CN107569985B - Reaction cracker - Google Patents
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- CN107569985B CN107569985B CN201710891666.4A CN201710891666A CN107569985B CN 107569985 B CN107569985 B CN 107569985B CN 201710891666 A CN201710891666 A CN 201710891666A CN 107569985 B CN107569985 B CN 107569985B
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Abstract
A reaction cracker is characterized in that an air inlet cover, a communicating chamber, a nonlinear orifice plate, a nitrogen cracking reactor, a cracking heating power annular pipe, a flame spray melting head, a buffer plate, a medium reaction filler and an ultrasonic vibration plate are sequentially arranged in a furnace wall of the cracker from left to right; the left end of the communicating chamber is connected with the air inlet cover, and the right end of the communicating chamber is connected with a nonlinear orifice plate with a hole on the surface; the small-opening end of the nitrogen cracking reactor is fixedly connected to the nonlinear orifice plate, and a nitrogen releaser driven by an active motor is arranged in the nitrogen cracking reactor; the cracking heating power annular pipe is fixedly connected with a plurality of flame spray melting heads and is connected with a fuel gas supply pipeline; the surface of the buffer plate is provided with a through hole; the temperature sensor is positioned below the catalytic reaction filler; the surface of the ultrasonic oscillation plate is provided with a plurality of through holes, and an ultrasonic vibrator and an ultrasonic generator are arranged in the ultrasonic oscillation plate; the pressurizing nitrogen pipe is communicated with the buffer chamber from the outside through a nitrogen branch pipe, and a heater is arranged at the inner end of the pressurizing nitrogen pipe. The reaction cracker has ideal effect on processing carbon chloride.
Description
Technical Field
The invention relates to the technical field of environment-friendly equipment, in particular to a reaction cracker.
Background
Carbon tetrachloride (CCl)4) Is artificially synthesized low boiling point organic chlorohydrocarbon (specific gravity 1.591 g/cm)3Boiling point 77 deg.C) and is slightly soluble in water. Foreign research shows that: carbon tetrachloride is a typical liver poison and, at high concentrations, affects the central nervous system first and then the liver and kidneys. It has persistence, long-term residue and biological accumulation in environment, so it has been listed by us EPA as "priority control pollutant in carbon tetrachloride-containing groundwater" since 1979 and also by our country as 68 "priority control pollutant in water".
In the seventies of the last century, groundwater in some regions was contaminated with carbon tetrachloride due to the large quantity of manufactured and used pesticides, such as the mississin aquifer in the united states and aquifers near ottawa, canada, which are mostly present as non-aqueous phases (NAPLs) in the aquifer.
Currently, various devices for carbon tetrachloride treatment are emerging. The reactive cracker has also been developed as an important apparatus for the treatment of carbon tetrachloride. However, the existing burner for processing the reaction cracker has large volume, unreasonable structure and low compactness, has undesirable effect on processing gaseous carbon tetrachloride, and is not suitable for systematized processing of the carbon tetrachloride.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a reaction cracker which has the advantages of small volume, reasonable structure, high compactness, ideal treatment effect on carbon chloride and suitability for systematic treatment of carbon tetrachloride.
In order to achieve the aim, the invention provides a reaction cracker which comprises a funnel-shaped air inlet cover, a cylindrical cracker furnace wall and a temperature sensor, wherein the large opening end of the air inlet cover is arranged at the left end of an inner cavity of the cracker furnace wall towards the left, and the large opening end of the air inlet cover is connected with the left end of the cracker furnace wall; a communicating chamber, a nonlinear orifice plate, a nitrogen cracking reactor, a cracking heating power annular pipe, a flame spray melting head, a buffer plate, a medium reaction filler and an ultrasonic vibration plate are fixedly arranged in the inner cavity of the furnace wall of the cracker from left to right in sequence;
the communicating chamber is of a hollow tubular structure, the left end of the communicating chamber is fixedly connected with the small end of the air inlet cover, the right end of the communicating chamber is fixedly connected with the left end face of the nonlinear pore plate, and nonlinear pore channels are arranged on the surface of the nonlinear pore plate in a distributed manner;
the small end of the nitrogen cracking reactor is fixedly connected with the central area of the nonlinear orifice plate, the small end of the nitrogen cracking reactor corresponds to the peripheral area of the communicating chamber, and the large end of the nitrogen cracking reactor is arranged towards the direction of the cracking thermal annular pipe;
the nitrogen cracking reactor comprises a motor, a pressurized nitrogen pipe, a nitrogen releaser and a truncated cone-shaped outer cover, wherein the pressurized nitrogen pipe penetrates through the outer part of the furnace wall of the cracker, the inner end of the pressurized nitrogen pipe is connected with the buffer chamber through a nitrogen branch pipe, the inner end of the pressurized nitrogen pipe is provided with a heater, and the outer end of the pressurized nitrogen pipe is connected with a nitrogen bottle; a cylindrical rotating shaft is arranged on an axis line in the outer cover, a buffer chamber fixedly connected to the inside of the communicating chamber is arranged on the outer side of the small opening end of the outer cover, the inner end of the buffer chamber is sleeved on the outer side of the inner end of the rotating shaft, the motor is positioned in the communicating chamber and fixedly connected with the outer end of the buffer chamber, an output shaft of the motor penetrates through the buffer chamber, extends into the inner end of the rotating shaft and is fixedly connected with the rotating shaft through a plurality of radially-adjusted connecting rods, two ends of the rotating shaft are respectively and fixedly connected with a circular support capable of rotating in the outer cover, so that the circular support consists of a circular hollow pipeline positioned on the outer ring and a communicating pipeline connecting the circular hollow pipeline with the inner cavity of the rotating shaft, and the outer diameter of the circular hollow pipeline of the circular support positioned on one side of the large opening end of the outer cover is; the nitrogen releasers are arranged around the rotating shaft and are of hollow columnar structures, and two ends of each nitrogen releaser are respectively communicated with the annular hollow pipelines of the two circular brackets; the surface of the nitrogen releaser is provided with a plurality of through holes communicated with the inner cavity of the nitrogen releaser;
the cracking heating power annular pipe is fixedly connected with a gas supply pipeline communicated with an inner cavity of the cracking heating power annular pipe, and the gas supply pipeline extends to the outside of the furnace wall of the cracker; the flame spray-melting heads are circumferentially and uniformly fixedly connected to the right end face of the cracking thermal annular tube;
the buffer plate is of a plate-shaped structure, and through holes which are communicated from left to right are formed in the surface of the buffer plate;
the temperature sensor is positioned below the catalytic reaction filler;
the ultrasonic oscillation plate is provided with a plurality of through holes distributed on the surface, and an ultrasonic vibrator and an ultrasonic generator are arranged in the ultrasonic oscillation plate;
an air outlet is arranged at the right end opening of the furnace wall of the cracker.
In the technical scheme, the gathering action of the bell mouth shape of the air inlet cover can gather the carbon tetrachloride-containing waste gas, pass through the communicating chamber, then pass through the nonlinear orifice plate, and enter the medium nitrogen cracking reactor; high-pressure nitrogen can be introduced through the pressurized nitrogen pipe and can be heated under the action of the heater; the motor drives the nitrogen releaser in the outer cover to rotate, so that the heated high-pressure nitrogen can be uniformly released and can be in full contact with and react with carbon tetrachloride to generate diazomethane gas (H2CNN) and chlorine (Cl2) under the action of high temperature, and the carbon tetrachloride can be effectively treated. The flame spray head is arranged to ignite residual carbon tetrachloride for further processing. The buffer board can form a plurality of air flows into the medium reaction filler with carbon tetrachloride gas which is not combusted and decomposed, so as to adsorb the carbon tetrachloride, the treated gas passes through the ultrasonic oscillation board, and the ultrasonic oscillation board can promote the further decomposition of the residual carbon tetrachloride through high-frequency vibration.
Further, in order to promote the efficient degradation of carbon tetrachloride, the catalytic reaction filler is prepared from the following components in parts by weight:
252-477 parts of sodium-removed ionized water, 44-86 parts of fatty amide polyoxyethylene ether, 47-156 parts of dihydroxy succinic acid, 43-60 parts of N-ethyl O/p-toluenesulfonamide, 46-103 parts of N, O-bis (trimethylsilyl) acetamide, 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino ] -9, 10-dioxo-2-anthracenesulfonic acid sodium salt, 49-110 parts of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene dioxide-2-sulfonic acid, 46-69 parts of 3, 5-diaminobenzoic acid, 51-106 parts of dysprosium nanoparticles, 44-86 parts of 1-amino-2-chloro-4-hydroxyanthraquinone, 34-77 parts of 2- [ (4-chloro-nitrophenyl) azo ] -N- (2, 4-dimethylphenyl) -3-oxobutanamide, 35-71 parts of potassium triacontanol phosphate, 46-86 parts of N- [ (5-methyl-1H-benzotriazol-1-yl) methyl ] diethanolamine, 53-97 parts of a 2-hydroxyethyl acrylate end-capped polymer of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and 76-130 parts of monoalkyl phosphate potassium salt with the mass concentration of 43-310 ppm.
Furthermore, in order to promote the high-efficiency degradation of carbon tetrachloride, the particle size of the dysprosium nanoparticles is 51.3-61.1 μm.
Further, in order to obtain a catalytic reaction filler with good treatment effect and excellent performance, the catalytic reaction filler is prepared by the following steps:
step 1: adding sodium ion-removed water and fatty amide polyoxyethylene ether into a stirring type reactor, starting a stirrer in the stirring type reactor, setting the rotating speed to be 45-91 rpm, starting a repeated heater in the stirring type reactor, raising the temperature to 60.4-61.4 ℃, adding dihydroxy succinic acid, uniformly stirring, carrying out halogenation acylation reaction for 37-48 minutes, adding N-ethyl o/p-toluenesulfonamide, and introducing the solution with the flow rate of 36.6m3/min～77.2m30.4-0.1 hour of xenon gas per minute; then adding N, O-bis (trimethylsilyl) acetamide into the stirring reactor, starting a repeated heater in the stirring reactor again to increase the temperature to 77.4-110.4 ℃, preserving the temperature for 37-48 minutes, and adding 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino]Adjusting the pH value of the solution in the stirring type reactor to 4.8-8.9 and keeping the temperature for 37-277 minutes by using-9, 10-dioxo-2-anthracene sulfonic acid sodium salt;
step 2: taking dysprosium nanoparticles, and carrying out ultrasonic treatment on the dysprosium nanoparticles for 0.4-0.1 hour under the condition that the power is 5.773 KW-11.218 KW; dysprosium nanoparticles are added into another stirring type reactorAdding 1-amino-2-chloro-4-hydroxyanthraquinone dispersed dysprosium nanoparticles with mass concentration of 47.9-277.2 ppm, starting a repeated heater in a stirring type reactor to ensure that the temperature of the solution is between 4.86 × 10 ℃ and 8.94 × 10 ℃, starting a stirrer in the stirring type reactor, and using 4.84 × 102rpm～8.97×102Stirring at rpm, adjusting pH to 4.8-8.9, stirring at constant temperature for 0.5-1.1 hr, stopping reaction, standing for 5.7 × 10-11.2 × 10 min to remove impurities, adding N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] into the suspension]Adjusting the pH value of diethanolamine to 1.6-2.2, eluting the formed precipitate with sodium ion water, and passing through a centrifuge at the rotating speed of 4.129 × 103rpm～***×103Solids were obtained at rpm, 2.22 × 102℃～3.79×102Drying at the temperature of DEG C, grinding, and sieving with a sieve of 500-620 meshes for later use;
and 3, step 3: taking 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and the dysprosium nano-particles after the step 2 treatment, after being uniformly mixed, alpha radiation reflection irradiation is adopted, the energy of the alpha radiation reflection irradiation is 34.527 MeV-62.184 MeV, the dosage is 82.558 kGy-122.856 kGy, the irradiation time is 46-71 minutes, obtaining a 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticle mixture with changed properties; placing a mixture of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles in another stirring type reactor, starting a repeated heater in the stirring type reactor, setting the temperature to be 45-91 ℃, starting a stirrer in the stirring type reactor, adjusting the rotating speed to be 37-432 rpm, adjusting the pH to be 4.8-8.9, and dehydrating for 46-60 minutes for later use;
and 4, step 4: modifying the 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] group obtained in step 3]Amino group]Methyl radical]Phenyl radical]Amino group]The (E) -9, 10-anthracene dioxide-2-sulfonic acid, the 3, 5-diaminobenzoic acid and the dysprosium nanoparticles are uniformly mixed and fed to the second stepIn the stirring type reactor in the step 1, the flow-adding speed is 182.8 mL/min-910.9 mL/min; starting a stirring type reactor stirrer, and setting the rotating speed to be 51-91 rpm; stirring for 4-8 minutes; then adding 2- [ (4-chloro-nitrophenyl) azo]-N- (2, 4-dimethylphenyl) -3-oxobutanamide, starting a repeated heater in the stirring reactor, heating to 81.3-118.5 ℃, adjusting the pH to 4.8-8.9, introducing xenon with the ventilation volume of 36.4m3/min～77.9m3Keeping the temperature and standing for 71-101 minutes; starting the stirring type reactor stirrer again, wherein the rotating speed is 46-91 rpm, adding potassium triacontanol phosphate to ensure that the threshold value of hydrophilic-hydrophilic alcohol ester of the reaction liquid is 5-11, adjusting the pH value to 4.8-8.9, and keeping the temperature and standing for 70-110 minutes;
step 5, starting a stirrer in the stirring type reactor, setting the rotating speed to be 43-110 rpm, starting a repeated heater in the stirring type reactor, and setting the temperature in the stirring type reactor to be 4.625 × 102℃～9.620×102Keeping the temperature at 70-110 minutes, adding a polymer capped by 2-hydroxyethyl acrylate of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and carrying out halogenation acylation reaction for 37-48 minutes; then adding potassium monoalkyl phosphate, starting a repeated heater in the stirring type reactor, setting the temperature in the stirring type reactor to be 121.6-177.6 ℃, adjusting the pH to be 4.8-8.9, adjusting the pressure to be 0.435-0.448 MPa, and reacting for 0.4-0.9 h; then reducing the pressure to 0MPa, reducing the temperature to 54.4-59.4 ℃, discharging, and putting into an injection molding machine to obtain the catalyst-promoted reaction filler.
Further, the diameter of the large opening end of the air inlet cover is 10-20 cm: the air inlet cover is made of stainless steel; the communicating chamber is made of stainless steel and has a diameter of 5-10 cm.
Further, the model of the temperature sensor is PT 100.
Furthermore, in order to enable the airflow to present a plurality of strands of rotary vortexes, the flow velocity of the airflow is sequentially increased from the circumference to the circle center, a specific airflow is formed to pass through the nitrogen cracking reactor, the number of nonlinear pore channels on the surface of the nonlinear pore plate is 10-30, the pore diameter inside each nonlinear pore channel is 5-10 mm, and the nonlinear pore channels are distributed according to a Sine-Gordon nonlinear equation.
Further, the diameter of the large opening end of the nitrogen cracking reactor is 10-20 cm; the diameter of the cracking heating power annular tube is 10-20 cm; the number of the flame spray-melting heads is 10-20.
Further, the buffer plate is of a high-temperature resistant ceramic circular plate structure; the ultrasonic oscillation plate is of a disc structure, the diameter of the ultrasonic oscillation plate is 10-20 cm, the thickness of the ultrasonic oscillation plate is 10-20 m, and the diameter of a through hole in the upper portion of the ultrasonic oscillation plate is 2-10 mm; the diameter of the through hole in the surface of the ultrasonic oscillation plate is 2-10 mm.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic structural view of a non-linear cell according to the present invention;
FIG. 3 is a schematic view of the structure of a nitrogen-cracking reactor in the present invention.
In the figure: 6-1, an air inlet cover, 6-2, a communicating chamber, 6-3, a nonlinear orifice plate, 6-3-1, a nonlinear pore passage, 6-3-2, a duct track, 6-4, a nitrogen cracking reactor, 6-4-1, a motor, 6-4-3, a heater, 6-4-4, a nitrogen branch pipe, 6-4-5, a nitrogen releaser, 6-4-6, a rotating shaft, 6-4-7, a circular bracket, 6-4-8, an outer cover, 6-4-9, a buffer chamber, 6-5, a cracking thermal annular pipe, 6-6, a flame spray-melt head, 6-7, a buffer plate, 6-8, a temperature sensor, 6-9, an ultrasonic vibration plate, 6-10 and a cracker furnace wall, 6-11 parts of gas outlet, 6-12 parts of pressurized nitrogen pipe, 6-13 parts of catalytic reaction filler.
Detailed Description
The present invention will be further explained below.
As shown in figure 1, the reaction cracker comprises a funnel-shaped air inlet cover 6-1, a cylindrical cracker furnace wall 6-10 and a temperature sensor 6-8, wherein the large opening end of the air inlet cover 6-1 is arranged at the left end of an inner cavity of the cracker furnace wall 6-10 towards the left, and the large opening end of the air inlet cover 6-1 is connected with the left end of the cracker furnace wall 6-10; a communicating chamber 6-2, a nonlinear orifice plate 6-3, a nitrogen cracking reactor 6-4, a cracking heating power annular pipe 6-5, a flame spray melting head 6-6, a buffer plate 6-7, a medium reaction filler 6-13 and an ultrasonic oscillation plate 6-9 are fixedly arranged in the inner cavity of the furnace wall 6-10 of the cracker from left to right in sequence;
the communicating chamber 6-2 is of a hollow tubular structure, the left end of the communicating chamber is fixedly connected with the small end of the air inlet cover 6-1, the right end of the communicating chamber is fixedly connected with the left end face of the nonlinear pore plate 6-3, and as shown in fig. 2, nonlinear pore channels 6-3-1 are arranged on the surface of the nonlinear pore plate 6-3 in a distributed manner;
the small end of the nitrogen cracking reactor 6-4 is fixedly connected to the central area of the nonlinear orifice plate 6-3, the small end of the nitrogen cracking reactor 6-4 is correspondingly arranged in the peripheral area of the communicating chamber 6-2, and the large end of the nitrogen cracking reactor 6-4 is arranged towards the direction of the cracking thermal annular pipe 6-5;
as shown in fig. 3, the nitrogen cracking reactor 6-4 comprises a motor 6-4-1, a pressurized nitrogen gas pipe 6-12, a nitrogen gas releaser 6-4-5, a truncated cone-shaped outer cover 6-4-8, the pressurized nitrogen gas pipe 6-12 penetrates from the outside of the furnace wall 6-10 of the cracker, the inner end of the pressurized nitrogen gas pipe is connected with a buffer chamber 6-4-9 through a nitrogen gas branch pipe 6-4-4, the inner end of the pressurized nitrogen gas pipe 6-12 is provided with a heater 6-4-3, the outer end of the pressurized nitrogen gas pipe is connected with a nitrogen gas bottle, the pressurized nitrogen gas pipe 6-12 is used for introducing high-pressure nitrogen gas from the outside, the heater 6-4-3 heats the introduced nitrogen gas to 86-92 ℃, and the buffer chamber 6-4-9 buffers the introduced nitrogen gas inside; a cylindrical rotating shaft 6-4-6 is arranged on the axis line in the outer cover 6-4-8, a buffer chamber 6-4-9 fixedly connected to the inside of the communicating chamber 6-2 is arranged on the outer side of the small opening end of the outer cover 6-4-8, the inner end of the buffer chamber 6-4-9 is sleeved on the outside of the inner end of the rotating shaft 6-4-6, the motor 6-4-1 is positioned in the communicating chamber 6-2 and fixedly connected with the outer end of the buffer chamber 6-4-9, the output shaft of the motor 6-4-1 penetrates through the buffer chamber 6-4-9 to extend into the inner end of the rotating shaft 6-4-6 and is fixedly connected with the rotating shaft 6-4-6 through a plurality of radially adjusted connecting rods, the outer diameter of the output shaft of the motor 6-4-1 is smaller than the inner diameter of the inner cavity of the rotating shaft 6-4-6, the motor 6-4-1 is driven to rotate at a low speed of 10-50 rpm; two ends of the rotating shaft 6-4-6 are respectively fixedly connected with a circular bracket 6-4-7 which can rotate in the outer cover 6-4-8, so that the circular bracket 6-4-7 consists of an annular hollow pipeline positioned at the outer ring and a communicating pipeline connecting the annular hollow pipeline and the inner cavity of the rotating shaft 6-4-6, and is positioned at one side of the large opening end of the outer cover 6-4-8The outer diameter of the annular hollow pipeline of the bracket 6-4-7 is larger than that of the annular hollow pipeline of the circular bracket 6-4-7 positioned at one side of the small opening end of the outer cover 6-4-8; the plurality of nitrogen releasers 6-4-5 are arranged around the rotating shaft 6-4-6, the nitrogen releasers 6-4-5 are of hollow columnar structures, and two ends of each nitrogen releaser 6-4-5 are respectively communicated with the annular hollow pipelines of the two circular brackets 6-4-7; the surface of the nitrogen releaser 6-4-5 is provided with a plurality of through holes communicated with the inner cavity of the nitrogen releaser; the section of the nitrogen releaser 6-4-5 is oval, the nitrogen releaser 6-4-5 releases the heated nitrogen through the through hole, and then the high-temperature nitrogen reacts with carbon tetrachloride to generate diazomethane gas H2CNN and chlorine Cl2；
The cracking heating power annular pipe 6-5 is fixedly connected with a fuel gas supply pipeline communicated with an inner cavity of the cracking heating power annular pipe, and the fuel gas supply pipeline extends to the outside of the furnace wall 6-10 of the cracker; the flame spray-melting heads 6-6 are circumferentially and uniformly fixedly connected to the right end face of the cracking thermal annular pipe 6-5; the flame spray melting head 6-6 generates flame to burn residual carbon tetrachloride gas;
the buffer plate 6-7 is of a plate-shaped structure, and through holes which are communicated from left to right are formed in the buffer plate 6-7 on the surface of the buffer plate; high-temperature gas generated by the flame spray melting head 6-6 slowly enters the catalytic reaction filler 6-13 through the buffer plate 6-7;
the temperature sensor 6-8 is positioned below the catalytic reaction filler 6-13;
the ultrasonic oscillation plate 6-9 is provided with a plurality of through holes distributed on the surface, and an ultrasonic oscillator and an ultrasonic generator are arranged in the ultrasonic oscillation plate; the ultrasonic vibrator is a product in the prior art, the model number of the ultrasonic vibrator is KS-2155-51K, and the ultrasonic vibrator is produced by Sen electronic plastics Co., Ltd, Dongguan city; the ultrasonic generator is a product in the prior art, has the model number of AFT-60w, and is produced by the Epsoviet ultrasonic equipment Limited in Shenzhen. The ultrasonic oscillation plates 6-9 promote the decomposition of carbon tetrachloride by high-frequency vibration.
An air outlet 6-11 is arranged at the right end opening of the furnace wall 6-10 of the cracker.
The arrangement of the pressurized nitrogen pipe can conveniently introduce external nitrogen, and the introduced nitrogen not only can increase the pressure in the chaotic mixer, but also can be used as a carrier of carbon tetrachloride entering the chaotic mixer so as to promote the carbon tetrachloride to uniformly disperse through the non-uniform distribution system type fence, thereby promoting the carbon tetrachloride to be uniformly dispersed in the nitrogen cracking reactor; the cracking potential annular tube and the flame spray melting port on the upper part of the cracking potential annular tube can provide high-temperature flame when gas is combusted, so that carbon tetrachloride passing through can be effectively cracked; the arrangement of the buffer plate can lead carbon tetrachloride which is not cracked to be rapidly degraded through ultrasonic waves when passing through the through hole. The media promotion reaction filler can promote carbon tetrachloride to be adsorbed by the filler, and the arrangement of the ultrasonic oscillation plate can realize the return of ultrasonic waves, so that the further degradation of the carbon tetrachloride can be promoted.
In order to promote the filler of the high-efficiency degradation of carbon tetrachloride, the catalyst reaction filler 6-13 comprises the following components in parts by weight:
252-477 parts of sodium-removed ionized water, 44-86 parts of fatty amide polyoxyethylene ether (FAEO), 47-156 parts of dihydroxy succinic acid, 43-60 parts of N-ethyl O/p-toluene sulfonamide, 46-103 parts of N, O-bis (trimethylsilyl) acetamide, 49-110 parts of 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino ] -9, 10-dioxo-2-anthracene sulfonic acid sodium salt, 46-69 parts of 1-amino-9, 10-dihydro-4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 43-88 parts of 3, 5-diaminobenzoic acid, 51-106 parts of dysprosium nanoparticles, 44-86 parts of 1-amino-2-chloro-4-hydroxyanthraquinone, 34-77 parts of 2- [ (4-chloro-nitrophenyl) azo ] -N- (2, 4-dimethylphenyl) -3-oxobutanamide, 35-71 parts of potassium triacontanol phosphate, 46-86 parts of N- [ (5-methyl-1H-benzotriazol-1-yl) methyl ] diethanolamine, 53-97 parts of a 2-hydroxyethyl acrylate end-capped polymer of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and 76-130 parts of monoalkyl phosphate potassium salt with the mass concentration of 43-310 ppm.
In order to promote the filler for efficiently degrading carbon tetrachloride, the particle size of the dysprosium nanoparticles is 51.3-61.1 μm.
In order to obtain a manufacturing method of a catalytic reaction filler which is simple in process and suitable for industrial production, the catalytic reaction filler 6-13 is prepared by the following steps:
step 1: adding sodium ion-removed water and fatty amide polyoxyethylene ether (FAEO) into a stirring type reactor, starting a stirrer in the stirring type reactor, setting the rotating speed to be 45-91 rpm, starting a repeated heater in the stirring type reactor, raising the temperature to 60.4-61.4 ℃, adding dihydroxy succinic acid, uniformly stirring, carrying out halogenation acylation reaction for 37-48 minutes, adding N-ethyl o/p-toluenesulfonamide, and introducing the mixture with the flow rate of 36.6m3/min～77.2m30.4-0.1 hour of xenon gas per minute; then adding N, O-bis (trimethylsilyl) acetamide into the stirring reactor, starting a repeated heater in the stirring reactor again to increase the temperature to 77.4-110.4 ℃, preserving the temperature for 37-48 minutes, and adding 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino]Adjusting the pH value of the solution in the stirring type reactor to 4.8-8.9 and keeping the temperature for 37-277 minutes by using-9, 10-dioxo-2-anthracene sulfonic acid sodium salt;
step 2, taking another dysprosium nanoparticle, carrying out ultrasonic treatment on the dysprosium nanoparticle for 0.4-0.1 hour under the condition that the power is 5.773 KW-11.218 KW, adding the dysprosium nanoparticle into another stirring type reactor, adding 1-amino-2-chlorine-4-hydroxyanthraquinone with the mass concentration of 47.9 ppm-277.2 ppm to disperse the dysprosium nanoparticle, starting a repeated heater in the stirring type reactor to ensure that the temperature of the solution is between 4.86 × 10 ℃ and 8.94 × 10 ℃, starting a stirrer in the stirring type reactor, and carrying out ultrasonic treatment on the dysprosium nanoparticle by using 4.84 × 102rpm～8.97×102Stirring at rpm, adjusting pH to 4.8-8.9, stirring at constant temperature for 0.5-1.1 hr, stopping reaction, standing for 5.7 × 10-11.2 × 10 min to remove impurities, adding N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] into the suspension]Adjusting the pH value of diethanolamine to 1.6-2.2, eluting the formed precipitate with sodium ion water, and passing through a centrifuge at the rotating speed of 4.129 × 103rpm～***×103Solids were obtained at rpm, 2.22 × 102℃～3.79×102Drying at the temperature of DEG C, grinding, and sieving with a sieve of 500-620 meshes for later use;
and 3, step 3: taking 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and the dysprosium nano-particles after the step 2 treatment, after being uniformly mixed, alpha radiation reflection irradiation is adopted, the energy of the alpha radiation reflection irradiation is 34.527 MeV-62.184 MeV, the dosage is 82.558 kGy-122.856 kGy, the irradiation time is 46-71 minutes, obtaining a 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticle mixture with changed properties; placing a mixture of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles in another stirring type reactor, starting a repeated heater in the stirring type reactor, setting the temperature to be 45-91 ℃, starting a stirrer in the stirring type reactor, adjusting the rotating speed to be 37-432 rpm, adjusting the pH to be 4.8-8.9, and dehydrating for 46-60 minutes for later use;
and 4, step 4: modifying the 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] group obtained in step 3]Amino group]Methyl radical]Phenyl radical]Amino group]Uniformly mixing 9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles, and adding the mixture into the stirring type reactor in the step 1 at a flow velocity of 182.8-910.9 mL/min; starting a stirring type reactor stirrer, and setting the rotating speed to be 51-91 rpm; stirring for 4-8 minutes; then adding 2- [ (4-chloro-nitrophenyl) azo]-N- (2, 4-dimethylphenyl) -3-oxobutanamide, starting a repeated heater in the stirring reactor, heating to 81.3-118.5 ℃, adjusting the pH to 4.8-8.9, introducing xenon with the ventilation volume of 36.4m3/min～77.9m3Keeping the temperature and standing for 71-101 minutes; starting the stirring type reactor stirrer again, wherein the rotating speed is 46-91 rpm, adding potassium triacontanol phosphate to ensure that the threshold value of hydrophilic-hydrophilic alcohol ester of the reaction liquid is 5-11, adjusting the pH value to 4.8-8.9, and keeping the temperature and standing for 70-110 minutes;
step 5, starting a stirrer in the stirring type reactor, setting the rotating speed to be 43-110 rpm, starting a repeated heater in the stirring type reactor, and setting the temperature in the stirring type reactor to be 4.625 × 102℃～9.620×102Keeping the temperature for 70-110 minutes, and then adding 3-methyltetrahydrochyseneCarrying out halogenation acylation reaction on the polymer terminated by 2-hydroxyethyl acrylate of furan, 1, 3-diisocyanatotoluene and tetrahydrofuran for 37-48 minutes; then adding potassium monoalkyl phosphate, starting a repeated heater in the stirring type reactor, setting the temperature in the stirring type reactor to be 121.6-177.6 ℃, adjusting the pH to be 4.8-8.9, adjusting the pressure to be 0.435-0.448 MPa, and reacting for 0.4-0.9 h; then reducing the pressure to 0MPa, reducing the temperature to 54.4-59.4 ℃, discharging, and putting into an injection molding machine to obtain the catalytic reaction filler 6-13.
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
The catalytic reaction filler 6-13 is prepared according to the following steps in parts by weight:
step 1: 252 parts of sodium ion-removed water and 44 parts of fatty amide polyoxyethylene ether (FAEO) are added into a stirring type reactor, a stirrer in the stirring type reactor is started, the rotating speed is set to be 45rpm, a repeated heater in the stirring type reactor is started, the temperature is raised to 60.4 ℃, 47 parts of dihydroxy succinic acid are added and stirred uniformly, the halogenation acylation reaction is carried out for 37 minutes, 43 parts of N-ethyl o/p-toluenesulfonamide is added, and the flow rate is 36.6m30.4 hour of xenon at/min; then 46 parts of N, O-bis (trimethylsilyl) acetamide was added to the stirred reactor, the repeated heater in the stirred reactor was again started to raise the temperature to 77.4 ℃ and the temperature was maintained for 37 minutes, and 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino group was added]49 parts of 9, 10-dioxo-2-anthracene sulfonic acid sodium salt, adjusting the pH value of the solution in the stirring type reactor to 4.8, and keeping the temperature for 37 minutes;
step 2: taking 51 parts of dysprosium nanoparticles, and carrying out ultrasonic treatment on the dysprosium nanoparticles for 0.4 hour under the power of 5.7736 KW; adding dysprosium nanoparticles into another stirring type reactor, and adding the dysprosium nanoparticles into the stirring type reactor according to the mass concentration44 parts of 1-amino-2-chloro-4-hydroxyanthraquinone at 47.9ppm, dysprosium nanoparticles dispersed, a repetitive heater in a stirred reactor was started to bring the solution temperature to 4.86 × 10 ℃, a stirrer in the stirred reactor was started and the stirring was continued at 4.84 × 102Stirring at rpm, adjusting pH to 4.8, stirring under constant temperature for 0.5 hr, stopping reaction, standing for 5.7 × 10 min to remove impurities, adding N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] methyl]46 portions of diethanolamine, adjusting the pH value to 1.6, eluting the formed precipitate with sodium ion water, passing through a centrifuge at the rotating speed of 4.129 × 103Solids were obtained at rpm, 2.22 × 102Drying at the temperature of DEG C, grinding and sieving with a 500-mesh sieve for later use;
and 3, step 3: taking 46 parts of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 43 parts of 3, 5-diaminobenzoic acid and 51 parts of dysprosium nano-particles after the step 2 treatment, after being mixed evenly, alpha radiation reflection irradiation is adopted, the energy of the alpha radiation reflection irradiation is 34.527MeV, the dose is 82.558kGy, the irradiation time is 46 minutes, obtaining a 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticle mixture with changed properties; placing the mixture of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles in another stirring type reactor, starting a repeated heater in the stirring type reactor, setting the temperature to be 45 ℃, starting a stirrer in the stirring type reactor, adjusting the pH to 4.8 at the rotating speed of 37rpm, and dehydrating for 46 minutes for later use;
and 4, step 4: modifying the 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] group obtained in step 3]Amino group]Methyl radical]Phenyl radical]Amino group]Uniformly mixing 9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles, and adding the mixture into the stirring type reactor in the step 1 at the flow velocity of 182.8 mL/min; starting a stirring type reactor stirrer, and setting the rotating speed to be 51 rpm; stirring for 4 minutes; then adding 2- [ (4-chloro-nitrophenyl) azo]-N- (2, 4-dimethylphenyl) -3-oxobutan34 portions of amide, starting a repeated heater in the stirring type reactor, raising the temperature to 81.3 ℃, adjusting the pH to 4.8, and introducing xenon with the ventilation volume of 36.4m3Min, keeping the temperature and standing for 71 minutes; starting the stirrer of the stirring type reactor again, wherein the rotating speed is 46.6rpm, adding 35 parts of potassium triacontanol phosphate to ensure that the threshold value of hydrophilic-hydrophilic alcohol ester of the reaction liquid is 5, adjusting the pH value to 4.8, and keeping the temperature and standing for 70 minutes;
step 5, starting the stirrer in the stirred reactor, setting the rotating speed to be 43rpm, starting the repeated heater in the stirred reactor, setting the temperature in the stirred reactor to be 4.625 × 102Keeping the temperature at 70 ℃ for 70 minutes, adding 53 parts of polymer capped by 2-hydroxyethyl acrylate of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and carrying out halogenation acylation reaction for 37 minutes; then 76 parts of 43ppm of mono-alkyl potassium phosphate is added, a repeated heater in the stirring type reactor is started, the temperature in the stirring type reactor is set to be 121.6 ℃, the pH value is adjusted to be 4.8, the pressure is 0.435MPa, and the reaction time is 0.4 hour; and then reducing the pressure to 0MPa, cooling to 54℃, discharging, and putting into an injection molding machine to obtain the catalyst reaction filler 6-13.
Wherein the diameter of the dysprosium nanoparticles is 51.3 μm.
Example 2
The catalytic reaction filler 6-13 is prepared according to the following steps in parts by weight:
step 1: adding 477 parts of sodium ion-removed water and 86 parts of fatty amide polyoxyethylene ether (FAEO) into a stirring type reactor, starting a stirrer in the stirring type reactor, setting the rotating speed to be 91rpm, starting a repeated heater in the stirring type reactor, raising the temperature to 61.4 ℃, adding 156 parts of dihydroxy succinic acid, uniformly stirring, carrying out halogenation acylation reaction for 48 minutes, adding 60 parts of N-ethyl o/p-toluenesulfonamide, and introducing the mixture at the flow rate of 77.2m30.1 hour of xenon at/min; then 103 parts of N, O-bis (trimethylsilyl) acetamide is added into the stirring reactor, the repeated heater in the stirring reactor is started again, the temperature is increased to 110.4 ℃, the temperature is kept for 48 minutes, and 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino is added]-9, 10-dioxo-2-anthracene110 parts of sodium sulfonate, adjusting the pH value of the solution in the stirring type reactor to 8.9, and keeping the temperature for 277 minutes;
step 2, taking 106 parts of dysprosium nanoparticles, carrying out ultrasonic treatment on the dysprosium nanoparticles for 0.1 hour under the power of 11.218KW, adding the dysprosium nanoparticles into another stirring type reactor, adding 86 parts of 1-amino-2-chloro-4-hydroxyanthraquinone with the mass concentration of 277.2ppm, dispersing the dysprosium nanoparticles, starting a repeated heater in the stirring type reactor to ensure that the temperature of the solution is 8.9 × 10 ℃, starting a stirrer in the stirring type reactor, and carrying out ultrasonic treatment on 8.97 × 10 parts of dysprosium nanoparticles2Stirring at rpm, adjusting pH to 8.9, stirring under constant temperature for 1.1 hr, stopping reaction, standing for 11.2 × 10 min to remove impurities, adding N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] methyl]86 portions of diethanolamine, adjusting the pH value to 2.2, eluting the formed precipitate by using sodium ion water, passing through a centrifuge at the rotating speed of *** × 103The solids obtained at rpm were 3.79 × 102Drying at the temperature of DEG C, grinding and sieving with a 620-mesh sieve for later use;
and 3, step 3: taking 69 parts of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 88 parts of 3, 5-diaminobenzoic acid and 106 parts of dysprosium nanoparticles treated in the step 2, after being mixed evenly, alpha radiation reflection irradiation is adopted, the energy of the alpha radiation reflection irradiation is 62.184MeV, the dose is 122.856kGy, the irradiation time is 71 minutes, obtaining a 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticle mixture with changed properties; placing the mixture of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles in another stirring type reactor, starting a repeated heater in the stirring type reactor, setting the temperature to be 91 ℃, starting a stirrer in the stirring type reactor, adjusting the pH to 8.9 at the rotating speed of 432rpm, and dehydrating for 60 minutes for later use;
and 4, step 4: modifying the 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] group obtained in step 3]Amino group]Methyl radical]Phenyl radical]Amino group]Uniformly mixing 9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles, and adding the mixture into the stirring type reactor in the step 1 at the flow velocity of 910.9 mL/min; starting a stirring type reactor stirrer, and setting the rotating speed to 91 pm; stirring for 8 minutes; then adding 2- [ (4-chloro-nitrophenyl) azo]77 parts of (E) -N- (2, 4-dimethylphenyl) -3-oxobutanamide, starting a double heater in a stirred reactor, heating to 118.5 ℃, adjusting the pH to 8.9, and introducing xenon at a flow rate of 77.9m3Keeping the temperature and standing for 101 minutes; starting the stirrer of the stirring type reactor again, wherein the rotating speed is 91rpm, adding 71 parts of triacontanol potassium phosphate to ensure that the threshold value of hydrophilic-hydrophilic alcohol ester of the reaction liquid is 11, adjusting the pH value to 8.9, and keeping the temperature and standing for 110 minutes;
and 5, step 5: starting the stirrer in the stirred reactor, setting the speed at 110rpm, and adding N- [ (5-methyl-1H-benzotriazole-1-yl) methyl group to the stirred reactor while stirring]86 parts of diethanolamine, starting a repeated heater in the stirred reactor, and setting the temperature in the stirred reactor at 9.620 × 102Keeping the temperature at 110 ℃ for 110 minutes, adding 97 parts of polymer terminated by 2-hydroxyethyl acrylate of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and carrying out halogenation acylation reaction for 48 minutes; then, 130 parts of 310ppm potassium monoalkyl phosphate is added, a repeated heater in the stirring reactor is started, the temperature in the stirring reactor is set to be 177.6 ℃, the pH value is adjusted to be 8.9, the pressure is 0.448MPa, and the reaction time is 0.9 hour; then reducing the pressure to 0MPa, reducing the temperature to 59.4 ℃, discharging, and putting into an injection molding machine to obtain the catalyst reaction filler 6-13.
Wherein the diameter of the dysprosium nanoparticles is 61.1 μm.
Example 3
The catalytic reaction filler 6-13 is prepared according to the following steps in parts by weight:
step 1: adding 285 parts of sodium ion-removed water and 62 parts of fatty amide polyoxyethylene ether (FAEO) into a stirring type reactor, starting a stirrer in the stirring type reactor, setting the rotating speed to be 70rpm, starting a repeated heater in the stirring type reactor, raising the temperature to 61.0 ℃,adding 120 parts of dihydroxy succinic acid, stirring uniformly, carrying out halogenation acylation reaction for 45 minutes, adding 50 parts of N-ethyl o/p-toluenesulfonamide, and introducing the mixture at the flow rate of 66.4m30.2 hour of xenon at/min; then 80 parts of N, O-bis (trimethylsilyl) acetamide is added into the stirring type reactor, the repeated heater in the stirring type reactor is started again, the temperature is increased to 90.5 ℃, the temperature is kept for 44 minutes, and 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino is added]90 parts of 9, 10-dioxo-2-anthracene sulfonic acid sodium salt, adjusting the pH value of the solution in the stirring type reactor to 7.0, and keeping the temperature for 95 minutes;
2, taking 85 parts of dysprosium nanoparticles, carrying out ultrasonic treatment on the dysprosium nanoparticles for 0.3 hour under the power of 7.400KW, adding the dysprosium nanoparticles into another stirring type reactor, adding 775 parts of 1-amino-2-chloro-4-hydroxyanthraquinone with the mass concentration of 79.8ppm, dispersing the dysprosium nanoparticles, starting a repeated heater in the stirring type reactor to ensure that the temperature of the solution is 7.74 × 10 ℃, starting a stirrer in the stirring type reactor, and carrying out ultrasonic treatment on 7.00 × 102Stirring at the rpm speed, adjusting the pH value to 7.2, and stirring for 0.8 hour under heat preservation; then stopping the reaction and standing for 80 minutes to remove impurities; adding the suspension to N- [ (5-methyl-1H-benzotriazol-1-yl) methyl]66 portions of diethanolamine, adjusting pH value to 1.9, eluting formed precipitate with sodium ion water, passing through centrifuge at 7.900 × 103Obtaining solid matter at rpm, 3.00 × 102Drying at the temperature of DEG C, grinding and sieving by a 600-mesh sieve for later use;
and 3, step 3: taking 60 parts of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 78 parts of 3, 5-diaminobenzoic acid and 90 parts of dysprosium nano-particles after the step 2 treatment, after being mixed evenly, alpha radiation reflection irradiation is adopted, the energy of the alpha radiation reflection irradiation is 50.500MeV, the dose is 100.000kGy, the irradiation time is 55 minutes, obtaining a 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticle mixture with changed properties; placing the mixture of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles in another stirring type reactor, starting a repeated heater in the stirring type reactor, setting the temperature to be 80 ℃, starting a stirrer in the stirring type reactor, regulating the pH to be 7.5 at the rotation speed of 200rpm, and dehydrating for 55 minutes for later use;
and 4, step 4: modifying the 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-methylphenyl) sulfonyl ] group obtained in step 3]Amino group]Methyl radical]Phenyl radical]Amino group]Uniformly mixing 9, 10-anthracene dioxide-2-sulfonic acid, 3, 5-diaminobenzoic acid and dysprosium nanoparticles, and adding the mixture into the stirring type reactor in the step 1 at the flow velocity of 320.5 mL/min; starting a stirring type reactor stirrer, and setting the rotating speed to be 60 rpm; stirring for 6 minutes; then adding 2- [ (4-chloro-nitrophenyl) azo]60 parts of (E) -N- (2, 4-dimethylphenyl) -3-oxobutanamide, starting a repeated heater in a stirring reactor, heating to 100.0 ℃, adjusting the pH to 8.1, and introducing xenon at an aeration rate of 70.5m3Min, keeping the temperature and standing for 90 minutes; starting the stirring 85.77936 of the stirring type reactor again, adjusting the pH to 8.2, and keeping the temperature and standing for 85 minutes;
step 5, starting the stirrer in the stirring type reactor, setting the rotating speed to be 100rpm, starting the repeated heater in the stirring type reactor, setting the temperature in the stirring type reactor to be 6.250 × 102Keeping the temperature at 85 ℃ for 85 minutes, adding 80 parts of polymer blocked by 2-hydroxyethyl acrylate of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and carrying out halogenation acylation reaction for 40 minutes; then adding 89 parts of 150ppm of monoalkyl phosphate potassium salt, starting a repeated heater in the stirring type reactor, setting the temperature in the stirring type reactor to be 150.5 ℃, adjusting the pH to be 8.5, adjusting the pressure to be 0.440MPa, and reacting for 0.7 hour; then reducing the pressure to 0MPa, reducing the temperature to 55.0 ℃, discharging, and putting into an injection molding machine to obtain the catalyst reaction filler 6-13.
Wherein the diameter of the dysprosium nanoparticles is 58.0 μm.
Comparative example:
the control example is a commercially available reaction-promoting filler of a certain brand.
Comparing the use effects of the catalytic reaction fillers 6-13 prepared in the embodiments 1-3 with those of the comparative example. The high temperature resistance and the carbon tetrachloride degradation rate improvement efficiency of the two are counted, and the result is shown in table 1.
As can be seen from Table 1, the indexes of the catalytic reaction filler 6-13 prepared by the invention, such as high temperature resistance, carbon tetrachloride degradation rate improvement efficiency and the like, are superior to those of products produced by the prior art.
The diameter of the large opening end of the air inlet cover 6-1 is 10-20 cm: the air inlet cover 6-1 is made of stainless steel; the communicating chamber 6-2 is made of stainless steel and has a diameter of 5-10 cm.
The model of the temperature sensor 6-8 is PT 100.
The number of the nonlinear pore channels 6-3-1 on the surface of the nonlinear pore plate 6-3 is 10-30, the pore diameter inside the nonlinear pore channels 6-3-1 is 5-10 mm, and the nonlinear pore channels 6-3-1 are distributed according to a Sine-Gordon nonlinear equation. The duct track 6-3-2 of the nonlinear duct 6-3-1 is designed according to a Sine-Gordon nonlinear equation which is as follows:
the ducted locus 6-3-2 causes the passing air flow to assume a rotating vortex, and the flow velocity thereof increases in sequence from the circumference to the center of the circle.
The diameter of the large opening end of the nitrogen cracking reactor 6-4 is 10-20 cm; the diameter of the cracking heating power annular tube 6-5 is 10-20 cm; the number of the flame spray melting heads 6-6 is 10-20.
The buffer plates 6-7 are high-temperature resistant ceramic round plate structures; the ultrasonic oscillation plate 6-9 is of a disc structure, the diameter of the ultrasonic oscillation plate is 10-20 cm, the thickness of the ultrasonic oscillation plate is 10-20 m, and the diameter of an upper through hole of the ultrasonic oscillation plate is 2-10 mm; the diameter of the through hole on the surface of the ultrasonic vibration plate 6-9 is 2-10 mm.
The working process is as follows:
step 1: the waste gas containing carbon tetrachloride enters the equipment from an air inlet hood 6-1 at one side of the gas phase reaction cracker, and the waste gas containing carbon tetrachloride is gathered and passes through a communicating chamber 6-2 under the gathering action of a horn mouth shape of the air inlet hood 6-1, then passes through a nonlinear orifice plate 6-3 and enters a nitrogen cracking reactor 6-4;
step 2: when the air flows through the nonlinear pore plate 6-3, due to the through holes of the nonlinear pore channel 6-3-1 on the nonlinear pore plate 6-3, the air flows are distributed according to a Sine-Gordon nonlinear equation, so that the air flows form a plurality of strands of rotary eddy currents, and the flow velocity of the air flows is increased in sequence from the circumference to the circle center; forming a specific gas stream through a nitrogen cracking reactor 6-4;
and 3, step 3: after the carbon tetrachloride-containing waste gas enters a nitrogen cracking reactor 6-4, high-pressure nitrogen is introduced from the outside through a pressurized nitrogen pipe 6-12, the nitrogen is heated to 86-92 ℃ by a heater 6-4-3 and enters a nitrogen releaser 6-4-5 through a nitrogen branch pipe 6-4-4, a buffer chamber 6-4-9, a rotating shaft 6-4-6 and a round bracket 6-4-7; meanwhile, the motor 6-4-1 drives the nitrogen releaser 6-4-5 to rotate at the rotating speed of 10-50 rpm through the rotating shaft 6-4-6 and the round bracket 6-4-7; the high-pressure nitrogen released by the nitrogen releaser 6-4-5 reacts with carbon tetrachloride under the action of high temperature to generate diazomethane gas (H)2CNN) and chlorine gas (Cl)2)；
And 4, step 4: the residual carbon tetrachloride-containing gas passes through flame spray melting heads 6-6 arranged in a combustion area, and carbon tetrachloride components in the carbon tetrachloride-containing waste gas are ignited by combustion;
and 5, step 5: the gas containing carbon tetrachloride which is not combusted and decomposed is buffered by a buffer plate 6-7, a plurality of gas flows are uniformly formed and enter a medium reaction filler 6-13, the carbon tetrachloride component is adsorbed, and the treated gas enters an ultrasonic oscillation plate 6-9;
and 6, step 6: meanwhile, the temperature sensor 6-8 monitors the combustion temperature of the flame spraying and melting head 6-6 in real time and feeds the temperature back to the control center;
and 7, step 7: the gas entering the ultrasonic vibration plates 6-9 is subjected to the cracking action of high-frequency vibration waves to decompose carbon tetrachloride.
Claims (8)
1. A reaction cracker comprises a funnel-shaped air inlet cover (6-1) and a cylindrical cracker furnace wall (6-10), and is characterized by also comprising a temperature sensor (6-8), wherein the large opening end of the air inlet cover (6-1) is arranged at the left end of the inner cavity of the cracker furnace wall (6-10) towards the left, and the large opening end of the air inlet cover (6-1) is connected with the left end of the cracker furnace wall (6-10); a communicating chamber (6-2), a nonlinear pore plate (6-3), a nitrogen cracking reactor (6-4), a cracking heating power annular pipe (6-5), a flame spray melting head (6-6), a buffer plate (6-7), a medium reaction filler (6-13) and an ultrasonic oscillation plate (6-9) are sequentially and fixedly arranged in an inner cavity of the furnace wall (6-10) of the cracker from left to right;
the communicating chamber (6-2) is of a hollow tubular structure, the left end of the communicating chamber is fixedly connected with the small opening end of the air inlet cover (6-1), the right end of the communicating chamber is fixedly connected with the left end face of the nonlinear pore plate (6-3), and nonlinear pore channels (6-3-1) are arranged on the surface of the nonlinear pore plate (6-3) in a distributed manner;
the small end of the nitrogen cracking reactor (6-4) is fixedly connected to the central area of the nonlinear orifice plate (6-3), the small end of the nitrogen cracking reactor (6-4) corresponds to the peripheral area of the communicating chamber (6-2), and the large end of the nitrogen cracking reactor (6-4) is arranged towards the cracking heating power annular pipe (6-5);
the nitrogen cracking reactor (6-4) comprises a motor (6-4-1), a pressurized nitrogen pipe (6-12), a nitrogen releaser (6-4-5), a truncated cone-shaped outer cover (6-4-8), and the pressurized nitrogen pipe (6-12) penetrates through the outer part of the furnace wall (6-10) of the cracker, the inner end of the pressurized nitrogen pipe is connected with the buffer chamber (6-4-9) through a nitrogen branch pipe (6-4-4), the inner end of the pressurized nitrogen pipe (6-12) is provided with a heater (6-4-3), and the outer end of the pressurized nitrogen pipe is connected with a nitrogen bottle; a cylindrical rotating shaft (6-4-6) is arranged on the axis in the outer cover (6-4-8), a buffer chamber (6-4-9) fixedly connected to the inside of the communicating chamber (6-2) is arranged on the outer side of the small opening end of the outer cover (6-4-8), the inner end of the buffer chamber (6-4-9) is sleeved outside the inner end of the rotating shaft (6-4-6), the motor (6-4-1) is positioned in the communicating chamber (6-2) and fixedly connected with the outer end of the buffer chamber (6-4-9), an output shaft of the motor (6-4-1) penetrates through the buffer chamber (6-4-9) to extend into the inner end of the rotating shaft (6-4-6) and is fixedly connected with the rotating shaft (6-4-6) through a plurality of radially-arranged connecting rods, the two ends of the rotating shaft (6-4-6) are respectively fixedly connected with a circular support (6-4-7) which can rotate in the outer cover (6-4-8), so that the circular support (6-4-7) consists of an annular hollow pipeline positioned at the outer ring and a communicating pipeline connecting the annular hollow pipeline and the inner cavity of the rotating shaft (6-4-6), and the outer diameter of the annular hollow pipeline of the circular support (6-4-7) positioned at one side of the large opening end of the outer cover (6-4-8) is larger than that of the annular hollow pipeline of the circular support (6-4-7) positioned at one side of the small opening end of the outer cover (6-4-8); the plurality of nitrogen releasers (6-4-5) are arranged around the rotating shaft (6-4-6), the nitrogen releasers (6-4-5) are of hollow columnar structures, and two ends of each nitrogen releaser (6-4-5) are respectively communicated with the annular hollow pipelines of the two circular brackets (6-4-7); the surface of the nitrogen releaser (6-4-5) is provided with a plurality of through holes communicated with the inner cavity of the nitrogen releaser;
the cracking heating power annular pipe (6-5) is fixedly connected with a fuel gas supply pipeline communicated with an inner cavity of the cracking heating power annular pipe, and the fuel gas supply pipeline extends to the outside of the furnace wall (6-10) of the cracker; the flame spray-melting heads (6-6) are circumferentially and uniformly fixedly connected to the right end face of the cracking heating power annular pipe (6-5);
the buffer plate (6-7) is of a plate-shaped structure, and through holes which are communicated from left to right are formed in the surface of the buffer plate (6-7) in a distributed manner;
the temperature sensor (6-8) is positioned below the catalytic reaction filler (6-13);
the ultrasonic oscillation plate (6-9) is provided with a plurality of through holes all over the surface, and an ultrasonic vibrator and an ultrasonic generator are arranged in the ultrasonic oscillation plate;
an air outlet (6-11) is arranged at the right end opening of the furnace wall (6-10) of the cracker.
2. The reaction cracker according to claim 1, wherein the reaction promoting filler (6-13) comprises the following components in parts by weight: 252-477 parts of sodium-removed ionized water, 44-86 parts of fatty amide polyoxyethylene ether, 47-156 parts of dihydroxy succinic acid, 43-60 parts of N-ethyl O/p-toluenesulfonamide, 46-103 parts of N, O-bis (trimethylsilyl) acetamide, 1-amino-9, 10-dihydro-4- [ (2-tolyl) amino ] -9, 10-dioxo-2-anthracenesulfonic acid sodium salt, 49-110 parts of 1-amino-9, 10-dihydro-4- [ [4- [ [ methyl [ (4-tolyl) sulfonyl ] amino ] methyl ] phenyl ] amino ] -9, 10-dianthracene dioxide-2-sulfonic acid, 46-69 parts of 3, 5-diaminobenzoic acid, 51-106 parts of dysprosium nanoparticles, 44-86 parts of 1-amino-2-chloro-4-hydroxyanthraquinone, 34-77 parts of 2- [ (4-chloro-nitrophenyl) azo ] -N- (2, 4-dimethylphenyl) -3-oxobutanamide, 35-71 parts of potassium triacontanol phosphate, 46-86 parts of N- [ (5-methyl-1H-benzotriazol-1-yl) methyl ] diethanolamine, 53-97 parts of a 2-hydroxyethyl acrylate end-capped polymer of 3-methyltetrahydrofuran, 1, 3-diisocyanatotoluene and tetrahydrofuran, and 76-130 parts of monoalkyl phosphate potassium salt with the mass concentration of 43-310 ppm.
3. The reaction cracker according to claim 2, wherein the dysprosium nanoparticles have a particle size of 51.3 μm to 61.1 μm.
4. A reaction cracker according to claim 3, characterised in that the large open end diameter of the air inlet hood (6-1) is 10-20 cm: the air inlet cover (6-1) is made of stainless steel; the communicating chamber (6-2) is made of stainless steel and has a diameter of 5-10 cm.
5. A reaction cracker according to claim 4, characterised in that said temperature sensor (6-8) is of the type PT 100.
6. The reaction cracker according to claim 5, wherein the number of the nonlinear pore channels (6-3-1) on the surface of the nonlinear pore plate (6-3) is 10 to 30, the pore diameter inside the nonlinear pore channels (6-3-1) is 5 to 10mm, and the nonlinear pore channels (6-3-1) are arranged according to a Sine-Gordon nonlinear equation.
7. The reaction cracker according to claim 6, wherein the diameter of the large mouth end of the nitrogen cracking reactor (6-4) is 10-20 cm; the diameter of the cracking heating power annular tube (6-5) is 10-20 cm; the number of the flame spray melting heads (6-6) is 10-20.
8. The reaction cracker according to claim 7, wherein the buffer plate (6-7) is a refractory ceramic circular plate structure; the ultrasonic oscillation plate (6-9) is of a disc structure, the diameter of the ultrasonic oscillation plate is 10-20 cm, the thickness of the ultrasonic oscillation plate is 10-20 m, and the diameter of a through hole in the upper part of the ultrasonic oscillation plate is 2-10 mm; the diameter of the through hole on the surface of the ultrasonic vibration plate (6-9) is 2-10 mm.
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