CN108940196A - A kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material - Google Patents

A kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material Download PDF

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CN108940196A
CN108940196A CN201810687286.3A CN201810687286A CN108940196A CN 108940196 A CN108940196 A CN 108940196A CN 201810687286 A CN201810687286 A CN 201810687286A CN 108940196 A CN108940196 A CN 108940196A
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activated carbon
carbon fiber
preparation
sodium bismuthate
loaded
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安俊健
黄梦璇
王梦玲
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Hubei University of Technology
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033Membrane, sheet, cloth, pad, lamellar or mat
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The present invention provides a kind of preparation methods of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material.The preparation method carries out as follows: 1, the preparation of activated carbon fibre;2, the preparation of activated carbon fiber-loaded sodium bismuthate.Ultrasonic power is carried out using ultrasound-in situ synthesis in the method, and activated carbon fiber-loaded sodium bismuthate uses bismuth source and activated carbon fibre for raw material.This method selects the photochemical catalyst sodium bismuthate with visible light catalytic performance for basic catalyst, and be supported in activated carbon fibre, it is good catalyst carrier that activated carbon fibre, which is used extensively, it can avoid the reunion of sodium bismuthate nano particle, to guarantee absorption and catalytic activity.

Description

A kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material
Technical field
The present invention relates to the technical fields of sewage treatment, are related specifically to a kind of activated carbon fiber-loaded sodium bismuthate absorption The preparation method of catalysis material.
Background technique
China be water resource possess big country be also water resource lack big country.Resources water shortage, economy water shortage, water quality lack Water is that China's water resource utilizes faced serious problems.The pollution of water resource has seriously affected being pacified with water health for people Entirely, the highest attention of state and society is caused.It offers convenience with the development of economy to people's lives, the dirt of industrial wastewater It is also increasingly severeer to contaminate situation, brings significant threat to China's water environment.Industrial wastewater is due to many kinds of, pollutant component And property is different with production process, variation is complicated, and main polluter is organic pollutant, and the influence to water body environment is non- Chang great.Water process new technology is explored, realizes the processing qualified discharge even Sewage treatment benefit of Industry Waste organic pollutants With being our present urgent problems.
High-level oxidation technology usually has Ozonation, Fenton reagent oxidizing process, photochemical oxidation method, photochemical catalytic oxidation Method, Ultrasonic Radiation oxidizing process etc..As people increasingly pay close attention to environment water problems, there is an urgent need for a kind of economy to have by people Effect and the few processing method of by-product.In water treatment technology, it is seen that photocatalytic method is as a kind of advanced oxidation processes due to can It generates non-selective oxidation agent (hydroxyl radical free radical) and is concerned.Since the fibre diameter of activated carbon fiber is thin, specific surface area Greatly, microcellular structure is flourishing, aperture is small and narrowly distributing, adsorption capacity are big, inhaling de- speed, fast, regeneration is easy.It is to ppb grades of trace Substance absorption is especially effective, and adsorption efficiency is high at low concentrations.Sodium bismuthate activated carbon fibre compound is used for in waste water Organic pollution materials, which carry out advanced treating, has preferable application value.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material.This Invention utilizes the strong absorption of activated carbon fibre using sodium bismuthate and the compound of activated carbon fibre as absorption and catalytic degradation material Performance and the visible light catalytic performance of sodium bismuthate achieve the purpose that absorption and degradation organic pollutants.
Design philosophy of the invention is to prepare activated carbon fibre first, then prepare work by ultrasound-in situ synthesis Property Carbon fibe load sodium bismuthate adsoption catalysis paper material.It is under strong stirring that its is few using bismuth nitrate or bismuth hydroxide as bismuth source Amount is repeatedly added in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads, and 20-30 DEG C of temperature control, ultrasonic reaction 60-80 Min is impregnated with ammonium phosphate the purpose is to make sodium bismuthate growth in situ in activated carbon fibre and increases its durability.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material, it is characterised in that: the preparation method It carries out as follows:
1, the preparation of activated carbon fibre
The cotton fabric for weighing solid 300-400 g is placed in the acid solution that mass percent concentration is 60-80%, is made solid in mixture Quality-concentration expressed in percentage by volume of body is 5-25%(w/v), is stirred, 4-7 minute, after aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution, by by pretreated cotton fabric, dry 20-26 is small in 70 DEG C -90 DEG C of baking oven When, it then releases and cools down 11-15 hours at ambient temperature, it is dense that cooling cotton fabric is immersed into mass percent at room temperature (the NH that degree is 7.5%4)2HPO42-4 hours in solution, then extracts and dry 20-26 hours at 70 DEG C -90 DEG C, be cooled to After environment temperature, it is transferred into aluminium oxide boat and is put into Muffle furnace, use N2As protective gas, flow velocity 600 ML/min is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, keeps the temperature 30 60 minutes progress carbon Change, then 700-800 DEG C is heated to the rate of 10 DEG C/min, in CO2It keeps being activated for 30-60 minutes under atmosphere, flow velocity For 0.5L/min, in N2It flows down after being naturally cooling to 300 DEG C, product is taken out to from furnace and is cooled to environment temperature, is then used Distilling water washing to pH value is 7-7.2, finally 20-26 hours dry at 70 DEG C -90 DEG C, obtains activated carbon fibre (ACF);
2, the preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g step (1) and obtain The activated carbon fibre ultrasonic disperse obtained is cooled to 3 DEG C -10 DEG C with ice water, is passed through chlorine under stiring into sodium hydroxide solution Reach saturation, then add the sodium hydroxide of 10-15 g, controls temperature at 10 DEG C -20 DEG C, by the crystal and activity of precipitation The mixture of Carbon fibe, which separates, to be filtered, and the sodium hypochlorite that activated carbon fiber tentatively loads is obtained;It is under vigorous stirring that bismuth source is few Amount is repeatedly added in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads, and 20-30 DEG C of temperature control, ultrasonic reaction 60-80 Minute, the sodium bismuthate precipitating of yellow is obtained, its stratification is eluted, mistake with the sodium hydroxide that mass percent concentration is 1% It is 24-30 hours dry in vacuum oven again after filter, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
Acid solution in the step (1) be sulfuric acid solution, boric acid solution, acetum, formic solutions, nitric acid solution, Any one in hydrochloric acid solution.
Ultrasonic power in the step 2 is carried out using ultrasound-in situ synthesis.
Activated carbon fiber-loaded sodium bismuthate in the step 2 uses bismuth source and activated carbon fibre for raw material.
Bismuth source in the step 2 uses Bi (NO3)3, Bi (OH)3For raw material.
Technical solutions according to the invention prepare the detailed process of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material, point For the preparation of activated carbon fibre and two key steps of preparation of activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material, phosphorus is used Sour ammonium, which impregnates, increases durability, and is carried out to the absorption of rhodanine B and degradation effect to preparation process according to prepared material Corresponding adjustment.
Compared with prior art, the positive effect of the present invention are as follows:
1, it selects the photochemical catalyst sodium bismuthate with visible light catalytic performance for basic catalyst, and is supported on active carbon fibre In dimension, activated carbon fibre is good catalyst carrier, can avoid the reunion of sodium bismuthate nano particle, to protect with extensively Card absorption and catalytic activity;
2, select activated carbon fibre as catalytic carrier, activated carbon fibre micropore size is small and uniform, and structure is simple, specific surface area Greatly, for adsorbing small-molecule substance, the rate of adsorption is fast, is easy desorption, helps to generate stronger absorption to organic pollutant, In addition huge specific surface area itself, necessarily to organic pollutant absorption property with super strength, strong absorption can generate good Catalytic degradation effect;
3, method and process used in the present invention is simple, easy to operate, can utilize the strong absorption and catalysis of the catalyst well Performance realizes efficient degradation and mineralising to organic pollutant.
Detailed description of the invention
The synthesis and application of Fig. 1, activated carbon fiber-loaded sodium bismuthate adsoption catalysis material;
Fig. 2, activated carbon fibre SEM figure;
Fig. 3, activated carbon fiber-loaded sodium bismuthate adsoption catalysis material TEM figure;
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (the activated carbon fibre preparation of Fig. 4, different activities Carbon fiber dimension hplc Using nitric acid aging fiber, using bismuth nitrate as bismuth source, ultrasound-in situ synthesis preparation) the adsorbance variation of methyl orange (is inhaled Sub conditione: pH 5, temperature: 25 DEG C);
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (the activated carbon fibre preparation of Fig. 5, different activities Carbon fiber dimension hplc Using nitric acid aging fiber, using bismuth nitrate as bismuth source, ultrasound-in situ synthesis preparation) to the degradation kinetics (activity of methyl orange The mass content of Carbon fibe: (1) 0, (2) 0.2, (3) 0.6, (4) 0.8, (5) 1.0, pH 5, temperature: 25 DEG C);
Fig. 6, different activities Carbon fiber dimension hplc activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (activated carbon fibre preparation make With sulfuric acid aging fiber, using bismuth hydroxide as bismuth source, ultrasound-in situ synthesis preparation) the adsorbance variation of methyl orange (is inhaled Sub conditione: pH 5, temperature: 25 DEG C);
Fig. 7, different activities Carbon fiber dimension hplc activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (using bismuth hydroxide as bismuth Source, the preparation of ultrasound-in situ synthesis) to the degradation kinetics of methyl orange, (activated carbon fibre preparation uses sulfuric acid aging fiber, living The mass content of property Carbon fibe: (1) 0, (2) 0.2, (3) 0.6, (4) 0.8, (5) 1.0, pH 5, temperature: 25 DEG C).
The activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (activated carbon fibre of Fig. 8, different activities Carbon fiber dimension hplc Preparation uses boric acid aging fiber, using bismuth nitrate as bismuth source, ultrasound-in situ synthesis preparation) and the adsorbance of methyl orange is changed (adsorption conditions: pH 5, temperature: 25 DEG C);
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (the activated carbon fibre preparation of Fig. 9, different activities Carbon fiber dimension hplc Using boric acid aging fiber, using bismuth nitrate as bismuth source, ultrasound-in situ synthesis preparation) to the degradation kinetics (activity of methyl orange The mass content of Carbon fibe: (1) 0, (2) 0.2, (3) 0.6, (4) 0.8, (5) 1.0, pH 5, temperature: 25 DEG C);
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (the activated carbon fibre preparation of Figure 10, different activities Carbon fiber dimension hplc Using formic acid aging fiber, using bismuth hydroxide as bismuth source, ultrasound-in situ synthesis preparation) adsorbance of methyl orange is changed (adsorption conditions: pH 5, temperature: 25 DEG C);
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material (the activated carbon fibre preparation of Figure 11, different activities Carbon fiber dimension hplc Using formic acid aging fiber, using bismuth hydroxide as bismuth source, ultrasound-in situ synthesis preparation) it is (living to the degradation kinetics of methyl orange The mass content of property Carbon fibe: (1) 0, (2) 0.2, (3) 0.6, (4) 0.8, (5) 1.0, pH 5, temperature: 25 DEG C).
Specific embodiment
Clear, complete description further is carried out to technical solution of the present invention with reference to the accompanying drawings and examples.
Embodiment one:
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material is prepared by bismuth source of bismuth nitrate
1, the preparation of activated carbon fibre
The cotton fabric (CW) for weighing 300-400 g is placed in the nitric acid solution that mass percent concentration is 60%, is made in mixture Quality-concentration expressed in percentage by volume of solid is 5%(w/v), after stirring 4-7 minute, aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution.It will be dry in 70 DEG C -90 DEG C of baking oven by pretreated cotton fabric (PCW) It 20-26 hours, then releases and cools down 11-15 hours at ambient temperature, cooling cotton fabric (PCW) is immersed at room temperature (the NH that mass percent concentration is 7.5%4)2HPO42-4 hours in solution, is then extracted at 70 DEG C -80 DEG C and dry 20- It 26 hours, after being cooled to environment temperature, is transferred into aluminium oxide boat and is put into Muffle furnace, use N2Make protective gas, Flow velocity is 600 mL/min, is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, heat preservation 30 60min is carbonized;Then it is heated to 700-800 DEG C with the rate of 10 DEG C/min, in CO2Under atmosphere keep 30-60min into Row activation, flow velocity 0.5L/min.In N2It flows down after being naturally cooling to 300 DEG C, product is taken out from furnace and is cooled to environment Then temperature is washed with distilled water to pH most 7-7.2, finally 20-26 hours dry at 70 DEG C -90 DEG C, obtains active carbon Fiber (ACF).
2, the preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g active carbon fibre Ultrasonic disperse is tieed up into sodium hydroxide solution, 3 DEG C -10 DEG C is cooled to ice water, is passed through chlorine under stiring and reaches saturation, then The sodium hydroxide of 10-15 g is added, controls temperature at 10 DEG C -20 DEG C, by the mixture of the crystal of precipitation and activated carbon fibre Separation filters, and obtains the sodium hypochlorite that activated carbon fiber tentatively loads;Using bismuth nitrate as bismuth source, under vigorous stirring by bismuth nitrate It is repeatedly added in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads on a small quantity, 20-30 DEG C of temperature control, ultrasonic reaction 60- 80 minutes, the sodium bismuthate precipitating of yellow is obtained, its stratification is eluted with the sodium hydroxide that mass percent concentration is 1%, It is 24-30 hours dry in vacuum oven again after filtering, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
3, sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic contamination The adsorption assessment of object (methyl orange):
It is absorption object with methyl orange referring to attached drawing 4, research sodium bismuthate based active carbon fiber loads sodium bismuthate adsoption catalysis paper wood Expect the adsorption effect to it, and according to the effect of absorption, phase is carried out to the preparation process of sodium bismuthate base visible light catalytic paper material The adjustment answered.
4, sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic contamination The degradation of object (methyl orange) is evaluated:
It is degradation object, research sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded bismuthic acid with methyl orange referring to attached drawing 5 Sodium adsoption catalysis paper material is to its degradation effect, and according to the effect of degradation, to sodium bismuthate base (bismuth nitrate is bismuth source) activity The preparation process of Carbon fibe load sodium bismuthate adsoption catalysis paper material is adjusted correspondingly.
Embodiment two:
Sodium bismuthate base visible light catalytic paper material is prepared by bismuth source of bismuth hydroxide
1, the preparation of activated carbon fibre
The cotton fabric (CW) for weighing 300-400 g is placed in the sulfuric acid solution that mass percent concentration is 70%, is made in mixture Quality-concentration expressed in percentage by volume of solid is 10%(w/v), after stirring 4-7 minute, aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution.It will be dry in 70 DEG C -90 DEG C of baking oven by pretreated cotton fabric (PCW) It 20-26 hours, then releases and cools down 11-15 hours at ambient temperature, cooling cotton fabric (PCW) is immersed at room temperature (the NH that mass percent concentration is 7.5%4)2HPO42-4 hours in solution (7.5%), then extracted simultaneously at 70 DEG C -90 DEG C It is 20-26 hours dry, after being cooled to environment temperature, it is transferred into aluminium oxide boat and is put into Muffle furnace.Use N2Go bail for Gas is protected, flow velocity is 600 mL/min, is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, heat preservation It is carbonized within 30 60 minutes.Then it is heated to 700-800 DEG C with the rate of 10 DEG C/min, in CO230-60 is kept under atmosphere Minute is activated, and flow velocity is 0.5 L/min.In N2It flows down after being naturally cooling to 300 DEG C, product is taken out and cooled down from furnace To environment temperature.Then being washed with distilled water to pH value is 7-7.2, finally, it is 20-26 hours dry at 70 DEG C -80 DEG C, it is lived Property Carbon fibe (ACF).
2, the preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g active carbon fibre Ultrasonic disperse is tieed up into sodium hydroxide solution, 3 DEG C -10 DEG C is cooled to ice water, is passed through chlorine under stiring and reaches saturation, so The sodium hydroxide of 10-15 g is added afterwards, controls temperature at 10 DEG C -20 DEG C, by the mixing of the crystal of precipitation and activated carbon fibre Object separation filters, and obtains the sodium hypochlorite that activated carbon fiber tentatively loads;Using bismuth hydroxide as bismuth source, under vigorous stirring by hydrogen Bismuth oxide is repeatedly added on a small quantity in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads, and 20-30 DEG C of temperature control, ultrasound is anti- It answers 60-80 minutes, obtains the sodium bismuthate precipitating of yellow, by its stratification, the sodium hydroxide for being 1% with mass percent concentration Elution, it is 24-30 hours dry in vacuum oven again after filtering, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
3, sodium bismuthate base (bismuth hydroxide is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic dirt Contaminate the adsorption assessment of object (methyl orange):
It is absorption object with methyl orange referring to attached drawing 6, research sodium bismuthate based active carbon fiber loads sodium bismuthate adsoption catalysis paper wood Expect the adsorption effect to it, and according to the effect of absorption, sodium bismuthate adsoption catalysis paper wood is loaded to sodium bismuthate based active carbon fiber The preparation process of material is adjusted correspondingly.
4, sodium bismuthate base (bismuth hydroxide is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic dirt Contaminate the degradation evaluation of object (methyl orange):
It is degradation object, research sodium bismuthate base (bismuth hydroxide is bismuth source) activated carbon fiber-loaded bismuth with methyl orange referring to attached drawing 7 Sour sodium adsoption catalysis paper material is to its degradation effect, and according to the effect of degradation, to sodium bismuthate base (bismuth hydroxide is bismuth source) The preparation process of activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is adjusted correspondingly.
Embodiment three
Activated carbon fiber-loaded sodium bismuthate adsoption catalysis material is prepared by bismuth source of bismuth nitrate
1, the preparation of activated carbon fibre
The cotton fabric (CW) for weighing 300-400 g is placed in the boric acid solution that mass percent concentration is 80%, is made in mixture Quality-concentration expressed in percentage by volume of solid is 15%(w/v), after stirring 4-7 minute, aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution.It will be dry in 70 DEG C -90 DEG C of baking oven by pretreated cotton fabric (PCW) It 20-26 hours, then releases and cools down 11-15 hours at ambient temperature, cooling cotton fabric (PCW) is immersed at room temperature (the NH that mass percent concentration is 7.5%4)2HPO42-4 hours in solution, is then extracted at 70 DEG C -80 DEG C and dry 20- It 26 hours, after being cooled to environment temperature, is transferred into aluminium oxide boat and is put into Muffle furnace, use N2Make protective gas, Flow velocity is 600 mL/min, is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, heat preservation 30 60min is carbonized;Then it is heated to 700-800 DEG C with the rate of 10 DEG C/min, in CO2Under atmosphere keep 30-60min into Row activation, flow velocity 0.5L/min.In N2It flows down after being naturally cooling to 300 DEG C, product is taken out from furnace and is cooled to environment Then temperature is washed with distilled water to pH most 7-7.2, finally 20-26 hours dry at 70 DEG C -90 DEG C, obtains active carbon Fiber (ACF).
2, the preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g active carbon fibre Ultrasonic disperse is tieed up into sodium hydroxide solution, 3 DEG C -10 DEG C is cooled to ice water, is passed through chlorine under stiring and reaches saturation, then The sodium hydroxide of 10-15 g is added, controls temperature at 10 DEG C -20 DEG C, by the mixture of the crystal of precipitation and activated carbon fibre Separation filters, and obtains the sodium hypochlorite that activated carbon fiber tentatively loads;Using bismuth nitrate as bismuth source, under vigorous stirring by bismuth nitrate It is repeatedly added in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads on a small quantity, 20-30 DEG C of temperature control, ultrasonic reaction 60- 80 minutes, the sodium bismuthate precipitating of yellow is obtained, its stratification is eluted with the sodium hydroxide that mass percent concentration is 1%, It is 24-30 hours dry in vacuum oven again after filtering, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
3, sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic contamination The adsorption assessment of object (methyl orange):
It is absorption object with methyl orange referring to attached drawing 8, research sodium bismuthate based active carbon fiber loads sodium bismuthate adsoption catalysis paper wood Expect the adsorption effect to it, and according to the effect of absorption, phase is carried out to the preparation process of sodium bismuthate base visible light catalytic paper material The adjustment answered.
4, sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic contamination The degradation of object (methyl orange) is evaluated:
It is degradation object, research sodium bismuthate base (bismuth nitrate is bismuth source) activated carbon fiber-loaded bismuthic acid with methyl orange referring to attached drawing 9 Sodium adsoption catalysis paper material is to its degradation effect, and according to the effect of degradation, to sodium bismuthate base (bismuth nitrate is bismuth source) activity The preparation process of Carbon fibe load sodium bismuthate adsoption catalysis paper material is adjusted correspondingly.
Example IV
Sodium bismuthate base visible light catalytic paper material is prepared by bismuth source of bismuth hydroxide
1, the preparation of activated carbon fibre
The cotton fabric (CW) for weighing 300-400 g is placed in the formic solutions that mass percent concentration is 90%, is made in mixture Quality-concentration expressed in percentage by volume of solid is 25%(w/v), after stirring 4-7 minute, aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution.It will be dry in 70 DEG C -90 DEG C of baking oven by pretreated cotton fabric (PCW) It 20-26 hours, then releases and cools down 11-15 hours at ambient temperature, cooling cotton fabric (PCW) is immersed at room temperature (the NH that mass percent concentration is 7.5%4)2HPO42-4 hours in solution (7.5%), then extracted simultaneously at 70 DEG C -90 DEG C It is 20-26 hours dry, after being cooled to environment temperature, it is transferred into aluminium oxide boat and is put into Muffle furnace.Use N2Go bail for Gas is protected, flow velocity is 600 mL/min, is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, heat preservation It is carbonized within 30 60 minutes.Then it is heated to 700-800 DEG C with the rate of 10 DEG C/min, in CO230-60 is kept under atmosphere Minute is activated, and flow velocity is 0.5 L/min.In N2It flows down after being naturally cooling to 300 DEG C, product is taken out and cooled down from furnace To environment temperature.Then being washed with distilled water to pH value is 7-7.2, finally, it is 20-26 hours dry at 70 DEG C -80 DEG C, it is lived Property Carbon fibe (ACF).
2, the preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g active carbon fibre Ultrasonic disperse is tieed up into sodium hydroxide solution, 3 DEG C -10 DEG C is cooled to ice water, is passed through chlorine under stiring and reaches saturation, so The sodium hydroxide of 10-15 g is added afterwards, controls temperature at 10 DEG C -20 DEG C, by the mixing of the crystal of precipitation and activated carbon fibre Object separation filters, and obtains the sodium hypochlorite that activated carbon fiber tentatively loads;Using bismuth hydroxide as bismuth source, under vigorous stirring by hydrogen Bismuth oxide is repeatedly added on a small quantity in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads, and 20-30 DEG C of temperature control, ultrasound is anti- It answers 60-80 minutes, obtains the sodium bismuthate precipitating of yellow, by its stratification, the sodium hydroxide for being 1% with mass percent concentration Elution, it is 24-30 hours dry in vacuum oven again after filtering, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
3, sodium bismuthate base (bismuth hydroxide is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic dirt Contaminate the adsorption assessment of object (methyl orange):
It is absorption object with methyl orange referring to attached drawing 10, research sodium bismuthate based active carbon fiber loads sodium bismuthate adsoption catalysis paper Material loads sodium bismuthate adsoption catalysis paper to sodium bismuthate based active carbon fiber to its adsorption effect, and according to the effect of absorption The preparation process of material is adjusted correspondingly.
4, sodium bismuthate base (bismuth hydroxide is bismuth source) activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is to organic dirt Contaminate the degradation evaluation of object (methyl orange):
It is degradation object with methyl orange referring to attached drawing 11, research sodium bismuthate base (bismuth hydroxide is bismuth source) is activated carbon fiber-loaded Sodium bismuthate adsoption catalysis paper material is to its degradation effect, and according to the effect of degradation, and to sodium bismuthate base, (bismuth hydroxide is bismuth Source) preparation process of activated carbon fiber-loaded sodium bismuthate adsoption catalysis paper material is adjusted correspondingly.
All features disclosed in this specification or disclosed all methods, step and volume, in addition to mutually exclusive spy Other than sign and/or step, volume, it can combine in any way.Disclosed in this specification (including claim, abstract) Any feature can be replaced by other alternative features that are equivalent or have similar purpose unless specifically stated.It is i.e. unless special It does not describe, each feature is an example in a series of equivalent or similar characteristics.
Described above is only the non-limiting embodiment of invention, a large amount of embodiment can also be derived, for this field Those of ordinary skill for, not departing from the invention design and under the premise of do not make creative work, can also do The embodiment of several modifications and improvements out, these are all within the scope of protection of the present invention.

Claims (5)

1. a kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material, it is characterised in that: the preparation side Method carries out as follows:
(1) preparation of activated carbon fibre
The cotton fabric for weighing solid 300-400 g is placed in the acid solution that mass percent concentration is 60-80%, is made solid in mixture Quality-concentration expressed in percentage by volume of body is 5-25%(w/v), is stirred, 4-7 minute, after aging 1-2 hours, is drawn off and with steaming Distilled water is washed for several times to remove residual solution, by by pretreated cotton fabric, dry 20-26 is small in 70 DEG C -90 DEG C of baking oven When, it then releases and cools down 11-15 hours at ambient temperature, it is dense that cooling cotton fabric is immersed into mass percent at room temperature (the NH that degree is 7.5%4)2HPO42-4 hours in solution, then extracts and dry 20-26 hours at 70 DEG C -90 DEG C, be cooled to After environment temperature, it is transferred into aluminium oxide boat and is put into Muffle furnace, use N2As protective gas, flow velocity 600 ML/min is heated up with the speed of 5 DEG C/min, and temperature rises to 500 800 DEG C from 25 DEG C, keeps the temperature 30 60 minutes progress carbon Change, then 700-800 DEG C is heated to the rate of 10 DEG C/min, in CO2It keeps being activated for 30-60 minutes under atmosphere, flow velocity For 0.5L/min, in N2It flows down after being naturally cooling to 300 DEG C, product is taken out to from furnace and is cooled to environment temperature, is then used Distilling water washing to pH value is 7-7.2, finally 20-26 hours dry at 70 DEG C -90 DEG C, obtains activated carbon fibre (ACF);
(2) preparation of activated carbon fiber-loaded sodium bismuthate
Sodium hypochlorite is prepared first, and the solid sodium hydroxide for weighing 10-20 g is dissolved in the water, then weighs 2-6g step (1) and obtain The activated carbon fibre ultrasonic disperse obtained is cooled to 3 DEG C -10 DEG C with ice water, is passed through chlorine under stiring into sodium hydroxide solution Reach saturation, then add the solid sodium hydroxide of 10-15 g, control temperature at 10 DEG C -20 DEG C, by the crystal of precipitation and The mixture of activated carbon fibre, which separates, to be filtered, and the sodium hypochlorite that activated carbon fiber tentatively loads is obtained;Under vigorous stirring by bismuth Source is repeatedly added on a small quantity in the sodium hypochlorite mixing test solution that activated carbon fibre tentatively loads, and 20-30 DEG C of temperature control, ultrasonic reaction 60-80 minutes, the sodium bismuthate precipitating of yellow is obtained, its stratification is drenched with the sodium hydroxide that mass percent concentration is 1% It washes, it is 24-30 hours dry in vacuum oven again after filtering, obtain the finished product of activated carbon fiber-loaded sodium bismuthate.
2. the preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material according to claim 1, feature exist It is that sulfuric acid solution, boric acid solution, acetum, formic solutions, nitric acid solution, hydrochloric acid are molten in: acid solution in the step (1) Any one in liquid.
3. the preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material according to claim 1, feature exist In: the ultrasonic power in the step (2) is carried out using ultrasound-in situ synthesis.
4. the preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material according to claim 1, feature exist In: the activated carbon fiber-loaded sodium bismuthate in the step (2) uses bismuth source and activated carbon fibre for raw material.
5. the preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material according to claim 1, feature exist In: the bismuth source in the step (2) uses Bi (NO3)3, Bi (OH)3For raw material.
CN201810687286.3A 2018-06-28 2018-06-28 A kind of preparation method of activated carbon fiber-loaded sodium bismuthate adsoption catalysis material Pending CN108940196A (en)

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Application publication date: 20181207