Add successively in water in the virgin iron ore after above-mentioned water-resisting agent, pulverizing and 0.8 kg chitin, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 3 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, obtained plastering.By plastering according to its folding strength of cement products ruggedness test standard testing and ultimate compression strength and waterproof ability.Hang in mercury lamp (being placed in the Glass tubing of water coolant) closed cabinet one, by the gypsum block case for preparing, distance mercury lamp 20 cm, passes into acetone, measures the content of acetone in casing after 12h.Experimental result: according to plastering ruggedness test standard, measuring its folding strength is 2.90 MPa, and ultimate compression strength is 9.75 MPa.Measuring its folding strength after 24 h water resistance tests is 1.32 MPa, and ultimate compression strength is 7.46 MPa.After not placing gypsum block 12h, acetone content reduces by 5.4%, and after placing gypsum block 12h, acetone content reduces by 15.5%.
embodiment 7
100 kg titanium white gypsum calcinations to 580 DEG C, pulverize, vibration screening, makes it at 60 microns.Be placed in autoclave, pass into saturation steam, after 120 DEG C and 2.1 kPa vapour pressures are incubated 3 hours, pearl is ground, 138 DEG C of dryings, and grinding and pulverizing, vibration screening to 3 micron.Pyrite 8 kg, limonite 4.5 kg are pulverized, vibration screening, make it at 15 microns.Allyl acetate 0.8 kg is added water after mixing, add 0.3 kg Sodium dodecylbenzene sulfonate, be warming up to 80 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, in the virgin iron ore after pulverizing and 0.2 kg chitin, 0.6 kg glucose solution, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 4 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, obtained plastering.By plastering according to its folding strength of plastering ruggedness test standard testing and ultimate compression strength and waterproof ability.Hang in mercury lamp (being placed in the Glass tubing of water coolant) closed cabinet one, by the gypsum block case for preparing, distance mercury lamp 20 cm, passes into acetone, measures the content of acetone in casing after 12h.Experimental result: according to plastering ruggedness test standard, measuring its folding strength is 2.25 MPa, and ultimate compression strength is 9.91 MPa.Measuring its folding strength after 24 h water resistance tests is 1.52 MPa, and ultimate compression strength is 7.99 MPa.After not placing gypsum block 12h, acetone content reduces by 5.3%, and after placing gypsum block 12 h, acetone content reduces by 14.6%.
embodiment 8
100 kg titanium white gypsum calcinations to 400 DEG C, pulverize, vibration screening, makes it at 30 microns.Be placed in autoclave, pass into saturation steam, after 125 DEG C and 2.8 kPa vapour pressures are incubated 3 hours, pearl is ground, 140 DEG C of dryings, and grinding and pulverizing, vibration screening to 10 micron.Spathic iron ore 2 kg, rhombohedral iron ore 18.5 kg are pulverized, vibration screening, make it at 20 microns.Organic waterproof agent butyl acrylate 2.8 kg is added water after mixing, add 0.2 kg Sodium dodecylbenzene sulfonate, be warming up to 70 DEG C and be incubated 1h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, in the virgin iron ore after pulverizing and 0.5 kg chitosan, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 3 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 3 days, through the empty maintenance of overdrying after the demoulding, obtained plastering.By plastering according to its folding strength of cement products ruggedness test standard testing and ultimate compression strength and waterproof ability.Hang in mercury lamp (being placed in the Glass tubing of water coolant) closed cabinet one, by the gypsum block case for preparing, distance mercury lamp 20 cm, passes into acetone, measures the content of acetone in casing after 12h.Experimental result: according to plastering ruggedness test standard, measuring its folding strength is 2.66 MPa, and ultimate compression strength is 10.30 MPa.Measuring its folding strength after 24 h water resistance tests is 1.92 MPa, and ultimate compression strength is 8.84 MPa.After not placing gypsum block 12h, acetone content reduces by 5.3%, and after placing gypsum block 12 h, acetone content reduces by 13.8 %.
embodiment 9
100 kg titanium white gypsum calcinations to 550 DEG C, pulverize, vibration screening, makes it at 60 microns.Be placed in autoclave, pass into saturation steam, after 135 DEG C and 3.5 kPa vapour pressures are incubated 4 hours, pearl is ground, 140 DEG C of dryings, and grinding and pulverizing, vibration screening to 8 micron.Yellow iron 15 kg, limonite ore 2 kg and rhombohedral iron ore 2 kg are pulverized, vibration screening, makes it at 20 microns.Organic waterproof agent butyl acrylate 0.6 kg, allyl acetate 0.8 kg are added water after mixing, add 0.4 kg Sodium dodecylbenzene sulfonate, be warming up to 55 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, stir in the virgin iron ore after pulverizing, 0.75 kg alkylphenol polyoxyethylene and chitin 0.6 kg, chitosan 0.1 kg solution, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 2 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 2-3 days, obtain foaming plaster goods through the maintenance demoulding.By plastering according to its folding strength of cement products ruggedness test standard testing and ultimate compression strength and waterproof ability.Hang in mercury lamp (being placed in the Glass tubing of water coolant) closed cabinet one, by the gypsum block case for preparing, distance mercury lamp 20 cm, passes into acetone, measures the content of acetone in casing after 12h.Experimental result: according to plastering ruggedness test standard, measuring its folding strength is 3.01 MPa, and ultimate compression strength is 10.65 MPa.Measuring its folding strength after 24 h water resistance tests is 2.06 MPa, and ultimate compression strength is 8.46 MPa.Density of building block is 328 kg/m
3, thermal conductivity is 0.060 w/mK.After not placing gypsum block 12h, acetone content reduces by 5.4%, and after placing gypsum block 12h, acetone content reduces by 14.1 %.
embodiment 10
100 kg titanium white gypsum calcinations to 300 DEG C, pulverize, vibration screening, makes it at 40 microns.Be placed in autoclave, pass into saturation steam, after 110 DEG C and 2.1 kPa vapour pressures are incubated 2 hours, pearl is ground, 135 DEG C of dryings, and grinding and pulverizing, vibration screening to 15 micron.Magnetite 2 kg, rhombohedral iron ore 13 kg are pulverized, vibration screening, make it at 8 microns.Organic waterproof agent butyl acrylate 2.7 kg, allyl acetate 1.2 kg are added water after mixing, add 0.3 kg Sodium dodecylbenzene sulfonate, be warming up to 66 DEG C and be incubated 1 h after high-speed stirring 40 min, be down to room temperature and regulate pH 7.5, filtering.In water, add above-mentioned water-resisting agent successively, the virgin iron ore after pulverizing, in 1.0 kg alkylphenol polyoxyethylene and chitosan 0.3kg, glucose 0.5kg solution, stir, make it fully mix.Obtained semi-hydrated gypsum is joined in above-mentioned solution, is poured into after stirring 2 min in mould, vibratory compaction, is placed in climatic chamber, at about 25 DEG C through maintenance 2-3 days, obtain foaming plaster goods through the maintenance demoulding.By plastering according to its folding strength of cement products ruggedness test standard testing and ultimate compression strength and waterproof ability.Hang in mercury lamp (being placed in the Glass tubing of water coolant) closed cabinet one, by the gypsum block case for preparing, distance mercury lamp 20 cm, passes into acetone, measures the content of acetone in casing after 12h.Experimental result: according to plastering ruggedness test standard, measuring its folding strength is 2.90 MPa, and ultimate compression strength is 9.98 MPa.Measuring its folding strength after 24 h water resistance tests is 1.53 MPa, and ultimate compression strength is 8.70 MPa.Density of building block is 279 kg/m
3, thermal conductivity is 0.065 w/ mK.After not placing gypsum block 12h, acetone content reduces by 5.3%, and after placing gypsum block 12h, acetone content reduces by 12.9 %.
Claims (7)
1. one kind has the semi-hydrated gypsum of photocatalytic activity, it is characterized in that: raw material based on titanium white gypsum, through adding iron ore, water-resisting agent, retardant, the obtained semi-hydrated gypsum with photocatalysis performance after whipping agent, by weight, 100 parts, titanium white gypsum, iron ore 4-25 part, water-resisting agent 0.6-5.8 part, retardant 0.5-2.8 part, whipping agent 0.1-1.3 part.
2. the semi-hydrated gypsum with photocatalytic activity according to claim 1, is characterized in that: described iron ore is one or more in magnetite, rhombohedral iron ore, pyrite, limonite and spathic iron ore.
3. the semi-hydrated gypsum with photocatalytic activity according to claim 1, is characterized in that: described water-resisting agent is butyl acrylate and/or allyl acetate.
4. the semi-hydrated gypsum with photocatalytic activity according to claim 1, is characterized in that: described retardant be in chitin, chitosan and glucose one or more.
5. the semi-hydrated gypsum with photocatalytic activity according to claim 1, is characterized in that: described whipping agent is alkylphenol polyoxyethylene.
6. there is a preparation method for the semi-hydrated gypsum goods of photocatalytic activity, it is characterized in that, comprise the following steps:
(1) by titanium white gypsum calcination 1-2h at 300-700 DEG C, pulverize after cooling, vibration screening to granularity is 5-100 micron, is placed in autoclave, passes into saturation steam by this titanium white gypsum particle, under the vapour pressure of 110-130 DEG C and 1.2-3.5 kPa, insulation 1-5h, ball milling after cooling, dry 1-2h at 130-135 DEG C, ball milling vibration screening to granularity is 0.5-50 micron again, and obtained semi-hydrated gypsum is stand-by;
(2) one or more mixed ores in magnetite, rhombohedral iron ore, pyrite, limonite, spathic iron ore are pulverized and sieved and at 300-600 DEG C, calcine 1-3 h after granularity is 5-100 micron, being milled to iron ore particle degree after cooling is 5-20 micron, and obtained iron ore is stand-by;
(3) water-resisting agent is added water mixing after, drip Sodium dodecylbenzene sulfonate, and after stirring 40 min with the speed of 120-200r/min, be warming up to 75-85 DEG C, be incubated 1 h, be down to room temperature and regulate pH to 7.5, filter, obtained water-resisting agent filtrate, stand-by, wherein the weight ratio of water-resisting agent, water, Sodium dodecylbenzene sulfonate is 10:80:0.1 ~ 1;
(4) the water-resisting agent filtrate in the iron ore in step (2), step (3), retardant are added to the water, 40 ~ 60min is stirred with the speed of 80 ~ 100 r/ min, obtained mixed slurry, wherein the weight ratio of iron ore, water-resisting agent filtrate, retardant, water is 4-25:0.6-5.8:0.5-2.8:50-70;
(5) in semi-hydrated gypsum in step (1), add the mixed slurry in step (4), be poured in mould after stirring 2-5 min, vibratory compaction, be placed in climatic chamber, at 25 ± 3 DEG C through maintenance 2-3 days, maintenance after the demoulding, the obtained semi-hydrated gypsum goods with photocatalytic activity.
7. there is a preparation method for the semi-hydrated gypsum goods of photocatalytic activity, it is characterized in that, comprise the following steps:
(1) by titanium white gypsum calcination 1-2h at 300-700 DEG C, pulverize after cooling, vibration screening to granularity is 5-100 micron, is placed in autoclave, passes into saturation steam by this titanium white gypsum particle, under the vapour pressure of 110-130 DEG C and 1.2-3.5 kPa, insulation 1-5h, ball milling after cooling, dry 1-2h at 130-135 DEG C, ball milling vibration screening to granularity is 0.5-50 micron again, and obtained semi-hydrated gypsum is stand-by;
(2) one or more mixed ores in magnetite, rhombohedral iron ore, pyrite, limonite, spathic iron ore are pulverized and sieved and at 300-600 DEG C, calcine 1-3 h after granularity is 5-100 micron, being milled to iron ore particle degree after cooling is 5-20 micron, and obtained iron ore is stand-by;
(3) water-resisting agent is added water mixing after, drip Sodium dodecylbenzene sulfonate, and after stirring 40 min with the speed of 120-200r/min, be warming up to 75-85 DEG C, be incubated 1 h, be down to room temperature and regulate pH to 7.5, filter, obtained water-resisting agent filtrate, stand-by, wherein the weight ratio of water-resisting agent, water, Sodium dodecylbenzene sulfonate is 10:80:0.1 ~ 1;
(4) the water-resisting agent filtrate in the iron ore in step (2), step (3), retardant are added to the water, 40 ~ 60min is stirred with the speed of 80 ~ 100r/min, obtained mixed slurry, wherein the weight ratio of iron ore, water-resisting agent filtrate, retardant, water is 4-25:0.6-5.8:0.5-2.8:50-70;
(5) in the mixed slurry of step (4), add whipping agent alkylphenol polyoxyethylene, stir, wherein mixed slurry is 100:0.1-1.0 with the weight ratio of alkylphenol polyoxyethylene;
(6) in semi-hydrated gypsum in step (1), add the mixed slurry in step (5), be poured in mould after stirring 2-5min, vibratory compaction, be placed in climatic chamber, at 25 ± 3 DEG C of maintenance 2-3 days, maintenance after the demoulding, the obtained semi-hydrated gypsum goods with photocatalytic activity.
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| CN107775789B (en) * | 2017-11-03 | 2020-06-09 | 钦州学院 | Manufacturing process of high-strength nixing pottery gypsum mold |
| CN111943619A (en) * | 2020-07-09 | 2020-11-17 | 重庆大学 | Method for preparing foamed brick by using titanium gypsum |
| CN112128026B (en) * | 2020-09-24 | 2021-05-14 | 中惠利邦环境技术有限公司 | Porous spherical body capable of realizing fuel saving of fuel-powered vehicle and synergistically reducing emission of exhaust pollutants, and preparation method and application thereof |
| CN116102286B (en) * | 2022-12-14 | 2024-04-09 | 山东华诚高科胶粘剂有限公司 | Gypsum retarder and preparation method thereof |
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