CN114031055A - Chlorination kettle cleaning process for phosphorus trichloride production - Google Patents
Chlorination kettle cleaning process for phosphorus trichloride production Download PDFInfo
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- CN114031055A CN114031055A CN202111310554.8A CN202111310554A CN114031055A CN 114031055 A CN114031055 A CN 114031055A CN 202111310554 A CN202111310554 A CN 202111310554A CN 114031055 A CN114031055 A CN 114031055A
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/0804—Cleaning containers having tubular shape, e.g. casks, barrels, drums
- B08B9/0817—Cleaning containers having tubular shape, e.g. casks, barrels, drums by agitating or tumbling containers filled with liquid or liquid and abrasive, e.g. chain
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Abstract
The invention relates to a cleaning process of a chlorination kettle for producing phosphorus trichloride, which belongs to the technical field of phosphorus trichloride production and comprises the following steps: step S1, after the chlorination kettle reaches a kettle cleaning condition, a reaction liquid port and a vacuumizing port are reserved, and the rest pipe ports are sealed by blind plates; step S2, dropwise adding a caustic soda aqueous solution into the chlorination kettle, vacuumizing the interior of the chlorination kettle by using a vacuumizing unit in the process of dropwise adding the caustic soda aqueous solution, and keeping the negative pressure in the reaction kettle to finish primary cleaning; step S3, discharging the substances in the chlorination kettle, removing the vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 0.5-1h, standing for 3-5h, discharging cleaning waste liquid, and finishing secondary cleaning; step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle; the cleaning process can reduce the generation of by-product acid in the kettle cleaning process, reduce the corrosion of equipment, prolong the service life of the reaction kettle, avoid the accumulation of hydrogen in the system and eliminate potential safety hazards.
Description
Technical Field
The invention belongs to the technical field of phosphorus trichloride production, and particularly relates to a cleaning process of a chlorination kettle for phosphorus trichloride production.
Background
Phosphorus trichloride is often used in the inorganic salt industryAn important product is also called phosphorus chloride, which is called phosphorus chloride for short. The molecular formula is as follows: PCl3Is colorless and transparent fuming liquid with pungent taste. Toxic and corrosive, can be dissolved in benzene, ether, chloroform, carbon disulfide and carbon tetrachloride, has strong reaction with water, and emits white smoke-shaped hydrogen chloride gas with irritation and corrosiveness. Phosphorus trichloride reacts with a plurality of organic matters to generate phosphate, which is a raw material for producing a plurality of organophosphorus pesticides, can be used for manufacturing pesticides dipterex, phosphorus sulfochloride, phosphorus oxychloride, phosphorous acid, phosphite ester and other phosphide, and can also be used as a chlorinating agent, a semiconductor doping source, a catalyst in ether analysis, the preparation of high-purity phosphorus and the like.
Phosphorus trichloride can be decomposed into hydrochloric acid and phosphoric acid when meeting water or deliquescing, other metals except nickel and lead are strongly corroded, and the metals are deteriorated to form inflammable hydrogen, so that a chlorination kettle for phosphorus trichloride production needs to be frequently cleaned to prevent the metals from being corroded and damaged.
Disclosure of Invention
The invention aims to provide a process for cleaning a chlorination kettle for producing phosphorus trichloride, which aims to solve the technical problems in the background.
The purpose of the invention can be realized by the following technical scheme:
a cleaning process of a chlorination kettle for phosphorus trichloride production comprises the following steps:
step S1, finishing the material treatment in the chlorination kettle, and leaving a reaction liquid port and a vacuumizing port after reaching the kettle cleaning condition, wherein the rest pipe ports are sealed by blind plates;
step S2, dropwise adding caustic soda aqueous solution into the chlorination kettle through the reaction solution port at the dropping speed of 0.5kg/h, removing HCl gas overflowing in the dropwise adding process by using a vacuum unit, setting absorption solution by using the vacuum unit, wherein the absorption solution is 35% by mass of sodium hydroxide solution, keeping the negative pressure in the reaction kettle, and finishing the primary cleaning;
s3, discharging the substances in the chlorination kettle, removing the vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 0.5-1h at the rotation speed of 200 plus 300rpm, standing for 3-5h, discharging the cleaning waste liquid, and finishing secondary cleaning;
and step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle.
Further, the weight fraction of the caustic soda aqueous solution is 10-15%.
Further, the cleaning agent comprises the following raw materials in parts by weight: 30-50 parts of distilled water, 10-15 parts of hydroxypropyl cellulose, 5-8 parts of sodium bicarbonate, 1-3 parts of modified bentonite and 1-5 parts of surfactant.
Further, the modified bentonite is prepared by the following steps:
step A1, adding 2-pyridylacetic acid, 1, 3-dibromopropane and n-butanol into a reaction kettle, heating to 70 ℃, stirring for 20min at the rotating speed of 60-100r/min, placing the reaction kettle into a microwave reactor, stirring for reaction for 6-8h at the microwave power of 900W and the reaction temperature of 140 ℃, removing the solvent by rotary evaporation after the reaction is finished, adding ethyl acetate into the rotary evaporation product while hot for dissolving and recrystallizing, performing suction filtration, washing a filter cake for 3-5 times by using acetone, and drying at the temperature of 75-80 ℃ to constant weight to obtain the gemini surfactant;
wherein the dosage ratio of the 2-pyridylacetic acid to the 1, 3-dibromopropane to the n-butanol is 0.2 mol: 0.1 mol: carrying out quaternization reaction on 60-80mL of 2-pyridylacetic acid and 1, 3-dibromopropane to obtain a gemini pyridine quaternary ammonium salt surfactant;
step A2, dispersing bentonite in deionized water, stirring for 30min, adding a magnesium chloride solution with the mass fraction of 20% under the protection of nitrogen, stirring and reacting for 2h in a water bath at 60 ℃, then heating to 75 ℃, adjusting the pH value to 10 by using a sodium hydroxide solution with the concentration of 5mol/L, continuously stirring for 1h, naturally cooling to room temperature, filtering, washing a filter cake for 3-5 times by using the deionized water, drying to constant weight at 60 ℃, and then calcining for 30-40min in a muffle furnace at 380-420 ℃ to obtain doped bentonite;
wherein the dosage ratio of the bentonite to the deionized water to the magnesium chloride solution is 5.0 g: 500 mL: 10-20mL, depositing a magnesium hydroxide compound on the surface of the bentonite by adopting a hydrothermal coprecipitation method, and calcining at high temperature to obtain the bentonite with magnesium oxide deposited on the surface, namely doped bentonite;
step A3, adding doped bentonite and deionized water into a three-neck flask, performing ultrasonic dispersion for 20min at the frequency of 40-50kHz, then adding dodecyl dimethyl betaine and gemini surfactant, heating to 40 ℃, stirring for reaction for 3h, filtering, washing a filter cake with deionized water for 3-5 times, drying at 60 ℃, and grinding and sieving with a 60-mesh sieve to obtain modified bentonite;
wherein the dosage ratio of the doped bentonite, the deionized water, the dodecyl dimethyl betaine and the gemini surfactant is 5.0 g: 500 mL: 0.5-0.8 g: 0.3-0.5 g; because the bentonite has excellent expansibility and has a layered structure and a larger specific area in water, the dodecyl dimethyl betaine and the gemini surfactant contain two hydrophilic functional groups of a hydrophobic carbon chain, a positive charge quaternary ammonium group and a negative charge carboxyl group, and are combined with the doped bentonite in an ion exchange action or electrostatic attraction way to obtain the modified bentonite.
Further, the surfactant is one or more of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene and fatty acid methyl ester polyoxyethylene mixed according to any proportion.
The invention has the beneficial effects that:
the invention provides a chlorinated kettle cleaning process for phosphorus trichloride production, which comprises three cleaning steps, wherein the chlorinated kettle is vacuumized, caustic soda solution is added dropwise to neutralize acid in a reaction kettle, and cleaning agent is added to remove organic impurities and phosphate in the chlorinated kettle, wherein the cleaning agent is characterized in that modified bentonite is added into the cleaning agent, the modified bentonite is a mixture of magnesium oxide deposited on the surface and dodecyl dimethyl betaine and a gemini surfactant on the surface, the bentonite has excellent expansibility, is of a layered structure and a large specific area in water, has a high adsorption effect on the phosphate after being doped with the magnesium oxide, and is mainly attributed that the magnesium oxide can generate a carboxylation reaction with-OH in an aqueous solution, presents different charge characteristics under different pH environments, and when the pH is less than 12, the magnesium oxide shows positive charges, can generate electrostatic adsorption with phosphates showing negative charges and form a mononuclear or polynuclear compound, and the surface of the modified bentonite contains quaternary ammonium groups with positive charges and carboxyl groups with negative charges, and can be combined with anions and cations in an aqueous solution through the electrostatic action, so that the kettle cleaning process is thorough, the generation of side acids in the kettle cleaning process can be reduced, the corrosion of equipment is reduced, the service life of a reaction kettle is prolonged, the accumulation of hydrogen in a system is avoided, and potential safety hazards are eliminated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow diagram of a cleaning process of a chlorination reactor for phosphorus trichloride production.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example provides a modified bentonite prepared by the following steps:
step A1, adding 0.2mol of 2-pyridylacetic acid, 0.1mol of 1, 3-dibromopropane and 60mL of n-butyl alcohol into a reaction kettle, heating to 70 ℃, stirring at the rotating speed of 60r/min for 20min, placing the reaction kettle into a microwave reactor, stirring and reacting at the microwave power of 900W and the reaction temperature of 140 ℃ for 6h, after the reaction is finished, removing the solvent by rotary evaporation, adding ethyl acetate into the rotary evaporation product while hot for dissolving and recrystallizing, performing suction filtration, washing a filter cake for 3 times by using acetone, and drying at 75 ℃ to constant weight to obtain the gemini surfactant;
step A2, dispersing 5.0g of bentonite in 500mL of deionized water, stirring for 30min, adding 10mL of magnesium chloride solution with the mass fraction of 20% under the protection of nitrogen, stirring for reaction for 2h in water bath at 60 ℃, then heating to 75 ℃, adjusting the pH value to 10 by using sodium hydroxide solution with the concentration of 5mol/L, continuously stirring for 1h, naturally cooling to room temperature, filtering, washing a filter cake with deionized water for 3 times, drying to constant weight at 60 ℃, and then calcining for 30min in a muffle furnace at 380 ℃ to obtain doped bentonite;
step A3, adding 5.0g of doped bentonite and 500mL of deionized water into a three-neck flask, performing ultrasonic dispersion for 20min at the frequency of 40kHz, then adding 0.5g of dodecyl dimethyl betaine and 0.3g of gemini surfactant, heating to 40 ℃, stirring for reaction for 3h, filtering, washing a filter cake with deionized water for 3 times, drying at 60 ℃, grinding and sieving with a 60-mesh sieve to obtain the modified bentonite.
Example 2
This example provides a modified bentonite prepared by the following steps:
step A1, adding 0.2mol of 2-pyridylacetic acid, 0.1mol of 1, 3-dibromopropane and 70mL of n-butanol into a reaction kettle, heating to 70 ℃, stirring at the rotating speed of 80r/min for 20min, placing the reaction kettle into a microwave reactor, carrying out stirring reaction at the microwave power of 900W and the reaction temperature of 140 ℃ for 7h, carrying out rotary evaporation to remove the solvent after the reaction is finished, adding ethyl acetate into the rotary evaporation product while the reaction is hot to dissolve and recrystallize, carrying out suction filtration, washing a filter cake for 4 times by using acetone, and drying at 78 ℃ to constant weight to obtain the gemini surfactant;
step A2, dispersing 5.0g of bentonite in 500mL of deionized water, stirring for 30min, adding 15mL of magnesium chloride solution with the mass fraction of 20% under the protection of nitrogen, stirring for reaction for 2h in water bath at 60 ℃, then heating to 75 ℃, adjusting the pH value to 10 by using sodium hydroxide solution with the concentration of 5mol/L, continuously stirring for 1h, naturally cooling to room temperature, filtering, washing a filter cake with deionized water for 4 times, drying at 60 ℃ to constant weight, and calcining in a 400 ℃ muffle furnace for 35min to obtain doped bentonite;
and A3, adding 5.0g of doped bentonite and 500mL of deionized water into a three-neck flask, performing ultrasonic dispersion for 20min at the frequency of 45kHz, then adding 0.7g of dodecyl dimethyl betaine and 0.4g of gemini surfactant, heating to 40 ℃, stirring for reaction for 3h, filtering, washing a filter cake with the deionized water for 4 times, drying at 60 ℃, grinding and sieving with a 60-mesh sieve to obtain the modified bentonite.
Example 3
This example provides a modified bentonite prepared by the following steps:
step A1, adding 0.2mol of 2-pyridylacetic acid, 0.1mol of 1, 3-dibromopropane and 80mL of n-butanol into a reaction kettle, heating to 70 ℃, stirring at the rotation speed of 100r/min for 20min, placing the reaction kettle into a microwave reactor, stirring and reacting at the microwave power of 900W and the reaction temperature of 140 ℃ for 8h, after the reaction is finished, removing the solvent by rotary evaporation, adding ethyl acetate into the rotary evaporation product while hot for dissolving and recrystallizing, performing suction filtration, washing a filter cake for 5 times by using acetone, and drying at the temperature of 80 ℃ to constant weight to obtain the gemini surfactant;
step A2, dispersing 5.0g of bentonite in 500mL of deionized water, stirring for 30min, adding 20mL of magnesium chloride solution with the mass fraction of 20% under the protection of nitrogen, stirring for reaction for 2h in water bath at 60 ℃, then heating to 75 ℃, adjusting the pH value to 10 by using sodium hydroxide solution with the concentration of 5mol/L, continuously stirring for 1h, naturally cooling to room temperature, filtering, washing a filter cake with deionized water for 5 times, drying to constant weight at 60 ℃, and then calcining for 40min in a muffle furnace at 420 ℃ to obtain doped bentonite;
and A3, adding 5.0g of doped bentonite and 500mL of deionized water into a three-neck flask, performing ultrasonic dispersion for 20min at the frequency of 50kHz, then adding 0.8g of dodecyl dimethyl betaine and 0.5g of gemini surfactant, heating to 40 ℃, stirring for reaction for 3h, filtering, washing a filter cake with the deionized water for 5 times, drying at 60 ℃, grinding and sieving with a 60-mesh sieve to obtain the modified bentonite.
Comparative example 1
This example provides a modified bentonite prepared by the following steps:
adding 5.0g of bentonite and 500mL of deionized water into a three-neck flask, ultrasonically dispersing for 20min at the frequency of 50kHz, then adding 0.8g of dodecyl dimethyl betaine and 0.5g of gemini surfactant, heating to 40 ℃, stirring for reacting for 3h, filtering, washing a filter cake for 5 times by using the deionized water, drying at 60 ℃, and grinding and sieving by using a 60-mesh sieve to obtain the modified bentonite.
Comparative example 2
The comparative example is sodium bentonite sold by Tuolin mineral product processing factories in Lingshou county.
The bentonite of examples 1-3 and comparative examples 1-2 were subjected to phosphate adsorption test to prepare 5 groups of phosphate solutions having an initial concentration of 500mg/L and an initial pH of 7.0, 4g of the bentonite of examples 1-3 and comparative examples 1-2 were added, respectively, and stirred at 40 ℃ and 100rpm for 48 hours to record the saturated adsorption amount of each group of bentonite, and the test results are shown in Table 1:
TABLE 1
| Group of | Saturated adsorption capacity (mg/g) |
| Example 1 | 88.57 |
| Example 2 | 88.46 |
| Example 3 | 88.51 |
| Comparative example 1 | 71.26 |
| Comparative example 2 | 47.62 |
As can be seen from Table 1, the modified bentonites prepared in examples 1-3 have higher phosphate adsorption than those prepared in comparative examples 1-2, indicating that the detergents prepared according to the present invention can effectively remove phosphate impurities in the chlorination reactor.
Example 4
Referring to fig. 1, a process for cleaning a chlorination reactor for producing phosphorus trichloride includes the following steps:
step S1, finishing the material treatment in the chlorination kettle, and leaving a reaction liquid port and a vacuumizing port after reaching the kettle cleaning condition, wherein the rest pipe ports are sealed by blind plates;
step S2, dropwise adding caustic soda aqueous solution into the chlorination kettle through the reaction solution port at the dropping speed of 0.5kg/h, removing HCl gas overflowing in the dropwise adding process by using a vacuum unit, setting absorption solution by using the vacuum unit, wherein the absorption solution is 35% by mass of sodium hydroxide solution, keeping the negative pressure in the reaction kettle, and finishing the primary cleaning;
step S3, discharging the substances in the chlorination kettle, removing a vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 0.5h at the rotating speed of 200rpm, standing for 3h, discharging cleaning waste liquid, and finishing secondary cleaning;
and step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle.
Wherein the mass fraction of the caustic soda aqueous solution is 10 percent.
The cleaning agent comprises the following raw materials in parts by weight: 30 parts of distilled water, 10 parts of hydroxypropyl cellulose, 5 parts of sodium bicarbonate, 1 part of modified bentonite in example 1 and 1 part of surfactant.
Example 5
A cleaning process of a chlorination kettle for phosphorus trichloride production comprises the following steps:
step S1, finishing the material treatment in the chlorination kettle, and leaving a reaction liquid port and a vacuumizing port after reaching the kettle cleaning condition, wherein the rest pipe ports are sealed by blind plates;
step S2, dropwise adding caustic soda aqueous solution into the chlorination kettle through the reaction solution port at the dropping speed of 0.5kg/h, removing HCl gas overflowing in the dropwise adding process by using a vacuum unit, setting absorption solution by using the vacuum unit, wherein the absorption solution is 35% by mass of sodium hydroxide solution, keeping the negative pressure in the reaction kettle, and finishing the primary cleaning;
step S3, discharging the substances in the chlorination kettle, removing a vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 0.8h at the rotation speed of 250rpm, standing for 4h, discharging cleaning waste liquid, and finishing secondary cleaning;
and step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle.
Wherein the mass fraction of the caustic soda aqueous solution is 12 percent.
The cleaning agent comprises the following raw materials in parts by weight: 40 parts of distilled water, 12 parts of hydroxypropyl cellulose, 7 parts of sodium bicarbonate, 2 parts of modified bentonite in example 1 and 2 parts of a surfactant.
Example 6
A cleaning process of a chlorination kettle for phosphorus trichloride production comprises the following steps:
step S1, finishing the material treatment in the chlorination kettle, and leaving a reaction liquid port and a vacuumizing port after reaching the kettle cleaning condition, wherein the rest pipe ports are sealed by blind plates;
step S2, dropwise adding caustic soda aqueous solution into the chlorination kettle through the reaction solution port at the dropping speed of 0.5kg/h, removing HCl gas overflowing in the dropwise adding process by using a vacuum unit, setting absorption solution by using the vacuum unit, wherein the absorption solution is 35% by mass of sodium hydroxide solution, keeping the negative pressure in the reaction kettle, and finishing the primary cleaning;
step S3, discharging the substances in the chlorination kettle, removing a vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 1h at the rotating speed of 300rpm, standing for 5h, discharging cleaning waste liquid, and finishing secondary cleaning;
and step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle.
Wherein the mass fraction of the caustic soda aqueous solution is 15 percent.
The cleaning agent comprises the following raw materials in parts by weight: 50 parts of distilled water, 15 parts of hydroxypropyl cellulose, 5-8 parts of sodium bicarbonate, 3 parts of modified bentonite in example 1 and 5 parts of a surfactant.
The invention provides a chlorination kettle cleaning process for phosphorus trichloride production, which comprises three cleaning steps, wherein the chlorination kettle is vacuumized, caustic soda solution is added dropwise to neutralize acid in a reaction kettle, a cleaning agent is added to remove organic impurities and phosphate in the chlorination kettle, then manual kettle cleaning is carried out, the by-product acid and the phosphate are removed through the previous two cleaning steps, other impurities in the chlorination kettle are cleaned, a foundation is laid for the subsequent manual kettle cleaning, the chlorination kettle cleaning is completely completed through the manual kettle cleaning, and preparation is made for high-quality phosphorus trichloride production.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A cleaning process of a chlorination kettle for phosphorus trichloride production is characterized by comprising the following steps:
step S1, after the chlorination kettle reaches a kettle cleaning condition, a reaction liquid port and a vacuumizing port are reserved, and the rest pipe ports are sealed by blind plates;
step S2, dropwise adding a caustic soda aqueous solution into the chlorination kettle, vacuumizing the interior of the chlorination kettle by using a vacuumizing unit, and keeping the negative pressure in the reaction kettle to finish primary cleaning;
step S3, discharging the substances in the chlorination kettle, removing the vacuum unit, adding a cleaning agent into the chlorination kettle, stirring and mixing for 0.5-1h, standing for 3-5h, discharging cleaning waste liquid, and finishing secondary cleaning;
step S4, opening a manhole cover of the chlorination kettle, and manually washing the kettle;
the cleaning agent comprises the following raw materials in parts by weight: 30-50 parts of distilled water, 10-15 parts of hydroxypropyl cellulose, 5-8 parts of sodium bicarbonate, 1-3 parts of modified bentonite and 1-5 parts of surfactant.
2. The chlorination reactor cleaning process for phosphorus trichloride production according to claim 1, wherein the modified bentonite is prepared by the following steps:
step A1, mixing 2-pyridylacetic acid, 1, 3-dibromopropane and n-butanol, heating to 70 ℃, stirring for 20min, reacting for 6-8h under stirring at the microwave power of 900W and the temperature of 140 ℃, performing rotary evaporation, recrystallization, suction filtration, washing a filter cake, and drying to obtain a gemini surfactant;
step A2, dispersing bentonite in deionized water, adding a magnesium chloride solution under the protection of nitrogen, stirring and reacting for 2 hours in a water bath at 60 ℃, then heating to 75 ℃, adjusting the pH value to 10 by using a sodium hydroxide solution, continuing stirring for 1 hour, cooling, filtering, washing and drying a filter cake, and calcining at the temperature of 380-420 ℃ to obtain doped bentonite;
and A3, ultrasonically dispersing the doped bentonite and deionized water, adding dodecyl dimethyl betaine and a gemini surfactant, heating to 40 ℃, stirring for reacting for 3 hours, filtering, washing a filter cake, drying, grinding and sieving to obtain the modified bentonite.
3. The chlorination kettle cleaning process for phosphorus trichloride production according to claim 2, wherein in the step A1, the using amount ratio of 2-pyridylacetic acid, 1, 3-dibromopropane and n-butanol is 0.2 mol: 0.1 mol: 60-80 mL.
4. The chlorination reactor cleaning process for phosphorus trichloride production according to claim 2, wherein the amount ratio of bentonite, deionized water and magnesium chloride solution in step a2 is 5.0 g: 500 mL: 10-20 mL.
5. The chlorination reactor cleaning process for phosphorus trichloride production according to claim 2, wherein the mass fraction of the magnesium chloride solution in step a2 is 20%.
6. The process of claim 2, wherein the amount ratio of bentonite, deionized water, dodecyl dimethyl betaine and gemini surfactant doped in the step A3 is 5.0 g: 500 mL: 0.5-0.8 g: 0.3-0.5 g.
7. The process for cleaning the chlorination reactor for producing phosphorus trichloride as claimed in claim 1, wherein the surfactant is one or more of alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether and fatty acid methyl ester polyoxyethylene ether, which are mixed in any proportion.
8. The cleaning process of the chlorination reactor for producing phosphorus trichloride according to claim 1, wherein the mass fraction of the caustic soda aqueous solution in the step S2 is 10-15%.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4166039A (en) * | 1973-10-15 | 1979-08-28 | The Proctor & Gamble Company | Detergent composition and process |
| CN103752274A (en) * | 2013-12-12 | 2014-04-30 | 西北农林科技大学 | Amphiprotic-Gemini type cationic composite adsorbent, and preparation method thereof |
| CN105502319A (en) * | 2014-09-25 | 2016-04-20 | 湖北泰盛化工有限公司 | Chlorination kettle washing system |
| CN105668533A (en) * | 2016-03-19 | 2016-06-15 | 安徽东至广信农化有限公司 | Reactor cleaning method for phosphorus trichloride production |
| CN109395693A (en) * | 2017-08-18 | 2019-03-01 | 湖州欧美新材料有限公司 | A kind of adsorbent, preparation method and application |
| CN112642408A (en) * | 2020-12-29 | 2021-04-13 | 张建峰 | Preparation method of MgO-loaded bentonite-sodium alginate composite ball |
-
2021
- 2021-11-05 CN CN202111310554.8A patent/CN114031055B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4166039A (en) * | 1973-10-15 | 1979-08-28 | The Proctor & Gamble Company | Detergent composition and process |
| CN103752274A (en) * | 2013-12-12 | 2014-04-30 | 西北农林科技大学 | Amphiprotic-Gemini type cationic composite adsorbent, and preparation method thereof |
| CN105502319A (en) * | 2014-09-25 | 2016-04-20 | 湖北泰盛化工有限公司 | Chlorination kettle washing system |
| CN105668533A (en) * | 2016-03-19 | 2016-06-15 | 安徽东至广信农化有限公司 | Reactor cleaning method for phosphorus trichloride production |
| CN109395693A (en) * | 2017-08-18 | 2019-03-01 | 湖州欧美新材料有限公司 | A kind of adsorbent, preparation method and application |
| CN112642408A (en) * | 2020-12-29 | 2021-04-13 | 张建峰 | Preparation method of MgO-loaded bentonite-sodium alginate composite ball |
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| CN115889369A (en) * | 2023-02-24 | 2023-04-04 | 山西钢科碳材料有限公司 | Cleaning method of gel in acrylonitrile polymerization reactor |
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