CN109205670B - Inorganic fibrous bismuth compound and application thereof - Google Patents
Inorganic fibrous bismuth compound and application thereof Download PDFInfo
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Abstract
The invention discloses an inorganic fibrous bismuth compound and application thereof, wherein bismuth oxide powder is used as a raw material to be treated in a hydrothermal system, and the degree of order and the phase composition of a fiber product are regulated and controlled by regulating the types and the dosage of additives and surfactants in the hydrothermal system, so that a nano-ordered inorganic fibrous bismuth compound is obtained. The inorganic fiber bismuth compound is used for preparing the hydrocolloid, the preparation process is simple, the reaction temperature is low, and the obtained hydrocolloid is uniform in component and has good stability.
Description
Technical Field
The invention belongs to the technical field of inorganic bismuth compounds, and relates to an inorganic ordered fibrous bismuth compound and application thereof.
Background
Bismuth is the most important stable metal element in the periodic table of elements, has special physicochemical properties, is nontoxic and non-cancerous, and is called as a green metal. Thus, bismuth compounds, particularly inorganic bismuth compounds such as bismuth oxide, bismuth subcarbonate, bismuth subnitrate, bismuth oxysulfate, bismuth oxychloride, and various salts of oxyacids such as bismuth vanadate, bismuth tungstate, bismuth oxybromide, bismuth phosphate, bismuth niobate, and the like, are also widely used in various industries. Such as bismuth oxide, is one of the most important bismuth compounds, the main source of which is the by-product of copper or lead smelting. Bismuth oxide can be reduced to metallic bismuth by hydrogen and can also be used for preparing other ternary bismuth compounds. The bismuth oxide is mainly used for electronic ceramic powder materials, electrolyte materials, photoelectric materials, high-temperature superconducting materials, catalysts, chemical fiber flame retardants, additives of environment-friendly batteries and the like. Bismuth subcarbonate is used as an astringent, an antidiarrheal, an X-ray diagnostic opacifier in the pharmaceutical industry, an enamel flux, a glaze additive in the ceramic industry, and also as an antibacterial material and a photocatalytic material. Bismuth oxychloride is a novel high-grade environment-friendly pearlescent material, is insoluble in water, non-toxic, low in oil absorption and strong in skin adhesion, and is an important raw material in cosmetics. In addition, bismuth oxychloride can be widely used as an astringent, a preservative, and a pigment for automobile interior materials, electronic devices, sporting goods, furniture paints, and the like. Bismuth vanadate is widely used as a coloring agent for foods, toys, automotive finishes, coatings and the like because of its non-toxic and high environmental protection properties, and is also a novel photocatalytic material.
In conclusion, the bismuth compound needs to be compounded with other components in practical use. Because various bismuth compounds have large molecular weight and large density (such as 8.9 relative density of alpha-bismuth oxide, 8.55 relative density of beta-bismuth oxide, 6.86 relative density of bismuth subcarbonate and 7.72 relative density of bismuth oxychloride), are insoluble in water, are easy to settle and layer when applied in a colloid form, and are difficult to realize uniform dispersion and stably exist in a colloid system. The nano-crystallization and surface modification are effective methods for solving the problems, the geometric dimension of bismuth compound powder is reduced to be less than 100nm by various chemical or physical methods, such as nano-fiber, nano-sheet, spherical nano-powder and the like, hydrophobic powder is obtained by reaction surface modification, stable inorganic colloid is obtained by grinding the powder after surface modification into particles through colloid, and the process is used for preparing spherical and spheroidal baseThe nano particle aggregate has good effect; however, the process cannot obtain effective stable colloid for the disordered and aggregated fibrous bismuth compound, and the reason is that the shearing action of the colloid mill cannot open the disordered fiber aggregate to obtain monodisperse nano fibers. Literature (template-free hydrothermal preparation of Bi)24O31Cl10Nanofibers, mining engineering, 2017,37: 113-.
Aiming at the problems, micron-grade submicron bismuth oxide powder is treated in a hydrothermal system with synergistic action of inorganic ions and a surfactant, the bismuth oxide powder is converted into ordered nano fibers, the bulk density is reduced, the ordered nano fibers are compounded and dispersed in deionized water with a dispersing agent, and a uniformly distributed and stable single fiber bismuth compound colloid system is obtained after ultrasonic shearing dispersion or high-speed shearing dispersion.
Disclosure of Invention
In order to solve the problems that the disordered fiber bismuth compound in the prior art has high density and is difficult to shear and dissociate to obtain uniformly dispersed single fibers and stably exists in other systems, the invention aims to provide the inorganic fiber bismuth compound, which is obtained by performing hydrothermal treatment on bismuth oxide powder and orderly growing in the same direction under the synergistic effect of an additive and a surfactant in the hydrothermal treatment process.
The invention also aims to provide the application of the inorganic fibrous bismuth compound, which is to uniformly disperse the ordered inorganic fibrous bismuth compound in the aqueous solution to form a stable aqueous colloid, wherein the inorganic fibrous bismuth compound is in a single fiber dispersion state in the colloid, the size distribution is uniform, the aqueous colloid can be stably stored at room temperature, and the subsequent use process is nontoxic and pollution-free.
In order to achieve the technical purpose, the invention adopts the technical scheme that:
an inorganic fibrous bismuth compound prepared by the steps of:
(1) adding an additive and a surfactant into a solvent, adjusting the pH value to 1-5 with acid to obtain a solution A,
(2) adding bismuth oxide powder into the solution A to obtain suspension B;
(3) carrying out hydrothermal treatment on the suspension B to obtain a nano inorganic ordered fibrous bismuth compound;
the additive is selected according to the requirements of the chemical composition of the inorganic ordered fibrous bismuth compound; the concentration of the surfactant is 1.0-4.0 times of the critical micelle concentration of the surfactant. The ordered state of the fiber bismuth compound is obtained by controlling the ordered self-assembly characteristic when the concentration of the surfactant is greater than the critical micelle concentration.
Preferably, when the inorganic fibrous bismuth compound is bismuth oxychloride, the selected additive comprises at least one of an alkali metal chloride, ammonium chloride, an alkaline earth metal chloride;
preferably, when the inorganic fibrous bismuth compound is (BiO)2CO3The selected additive comprises a mixture of at least one of an alkali metal carbonate, ammonium bicarbonate, alkaline earth metal bicarbonate and at least one of an alkali metal chloride.
Preferably, when the inorganic fibrous bismuth compound is Bi2O3When selected, the additive comprises a mixture of at least one of an alkali metal chloride, an alkaline earth metal chloride, and at least one of an alkali metal sulfate, ammonium sulfate, and an alkaline earth metal sulfate.
Preferably, when the inorganic fibrous bismuth compound is bismuth oxysulfate, the selected additive comprises at least one of an alkali metal sulfate, ammonium sulfate, and an alkaline earth metal sulfate.
Preferably, when the inorganic fibrous bismuth compound is a metal bismuth oxoacid, the selected additives include: the metal oxyacid salt of an alkali metal, at least one of the metal oxyacids and at least one of the alkali metal chlorides, the metal in the metal oxyacid preferably comprising molybdenum, vanadium or tungsten.
Preferably, the surfactant in step (1) is at least one of an anionic surfactant, a cationic surfactant, a zwitterionic surfactant and a nonionic surfactant.
The cationic surfactant is preferably: C10-C18 alkyl quaternary ammonium salt surfactant.
The anionic surfactant is preferably: sodium C10-C18 alkylsulfonate.
The nonionic surfactant is preferably: at least one of PVP and polyvinyl alcohol.
The surfactant in the step (1) is preferably a cationic surfactant; further preferably, the surfactant is at least one of cetyltrimethylammonium chloride, tetradecyltrimethylammonium bromide, hexadecyltrimethylammonium hydroxide and dodecyltrimethylammonium chloride.
Preferably, the acid used in step (1) is an inorganic acid, such as hydrochloric acid, sulfuric acid or nitric acid; or an organic acid such as acetic acid. The pH value of the solution is adjusted mainly to adjust the reactivity of the powder.
Preferably, the particle size of the bismuth oxide powder in the step (2) is 0.1-50 μm, and the molar ratio of the bismuth oxide powder to the alkali metal ions, the alkaline earth metal ions or the ammonium ions is 1: 5-20.
Preferably, the solid content in the hydrothermal reaction in the step (2) is 10-150 g/L, the reaction temperature is 80-160 ℃, and the reaction time is 1-6 h.
Preferably, the inorganic fibrous bismuth compound is BiOCl or Bi4O5Cl2、Bi24O31Cl10、Bi3O4Cl、Bi12O17Cl2、(BiO)2SO4、Bi6S2O15、(BiO)2CO3、Bi2MoO6、BiVO4、Bi2WO6And Bi2O3At least one of the fibers.
The inorganic fibrous bismuth compound of the invention adopts bismuth oxide powder to carry out hydrothermal treatment, controls the variety and the dosage of inorganic salt additives and the dosage of surfactants to regulate the phase composition and the order degree of a fiber product, and orderly grows in the same direction under the synergistic action of the additives and the surfactants, thereby obtaining the nano-ordered inorganic fibrous bismuth compound.
The invention also provides application of the inorganic ordered fibrous bismuth compound, which is a stable aqueous colloid formed by uniformly dispersing the nano inorganic fibrous bismuth compound in an aqueous solution.
Preferably, a dispersing agent is added when the inorganic fibrous bismuth compound is uniformly dispersed, and the inorganic fibrous bismuth compound is in a single fiber dispersion state in a colloid, wherein the diameter of a single fiber is 30-50 nm. In the invention, the nano-ordered inorganic fibrous bismuth compound can realize single fiber dissociation after being dispersed, and is in a single fiber dispersion state.
Preferably, the inorganic fiber bismuth compound aqueous colloid contains 5-25% of inorganic fiber bismuth compound by mass, 0.5-5% of dispersant by mass and the balance of deionized water.
Preferably, the dispersant is at least one of a nonionic surfactant, an amphoteric surfactant and an anionic surfactant.
Preferably, the dispersant is a nonionic surfactant: the method comprises the following steps: polyol fatty acid ester: octadecylamine, glyceric acid ester, sorbic acid ester and glycol acid ester; or polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, and the like.
The anionic surfactant is preferably: sodium oleate.
Preferably, when the inorganic fibrous bismuth compound is used for preparing the aqueous colloid, ultrasonic dispersion or high-speed mechanical stirring dispersion is adopted;
the high-speed mechanical stirring speed is 300-5000 rpm, and the stirring time is 0.5-5 h;
the ultrasonic dispersion frequency is 20-100 kHz, and the sound intensity is>10w/m2The dispersion time is 0.1-3 h.
Compared with the prior known technology, the inorganic fiber bismuth compound and the application thereof provided by the invention have the following advantages:
(1) according to the inorganic fibrous bismuth compound, bismuth oxide powder is subjected to hydrothermal treatment, and the phase composition of a fiber product is regulated and controlled by controlling the type and the amount of an inorganic salt additive; simultaneously adding a surfactant to ensure that the concentration of the surfactant is 1.0-4.0 times of the critical micelle concentration of the surfactant, spontaneously aggregating the non-polar end of the surfactant into a micelle or micelle, controlling the ordering of fiber arrangement through the self-assembly characteristic of the surfactant, and orderly growing in the same direction under the synergistic action of the additive and the surfactant to obtain the nano-ordered inorganic fibrous bismuth compound.
(2) The method comprises the steps of uniformly dispersing an ordered inorganic fibrous bismuth compound in an aqueous solution under the action of a dispersing agent to form a stable aqueous colloid, wherein the inorganic fibrous bismuth compound is in a single-fiber dispersion state in the colloid, the diameter of a single fiber is 30-50nm, the size distribution is uniform, and the aqueous colloid can be stably stored at room temperature for more than 15 days without layering and sedimentation.
(3) The preparation method of the hydrocolloid is simple, the production cost is low, the subsequent use process is nontoxic and pollution-free, and the hydrocolloid can be used in any aqueous system.
Drawings
FIG. 1: example 1 preparation of (BiO) by hydrothermal method after adding surfactant to critical micelle concentration of 0.9 times2CO3A nanofiber SEM photograph (a), and a heterogeneous system layered (c) photograph thereof; ordered (BiO) preparation by hydrothermal method after adding surfactant to exceed critical micelle concentration by 2.52 times2CO3Nanofiber SEM photograph (b) and colloid thereof (d);
FIG. 2: example 2 preparation of Bi by hydrothermal method after adding surfactant to critical micelle concentration of 0.75 times2O3A nanofiber SEM photograph (a), and a heterogeneous system layered (c) photograph thereof; ordered Bi prepared by hydrothermal method after adding surfactant to exceed critical micelle concentration by 1.68 times2O3Nanofiber SEM photograph (b) and colloid thereof (d);
FIG. 3: in example 3, a surfactant is added to the critical micelle concentration of the bismuth oxychloride nanofiber with the concentration of 0.82 times, and then a bismuth oxychloride nanofiber SEM picture (a) and a heterogeneous system layering (c) picture are prepared by a hydrothermal method; and (b) preparing an ordered bismuth oxychloride nanofiber SEM photo (b) and colloid (d) thereof by a hydrothermal method after adding a surfactant to exceed the critical micelle concentration of the bismuth oxychloride nanofiber by 3.65 times.
Detailed Description
To further illustrate the content of the present invention, the present invention will be further described with reference to the following examples.
Example 1
The preparation method of the ordered bismuth compound fiber and the colloid thereof of the embodiment comprises the following specific steps:
(1) 8.8g NaCl and 1.6g Na were added2CO3Dissolved in 70mL of a solution containing 1.26g of cetyltrimethylammonium chloride (critical micelle concentration 1.6X 10)-2mol/L) of the mixture in deionized water, the concentration of the surfactant is 2.52 times of the critical micelle concentration, 1M HCl solution is used for adjusting the pH to 3, and 7g of Bi with the median diameter of 15 mu M is added2O3Heating the powder in a hydrothermal kettle to 140 ℃, preserving heat for 4h, cooling, and washing for 2 times by using deionized water to obtain the ordered bismuth subcarbonate nanofiber.
(2) 0.5g of octadecylamine was dissolved in 5mL of ethanol to obtain an octadecylamine ethanol solution.
(3) Prepared by the above method (BiO)2CO3The nanofibers were treated with octadecyl ammonium ethanol solution and redispersed in 70mL deionized water containing 1.5g glyceryl oleate, then 0.4g sodium oleate was added and dispersed by sonication for 20min to give a uniformly dispersed (BiO)2CO3The diameter of a single fiber of the nanofiber hydrocolloid is 30-50nm, the ultrasonic frequency is 90kHz, and the sound intensity is 15w/m2(ii) a The dispersing time is 2 h. Ordered (BiO) after adding the surfactant to exceed the critical micelle concentration by 2.52 times2CO3The photograph of the heterogeneous system layering (c) after nanofiber colloid (d) and addition of surfactant to its critical micelle concentration of 0.9 times is shown in fig. 1. (d) The aqueous colloid in (A) can be stably stored for more than 15 days at room temperature without layering and sedimentation.
Example 2
The preparation method of the ordered bismuth compound fiber and the colloid thereof of the embodiment comprises the following specific steps:
(1) 3.65g of KCl and 7.6g K were weighed2SO4Dissolved in 70mL potassium oleate (critical micelle concentration 4.5X 10)- 3mol/L)0.17g of deionized water, the concentration of the surfactant is 1.68 times of the critical micelle concentrationReuse H2SO4(1.0M) to adjust the pH to 2.0-3.0, and 5g of Bi having a median diameter of 2 μ M was added2O3Magnetically stirring the powder at room temperature for 5min, transferring into a polytetrafluoroethylene reaction kettle, stirring and crystallizing at 140 ℃ for 4 h;
(2) 0.5g of octadecylamine was dissolved in 5mL of ethanol to obtain an octadecylamine ethanol solution.
(3) Washing the hydrothermal product with deionized water for 3 times, treating the product with an octadecylamine ethanol solution, dispersing the product in 70mL of deionized water again, adding 1g of glycol acid ester and 0.5g of sodium oleate, performing high-speed mechanical dispersion at a stirring speed of 3000rpm for 2 hours to obtain uniformly and stably dispersed Bi2O3The nanofiber hydrocolloid has a single fiber diameter of 30-50 nm. Ordered Bi after adding a surfactant to exceed the critical micelle concentration by 1.68 times2O3The photograph of the heterogeneous system layering (c) after the nanofiber colloid (d) and the added surfactant reach 0.75 times their critical micelle concentration is shown in fig. 2. (d) The aqueous colloid in (A) can be stably stored for more than 15 days at room temperature without layering and sedimentation.
Example 3
The preparation method of the ordered fiber bismuth compound and the colloid thereof comprises the following specific steps:
(1) 13.2g NaCl was dissolved in 70mL of a solution containing dodecyltrimethylammonium chloride (critical micelle concentration 1.6X 10)- 2mol/L)1.08g of deionized water, the concentration of the surfactant is 3.65 times of the critical micelle concentration, 1M HCl solution is used for adjusting the pH to 3, and 7g of Bi with the median diameter of 0.5 mu M is added2O3Heating the powder in a hydrothermal kettle to 160 ℃, preserving the heat for 2 hours, cooling, and washing for 2 times by using deionized water to obtain the bismuth oxychloride nanofiber.
(2) 0.5g of octadecylamine was dissolved in 5mL of ethanol to obtain an octadecylamine ethanol solution.
(3) Treating the bismuth oxychloride nano-fiber by using an octadecyl ammonium ethanol solution, adding the treated bismuth oxychloride nano-fiber into deionized water, adding 1g of polyvinyl alcohol and 0.5g of sodium oleate, and performing ultrasonic dispersion for 25min to obtain a bismuth oxychloride nano-fiber hydrocolloid, wherein the diameter of a single fiber is 30-50nm, the ultrasonic frequency is 90kHz, and the sound intensity is 11w/m2(ii) a Time of dispersionAnd 3 h. The photographs of the ordered bismuth oxychloride nanofiber colloid (d) after the addition of the surfactant exceeding the critical micelle concentration by 3.65 times and the multiphase system layered (c) after the addition of the surfactant reaching the critical micelle concentration by 0.82 time are shown in fig. 3. (d) The aqueous colloid in (A) can be stably stored for more than 15 days at room temperature without layering and sedimentation.
Example 4
The preparation method of the ordered fiber bismuth compound and the colloid thereof comprises the following specific steps:
(1) 13.65g of Na2SO4Dissolving in 70mL solution containing sodium hexadecylsulfonate (critical micelle concentration 5.8X 10)-4mol/L)0.04g of deionized water, the concentration of the surfactant is 3.0 times of the critical micelle concentration, 0.5M H is used2SO4The pH of the solution was adjusted to 3, and 7g of Bi having a median diameter of 0.5 μm were added2O3Heating the powder in a hydrothermal kettle to 90 ℃, preserving heat for 4h, cooling, and washing for 2 times by using deionized water to obtain the ordered bismuth oxysulfate nanofiber.
(2) 0.5g of octadecylamine was dissolved in 5mL of ethanol to obtain an octadecylamine ethanol solution.
(3) Treating the bismuth oxysulfate nanofiber with an ethanol solution of octadecylamine, adding into deionized water, adding 0.85g of polyethylene glycol, and performing ultrasonic dispersion for 25min to obtain bismuth oxysulfate nanofiber hydrocolloid, wherein the diameter of a single fiber is 20-50nm, the ultrasonic frequency is 50kHz, and the sound intensity is 15w/m2(ii) a The dispersing time is 3 h. The obtained hydrocolloid can be stably stored at room temperature for more than 15 days without layering and sedimentation.
Example 5
The preparation method of the ordered fiber bismuth compound and the colloid thereof comprises the following specific steps:
(1) 11.53g NaCl was dissolved in 70mL sodium tungstate 4.17g, sodium dodecylsulfate (critical micelle concentration 9.0X 10)-3mol/L)0.4g of deionized water, the surfactant concentration being 2.33 times its critical micelle concentration, 0.5M H2SO4The pH of the solution was adjusted to 3, and 7g of Bi having a median diameter of 0.5 μm were added2O3Heating the powder in a hydrothermal kettle to 100 deg.C, keeping the temperature for 2h, cooling, and usingAnd washing with ions for 2 times to obtain the ordered bismuth tungstate nanofiber.
(2) 0.5g of octadecylamine was dissolved in 5mL of ethanol to obtain an octadecylamine ethanol solution.
(3) And (2) treating the bismuth tungstate nanofiber by using an octadecyl ammonium ethanol solution, adding the treated bismuth tungstate nanofiber into deionized water, adding 1.2g of polyvinylpyrrolidone, and performing high-speed mechanical dispersion at a stirring speed of 5000rpm for 4 hours to obtain a bismuth tungstate nanofiber hydrocolloid with a single fiber diameter of 30-50 nm. The obtained hydrocolloid can be stably stored at room temperature for more than 15 days without layering and sedimentation.
Claims (8)
1. An inorganic fibrous bismuth compound characterized in that: is prepared by the following steps:
(1) adding an additive and a surfactant into a solvent, adjusting the pH value to 1-5 with acid to obtain a solution A,
(2) adding bismuth oxide powder into the solution A to obtain suspension B;
(3) carrying out hydrothermal treatment on the suspension B to obtain a nano inorganic fibrous bismuth compound;
the additive is selected according to the requirement of chemical composition of the inorganic fibrous bismuth compound; the concentration of the surfactant is 1.0-4.0 times of the critical micelle concentration of the surfactant;
when the inorganic fibrous bismuth compound is bismuth oxychloride, the selected additive comprises at least one of alkali metal chloride, ammonium chloride, and alkaline earth metal chloride;
when the inorganic fibrous bismuth compound is (BiO)2CO3The selected additives include a mixture of at least one of an alkali metal carbonate, ammonium bicarbonate, alkaline earth metal bicarbonate and at least one of an alkali metal chloride;
when the inorganic fibrous bismuth compound is Bi2O3When the additive is selected, the selected additive comprises a mixture of at least one of alkali metal chloride and alkaline earth metal chloride and at least one of alkali metal sulfate, ammonium sulfate and alkaline earth metal sulfate;
when the inorganic fibrous bismuth compound is bismuth oxysulfate, the selected additive comprises at least one of alkali metal sulfate, ammonium sulfate and alkaline earth metal sulfate;
when the inorganic fibrous bismuth compound is a metallic bismuth oxoacid, the additives selected include: at least one of metal oxyacid salts of alkali metals, metal ammonium oxyacid salts and at least one of alkali metal chlorides, wherein the metal in the metal oxyacid salts comprises molybdenum, vanadium or tungsten;
the surfactant is at least one of an anionic surfactant, a cationic surfactant, a zwitterionic surfactant or a nonionic surfactant; the cationic surfactant is quaternary ammonium salt surfactant with C10-C18 alkyl; the anionic surfactant is C10-C18 sodium alkylsulfonate; the nonionic surfactant is at least one of PVP and polyvinyl alcohol.
2. The inorganic fibrous bismuth compound according to claim 1, characterized in that: the particle size of the raw material bismuth oxide powder is 0.1-50 mu m, and the molar ratio of the bismuth oxide powder to alkali metal ions or alkaline earth metal ions or ammonium ions is 1:5 to 20.
3. The inorganic fibrous bismuth compound according to claim 1, characterized in that: the solid content in the hydrothermal reaction is 1-150 g/L, the reaction temperature is 80-160 ℃, and the reaction time is 1-6 h.
4. The inorganic fibrous bismuth compound according to any one of claims 1 to 3, wherein: the inorganic fibrous bismuth compound is BiOCl and Bi4O5Cl2、Bi24O31Cl10、Bi3O4Cl、Bi12O17Cl2、(BiO)2SO4、Bi6S2O15、(BiO)2CO3、Bi2MoO6、BiVO4、Bi2WO6And Bi2O3At least one of the fibers.
5. Use of the inorganic fibrous bismuth compound of any of claims 1 to 3, characterized in that: the nano inorganic fibrous bismuth compound is uniformly dispersed in the water solution to form stable aqueous colloid.
6. Use of the inorganic fibrous bismuth compound according to claim 5, characterized in that: after the dispersing agent is added when the inorganic fibrous bismuth compound is uniformly dispersed, the inorganic fibrous bismuth compound is in a single fiber dispersed state in the colloid, and the diameter of a single fiber is 30-50 nm.
7. Use of the inorganic fibrous bismuth compound according to claim 6, characterized in that: the mass content of the inorganic ordered fibrous bismuth compound in the aqueous colloid is 5-25%, and the mass content of the dispersing agent is 0.5-5%.
8. Use of the inorganic fibrous bismuth compound according to claim 6, characterized in that: the dispersant is at least one of nonionic surfactant, amphoteric surfactant and anionic surfactant.
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