TWM566203U - System for production of silane with catalyst enhancement and total recycle of byproducts - Google Patents

Abstract

A catalyst for increasing the formation of decane and the complete recovery of by-product by process, wherein: the separation and purification of the decane mixture generated by the newly developed and designed purification system and technology is separated from the solid raw materials involved in the reaction, and then The methane is separated from the gas by its physical properties at a low temperature gas-liquid separation, and the methane methane fractionation system is used to recover the ammonia raw material in the methane and the purification of the methane and the removal of the impurities, and the gas-liquid separation The ethane and ammonia feedstocks are also fractionated and purified by a cesium ethane distillation system. The enthalpy conversion rate is improved with the unique catalyst technology developed, and new feed methods and equipment are developed, and ammonia is recovered. It is used again as a raw material for the reaction, thereby stabilizing the production capacity and purification process of methane and hydrazine.

Description

Catalyst to increase the formation of decane reaction and its system by-product recovery

This creation is about a system for the catalyst to increase the formation of decane and its complete recovery of by-products.

According to the bismuth magnesium alloy method, it is a known industrial process for the synthesis of semiconductor special gas raw materials such as methane and cesium. It is known to use yttrium magnesium alloy method to produce decane and its ethane reaction. The selection rate is too low, and the purity and cost of the high-purity methane production technology are reduced, and the environmental impact caused by the reaction slag storage and the complicated and energy-intensive processing procedures are used to produce decane by the bismuth magnesium alloy method. The process is difficult to meet economic benefits. Therefore, the improved bismuth magnesium alloy method is gradually developed, and the selectivity, yield and purity of the oxirane reaction production are improved, but the disposal problem of the reaction slag is still hindered by the decane production method, and There are still many technical-related problems in the production process. For example, decane is oxidized to form cerium oxide particles or crystals due to the operating conditions and environment of the process, resulting in a decrease in equipment efficiency and production efficiency and an increase in the frequency of cleaning and maintenance. Therefore, this creative design and development of advanced production technology and equipment systems, to make up for and improve the use of improved bismuth magnesium alloy method for the production of decane technology and process defects, and then develop into a perfect high-purity decane production methods and systems.

In view of this, the creator has been engaged in the manufacturing development and design experience of related products for many years. After detailed design and careful evaluation, the author has finally achieved a practical and practical creation.

The technical problem to be solved by the present invention is to provide a system for the catalyst to increase the formation of decane reaction and the complete recovery of by-product by-products in view of the above-mentioned shortcomings in the prior art.

The monooxane reaction system comprises a magnesium telluride powder suction bucket, a magnesium telluride automatic feeding device, a jacketed reaction tank, a condenser and a pneumatic pump, and the magnesium telluride powder suction bucket stores magnesium telluride and touch in an anaerobic state. The medium, and the mixing ratio of the catalyst is 15% to 30% of magnesium telluride, and the catalyst comprises 20~50wt% of tantalum powder and 50~80wt% of metal powder to form a bimetallic composite, and the magnesium telluride is automatically The feeding device is connected between the magnesium telluride powder suction bucket and the jacketed reaction tank, and the jacketed reaction tank is equipped with a mixer, and the top end of the jacketed reaction tank is connected to the condenser and connected to the bottom end The pneumatic pump, the jacketed reaction tank is first put into ammonium chloride powder, and is subjected to closed nitrogen replacement and vacuum deaeration operation, and then introduced into pure ammonia to control condensation of -30 ° C refrigerant to form liquid ammonia, and start the mixer. Pre-dissolving ammonium chloride and liquid ammonia, and inputting magnesium telluride and catalyst into the jacketed reaction tank at a fixed rate by the magnesium telluride automatic feeding device, thereby triggering reaction to generate methane and hydrogen gas mixture and The condenser produces and is supplemented by a 90°C heat medium. The liquid ammonia and the hydrazine ethane are regenerated and recovered through the condenser, and the slag after the reaction is discharged from the pneumatic pump and stored in a slag buffer tank, and a gas-liquid separation tank is connected to the condenser, and The upper end of the gas-liquid separation tank is connected to a methane temporary storage tank for storing vaporized helium methane, and the gas-liquid separation tank is connected with a temporary storage tank for storing liquefied ethane and liquid ammonia. The alkane distillation system comprises a depurinating ethane column, an ammonia purification column and an ethane purification column, the cesium ethane temporary storage tank is connected to the deuterium ethane column, and the upper end of the deuteration ethane column is connected to the ammonia purification tower And the lower end of the deuterated ethane column is connected to the hydrazine ethane purification tower, and the deuterated ethane column is separated into the ammonia purification tower by a pressure of 18 to 24 kg/cm ² and a temperature of 25 ° C to 70 ° C, and 矽The ethane is separated into the hydrazine ethane purification tower, and the ammonia purification tower separates a small amount of hydrazine methane to the hydrazine methane storage tank by a temperature difference, and the hydrazine ethane purification tower further purifies the hydrazine at a temperature of 30 ° C to 100 ° C. Ethane, and the purified cesium ethane is stored in a liquefied ethane buffer tank, thereby making 矽Alkoxy the reaction selectivity can reach 5 ~ 25vol%, and the ammonia is separated with the silicon oxide purification column purified liquid ammonia to an ammonia storage column buffer tank.

Wherein, the condenser is sequentially connected with a second condenser and a third condenser, and the preliminary decane separation is performed by using physical properties different in boiling temperature of each substance, and the first step is introduced at a constant pressure of 2-7 kg/cm ² . The second condenser was condensed at -30 ° C to condense with the third condenser at -75 ° C to form liquid helium ethane and liquefied ammonia, and gaseous methane and hydrogen, and separated in the gas-liquid separation tank.

Wherein, a filter is installed between the condenser and the second condenser, and the ammonia and the ethane which are cooked after the reaction is completed due to the methane gas mixture generated during the reaction of the jacketed reaction tank A small amount of raw material or slag powder carried by the differential pressure gas stream is used to intercept particles larger than 3 to 100 μm.

Among them, the liquefied ethane ethane buffer barrel can store 矽 ethane up to 4N8 (99.998%) purity, and the 矽 ethane can be liquefied by vacuum low temperature -75 ° C condensation when 矽 ethane filling demand The 矽 缓冲 buffer tank is filled into at least one cylinder, and the purification of a small amount of ethane and the removal of a trace amount of impure gas can also be performed by the same vacuum condensation technique.

The methane methane storage tank is connected with a helium methane fractionation system, and the methane methane fractionation system comprises a helium methane recovery tower, a methane molecular sieve and a methane purification tower, and the methane recovery tower is connected to the methane molecular sieve at the upper end. And the methane methane purification tower is connected to the methane methane purification tower, and the methane recovery tower stores the majority of ammonia in the liquid ammonia buffer tank at a pressure of 8-15 kg/cm ² and a temperature of -60 ° C to 40 ° C. The fractionated methane gas and a small amount of ammonia are adsorbed by the 3A~5A methane molecular sieve to remove ammonia and other impurities, and the methane is introduced into the methane purification tower and is cooled at a temperature of -160 ° C to -50 ° C. The contained hydrogen is separated and separated, and the purified methane is stored in a liquefied methane buffer tank.

Wherein, the enthalpy methane stored in the liquefied methane buffer tank can reach a purity of 6N (99.9999%), and the liquefied methane buffer tank adopts an inner and outer double-layer structure, and the inner layer stores liquefied methane, and the outer layer is vacuumed. A ring coil is arranged around the ring coil, and the temperature and pressure control of the refrigerant flow through the ring coil is up to -50 ° C, and the refrigerant is used as the condensation of helium methane when needed, and the liquefied methane buffer tank A vaporizer is connected to the methane filling requirement, and the methane is introduced into the vaporizer and controlled by a steady flow of -30 ° C refrigerant to a finished press, and pressurized by the finished press to 100~ A pressure of 160 kg/cm ² fills the methane methane into at least one cylinder or at least one tank car.

Wherein, the slag buffer tank is connected in sequence with a centrifugal filter, an ammonia aqueous solution buffer tank, a magnesium hydroxide filter and an ammonia water buffer tank, and the centrifugal filter and the magnesium hydroxide filter are simultaneously connected to have a dry a grinding device, and a high-pressure forming brick system is connected with the dry milling device, and the slag discharged into the slag buffer tank is firstly converted into insoluble magnesium hydroxide by adding water and stirring in the jacketed reaction tank. a solid powder and a salt product dissolved therein, and flowing the slurry slag into the centrifugal filter under the uninterrupted stirring of the slag buffer tank, and using the centrifugal filter to detach the liquid to make the slag The liquid portion flows to the buffer solution tank of the ammonia aqueous solution, and the solid portion is discharged to the dry milling device, and the dry milling device is heated and dried by the electric heating and the spiral stirring to remove the ammonia and detach the ammonia, and discharged to the high pressure. The forming brick system is used as a raw material for brick making, and the ammonia aqueous solution buffer tank is added with ammonia water, and the magnesium chloride in the solution can be reacted to be converted into ammonium chloride and magnesium hydroxide powder, and then passed through the hydrogen. Magnesium filter accuracy to 1 ~ 30μm The magnesium hydroxide powder particles are filtered and discharged to the dry milling device to prevent the solid powder particles from entering the ammonia water buffer tank, and only the ammonia water is stored in the ammonia water buffer tank.

Wherein, the ammonia buffer tank is connected with an ammonia separation and recovery system, the ammonia separation and recovery system is connected to the ammonia buffer tank by an ammonia recovery tower, and an ammonia distillation tower is connected to the upper end of the ammonia recovery tower, and the ammonia recovery tower is 0. Separating the ammonium chloride solution and the aqueous ammonia solution at a pressure of 5 kg/cm ² and a temperature of 50 ° C to 145 ° C, and discharging the aqueous ammonia solution from the top of the ammonia recovery column to the ammonia rectification column, and at the ammonia Purification and separation of ammonia and water at a temperature of -30 ° C to 130 ° C in the distillation column, and the purified ammonia at the top of the ammonia distillation column is stored in an ammonia raw material barrel for recycling, and the ammonia distillation tower is used in the tower. The bottom separated water and trace ammonia are returned to the ammonia buffer tank, and the ammonia recovery tower is sent from the ammonium chloride solution separated from the bottom of the tower to a multi-effect evaporation system, and the multi-effect evaporation system is passed through the multi-effect evaporation system at 120 ° C to 160 ° C. The steam is heated to cause the ammonium chloride solution to vaporize the moisture contained in the ammonium chloride solution, and the ammonium chloride has a water content of less than 1% by weight, and is recovered by a dryer as a reaction of the jacketed reaction tank. The raw material is used, and the water vapor is recovered by a recycled water buffer tank to provide the jacket The reaction tank is used in the slag solvent after the reaction.

Wherein, after the slag material is emptied, the jacketed reaction tank is cleaned by a nitrogen gas blow, vacuumed, and heated at a temperature of 90 ° C to clean the tank and effectively remove moisture to avoid moisture. It affects the oxidation reaction of decane formed in the next reaction with water to form cerium oxide, thereby increasing the decane reaction rate.

Wherein, the process equipment of the decane reaction whole process is connected and connected to a tail gas treatment system by a plurality of exhaust gas discharge lines, the tail gas treatment system comprises a washing tower, a high temperature oxidizer and a filtering device, and the tail (waste) gas is The composition containing ammonia and decane gas is branched to each stage of the tail gas treatment system, and the washing tower is adsorbed and removed by water for ammonia gas, and then formed. The ammonia water is introduced into the buffer solution of the ammonia solution for recovery, and is used as an additive for ammonium chloride salt conversion, and a trace amount of tail gas is discharged from the top of the tower to the high temperature oxidizer for destruction of decane gas, thereby converting it into cerium oxide. The non-hazardous substances are then intercepted and collected by the filtering equipment of the exhaust gas treatment system.

The first main purpose of this creation is to use a modified bismuth magnesium alloy method for decane production, to improve the conversion of ethane with the unique catalyst technology developed, and to implement new feeding methods and equipment for development. Improve the reaction rate of the raw materials and reduce the impact of the reaction system on the solid powder blockage problem, and effectively control and optimize the environment generated by the decane reaction with improved production operation technology to increase the production capacity of cesium ethane.

The second main purpose of this creation is to separate the decane mixture generated by the reaction and the solid raw material involved in the reaction by the newly developed separation and purification system and technology, and then carry out the methane from the gas mixture according to its physical properties. Low-temperature gas-liquid separation, and the recovery of ammonia raw materials in methane and the purification of methane and its impurities are removed using the methane methane fractionation system, and then stored as methane in a low-temperature vacuum mode, and separated by gas-liquid separation. The ethane and ammonia feedstocks are also fractionated and purified by a hydrazine distillation system, and the ammonia is recovered for use as a reaction raw material, thereby stabilizing the production and purification processes of hydrazine methane and hydrazine ethane, and effectively reducing production. cost.

The third main purpose of the creation is that the slag produced by the reaction is added to the water as a solvent after the end of the decane reaction, so that part of the slag content can be converted into a salt substance and dissolved in the ammonia water, and the slurry can be obtained. The fluid is used for subsequent separation and recovery, and a newly designed separation method is adopted. The solid-liquid separation of the slurry slag is carried out by centrifugal separation technology, and the separated solid product is dried to be used as a brick raw material. The liquid fluid is converted into a recoverable salt aqueous ammonia solution by adding ammonia, and the ammonium chloride salt solution, ammonia and water are separated by using a distillation system. Purification and recovery. The ammonium chloride salt solution is then subjected to moisture removal treatment and drying using a high-efficiency evaporation system, and is recycled as a raw material for the decane production reaction. In order to effectively reduce the environmental impact and production cost of slag storage.

The fourth main purpose of this creation is that the tail (waste) gas generated by the process is uniformly integrated into the exhaust gas treatment system through the exhaust gas discharge pipeline, and the ammonia gas in the exhaust gas is absorbed and removed by the ammonia adsorption removal technology and recovered as a salt solution. The addition liquid is used, and other decane waste gas is treated by oxidation treatment of the tail gas treatment system to be converted into non-hazardous gas or slag for disposal to reduce environmental pollution and harm.

Other objects, advantages and novel features of the present invention will become more apparent from the detailed description and the accompanying drawings.

[this creation]

11‧‧‧ decane reaction system

111‧‧‧Magnesium magnesium powder bucket

112‧‧‧Magnesium telluride automatic feeding device

113‧‧‧ jacketed reaction tank

114‧‧‧Condenser

115‧‧‧Pneumatic pump

116‧‧‧Mixer

117‧‧‧second condenser

118‧‧‧ Third condenser

119‧‧‧Filter

12‧‧‧ gas-liquid separation tank

13‧‧‧矽ethane distillation system

131‧‧‧Deacetylation tower

132‧‧‧Ammonia Purification Tower

133‧‧‧ 矽 ethane purification tower

134‧‧‧Liquid ammonia buffer tank

14‧‧‧Slag buffer tank

15‧‧‧ 矽 暂 temporary storage tank

16‧‧‧ Liquefied ethane buffer bucket

17‧‧‧Cylinders

21‧‧‧矽methane temporary storage tank

22‧‧‧矽Methane fractionation system

221‧‧‧矽Methane Recovery Tower

222‧‧‧矽Methane molecular sieve

223‧‧‧矽 methane purification tower

23‧‧‧ Liquefied methane buffer bucket

231‧‧‧Vaporizer

232‧‧‧ ring coil

24‧‧‧Finished Press

25‧‧‧Cylinders

26‧‧‧ tank truck

31‧‧‧ centrifugal filter

32‧‧‧Ammonia solution buffer tank

33‧‧‧Magnesium hydroxide filter

34‧‧‧Ammonia buffer bucket

35‧‧‧Dry grinding device

351‧‧‧High Pressure Forming Brick System

36‧‧‧Ammonia Separation and Recovery System

361‧‧‧Ammonia recovery tower

362‧‧‧Ammonia distillation tower

37‧‧‧Ammonia material barrel

38‧‧‧Multi-effect evaporation system

381‧‧‧Dryer

39‧‧‧Recycled water buffer tank

41‧‧‧Exhaust gas discharge pipeline

42‧‧‧Exhaust gas treatment system

421‧‧·washing tower

422‧‧‧High temperature oxidizer

423‧‧‧Filter equipment

The first picture shows the structure and flow chart of the ethane process.

Figure 2 is the structure and flow chart of the methane process.

Fig. 3 is a schematic view showing the structure of the liquefied methane buffer tank of the present invention.

Figure 4 is the structure and flow chart of the slag recycling process.

Figure 5 is the structure and flow chart of the tail gas recovery process of this creation.

In order to enable your review committee to have a better understanding and understanding of the purpose, characteristics and efficacy of this creation, please refer to the following [Simplified Description of the Drawings] for details:

First, please see the system shown in Figure 1, a catalyst to increase the formation of decane reaction and its system by-product recovery, including: a decane reaction system 11, a gas-liquid separation tank 12 and an ethane distillation system 13. The monooxane reaction system 11 includes a magnesium telluride powder suction drum 111, a magnesium telluride automatic feeding device 112, a jacketed reaction tank 113, a condenser 114, and a pneumatic pump 115. The magnesium telluride powder absorption tank 111 The magnesium oxide (Mg ₂ Si) and the catalyst are stored in an anaerobic state, and the anaerobic state is vacuum-filled and nitrogen-substituted after the sealing is sealed, and the mixing ratio of the catalyst is 15% to 30% of the magnesium telluride. The catalyst comprises a bimetallic composite of 20 to 50 wt% of bismuth powder (Si) and 50 to 80 wt% of metal powder, wherein the metal powder may be a metal element of an alkali metal group or an alkaline earth metal group, or may be used. a metal element in the transition metal, such as iron (Fe), or an alloy of elements in the group IIIA to VIA, and the magnesium telluride automatic feeding device 112 is connected to the magnesium telluride powder suction drum 111 and the jacketed reaction tank 113. Between the jacketed reaction tank 113 is equipped with a mixer 116, and the jacket type The top end of the reaction tank 113 is connected to the condenser 114 and connected to the pneumatic pump 115 at the bottom end, and the jacketed reaction tank 113 is first charged with ammonium chloride (NH ₄ Cl) powder, and is subjected to closed nitrogen replacement and vacuum deaeration operation. After introducing pure ammonia (NH ₃ ), controlling the condensation of the -30 ° C refrigerant to form liquid ammonia, and starting the mixer 116 to pre-dissolve the ammonium chloride and the liquid ammonia, so that the ammonium chloride is dissolved in the liquid ammonia to form ammonia and Chloride salt ion, and maintain the continuous operation of the mixer 116 to the clearance in the tank after the end of the reaction, in order to avoid the uneven dispersion of the powder during the reaction or the solidification and agglomeration caused by the reaction, and the magnesium carbide automatically enters The material device 112 inputs magnesium telluride and the catalyst into the jacketed reaction tank 113 at a fixed rate, that is, the magnesium telluride and the catalyst powder are fixed at a fixed rate of 0 to 150 kg/h, and a small amount of liquid ammonia controlled by the flow rate is used as a load. The fluid is evenly introduced into the jacketed reaction tank 113 to react with ammonium chloride, thereby preventing the magnesium halide powder from splashing when it comes into contact with the liquid ammonia in the tank, and causing the powder to adhere to the pipeline or the tank wall. Gradually lead to blockage of the pipeline, decane generation The process is an exothermic reaction. Therefore, the heat removal of the refrigerant at -30 ° C is continued in the reaction process in order to maintain the reaction temperature. In the course of the reaction, the liquid ammonia is also vaporized by the heat generated by the reaction, and The generated decane floats out of the jacketed reaction tank 113, resulting in a decrease in the reaction rate or a termination of the reaction. In order to maintain the amount of liquid ammonia during the reaction, the ammonia is condensed through the condenser 114 at -30 ° C. Re-liquefying back to the jacketed reaction tank 113, thereby triggering the reaction to form a mixture of helium methane (SiH4) and hydrogen (H ₂ ) and producing through the condenser 114, most of the produced Since the physical properties of the alkane are similar to those of ammonia, the condenser 114 is condensed and reliquefied back into the jacketed reaction vessel 113. Therefore, after the completion of the decane reaction, the liquid ammonia and the reaction involved in the reaction are required. The ruthenium ethane therein is recovered as much as possible, so that the refrigerant in the condenser 114 is converted to a heat medium at 90 ° C, so that the liquid ammonia and hydrazine in the jacketed reaction tank 113 can be stably heated and vaporized. With 90°C heat medium The liquid ammonia after the auxiliary reaction is digested with hydrazine ethane (Si ₂ H ₆ ) and recovered through the condenser 114. The proportion of the reaction raw materials used is usually determined by the weight of magnesium hydride, and magnesium hydride 1: ammonium chloride. 3~6: Liquid ammonia 9~12 is taken, and the reaction formula is: 矽methane reaction equation is as follows (main reaction): Mg ₂ Si _(s) +4NH ₄ Cl _(s) +8NH _3(l) →SiH _{4 (g)} +2 (MgCl ₂ ̇6NH ₃ ) _(s)

The enthalpy reaction equation is as follows (side reaction): 2Mg ₂ Si _(s) +8NH ₄ Cl _(s) +16NH _3(l) →Si ₂ H _6(g) +4(MgCl ₂ ̇6NH ₃ ) _(s) +H _2(g)

The slag after the reaction is discharged from the pneumatic pump 115 and stored in a slag buffer tank 14. The slag discharged into the slag buffer tank 14 is stirred with water in the jacketed reaction tank 113 to partially convert it into insoluble solvent. The magnesium hydroxide solid powder and the salt product dissolved therein, wherein the jacketed reaction tank 113 is subjected to nitrogen purge, vacuuming, and temperature rise of the heat medium at 90 ° C after the slag is emptied. The cleaning in the tank of the reaction tank 113 and the effective removal of moisture to prevent moisture from affecting the oxidation reaction of the decane formed in the next reaction with the water alkaline environment to form cerium oxide, thereby increasing the decane reaction rate, a gas-liquid separation The tank 12 is connected to the condenser 114. The condenser 114 is sequentially connected with a second condenser 117 and a third condenser 118. The preliminary decane separation is performed by using physical properties different in boiling temperature of each substance, and then 2 to 7 kg. The constant pressure of /cm ² is sequentially introduced into the second condenser 117 to condense at -30 ° C and condense with the third condenser 118 at -75 ° C to avoid the enthalpy of ethane dispersed in the gas phase and then in a gaseous state. Mixing methane and hydrogen in the gas-liquid separation device The cells are separated to form liquid helium ethane and liquefied ammonia, and gaseous methane and hydrogen. A filter 119 is disposed between the condenser 114 and the second condenser 117, because the jacketed reaction tank 113 is in the reaction process. The produced methane-methane gas mixture and the ammonia and cesium ethane which are distilled after the reaction is completed are accompanied by a small amount of raw material or slag powder carried by the differential pressure gas stream, and the filter 119 is used to intercept powders larger than 3 to 100 μm. The upper end of the gas-liquid separation tank 12 is connected to a methane temporary storage tank 21 for storing vaporized helium methane, and the gas-liquid separation tank 12 is connected to an ethane for storing liquefied ethane and liquid ammonia. The storage tank 15 comprises a deuterium ethane column 131, an ammonia purification column 132 and an ethane purification column 133. The ethane storage tank 15 is connected to the deuterium ethane column. 131, the upper end of the deuterated ethane column 131 is connected to the ammonia purification column 132, and the lower end of the deuterated ethane column 131 is connected to the oxime ethane purification column 133, and the deuterium ethane column 131 is at a pressure of 18 to 24 kg/cm ² The ammonia is separated into the ammonia purification column 132 at a temperature of 25 ° C to 70 ° C, and the separated liquid ammonia amount is 58 to 67 wt %. At the same time, the ruthenium ethane is separated into the oxime ethane purification column 133, and the ammonia purification column 132 is separated by a temperature difference to reflux a small amount of hydrazine methane to the hydrazine methane storage tank 21, and the cesium ethane purification column 133 is at a temperature of 30 The oxirane is further purified at a temperature of from ° C to 100 ° C, and the purified oxirane is stored in a liquefied ethane buffer tank 16 , whereby the reaction selectivity of the oxirane can be 5 to 25 vol %, and the liquefied ethane is liquefied. The buffer tank 16 can store 矽 ethane up to 4N8 (99.998%) purity. When 矽 ethane filling demand, 矽 ethane can be liquefied from the liquefied ethane buffer bucket by vacuum low temperature -75 ° C condensation. Filling into at least one cylinder 17 can also purify a small amount of ethane and a trace of impure gas by the same vacuum condensation technique, and the ammonia purification tower 132 and the ethane purification tower 133 are separated from the ammonia storage. The liquid ammonia buffer tank 134 is passed through the liquid ammonia buffer tank 134 to introduce the recovered ammonia into the jacketed reaction tank 113 for repeated use, thereby effectively reducing the production cost.

Another branch of the present invention performs a purification operation of methane, which is shown in Fig. 2. The methane methane storage tank 21 is connected to a methane fractionation system 22, which includes a helium methane recovery tower. 221, a methane molecular sieve 222 and a methane purification tower 223, the methane recovery column 221 is connected to the methane molecular sieve 222 at the upper end, and the methane purification column 223 is connected to the methane recovery column 223 by the methane molecular sieve 222. The majority of the ammonia is fractionally stored in the liquid ammonia buffer tank 134 at a pressure of 8 to 15 kg/cm ² and a temperature of -60 ° C to 40 ° C, that is, ammonia is used as a relatively heavy substance, and the methane is fractionated by fractionation. The bottom of the recovery column 221 is produced and sent to the ammonia buffer tank 134 for recovery, and the separated methane gas still contains about 2 to 10% by weight of a small amount of ammonia component, and the fractionated methane gas and a small amount of The ammonia is further adsorbed by the 3A~5A yttrium methane molecular sieve 222 to remove ammonia and other impurities, wherein the yttrium methane molecular sieve 222 can be heated to provide a vacuum after the switching to remove the adsorbed material, and then the yttrium methane is introduced into the 矽. Alkoxy purification column 223 and hydrogen at a low temperature of -160 deg.] C to -50 ℃ contained in the removed separation, purification of silicon so that the liquefied methane is stored in a buffer tub 23 silicon methane. The enthalpy methane stored in the liquefied methane buffer tank 23 can be purified to a purity of 6N (99.9999%), and the liquefied methane buffer 23 barrels adopt an inner and outer double-layer structure (shown in FIG. 3), and the inner layer is stored and liquefied. Methane is methane, and the outer layer is vacuumed and wound around a ring coil 232. The ring coil 232 is used to circulate the refrigerant to a temperature of -50 ° C for temperature control and pressure control, and when used, the refrigerant is used as methane. Condensation, and the liquefied methane buffer tank 23 is connected to a vaporizer 231. When the methane filling requirement is required, the methane is introduced into the vaporizer 231 and controlled by a steady flow of -30 ° C refrigerant to a finished press 24 . And the methane methane is filled into at least one cylinder 25 or at least one tank truck 26 by pressurizing the finished presser 24 to a pressure of 100 to 160 kg/cm ² , thereby facilitating the filling and transportation.

Another branch of the present invention performs the recovery operation of the slag material, and as shown in FIG. 4, the slag buffer tank 14 is sequentially connected in series with a centrifugal filter 31, an ammonia aqueous solution buffer tank 32, and a magnesium hydroxide. a filter 33 and an ammonia buffer tank 34, and the centrifugal filter 31 and the magnesium hydroxide filter 33 are simultaneously connected with a dry milling device 35, and a high-pressure forming brick system 351 is connected to the dry milling device 35. The slag discharged into the slag buffer tank 14 during operation is firstly converted into the insoluble magnesium hydroxide solid powder and the salt product dissolved therein by adding water and stirring in the jacketed reaction tank 113, and The slurry slag 14 is flowed into the centrifugal filter 31 without interruption, so that the slag can be more efficiently reacted with water to form a soluble salt, so that the formed solid powder can be uniformly distributed and The sedimentation is avoided, and the centrifugal filter 31 is used for the liquid separation, that is, the centrifugal filter 31 performs the deliquoring of the slag at a rotation speed of 300 to 1000 rpm, and the solid powder is intercepted by a filter medium of 200 to 400 mesh. Flowing the liquid portion of the slag to the aqueous ammonia solution a groove 32, and the solid slag is discharged to the dry milling device 35 in a scraping manner when the centrifugal filter 31 is formed to a suitable thickness, and the dry milling device 35 is electrically heated and spirally stirred for solid slag. The heat drying and the detachment of ammonia are discharged to the high-pressure forming brick making system 351 as a raw material for brick making, and can also be directly used as a desulfurizing agent for exhausting smoke, and the ammonia aqueous buffer tank 32 is added to the recovered ammonia water. The magnesium chloride in the solution can be reacted to form ammonium chloride and magnesium hydroxide powder, and the magnesium hydroxide powder is filtered through the magnesium hydroxide filter 33 with an accuracy of 1 to 30 μm and discharged to the dry milling device 35. And the excretion method is to blow the powder from the centrifugal filter 31 by using nitrogen gas, and discharge the powder particles to the dry milling device 35 by gravity, thereby preventing the solid powder particles from entering the ammonia buffer tank 34, only Ammonia water is stored in the ammonia buffer tank 34. The ammonia buffer tank 34 is connected to an ammonia separation and recovery system 36. The ammonia separation and recovery system 36 is connected to the ammonia buffer tank 34 by an ammonia recovery tower 361, and an ammonia distillation column 362 is connected to the upper end of the ammonia recovery tower 361. The ammonia recovery tower 361 separates the ammonium chloride solution and the ammonia aqueous solution at a pressure of 0 to 5 kg/cm ² and a temperature of 50 ° C to 145 ° C, and the separated ammonia water concentration is 10 to 30 wt %, which is a relatively light substance, so that ammonia The aqueous solution is discharged from the top of the ammonia recovery column 361 to the ammonia rectification column 362, and the ammonia and water are purified and separated in the ammonia rectification column 362 at a temperature of -30 ° C to 130 ° C. Up to 98% to 99% of the purity level of the industrial grade, and the purified ammonia at the top of the ammonia rectification column 362 is stored in an ammonia raw material tank 37 for recycling, and the ammonia rectification tower 362 is separated from the bottom of the water and A trace amount of ammonia is returned to the ammonia buffer tank 34, and the ammonia recovery column 361 is sent to the poly-effect evaporation system 38 by the ammonium chloride solution separated from the bottom of the column, and is passed through the multi-effect evaporation system 38 at 120 ° C to 160 ° C. The steam is heated to vaporize the water contained in the ammonium chloride solution to remove ammonium chloride, and the ammonium chloride The water rate can be less than 1% by weight, and is recovered by a dryer 381 as a reaction raw material of the jacketed reaction tank 113, and the water vapor is recovered by a recovery water buffer tank 39 to provide the jacketed reaction tank 113 for reaction. After the slag solvent is used.

At the end of the creation (waste) gas recovery operation, please see the picture shown in Figure 5, the process equipment of the decane reaction full process is integrated by a plurality of exhaust gas discharge lines 41 to connect an exhaust gas treatment system 42, the exhaust gas treatment system 42 includes a scrubbing tower 421, a high temperature oxidizer 422, and a filtering device 423, and the tail (waste) gas is split to various stages of the exhaust gas treatment system 42 according to a composition containing ammonia and decane gas, the scrubbing tower 421 being water The ammonia gas is removed by adsorption, and the formed ammonia water is introduced into the ammonia solution buffer tank 32 for recovery, and is used as an additive for ammonium chloride salt conversion, and a trace amount of tail gas is discharged from the top of the tower to the high temperature oxidizer. 422 is subjected to destruction of decane gas to convert it into a non-hazardous substance of cerium oxide, and then the filtering device of the exhaust gas treatment system 42 423 performs interception collection, thereby effectively treating the exhaust gas to reduce environmental pollution at a low cost.

In summary, this creation has indeed achieved a breakthrough structural design, and has improved new content, while at the same time achieving industrial use and progress, and this creation is not seen in any publication, but also novel, when In accordance with the provisions of the relevant laws and regulations of the Patent Law, a new type of patent application is filed according to law, and the examination authority of the bureau is required to grant legal patent rights.

Only the above-mentioned ones are only preferred embodiments of the present invention, and the scope of the creation of the present invention cannot be limited thereto; that is, the equal changes and modifications made by the majority of the patent application scope of the present invention should still belong to the present invention. Within the scope of the patent.

Claims (10)

A catalyst for increasing the formation of decane and the complete recovery of by-product by-process thereof, comprising: a decane reaction system comprising a magnesium sulphide powder suction bucket, a magnesium telluride automatic feeding device, and a jacketed type a reaction tank, a condenser and a pneumatic pump, wherein the magnesium telluride powder tank stores magnesium telluride and a catalyst in an oxygen-free state, and the mixing ratio of the catalyst is 15% to 30% of magnesium telluride, and the catalyst is composed of 20~50wt% of tantalum powder and 50~80wt% of metal powder form a bimetal composite, and the magnesium telluride automatic feeding device is connected between the magnesium telluride powder sucking barrel and the jacketed reaction tank, and the clip The jacketed reaction tank is equipped with a mixer, and the top end of the jacketed reaction tank is connected to the condenser and the bottom end is connected to the pneumatic pump, and the jacketed reaction tank is first charged with ammonium chloride powder and sealed nitrogen gas is replaced. And vacuum deaeration operation, after introducing pure ammonia, controlling the condensation of -30 °C refrigerant to form liquid ammonia, and starting the mixer to pre-dissolve ammonium chloride and liquid ammonia, and inputting the magnesium telluride automatic feeding device at a fixed rate Magnesium telluride and catalyst enter the jacket a reaction tank, thereby triggering a reaction to generate a mixture of methane and hydrogen, and producing the mixture via the condenser, and further heating the liquid ammonia and the hydrazine ethane after the auxiliary treatment at 90 ° C to recover the reaction through the condenser. The slag is discharged from the pneumatic pump and stored in a slag buffer tank; a gas-liquid separation tank connected to the condenser, and connected to the upper end of the gas-liquid separation tank for storing vaporized methane a methane temporary storage tank, and the gas-liquid separation tank is connected to a sulphur storage tank for storing liquefied ethane and liquid ammonia; and an ethane distillation system including a detachment system a ruthenium ethane column, an ammonia purification column and an ethane purification column, the 矽 ethane temporary storage tank is connected to the deuterium ethane column, the upper end of the deuterium ethane column is connected to the ammonia purification tower, and the detachment The lower end of the alkylene column is connected to the oxime purification tower, and the deuterated ethane column is separated into the ammonia purification tower under the conditions of a pressure of 18 to 24 kg/cm ² and a temperature of 25 to 70 ° C, and the hydrazine is separated into the hydrazine. An ethane purification tower, and the ammonia purification tower separates a small amount of hydrazine methane to the temperature difference a methane storage tank, and the oxirane purification tower further purifies the ruthenium ethane at a temperature of 30 ° C to 100 ° C, and stores the purified ruthenium ethane in a liquefied ethane buffer tank, thereby reacting the ruthenium ethane The selectivity can be 5~25 vol%, and the ammonia separated from the pyridine purification column is stored in a liquid ammonia buffer tank, and the recovered ammonia is introduced into the jacket reaction through the liquid ammonia buffer tank. The tank is reused, which in turn reduces its production costs. The system for raising decane reaction and the total recovery of by-product by process according to the catalyst of claim 1, wherein the condenser is sequentially connected with a second condenser and a third condenser, and the boiling point of each substance is utilized. The physical properties of different temperatures are subjected to preliminary decane separation, and the second condenser is introduced into the second condenser at a constant pressure of 2 to 7 kg/cm ^{2 to} condense at -30 ° C to condense with the third condenser at -75 ° C to form a liquid. Ethane and liquefied ammonia, as well as gaseous methane and hydrogen, are separated in the gas-liquid separation tank. a system for promoting decane reaction formation and full recovery of by-product by-product according to the catalyst of claim 2, wherein a filter is installed between the condenser and the second condenser, due to the jacket type The methane gas mixture generated in the reaction tank during the reaction process and the ammonia and cesium ethane which are distilled after the reaction is completed are accompanied by a small amount of raw material or slag powder carried by the differential pressure gas stream, and the filter is intercepted by more than 3 ~100μm particles. The system for raising decane reaction and the complete recovery of by-product by-product according to the catalyst of the first application of the patent scope, wherein the liquefied ethane ethane buffer tank can store 矽 ethane up to 4N8 (99.998%) purity When the demand for ethane is filled, the condensed ethane can be filled into the at least one cylinder by the liquefied ethane buffer tank by vacuum low-75 ° C condensation, and the same vacuum condensation technology can be used for small amount Purification of the alkane and removal of traces of impure gas. The system for raising decane reaction and the total recovery of by-product by-product according to the catalyst of claim 1, wherein the methane methane storage tank is connected with a helium methane fractionation system comprising a methane a recovery tower, a methane molecular sieve and a methane purification tower. The upper end of the methane recovery tower is connected to the methane molecular sieve, and the methane methane sieve is connected to the methane purification tower. The methane recovery tower is pressurized at 8-15 kg/ Cm ² and varying temperature -60 ° C ~ 40 ° C, most of the ammonia is fractionated and stored in the liquid ammonia buffer tank, and the fractionated methane gas and a small amount of ammonia are adsorbed and removed by the 3A~5A methane molecular sieve. And other impurities, the methane is introduced into the methane purification tower and the hydrogen contained is removed at a low temperature of -160 ° C to -50 ° C, and the purified methane is stored in a liquefied methane buffer tank. a system for promoting the recovery of decane reaction and the total recovery of by-product by-product according to the catalyst described in claim 5, wherein the enthalpy methane stored in the liquefied methane buffer tank has a purity of 6N (99.9999%), and The liquefied methane buffer tank adopts an inner and outer double-layer structure, and the inner layer stores liquefied methane, and the outer layer is vacuumed and wound around a ring coil, and the circulating coil is used to circulate the refrigerant to a temperature of -50 ° C. Control and pressure control, and use the refrigerant as the condensation of helium methane when needed, and the liquefied methane buffer tank is connected with a vaporizer. When the methane filling demand is required, the methane is introduced into the vaporizer and the refrigerant is -30 ° C. The control of the steady flow is carried out to a finished press, and the methane is filled into at least one cylinder or at least one tank by the pressure of the finished press to 100 to 160 kg/cm ² . The system for raising decane reaction and the total recovery of by-product by-product according to the catalyst of claim 1, wherein the slag buffer tank is sequentially connected in series with a centrifugal filter, an ammonia solution buffer tank, and a hydrogen solution. a magnesium oxide filter and an ammonia water buffer tank, and the centrifugal filter and the magnesium hydroxide filter are simultaneously connected with a dry milling device, and connected by the dry milling device A high-pressure forming brick system is connected, and the slag discharged into the slag buffer tank is firstly mixed with water in the jacketed reaction tank to be partially converted into insoluble magnesium hydroxide solid powder and a salt product dissolved therein. And flowing the slurry slag into the centrifugal filter under the uninterrupted stirring of the slag buffer tank, and using the centrifugal filter to de-liquidize, the liquid portion of the slag is flowed to the ammonia solution buffer tank, and The solid portion is discharged to the dry milling device, and the dry milling device is heated and dried by the electric heating and spiral stirring to remove the solid slag and the ammonia is removed, and discharged to the high-pressure forming brick system as a raw material for brick making. Further, the ammonia aqueous solution buffer tank is added with ammonia water, and the magnesium chloride in the solution can be reacted to be converted into ammonium chloride and magnesium hydroxide powder, and the magnesium hydroxide powder is filtered by the magnesium hydroxide filter with an accuracy of 1 to 30 μm. Excreted to the dry milling device to prevent solid powder from entering the ammonia buffer tank, and only storing ammonia water into the ammonia buffer tank. The system for raising decane reaction and the total recovery of by-product by-product according to the catalyst described in claim 7 wherein the ammonia buffer tank is connected to an ammonia separation recovery system, and the ammonia separation recovery system is connected by an ammonia recovery tower. The ammonia buffer tank is connected with an ammonia rectification tower from the upper end of the ammonia recovery tower, and the ammonia recovery tower carries out the ammonium chloride solution and the ammonia solution at a pressure of 0 to 5 kg/cm ² and a temperature of 50 ° C to 145 ° C. Separating, discharging an aqueous ammonia solution from the top of the ammonia recovery tower to the ammonia rectification column, and purifying and separating ammonia and water at a temperature of -30 ° C to 130 ° C in the ammonia rectification column, and the ammonia The purified ammonia at the top of the distillation column is stored in an ammonia raw material tank for recycling, and the water and trace ammonia separated by the ammonia distillation column are refluxed to the ammonia water buffer tank, and the ammonia recovery tower is separated from the bottom of the tower. The ammonium chloride solution is sent to a multi-effect evaporation system, and is heated by steam of 120 ° C to 160 ° C through the multi-effect evaporation system, so that the ammonium chloride solution vaporizes the moisture contained in the ammonium chloride solution and is chlorinated. The moisture content of ammonium can be less than 1wt% and is controlled by a dryer The reaction yield as a raw material of the jacket type reaction vessel, and the water vapor recovered to a buffer tank supplies the recovered solvent using a jacketed reaction vessel after the reaction of the slag. The system for raising decane reaction and the complete recovery of by-product by the catalyst according to the catalyst of the first aspect of the patent application, wherein the jacketed reaction tank is flushed with nitrogen, vacuumed and 90 after the slag is emptied. °C heating of the heat medium to clean the tank in the jacketed reaction tank and effectively remove moisture to prevent moisture from affecting the oxidation reaction between the decane formed in the next reaction and the alkaline environment to form cerium oxide. Increase the decane reaction rate. The system for raising decane reaction and the complete recovery of by-product by process according to the catalyst of the first application of the patent scope, wherein the process equipment of the decane reaction full process is integrated and connected to a tail gas treatment system by a plurality of exhaust gas discharge pipelines. The exhaust gas treatment system comprises a washing tower, a high temperature oxidizer and a filtering device, and the tail (waste) gas is divided into various stages of the tail gas treating system according to a composition containing ammonia and decane gas, and the washing tower carries ammonia gas with water. The adsorption is removed, and the formed ammonia water is introduced into the ammonia solution buffer tank for recovery, and is used as an additive for ammonium chloride salt conversion, and a trace amount of tail gas is discharged from the top of the tower to the high temperature oxidizer for destruction of decane gas. It is converted into a non-hazardous substance of cerium oxide, which is then intercepted and collected by the filtering equipment of the exhaust gas treatment system.