TWM566204U - Trisilane synthesis and filtration purification system - Google Patents

Abstract

A system for the synthesis and filtration purification of hydrazine propane comprises: a hydrazine powder filtration treatment system, a hydrazine propane purification system and a decane conversion system, a deuterium methane distillation column of the hydrazine propane purification system, the first distillation column and The second distillation column purifies and purifies the hydrazine propane by the difference in the size and boiling point of the decane molecule, thereby achieving the effect of purifying the hydrazine propane with high purity, and the micro-nano-grade strontium powder produced by the reaction is filtered by the strontium powder processing system. The filter group is filtered and reversed by nitrogen gas regeneration, and the dosing system adds an aqueous sodium hydroxide solution to the filter group, and the residual micro-nano-grade strontium powder and sodium hydroxide aqueous solution are reacted to form a sodium citrate solution, and then Discharge into the slag bucket to improve the safety of the slagging process.

Description

Helium propane synthesis and filtration purification system

This creation is about a decane process system, especially a system for the synthesis and filtration purification of hydrazine propane which can improve the conversion of decane and its safe filtration treatment.

According to the fact that both Silane and Disilane are SEG (Special Electronic Grade Gas), their main functional use is for film deposition. Among them, the main application industries of methane and methane include LCD panels, solar cells, energy-saving glass and aeration industries, and ethane is mainly used in high-quality electronics industries including DRAM, foundry, LED wafers and germanium derivative chemicals. In other industries, the current market price of methane is US$ per kilogram, and ethane is tens of US dollars per kilogram. The reason is that the production technology of ethane products is difficult, and the market is in short supply and the market demand is expected to increase in the future. Therefore, the price difference is up to 100 times, and due to the excellent density of 矽 ethane and the low deposition temperature of 矽 methane, the conventional decane conversion reaction process still has some shortcomings, the main reasons are as follows: the decane conversion reaction In the process, hydrazine propane is also produced, and the conventional practice is to treat hydrazine propane as tail (waste) gas directly to the combustion tower for combustion treatment, mainly because the conventional technology has too high purification cost for hydrazine propane. Its purification does not meet economic costs, and the discharge of hydrazine propane along with other higher decanes will not only result in a reduction in the yield of finished products, but also an increase in the ring. The pollution is the technical problem that the creation wants to improve. Furthermore, the environmental impact caused by the reaction slag storage and the complicated and energy-intensive processing procedures, such as the operating conditions and environment of the decane process. Oxidation reaction produces bismuth powder, which will lead to equipment efficiency and production efficiency The reduction in the rate and the increase in the frequency of demolition and maintenance will also increase the risk of burning during dismantling and cleaning. Therefore, the conventional decane production process is difficult to meet economic benefits.

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 synthesis and filtration purification of hydrazine propane in view of the above-mentioned shortcomings existing in the prior art. .

A powder filtration treatment system is connected with a slag bucket and a dosing system by a filter group, and a large amount of micro-nano-grade strontium powder generated by excessive cleavage during the decane conversion reaction is directly filtered by the different aperture precision of the filter group. And removing the micro-nano-grade yttrium powder adhered to the filter by means of nitrogen reverse-blowing regeneration and storing in the slag discharging bucket, and then adding the sodium hydroxide aqueous solution by using the medicating system after the nitrogen reverse-blowing the regeneration filter group The filter group is configured to react residual micro-nano-grade strontium powder with sodium hydroxide aqueous solution to form a sodium citrate solution, and then discharge into the slag discharge tank, and after being discharged, the pure water is added and washed and attached to the filter. Residual sodium ions in the group, to avoid the sodium ions to contaminate the decane formed by the conversion reaction. The monopropane purification system is sequentially connected in series with a depurinating methane distillation column, a first distillation column, a second distillation column and a propane propane. a storage tank, the dehalogenation methane distillation column, the first distillation column and the second distillation column are separated and purified by the difference in size and boiling point of the decane molecule to purify the methane, hydrazine and hydrazine propane. Stored in the cesium propane storage tank, and the separated hydrazine methane recovery is further subjected to a decane conversion reaction. The decane conversion system comprises a preheater, a converter, a dehydrogenation distillation column, a methane replenishing tank and a compression. The methane replenishing tank is connected to one end of the preheater and is converted by the methane methane replenishing tank as a decane conversion reaction. In the process, the methane resource consumed by the methane is supplemented, and the other end of the preheater is connected to the converter, and the preheater is heated to a temperature of 400 ° C ~ 500 ° C of methane to decane conversion in the converter The reaction converts the methane partial portion into oxirane, hydrazine propane and higher order decane, and the converter is connected to the filter group of the mash filtration treatment system, and the mash formed by the reaction cleavage is intercepted in the filter group. Filtration, so as not to cause blockage of downstream equipment pipelines, and the filter group outlet is connected to the dehydrogenation distillation tower by the compressor, and the non-condensing and minimum molecular weight hydrogen gas is separated and removed at the top of the dehydrogenation distillation tower. And the bottom of the dehydrogenation distillation column is connected to the deuterium methane distillation column of the helium propane purification system, so that the methane separated by the deuteration methane distillation column is again transported into the preheater for a conversion reaction cycle, and the deuterium methane distillation The cesium propane and higher decane separated by the column are introduced into the hydrazine propane purification system for fractional purification.

The filter group is connected in series with three filters, and the filter is provided with filter cores of 25 to 200 μm, 1 to 20 μm, and 0.03 to 0.8 μm in size.

Wherein, the filter group is connected in series with three filters, and the filter sequentially sets a filter core using a filter particle size of 5 μm, 0.45 μm and 0.1 μm.

Wherein, the filter having different filter particle diameters has a plurality of filters, and at the same time, only one is activated, and the filter can switch the pressure difference caused by the filter core to intercept and intercept the excess powder, so that the filter can be switched to the outlet. The filter is used instead and the deactivated filter is regenerated.

Wherein, the helium propane temporary storage tank transports the helium propane into a steel cylinder by condensing and vacuuming for shipment.

Wherein, a ruthenium distillation system is connected to the top of the first distillation column, and the ethane is separated from the ruthenium methane by the oxirane distillation system.

Wherein the dehydrogenation distillation column of the decane conversion system and the hydrazine propane purification system use a liquid nitrogen refrigerant to create a cryogenic environment required to distill off the non-condensed hydrogen and helium methane having a lower boiling point, and the liquid nitrogen after the heat exchange is vaporized into The extremely low temperature nitrogen gas having a temperature close to -160 ° C can be reused in the first distillation column and the second distillation column to condense the hydrazine propane, and after the condensed hydrazine propane is sent to the shell side of the hydrazine propane storage tank as a cold-keeping fluid, Finally, it is supplied to the filter group as a nitrogen gas for reverse blown regeneration, whereby the liquid nitrogen is effectively utilized for cooling and blow-off.

The first main purpose of this creation is to use helium methane as a raw material for the conversion of helium propane. In the preheater of the decane conversion system, helium methane is heated and controlled by the pressure and heating to stabilize the pyrolysis of methane. Introduced into the converter, the hydroquinone molecule produced by the cracking is subjected to the reaction synthesis of hydrazine propane, and then the solid bismuth powder formed by the excessive cracking is filtered and intercepted by the filter group, and only the decane gas is fractionated and purified by entering the fractionation purification device. Effectively control the stability of the decane conversion reaction, and reduce the storage of the slag derived from the reaction and the impact of the slag on the environment.

The second main purpose of the present invention is to isolate the filter body from the vacuum before re-generating the filter set, and then vacuuming it, then filling it with nitrogen to perform the flushing and displacement to desorb the filter to intercept the conversion reaction. Pyrolysis of bismuth powder and the manufacture of an oxygen-free environment, reacting hydrazine with aqueous sodium hydroxide in an anaerobic environment to produce a water-soluble sodium citrate gelatinous substance, and thus, after nitrogen reversal regeneration to remove micronized strontium powder The sodium hydroxide aqueous solution is added to be immersed, and the micronized strontium powder is discharged to the slag discharge tank after being reacted in a large amount, and then pure water is added to the filter group to wash the residual residual sodium ions (Na ⁺ ) to avoid Sodium ion (Na ⁺ ) contaminates the decane formed by the conversion reaction, and finally can be safely removed. This can effectively remove the micro-nano-grade strontium powder to maintain the filter efficiency and improve the safety of the slagging process. The effect of sex, avoiding the oxidative combustion of bismuth powder exposed to the atmosphere.

The third main purpose of this creation is that the hydrazine propane purification system is serially connected. a difference between the size and the boiling point of the deuterium methane distillation column, the first distillation column, the second distillation column and the hydrazine propane storage tank, and the deuteration methane distillation column, the first distillation column and the second distillation column The methane, hydrazine and hydrazine propane are purified and separated, and the purified hydrazine propane is stored in the hydrazine propane storage tank to ensure that the purity of the hydrazine propane can reach 4N or more in accordance with international specifications, thereby achieving the high purity purification of hydrazine propane.

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

[this creation]

10‧‧‧矽 powder filtration treatment system

11‧‧‧Filter group

111‧‧‧Filter

12‧‧‧ slag bucket

13‧‧‧ Dosing system

20‧‧‧矽propane purification system

21‧‧‧ Deaerator Methane Distillation Tower

211‧‧‧ gas-liquid separation tank

22‧‧‧First Distillation Tower

23‧‧‧Second distillation tower

24‧‧‧矽 propane suspension tank

25‧‧‧Cylinders

30‧‧‧ decane conversion system

31‧‧‧Preheater

32‧‧‧Transformer

33‧‧‧Dehydrogenation distillation tower

34‧‧‧矽 methane refill bucket

35‧‧‧Compressor

40‧‧‧矽ethane distillation system

Figure 1 is a system flow diagram of the present decane conversion system.

Figure 2 is a system flow diagram of the present invention.

Figure 3 is a system flow diagram of the present 矽propane purification system.

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 views shown in Figures 1 and 2. A system for the synthesis and filtration purification of hydrazine propane comprises: a hydrazine powder filtration treatment system 10, a hydrazine propane purification system 20 and a decane conversion system 30, a mash filtration treatment system 10 to a filter group 11 A row of slag buckets 12 and a dosing system 13 are connected, and a large amount of micro-nano-grade bismuth powder (Si) generated by excessive cracking during the decane conversion reaction is filtered with a different precision of the filter group 11 and reversed by nitrogen. The micro-nano-grade tantalum powder attached to the filter 111 is removed by the method of blowing regeneration and stored in the slag discharge tank 12, and the nitrogen gas is used to reverse-regenerate the filter group 11, and the sodium hydroxide (NaOH) is used by the medicinal system 13 An aqueous solution is added to the filter group 11, and the residual micro-nano-grade niobium powder and an aqueous sodium hydroxide solution are reacted to form a sodium niobate (Na ₂ SiO ₃ ) solution, which is discharged into the slag discharge tank 12 and discharged. After adding pure water (H ₂ O) cleaning, it is attached to the Residual sodium ions (Na ⁺ ) on the filter group 11 prevent sodium ions (Na ⁺ ) from contaminating the decane formed by the conversion reaction. Its reaction formula is as follows: Si + ₂ NaOH + H ₂ O → Na ₂ SiO ₃ + H ₂

The filter group 11 is connected in series with three filters 111, and the filter 111 is sequentially provided with filter cores of 25 to 200 μm, 1 to 20 μm, and 0.03 to 0.8 μm filter diameter, and the filter 111 can also be The filter cores of 5 μm, 0.45 μm, and 0.1 μm filter particle diameters are sequentially disposed, and the filter 111 having different filter particle diameters has a plurality of filters, and at the same time, only one is activated, and the filter 111 intercepts too many powders due to the filter core. When the pressure difference between the inlet and outlet of the filter 111 is generated, the filter 111 can be switched for alternate use, and the deactivated filter 111 can be regenerated and cleaned. Further, since the powder contains micron-sized The different particle sizes of the nanometers are only regenerated by the reverse blow of nitrogen gas. The filter group 11 is insufficient to remove all of the nano-grade tantalum powder, so that the residual tantalum powder which is often left in contact with the filter 111 is reacted with air to cause oxidation. There is a danger of burning, so this creation overcomes the above-mentioned deficiency with a unique technique. Before performing the nitrogen backflush regeneration of the filter 111, the filter group 11 must be isolated and vacuumed, and nitrogen gas is injected for flushing. Replacement The filter 111 intercepts the tantalum powder cracked by the conversion reaction and creates an oxygen-free environment, and reacts the rhodium with the aqueous sodium hydroxide solution in an oxygen-free environment to produce a water-soluble sodium citrate (Na2SiO3) gelatinous substance, thus After the reverse blowing regeneration and removal of the micro-nano-grade tantalum powder, an aqueous sodium hydroxide solution is added for soaking, and the micro-nano-grade tantalum powder is discharged to the slag discharging barrel 12 after being reacted in a large amount, and then pure water is added to the filter 111. The attached residual sodium ion (Na ⁺ ) is cleaned and finally safely removed, thereby effectively removing the micro-nano-grade niobium powder to maintain the performance of the filter 111, and also improving the safety of the slagging process. Efficacy, to avoid bismuth powder exposed to the atmosphere and oxidative combustion.

Further, as shown in Figs. 1 and 3, a monopropane purification system 20 is sequentially connected in series with a depurinating methane distillation column 21, a first distillation column 22, a second distillation column 23, and a propane propane. The buffer tank 24, the deuterium methane distillation column 21, the first distillation column 22 and the second distillation column 23, the difference in size and boiling point of the decane molecule, the methane (SiH ₄ ), cesium ethane (Si) ₂ H ₆ ) is purified and separated from hydrazine propane (Si ₃ H ₈ ), and the purified hydrazine propane is stored in the hydrazine propane storage tank 24, and the hydrazine propane storage tank 24 transports the hydrazine propane in a condensed vacuum to a cylinder 25 The shipment is carried out internally, and the separated methane recovery is carried out again for the decane conversion reaction. Further, an oxirane distillation system 40 is connected to the top of the first distillation column 22, and the oxirane and the ruthenium methane are separated from the oxirane distillation system 40. Further, the liquid phase mixed liquid of the decane separated by the decane conversion system 30 enters the depurinated methane distillation column 21, and the depurinated methane distillation column 21 performs heat exchange using a heat medium of 100 ° C to 140 ° C to allow the decane mixed liquid. The methane in the methane can be completely vaporized, and the operating pressure of the deuterium methane distillation column 21 is controlled to be 3 to 10 kg/cm ² (g), so that the boiling point of methane is -90 ° C to -50 ° C, and the boiling point of helium is 20 ° C. At ~70 ° C, the flow rate of the refrigerant is controlled to maintain the temperature of the gas phase discharge of the top of the dehalogenated methane distillation column 21 at -80 ° C to -40 ° C, and the methane is separated and removed, and the methane is returned to the decane. The conversion reaction cycle is performed again in the conversion system 30, and the function of the first distillation column 22 is to separate the ruthenium ethane and the ruthenium propane. To ensure the stable source of the feed, the liquid phase discharge of the bottom of the depurinated methane distillation column 21 is not Directly transported into the first distillation column 22, but first into a gas-liquid separation tank 211, and then introduced into the first distillation column 22 via the flow control of the gas-liquid separation tank 211, at the first distillation column 22 at operating pressure 0~5kg/cm ² (g) and temperature 0 °C ~ 120 °C, distilled and collected for condensation The hydrazine liquid enters the second distillation column 23, and the content of the second distillation column 23 is hydrazine propane and higher decanes such as butane, but the high valane content is extremely small and still lacks market value, so it is not purified. As the exhaust gas is discharged, the second distillation column 23 uses a heat medium of 100 ° C to 140 ° C to heat the vaporized helium propane, and the room temperature cooling water is used as a refrigerant to carry out the condensation of the helium propane, and the second distillation column 23 tower The liquid helium propane was collected and discharged to the helium propane storage tank 24, whereby the purification efficiency of the helium propane up to 4N electronic grade purity was obtained.

The decane conversion system 30 includes a preheater 31, a converter 32, a dehydrogenation distillation column 33, a methane replenishing tank 34, and the like, as shown in Figs. 1, 2, and 3. a compressor 35, the helium methane replenishing tank 34 is connected to one end of the preheater 31, and the methane methane replenishing tank 34 is used as a supplementary source of helium methane raw material consumed by methane in the decane conversion reaction process, and the preheater 31 is further used. The other end of the converter is connected to the converter 32, and the preheater 31 is heated to a temperature of 400 to 500 ° C to carry out a decane conversion reaction in the converter 32 to convert the methane component into oxirane, hydrazine and For higher valanes, the decane conversion reaction formula is as follows: nSiH ₄ → H _{2 (g)} + Si _(s) + SiH _{2 (g)} + Si ₂ H _{6 (g)} + Si ₃ H _{8 (g)} + Si ₄ H _10(g) ‧‧‧

The converter 32 is connected to the filter group 11 of the powder filtration treatment system 10, and the tantalum powder generated by the reaction cracking is intercepted and filtered by the filter group 11, so that the downstream equipment line is not blocked, and the filter is blocked. The group 11 outlet is pressurized by the compressor 35 to 5 to 15 kg/cm ² (g) to be connected to the dehydrogenation distillation column 33, and the non-condensed hydrogen (H ₂ ) having the smallest molecular weight is separated at the top of the dehydrogenation distillation column 33. The bottom of the dehydrogenation distillation column 33 is connected to the depurinated methane distillation column 21 of the helium propane purification system 20, and the helium methane separated by the deuterated methane distillation column 21 is again transported into the preheater 31 for the reaction cycle. Further, the hydrazine propane and the higher decane separated by the deuterated methane distillation column 21 are introduced into the hydrazine propane purification system 20 for purification.

Continuing from Fig. 1, Fig. 2 and Fig. 3, the dehydrogenation distillation column 33 of the decane conversion system 30 and the hydrazine propane purification system 20 use liquid nitrogen refrigerant to create the extremely low required. The non-condensed hydrogen and helium methane having a lower boiling point are separated by distillation in a warm environment, and the liquid nitrogen after the heat exchange is vaporized into a very low-temperature nitrogen gas having a temperature of still close to -160 ° C, which can be reused in the first distillation column 22 and the second distillation. The tower 23 condenses the hydrazine propane, and after condensing the hydrazine propane, it is sent to the shell side of the hydrazine propane storage tank 24 as a cold-preserving fluid, and finally supplied to the filter group 11 for use as a reverse-blown and regenerated nitrogen gas, thereby effectively The liquid nitrogen is used for cooling and blasting.

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 (7)

The invention relates to a system for synthesizing and purifying helium, which comprises: a powder filtration treatment system, wherein the powder filtration treatment system is connected with a slag bucket and a dosing system by a filter group, and excessively cleavage during the decane conversion reaction process The generated micro-nano-grade tantalum powder is directly filtered by the different aperture precision of the filter group, and the micro-nano-grade tantalum powder attached to the filter is removed by nitrogen back-flow regeneration and stored in the draining bucket. After the nitrogen gas is blown back to the regeneration filter group, the sodium hydroxide aqueous solution is added to the filter group by the medicinal system, and the residual micro-nano-grade strontium powder and the sodium hydroxide aqueous solution are reacted to form a sodium citrate solution, and then discharged. Up to the slag discharge tank, and after washing, the residual sodium ions attached to the filter group are cleaned by adding pure water to avoid sodium ions contaminating the decane formed by the conversion reaction; a hydrazine purification system, the hydrazine propane purification system Directly connected in series with a depurinating methane distillation column, a first distillation column, a second distillation column and a propylene propane storage tank, and the decarburization methane distillation column, the first distillation column and the second steaming The column purifies and purifies the methane, hydrazine and hydrazine by the difference in the size and boiling point of the decane molecule, so that the purified hydrazine propane is stored in the hydrazine propane storage tank, and the separated hydrazine methane is recovered again for the decane conversion reaction; a decane conversion system, comprising: a preheater, a converter, a dehydrogenation distillation column, a methane replenishing tank, and a compressor, the methane methane replenishing tank being connected to one end of the preheater, and The methane replenishing tank is used as a supplementary source of methane recovery material for the methane recovery in the decane conversion reaction, and the other end of the preheater is connected to the converter, and the preheater is heated to a temperature of 400 ° C to 500 ° C of methane. The decane conversion reaction is carried out in the converter to convert the hydrazine methane portion into hydrazine ethane, hydrazine propane and higher order decane, and the converter is connected to the filter group of the bismuth powder filtration treatment system to cause the reaction to be cracked.矽 powder is intercepted in the filter group Filtration, so as not to cause blockage of downstream equipment pipelines, and the filter group outlet is connected to the dehydrogenation distillation tower by the compressor, and the non-condensing and minimum molecular weight hydrogen gas is separated and removed at the top of the dehydrogenation distillation tower. And the bottom of the dehydrogenation distillation column is connected to the deuterium methane distillation column of the helium propane purification system, so that the methane separated by the deuteration methane distillation column is again transported into the preheater for a conversion reaction cycle, and the deuterium methane distillation The cesium propane and higher decane separated by the column are introduced into the hydrazine propane purification system for fractional purification. The system for synthesizing and purifying oxime according to the first aspect of the patent application, wherein the filter group is connected in series with three filters, and the filter is sequentially provided with 25 to 200 μm, 1 to 20 μm, and 0.03~. Filter pore size of 0.8 μm filter. The system for synthesizing and purifying oxime according to the first aspect of the patent application, wherein the filter group is connected in series with three filters, and the filter is sequentially arranged to have a particle size of 5 μm, 0.45 μm and 0.1 μm. Filter heart. A system for the synthesis and filtration purification of hydrazine propane according to the second or third aspect of the patent application, wherein the filter having different filter particle sizes has a plurality of filters, and at the same time only one is activated, and the filter is filtered. When the heart adsorbs and intercepts too much powder to cause a pressure difference between the filter inlet and outlet, the filter can be switched for replacement and the deactivated filter can be regenerated. The system for syngas synthesis and filtration purification according to claim 1, wherein the ruthenium propane suspension tank transports the ruthenium propane in a condensed vacuum to a steel cylinder for shipment. A system for the synthesis and filtration purification of ruthenium propane according to claim 1, wherein the first distillation column is connected to an oxirane distillation system at the top, and is pure by the oxirane distillation system. Ethane and separation of methane. A system for the synthesis and filtration purification of ruthenium propane according to the scope of claim 1, wherein the dehydrogenation distillation column of the decane conversion system and the hydrazine propane purification system use a liquid nitrogen refrigerant to create a cryogenic environment required for distillation to separate the boiling point. The lower non-condensed hydrogen and helium methane, and the liquid nitrogen after the heat exchange is vaporized to a very low temperature nitrogen gas with a temperature close to -160 ° C, which can be reused in the first distillation column and the second distillation column to condense the helium propane and condense After the propane is propane, it is sent to the shell side of the helium propane storage tank as a cold-preserving fluid, and finally supplied to the filter group as a reverse-blown and regenerated nitrogen gas, thereby effectively utilizing the liquid nitrogen for cooling and blowing. .