CN113292472A - Recycling treatment method for dialkyl peroxide-white carbon black waste - Google Patents
Recycling treatment method for dialkyl peroxide-white carbon black waste Download PDFInfo
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- CN113292472A CN113292472A CN202110575399.6A CN202110575399A CN113292472A CN 113292472 A CN113292472 A CN 113292472A CN 202110575399 A CN202110575399 A CN 202110575399A CN 113292472 A CN113292472 A CN 113292472A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
- C07C407/003—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a recycling treatment method of dialkyl peroxide-white carbon black waste, belonging to the technical field of solid waste recycling. The dialkyl peroxide-white carbon black waste is mixed with a sodium hydroxide aqueous solution for salt forming reaction, and sodium hydroxide and silicon dioxide react to generate sodium silicate so that the white carbon black is decomposed and enters a water phase; then the salt-forming reaction product is stood, and oil-phase dialkyl peroxides in the salt-forming reaction product are separated from a water phase, so that the dialkyl peroxides are separated from an oil layer and can be used as recovered dialkyl peroxides to be applied to industrial production again; according to the invention, the pH value of the water layer is adjusted to 1-2 by using a hydrochloric acid solution, sodium silicate reacts with hydrochloric acid to generate silicon dioxide and the silicon dioxide is separated out to obtain a crude white carbon black product and a filtrate, wherein the filtrate contains sodium chloride. The results of the examples show that the purity of the recovered dialkyl peroxide obtained by the method provided by the invention is 95.6%.
Description
Technical Field
The invention relates to the technical field of solid waste recovery, in particular to a recycling method of dialkyl peroxide-white carbon black waste.
Background
Organic peroxides are widely used in chemical production. For example, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) -3-hexyne (hexyne bis "2, 5" vulcanizing agent for short), which is an important dialkyl organic peroxide, has high tensile strength and hardness and low elongation and compression set, is widely used as a high-temperature vulcanizing agent for vinyl rubber, a hardening agent for unsaturated polyester, and a vulcanizing agent for silicone rubber, fluororubber, urethane rubber, and ethylene-propylene rubber.
Because the dialkyl peroxides are active in chemical property, in actual production, the dialkyl peroxides are often prepared into dialkyl peroxide-white carbon black powder so as to be convenient for transportation, storage and use. In the preparation process of the dialkyl peroxide-white carbon black powder, the situation of leakage or pollution by mechanical impurities can exist, so that the product cannot be sold due to unqualified appearance. When the dialkyl peroxide-white carbon black powder is not stored properly, the powder is agglomerated and becomes unusable waste. The waste materials are flammable and explosive, and are easy to generate dust which is harmful to human bodies.
The dialkyl peroxide-white carbon black powder belongs to solid waste and cannot be directly discharged, but no effective recycling method for the dialkyl peroxide-white carbon black powder exists at present.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for recycling dialkyl peroxide-white carbon black waste. The method provided by the invention can effectively recycle the dialkyl peroxides in the waste materials to reduce the generation of solid wastes and reduce the environmental pollution.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a resource recycling method of dialkyl peroxide-white carbon black waste, which comprises the following steps:
(1) mixing dialkyl peroxide-white carbon black waste with a sodium hydroxide aqueous solution, and carrying out a salt forming reaction to obtain a salt forming reaction product;
(2) standing the salification reaction product, and separating an oil layer and a water layer, wherein the obtained oil layer contains recovered organic peroxide;
(3) and adjusting the pH value of the water layer to 1-2 by using a hydrochloric acid solution, and separating out solids to obtain a crude white carbon black product and a filtrate, wherein the filtrate contains sodium chloride.
Preferably, the method further comprises the following steps after obtaining the filtrate:
and adjusting the pH value of the filtrate to 5-7 by using a sodium hydroxide solution, and sequentially carrying out concentration and solid-liquid separation to obtain a sodium chloride solid and a saturated sodium chloride solution.
Preferably, the dialkyl peroxide and the white carbon black waste material contain, by mass, 55-65% of dialkyl peroxide and 35-45% of white carbon black.
Preferably, in the step (1), after the dialkyl peroxide-white carbon black waste is mixed with the aqueous solution of sodium hydroxide, the content of sodium hydroxide in the obtained mixture is 8.4-9 wt%.
Preferably, the mass concentration of the sodium hydroxide aqueous solution in the step (1) is 20-32%; the mass ratio of the dialkyl peroxide-white carbon black waste to the sodium hydroxide aqueous solution is 1: 3-4.
Preferably, the temperature of the salt forming reaction in the step (1) is 70-80 ℃, and the time is 15-30 min.
Preferably, the standing temperature in the step (2) is 20 ℃, and the standing time is 30-60 min.
Preferably, the solid-to-liquid ratio after concentration is 1: (0.5-2).
The invention provides a resource recycling method of dialkyl peroxide-white carbon black waste, which comprises the steps of mixing the dialkyl peroxide-white carbon black waste with a sodium hydroxide aqueous solution, carrying out a salt forming reaction, reacting sodium hydroxide with silicon dioxide to generate sodium silicate, and enabling the white carbon black to be decomposed and enter a water phase; then the salt-forming reaction product is stood, and oil-phase dialkyl peroxides in the salt-forming reaction product are separated from a water phase, so that the dialkyl peroxides are separated from an oil layer and can be used as recovered dialkyl peroxides to be applied to industrial production again; according to the invention, the pH value of the water layer is adjusted to 1-2 by using a hydrochloric acid solution, sodium silicate reacts with hydrochloric acid to generate silicon dioxide and the silicon dioxide is separated out to obtain a crude white carbon black product and a filtrate, wherein the filtrate contains sodium chloride. The results of the examples show that the purity of the recovered dialkyl peroxide obtained by the method provided by the invention is 95.6%.
Further, the pH value of the filtrate is adjusted to 5-7 by using a sodium hydroxide solution, and concentration and solid-liquid separation are sequentially carried out to obtain a sodium chloride solid and a saturated sodium chloride solution. The results of the examples show that the solid sodium chloride obtained by the invention has the purity of 98.9% and the whiteness of 82.3%, can be reused as industrial sodium chloride, and the obtained sodium chloride solution can be used for salt steaming.
The method provided by the invention can effectively carry out resource treatment on dialkyl peroxides and white carbon black in the waste material so as to reduce the generation of solid waste and reduce environmental pollution.
Detailed Description
The invention provides a resource recycling method of dialkyl peroxide-white carbon black waste, which comprises the following steps:
(1) mixing dialkyl peroxide-white carbon black waste with a sodium hydroxide aqueous solution, and carrying out a salt forming reaction to obtain a salt forming reaction product;
(2) standing the salification reaction product, and separating an oil layer and a water layer, wherein the obtained oil layer contains recovered organic peroxide;
(3) and adjusting the pH value of the water layer to 1-2 by using a hydrochloric acid solution, and separating out solids to obtain a crude white carbon black product and a filtrate, wherein the filtrate contains sodium chloride.
The dialkyl peroxide-white carbon black waste is mixed with a sodium hydroxide aqueous solution to carry out salt forming reaction, so as to obtain a salt forming reaction product. The present invention does not require any particular kind of dialkyl peroxide, and any dialkyl peroxide known to those skilled in the art may be used. In a specific embodiment of the present invention, the dialkyl peroxide is 2, 5-dimethyl-2, 5-bis (t-butylperoxy) -3-hexyne.
In the invention, the content of dialkyl peroxides in the dialkyl peroxide-white carbon black waste is preferably 55-65% by mass, and more preferably 60% by mass; the content of the white carbon black is preferably 35-45%, and more preferably 40%. The method has no special requirements on parameters such as particle size, viscosity and the like of the dialkyl peroxide-white carbon black waste, and the dialkyl peroxide-white carbon black waste with properties well known by the technical personnel in the field can be recycled by using the method provided by the invention.
The invention does not require any particular mixing means, such as stirring, known to the person skilled in the art. In the invention, after the dialkyl peroxide-white carbon black waste is mixed with the sodium hydroxide aqueous solution, the content of sodium hydroxide in the obtained mixture is preferably 8.4-9 wt%, and more preferably 8.6-8.8%. In the invention, the mass concentration of the sodium hydroxide aqueous solution is preferably 20-32%, and more preferably 25-30%; the mass ratio of the dialkyl peroxide-white carbon black waste to the sodium hydroxide aqueous solution is preferably 1: 3-4, and more preferably 1: 3.5.
In the invention, the temperature of the salt forming reaction is preferably 70-80 ℃, and more preferably 75 ℃; the time is preferably 15 to 30min, and more preferably 18 to 25 min.
After the salt-forming reaction product is obtained, the invention stands the salt-forming reaction product, separates an oil layer and a water layer, and the obtained oil layer contains recovered organic peroxide. In the invention, the standing temperature is preferably 20 ℃, and the standing time is preferably 30-60 min, and more preferably 40-50 min. In the present invention, the means for separating the oil layer and the water layer is preferably centrifugal separation, the rotation speed of the centrifugation is preferably 1000rpm, and the centrifugation time is preferably 10 min.
According to the invention, the pH value of the water layer is adjusted to 1-2 by using a hydrochloric acid solution, solid is precipitated, and a crude white carbon black product and a filtrate are obtained, wherein the filtrate contains sodium chloride. In the invention, the mass concentration of the hydrochloric acid solution is preferably 20-36%, and more preferably 25-30%. After the solid is precipitated, the solid-liquid mixture obtained is preferably filtered in the present invention.
After obtaining the filtrate, the invention also comprises: and adjusting the pH value of the filtrate to 5-7 by using a sodium hydroxide solution, and sequentially carrying out concentration and solid-liquid separation to obtain a sodium chloride solid and a saturated sodium chloride solution.
In the present invention, the solid-liquid mass ratio after the concentration is preferably 1: (0.5 to 2), more preferably 1: (1-1.5). In the present invention, the solid-liquid separation is preferably performed by centrifugation, the rotation speed of the centrifugation is preferably 1000rpm, and the centrifugation time is preferably 10 min.
After the sodium chloride solid is obtained, the obtained sodium chloride solid is preferably dried in the present invention. The present invention does not require special drying means, and sodium chloride is dried to a constant weight using drying means well known to those skilled in the art.
The following will explain the recycling method of dialkyl peroxide-white carbon black waste provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
389kg of water, 211kg of 32 wt% sodium hydroxide solution and 200kg of powdery waste are added into a 1000L reaction kettle, the mixture is uniformly mixed, a jacket is used for heating, when the temperature reaches 65 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 70 ℃, and the temperature is kept for 30min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 94.3%.
And then adding 36 wt% hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.2, separating out white solid, performing first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and filtrate, and recovering the crude white carbon black product.
And (3) adjusting the pH of the filtrate 1 obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-liquid ratio is 1: 0.5, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.3 percent and the whiteness of 80.2 percent.
Example 2
398kg of water, 215kg of 32 wt% sodium hydroxide solution and 175kg of powdery waste are added into a 1000L reaction kettle, after uniform mixing, a jacket is used for heating, when the temperature reaches 65 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 70 ℃, and the temperature is kept for 30min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 95.1%.
And then adding 36 wt% of hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.1 to separate out white solid, carrying out first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and filtrate, and recycling the crude white carbon black product.
Adjusting the pH of the filtrate obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-to-liquid ratio is 1: 1, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.6 percent and the whiteness of 80.8 percent.
Example 3
415kg of water, 225kg of 32 wt% sodium hydroxide solution and 160kg of powdery waste are added into a 1000L reaction kettle, after uniform mixing, a jacket is used for heating, when the temperature reaches 70 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 75 ℃, and the temperature is kept for 25min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 94.9%.
And then adding 36 wt% of hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.5 to separate out white solid, carrying out first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and filtrate, and recycling the crude white carbon black product.
Adjusting the pH of the filtrate obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-to-liquid ratio is 1: 2, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.5 percent and the whiteness of 81.3 percent.
Example 4
389kg of water, 211kg of 32 wt% sodium hydroxide solution and 200kg of powdery waste are added into a 1000L reaction kettle, the mixture is uniformly mixed, a jacket is used for heating, when the temperature reaches 75 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 80 ℃, and the temperature is kept for 15min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 95.3%.
And then adding 36 wt% hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.5, separating out white solid, performing first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and filtrate, and recovering the crude white carbon black product.
Adjusting the pH of the filtrate obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-to-liquid ratio is 1: 2, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.1 percent and the whiteness of 80.7 percent.
Example 5
398kg of water, 215kg of 32 wt% sodium hydroxide solution and 175kg of powdery waste are added into a 1000L reaction kettle, after uniform mixing, a jacket is used for heating, when the temperature reaches 65 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 70 ℃, and the temperature is kept for 30min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 95.6%.
And then adding 36 wt% of hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.6 to separate out white solid, carrying out first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and filtrate, and recycling the crude white carbon black product.
And (3) adjusting the pH of the filtrate 1 obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-liquid ratio is 1: 2, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.1 percent and the whiteness of 81.1 percent.
Example 6
415kg of water, 225kg of 32 wt% sodium hydroxide solution and 160kg of powdery waste are added into a 1000L reaction kettle, after uniform mixing, a jacket is used for heating, when the temperature reaches 70 ℃, the reaction starts to occur, the reaction releases heat, the reaction temperature is controlled to be 75 ℃, and the temperature is kept for 20min until the powdery waste is completely dissolved. Then cooling water in the reaction kettle is opened for cooling, the reaction liquid is cooled to 20 ℃, standing and layering are carried out, an oil layer and a water layer are obtained, the obtained oil layer is the recovered dialkyl peroxide, and the purity is 95.6%.
And then adding 36 wt% of hydrochloric acid into the water layer obtained by layering, adjusting the pH to 1.9 to separate out white solid, carrying out first centrifugal separation (the centrifugal speed is 1000rpm, and the centrifugal time is 10min) to obtain white solid which is a crude white carbon black product and a filtrate 1, and recycling the obtained crude white carbon black product.
And (3) adjusting the pH of the filtrate 1 obtained by centrifugation to 7 by using 32 wt% sodium hydroxide solution, and evaporating and concentrating the filtrate until the solid-liquid ratio is 1: 1, carrying out second centrifugal separation (the centrifugal speed is 1000rpm, the centrifugal time is 10min), and recycling the obtained liquid material which is a sodium chloride saturated solution for subsequent salt steaming; and drying the obtained solid material to obtain sodium chloride with the purity of 98.9 percent and the whiteness of 82.3 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A resource recycling treatment method of dialkyl peroxide-white carbon black waste comprises the following steps:
(1) mixing dialkyl peroxide-white carbon black waste with a sodium hydroxide aqueous solution, and carrying out a salt forming reaction to obtain a salt forming reaction product;
(2) standing the salification reaction product, and separating an oil layer and a water layer, wherein the obtained oil layer contains recovered organic peroxide;
(3) and adjusting the pH value of the water layer to 1-2 by using a hydrochloric acid solution, and separating out solids to obtain a crude white carbon black product and a filtrate, wherein the filtrate contains sodium chloride.
2. The recycling treatment method according to claim 1, further comprising, after obtaining the filtrate:
and adjusting the pH value of the filtrate to 5-7 by using a sodium hydroxide solution, and sequentially carrying out concentration and solid-liquid separation to obtain a sodium chloride solid and a saturated sodium chloride solution.
3. A resource recovery processing method according to claim 1 or 2, characterized in that the dialkyl peroxide and the white carbon black are contained in the dialkyl peroxide-white carbon black waste material in a mass percentage of 55-65% and 35-45%.
4. The resource recycling method according to claim 1 or 2, wherein in the step (1), after the dialkyl peroxide-white carbon black waste is mixed with the sodium hydroxide aqueous solution, the content of sodium hydroxide in the obtained mixture is 8.4-9 wt%.
5. A resource recovery processing method according to claim 1 or 2, characterized in that the mass concentration of the sodium hydroxide aqueous solution in the step (1) is 20-32%; the mass ratio of the dialkyl peroxide-white carbon black waste to the sodium hydroxide aqueous solution is 1: 3-4.
6. The method as claimed in claim 1, wherein the temperature of the salt forming reaction in step (1) is 70 to 80 ℃ for 15 to 30 min.
7. The resource recycling method according to claim 1, wherein the temperature of the standing in the step (2) is 20 ℃ and the time is 30-60 min.
8. The resource recovery processing method according to claim 2, wherein the solid-to-liquid ratio after concentration is 1: (0.5-2).
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