CN110449142B - Magnetic silicon dioxide porous adsorbent and preparation method and application thereof - Google Patents
Magnetic silicon dioxide porous adsorbent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a magnetic silicon dioxide porous adsorbent and a preparation method and application thereof. The preparation method of the magnetic silica porous adsorbent comprises the following steps: mixing silicon dioxide powder and an iron ion solution, adding a hot alkali solution at the temperature of 60-80 ℃, adjusting the pH value, fully reacting, cooling to room temperature, aging, washing to be neutral, drying and grinding to obtain the magnetic silicon dioxide porous adsorbent. According to the preparation method of the magnetic silica porous adsorbent, the inorganic silicon source silica powder is used as the raw material, so that the magnetic silica porous adsorbent is cheap and easy to obtain, is non-toxic and environment-friendly, does not generate related organic waste liquid in the preparation process, is environment-friendly, is synthesized by a surface deposition method in one step under a low-temperature condition, and is short in reaction time, low in energy consumption in the preparation process and low in cost. The magnetic silica porous adsorbent has good selectivity, the maximum adsorption amount to methylene blue is 121.23mg/g, and the maximum adsorption amount to malachite green is 163.52 mg/g.
Description
Technical Field
The invention relates to the technical field of printing and dyeing wastewater treatment, and particularly relates to a magnetic silica porous adsorbent and a preparation method and application thereof.
Background
The promulgation of ten items of water puts higher requirements on water pollution treatment, industrial wastewater is always closely concerned as a type of wastewater which is difficult to treat, printing and dyeing wastewater is a wastewater which accounts for a higher proportion of the total amount of industrial wastewater, and the printing and dyeing wastewater has high organic concentration, high chromaticity, stable chemical property and difficult biochemistry, and is industrial wastewater with high treatment difficulty. After the dyeing wastewater is subjected to physicochemical and biochemical treatment, the pollution index of the dyeing wastewater is greatly reduced, most of the dyeing wastewater can reach the emission standard, but the goal of realizing the pollution index by the conventional treatment method technology is more difficult along with the improvement of the standard emission. The adsorption method is favored in a plurality of technologies due to simple operation, low cost and high efficiency, and the selection of the adsorption material is the most critical in the adsorption method, so that the selection of an adsorption material with high efficiency, good selectivity and low cost is the decisive factor for determining the success of adsorption. The magnetic material has the advantages of strong magnetism, easy separation, reusability and the like, but the magnetic material has poor adsorption effect and adsorption selectivity. Silica is widely available on earth, is cheap and easy to obtain, is acid-base resistant and high in stability, and is a hotspot in the research field of adsorption materials by compounding silica and magnetic materials. Some new methods for preparing magnetic silica composite materials developed in recent years include a template method, a sol-gel method, a reverse microemulsion method and the like, and the methods are relatively complicated to prepare, take a long time and use a certain organic solvent, which may cause secondary pollution to the environment. For example, CN107583599A discloses a method for preparing, applying and regenerating a monodisperse mesoporous silica adsorbent, which is prepared by reacting CTAB, tee and TEOS and post-treating, and in the preparation process, the addition of organic substances causes the discharge of organic waste liquid, resulting in secondary pollution. What is desired in the art is a method for preparing an environment-friendly, easily synthesized and highly efficient silica magnetic adsorption material.
Disclosure of Invention
The invention aims to solve the technical problems of easy secondary pollution, poor adsorption treatment selectivity and low adsorption efficiency in the preparation process of the existing silicon dioxide magnetic adsorption material, and provides a preparation method of a magnetic silicon dioxide porous adsorbent.
The invention also aims to provide the magnetic silica porous adsorbent prepared by the method.
The invention also aims to provide application of the magnetic silica porous adsorbent in adsorption treatment of printing and dyeing wastewater.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of a magnetic silica porous adsorbent comprises the following steps: mixing silicon dioxide powder and an iron ion solution, adding a hot alkali solution at the temperature of 60-80 ℃, adjusting the pH to 10.00-12.00, cooling to room temperature after reaction, aging and washing to be neutral, drying and grinding to obtain the magnetic silicon dioxide porous adsorbent,
wherein the molar ratio of ferric iron to ferrous iron in the iron ion solution is 1.8-2.0: 1, the molar ratio of silicon dioxide powder to ferric iron is 1-3: 1, the reaction temperature is 60-80 ℃, and the reaction time is 60-120 min.
The pH value range and the reaction temperature of the invention not only influence the reaction but also influence the reaction generation speed.
The invention uses silicon dioxide powder as raw material for preparation, and the silicon dioxide powder as inorganic silicon source is nontoxic, cheap and easily available raw material. Meanwhile, the method adopts a surface deposition method, the magnetic silica porous high-efficiency adsorbent is synthesized by one-step reaction, no organic solvent is involved in the reaction process, the reaction process is carried out at low temperature, the reaction time is short, the energy consumption in the preparation process is low, the cost is low, and the method has the advantages of environmental protection. Meanwhile, the magnetic silica porous high-efficiency adsorbent prepared by the invention has magnetism, can rapidly carry out solid-liquid separation by utilizing a magnetic field, can desorb materials adsorbing dyes by using low-concentration acid, and has high recycling rate.
Wherein the molar ratio of the hot alkali to the ferric iron is preferably 8-9: 1.
Preferably, the molar ratio of the silicon dioxide powder to the ferric iron is 2-3: 1.
Preferably, the pH is adjusted to 11-12.
More preferably, the molar ratio of ferric and ferrous iron is 1.8:1, the molar ratio of silica powder to ferric iron is 2:1, the pH is adjusted to 11 and the reaction temperature is 60 ℃.
Also more preferably, the molar ratio of ferric and ferrous iron is 2:1, the molar ratio of silica powder to ferric iron is 3:1, the pH is adjusted to 12 and the reaction temperature is 80 ℃.
Preferably, the aging time is 1-3 h. Preferably 1 h.
The invention also protects the magnetic silicon dioxide porous adsorbent prepared by the preparation method.
The application of the magnetic silica porous adsorbent in adsorption removal of cationic dye in printing and dyeing wastewater is also within the protection scope of the invention.
The preferred cationic dyes adsorbed and removed by the magnetic silica porous adsorbent are methylene blue and malachite green.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a preparation method of a magnetic silicon dioxide porous adsorbent, which adopts inorganic silicon source silicon dioxide powder as a raw material, is cheap and easy to obtain, is non-toxic and environment-friendly, generates no related organic waste liquid in the preparation process, and is environment-friendly;
(2) the preparation method of the magnetic silicon dioxide porous adsorbent adopts a surface deposition method and one-step synthesis under a low temperature condition, and has the advantages of short reaction time, less energy consumption in the preparation process and low cost;
(3) the magnetic silica porous adsorbent has good selectivity, has higher adsorption capacity to cationic dyes, has the maximum adsorption capacity to methylene blue of 121.23mg/g, and has the maximum adsorption capacity to malachite green of 163.52 mg/g.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents used in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) 2.00g (0.005mol) of Fe was weighed out separately2(SO4)31.20g (0.02mol) of silicon dioxide powder and 1.40g (0.005mol) of FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 4. Firstly Fe2(SO4)3And twoAdding silicon oxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7H2O is stirred for a few minutes to completely dissolve the ferrous ions to obtain a mixed solution.
(2) 1.60g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, adjusting the pH value to 11, heating, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing and filtering until the pH value of the solution is neutral, drying for 12 hours at normal temperature in a vacuum drying oven, and grinding to obtain Fe 3+:SiO21:2 magnetic silica porous high efficiency adsorbents.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 1 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100 mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into every 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, and the calculation formula is as follows:
in the formula: qe is the adsorption capacity of the dye at equilibrium, mg/g; v is the wastewater volume, L; c0 is the initial concentration of dye, mg/L; ce is the equilibrium concentration of the dye, mg/L; m is the mass of the adsorbent, g.
The experimental result shows that the maximum adsorption capacity of the adsorbent to methylene blue is 115.20mg/g and the maximum adsorption capacity to malachite green is 151.50mg/g at 25 ℃.
Example 2
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) 2.00g (0.005mol) of Fe was weighed out separately2(SO4)31.20g (0.02mol) of silicon dioxide powder and 1.55g (0.0055mol) of FeSO 4·7H2O in molar ratio to Fe3+:Fe2+:SiO21.8:1: 3.6. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7H2Stirring for a few minutes to completely dissolve divalent iron ions to obtain a mixed solution.
(2) 1.6g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, adjusting the pH value to 11, heating, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing and filtering until the pH value of the solution is neutral, drying for 12 hours at normal temperature in a vacuum drying oven, and grinding to obtain the magnetic silica porous efficient adsorbent.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 2 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into each 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, the maximum adsorption capacity of the adsorbent to methylene blue is 121.23mg/g at 25 ℃, and the maximum adsorption capacity to malachite green is 163.52 mg/g.
Example 3
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) separately weighing Fe2(SO4)3Silicon dioxide powder and FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 3. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 70 deg.C, and adding FeSO4·7 H2O is stirred for a few minutes to completely dissolve the ferrous ions to obtain a mixed solution.
(2) 1.6g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, heating, adjusting the pH value to 11, controlling the temperature at 70 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing, filtering until the pH value of the solution is neutral, drying in a vacuum drying oven at normal temperature for 12 hours, and grinding to obtain the magnetic silica porous efficient adsorbent.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 3 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into each 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, the maximum adsorption capacity of the adsorbent to methylene blue is 108.61mg/g and the maximum adsorption capacity to malachite green is 141.30mg/g at 25 ℃.
Example 4
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) separately weighing Fe2(SO4)3Silicon dioxide powder and FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 6. Firstly Fe2(SO4)3And dioxygenAdding silicon oxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 80 deg.C, and adding FeSO4·7 H2O is stirred for a few minutes to completely dissolve the ferrous ions to obtain a mixed solution.
(2) 1.6g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, heating, adjusting the pH value to 12, controlling the temperature at 80 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing, filtering until the pH value of the solution is neutral, drying in a vacuum drying oven at normal temperature for 12 hours, and grinding to obtain the magnetic silica porous efficient adsorbent.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 3 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into each 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, and at 25 ℃, the maximum adsorption capacity of the adsorbent on methylene blue is 116.97mg/g, and the maximum adsorption capacity on malachite green is 155.06 mg/g.
Example 5
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) separately weighing Fe2(SO4)3Silicon dioxide powder and FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 2. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7 H2O stirring for a few minutes to separate ferrous ironAnd dissolving the seed completely to obtain a mixed solution.
(2) 1.6g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, heating, adjusting the pH value to 10, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing and filtering until the pH value of the solution is neutral, drying in a vacuum drying oven at normal temperature for 12 hours, and grinding to obtain the magnetic silica porous efficient adsorbent.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 3 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into each 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, the maximum adsorption capacity of the adsorbent to methylene blue is 96.59mg/g and the maximum adsorption capacity to malachite green is 114.85mg/g at 25 ℃.
Example 6
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) separately weighing Fe2(SO4)3Silicon dioxide powder and FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO21.8:1: 4.5. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7 H2O is stirred for a few minutes to completely dissolve the ferrous ions to obtain a mixed solution.
(2) 1.6g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, heating, adjusting the pH value to 11, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing, filtering until the pH value of the solution is neutral, drying in a vacuum drying oven at normal temperature for 12 hours, and grinding to obtain the magnetic silica porous efficient adsorbent.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 3 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the dye wastewater containing cations on dyes is measured. Preparing simulated wastewater with 10-100mg/L of dye solution, wherein the initial pH value of the wastewater sample is 6.00-7.00. In the experiment, 50mg of adsorbent is added into each 100mL of wastewater, the wastewater is magnetically separated after being oscillated for 2 hours at room temperature and at the rotating speed of 100-150 r/min, 2-3 mL of supernatant is taken, an ultraviolet spectrophotometer is adopted to measure the concentration of the residual dye solution in the solution and calculate the adsorption capacity, the maximum adsorption capacity of the adsorbent to methylene blue is 114.50mg/g at 25 ℃, and the maximum adsorption capacity to malachite green is 138.54 mg/g.
The embodiment shows that the preparation process is simple and convenient, the environment is protected, the cost is low, the obtained magnetic silica porous high-efficiency adsorbent has a good effect of adsorbing and removing cationic dyes, the adsorption capacity is high, and the magnetic silica porous high-efficiency adsorbent is a high-efficiency adsorbent for removing printing and dyeing wastewater and has a high use value in the market.
Comparative example 1
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) 2.00g (0.005mol) of Fe was weighed out separately2(SO4)31.20g (0.02mol) of silicon dioxide powder and 1.40g (0.005mol) of FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 4. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7H2Stirring for a few minutes to completely dissolve ferrous ions to obtain a mixed solution。
(2) 1.60g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, adjusting the pH value to 9, heating, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing, filtering until the pH value of the solution is neutral, drying for 12 hours at normal temperature in a vacuum drying oven, and grinding to obtain Fe 3+:SiO21:2 magnetic silica porous high efficiency adsorbents.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 1 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the adsorbent on the dyes is measured, wherein the maximum adsorption capacity of the adsorbent on methylene blue is 59.65mg/g and the maximum adsorption capacity on malachite green is 62.54mg/g at 25 ℃.
Comparative example 2
A preparation method of a magnetic silica porous adsorbent comprises the following steps:
(1) 2.00g (0.005mol) of Fe was weighed out separately2(SO4)31.20g (0.02mol) of silicon dioxide powder and 1.40g (0.005mol) of FeSO4·7H2O in molar ratio to Fe3+:Fe2+:SiO22:1: 4. Firstly Fe2(SO4)3Adding silicon dioxide powder into 100ml deionized water, ultrasonic dispersing for 10min, magnetically stirring to dissolve completely at 60 deg.C, and adding FeSO4·7H2O is stirred for a few minutes to completely dissolve the ferrous ions to obtain a mixed solution.
(2) 1.60g of sodium hydroxide was weighed and dissolved in 300ml of deionized water, and the temperature was controlled at 60 ℃ to serve as an alkali solution for the reaction.
(3) Slowly adding the mixed solution obtained in the step 1 into the alkali solution obtained in the step 2, continuously stirring after the mixed solution is added, adjusting the pH value to 13, heating, controlling the temperature at 60 ℃, reacting for 120 minutes, stopping heating, aging for 1 hour, washing and filtering until the pH value of the solution is neutral, Drying in a vacuum drying oven at normal temperature for 12 hours, and grinding to obtain Fe3+:SiO21:2 magnetic silica porous high efficiency adsorbents.
The magnetic silica powder porous high-efficiency adsorbent prepared in example 1 is used for treating dye wastewater containing cations simulated in a laboratory, and the adsorption performance of the adsorbent on the dyes is measured, wherein the maximum adsorption capacity of the adsorbent on methylene blue is 65.45mg/g and the maximum adsorption capacity on malachite green is 72.82mg/g at 25 ℃.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that other variations and modifications can be made on the basis of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (3)
1. The application of the magnetic silica porous adsorbent in adsorption removal of cationic dye in printing and dyeing wastewater is characterized in that the preparation method of the magnetic silica porous adsorbent comprises the following steps: mixing silicon dioxide powder and an iron ion solution, adding a hot alkali solution at the temperature of 60-80 ℃, adjusting the pH value to 11, fully reacting, cooling to room temperature, aging and washing to be neutral, drying and grinding to obtain the magnetic silicon dioxide porous adsorbent,
Wherein the molar ratio of ferric iron to ferrous iron in the iron ion solution is 2.0:1, the molar ratio of silicon dioxide powder to ferric iron is 2:1, the reaction temperature is 60 ℃, and the reaction time is 120 min.
2. Use according to claim 1, wherein the aging time is 1 to 3 hours.
3. The use of claim 1, wherein the cationic dyes are methylene blue and malachite green.
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