Organosilicon low-boiling-point substance mixing system adsorption separation evaluation device

Abstract

The utility model discloses an adsorptive separation evaluation device for an organic silicon low-boiling-point substance mixing system. A raw material storage tank is connected with the top inlet end of the vaporizing chamber through a feeding pump; vaporizing chamber outlet pipelines are respectively connected with the top end and the bottom end of the adsorption column; the top outlet pipeline of the adsorption column is connected with the inlet end of the condenser; the bottom outlet end of the condenser is connected with the inlet end of the collecting tank. A constant-temperature box is arranged outside the vaporizing chamber and the adsorption column and is used for stabilizing the temperature of the vaporizing chamber and the adsorption column. The nitrogen enters the vaporizing chamber at a certain flow rate under the pressure of nitrogen and is heated into gas, the gas enters the adsorption column at a constant temperature, a constant speed and a constant pressure to be in contact with an adsorbent in the adsorption column, and after impurities are adsorbed, a target product obtained at the tower top enters the condenser to be cooled into a liquid phase and then enters the collecting tank through the conversion valve. The organic silicon low-boiling-point substance mixing system adsorption separation evaluation device disclosed by the utility model can ensure that organic silicon low-boiling-point substances are not contacted with the outside, and the adsorption evaluation stability is high.

Description

Technical Field

[0001] The utility model patent relates to an adsorption effect evaluation device for the adsorption and separation of organosilicon low boilers, specifically a device that can stably evaluate the adsorption effect of an adsorbent on each component in organosilicon low boilers. Background Art

[0002] In the production process of organosilicon, the main product formed by the reaction of metallic silicon and methyl chloride is dimethyldichlorosilane, accounting for about 80%. At the same time, about 20% of organosilicon by-products, low boilers, are also produced, mainly composed of tetramethylsilane, dimethylchlorosilane, 2-methyl-2-butene, 2-methylbutane, 2-butene, 1-butene, etc. The produced organosilicon low boiler waste liquid has the characteristics of being easily decomposed when encountering water or light. And if it is treated as solid waste, it will significantly increase the total production cost of organosilicon. It should be noted that if each component in this waste liquid is separated and refined into various single products, it can turn waste into treasure and improve the product added value through classified recycling. The boiling point differences of nearly ten components in the waste liquid are between 1°C and 5°C. If distillation separation is used, both the equipment investment and separation energy consumption are extremely large. The waste liquid is a mixture of low boilers, and the melting points are all around -100°C, so crystallization separation cannot be used either. However, the molecular dynamic diameters and functional groups of each component have differences, which makes it possible to separate and purify each component using the adsorption method. Seeking an ideal adsorbent to separate and purify the target components is the key. However, organosilicon low boilers are easily decomposed when encountering water vapor and need to be operated in the dark throughout the process. They are liquids below 30°C, and these characteristics make it difficult to evaluate the effect of the adsorbent in separating organosilicon low boiler waste liquid. Summary of the Invention

[0003] A main object of the utility model is to provide an adsorption separation evaluation device for an organosilicon low boiler mixed system. The device includes a raw material storage tank, a vaporization chamber, an adsorption column, a condenser, and a collection tank, aiming to solve the problems of the accuracy and stability of the effect evaluation of the adsorbent in adsorbing and separating each component of the organosilicon low boiler waste liquid.

[0004] An adsorption separation evaluation device for an organosilicon low boiler mixed system,

[0005] The raw material storage tank is connected to the top inlet end of the vaporization chamber through a feed pump, and the outlet pipeline of the vaporization chamber is respectively connected to the top and bottom ends of the adsorption column;

[0006] The outlet pipeline at the top of the adsorption column is connected to the inlet end of the condenser;

[0007] The bottom outlet end of the condenser is connected to the inlet end of the collection tank. The cooling medium of the condenser includes but is not limited to water, silicone oil, ethanol, and liquid nitrogen.

[0008] A constant temperature box is arranged outside the vaporization chamber and the adsorption column to stabilize the temperatures of the vaporization chamber and the adsorption column. The vaporization chamber is heated by an aluminum block electric heater.

[0009] A nitrogen inlet pipe is provided on the raw material storage tank to achieve nitrogen protection inside the device. To prevent the sample from contacting air and causing inaccurate adsorption evaluation results, nitrogen protection is used in the front process of this device.

[0010] A vacuum system is provided at the top of the adsorption column to achieve the adjustment of the vacuum degree inside the adsorption column.

[0011] There is at least one adsorption column. When there are multiple adsorption columns, series or parallel adsorption is adopted between the adsorption columns. The adsorbent inside the adsorption column can be replaced, including but not limited to molecular sieve, activated carbon or metal-organic framework material.

[0012] A nitrogen inlet pipe and an evacuation pipe are provided at the upper part of the collection tank to achieve nitrogen protection inside the device.

[0013] According to an embodiment of the present invention, the raw material storage tank and the collection tank are made of stainless steel, and temperature and pressure test elements are provided at the collection tank, the vaporization chamber and the outlet end of the adsorption column.

[0014] According to an embodiment of the present invention, the nitrogen source used in the nitrogen protection system of the device is provided by bottled nitrogen.

[0015] According to an embodiment of the present invention, the collection tank and the condenser of the device use the same low-temperature water as the cold source.

[0016] According to an embodiment of the present invention, a vacuum pump is connected to the top end of the adsorption column of the device.

[0017] According to an embodiment of the present invention, the vaporization chamber and the adsorption column of the device are placed in the same constant temperature box, such as a constant temperature air bath, to ensure uniform temperature.

[0018] The device of the present utility model can be used for evaluating the separation effect of adsorbents, mainly for evaluating the component adsorption separation effect of a mixed system of organosilicon low-boiling substances. To prevent the mixed liquid of organosilicon low-boiling substances from denaturing when encountering air, the whole device is installed with nitrogen protection. The storage tank is used to hold the mixed liquid of organosilicon low-boiling substances. The vaporization chamber and the adsorption column are placed in an air bath constant temperature box. The vaporization chamber has a separate aluminothermic device to quickly vaporize the organosilicon low-boiling substances to a specified temperature. The mixed liquid of organosilicon low-boiling substances enters the storage tank through the feeding port. It enters the vaporization chamber through nitrogen pressure at a certain flow rate, is heated to a gas, and then enters the adsorption column at a constant temperature, constant speed and constant pressure, contacts the adsorbent in the adsorption column. When the impurities are adsorbed, the target product is obtained at the top of the column, enters the condenser, is cooled to the liquid phase, and then enters the collection tank through the diversion valve. The adsorption separation evaluation device for the mixed system of organosilicon low-boiling substances of the present invention can ensure that the organosilicon low-boiling substances do not contact the outside world, and has high adsorption evaluation stability. Brief Description of the Drawings

[0019] Figure 1 The structural schematic diagram of an adsorption separation evaluation device for an organosilicon low-boiling mixture system of the present utility model; 1 - raw material storage tank; 2 - feed pump; 3 - vaporization chamber; 4 - adsorption column; 5 - air bath; 6 - condenser; 7 - collection tank. Specific embodiments

[0020] Typical embodiments reflecting the features and advantages of the present invention will be described in detail in the following description. It should be understood that the present invention can have various variations in different embodiments, all of which do not depart from the scope of the present invention, and the descriptions and illustrations therein are for illustrative purposes in essence and not for limiting the present invention.

[0021] An embodiment of the present invention provides an adsorption separation evaluation device for an organosilicon low-boiling mixture system. This device can be used to evaluate the separation effect of an adsorbent, mainly for evaluating the component adsorption separation effect of an organosilicon low-boiling mixture system.

[0022] Example 1

[0023] As Figure 1 shown, the adsorption separation evaluation device for an organosilicon low-boiling mixture system according to an embodiment of the present invention includes a storage tank, a vaporization chamber, an adsorption column, a condenser, and a sampling system connected in sequence.

[0024] The raw material storage tank 1 is connected to the top inlet end of the vaporization chamber 3 through the feed pump 2, and the outlet pipeline of the vaporization chamber 3 is respectively connected to the top and bottom ends of the adsorption column 4; the flow rate of the organosilicon low-boiling mixture system pumped from the raw material storage tank 1 into the vaporization chamber 3 through the feed pump 2 is 0.05 mL / min to 1 mL / min.

[0025] The top outlet pipeline of the adsorption column 4 is connected to the inlet end of the condenser 6; the upper and lower ends of the adsorption column 4 are sealed with glass wool to fix the adsorbent. Temperature and pressure display and adjustment elements are installed on the vaporization chamber 3 and the adsorption column 4 to detect and control the temperature and pressure during the evaluation of the adsorption effect in real time. The height of the adsorption column 4 is 300 mm and the diameter is 13 mm.

[0026] The bottom outlet end of the condenser 6 is connected to the inlet end of the collection tank 7.

[0027] A constant temperature box 5 is arranged outside the vaporization chamber 3 and the adsorption column 4 to stabilize the temperature of the vaporization chamber 3 and the adsorption column 4. The temperature control range of the vaporization chamber is 20°C to 80°C, and the pressure range is 0 to 1 MPa.

[0028] A nitrogen inlet pipe is arranged on the raw material storage tank. After nitrogen enters the storage tank, the air in the storage tank is replaced to prevent reaction with water vapor in the air, for realizing nitrogen protection in the device.

[0029] A vacuum system is provided at the top of the adsorption column 4 for adjusting the vacuum degree inside the adsorption column 4.

[0030] The two series-connected adsorption columns of the adsorption column 4 are connected.

[0031] A nitrogen inlet pipe and an evacuation pipe are provided at the upper part of the collection tank 7 for realizing nitrogen protection inside the device.

[0032] Example 2

[0033] For the adsorption separation evaluation device of an organosilicon low-boiling mixture system in Example 1, the vaporization chamber temperature is 20°C, the pressure is 0.5 MPa, the flow rate of the organosilicon low-boiling mixture system is 0.05 mL / min, the cooling medium of the condenser is water, and the adsorbent inside the adsorption column is molecular sieve.

[0034] After running for 50 h as described above, the purity of the organosilicon low-boiling substances ≥ 99.999%.

[0035] Example 3

[0036] For the adsorption separation evaluation device of an organosilicon low-boiling mixture system in Example 1, the vaporization chamber temperature is 50°C, the pressure is 1 MPa, the flow rate of the organosilicon low-boiling mixture system is 0.5 mL / min, the cooling medium of the condenser is silicone oil, and the adsorbent inside the adsorption column is activated carbon.

[0037] After running for 70 h as described above, the purity of the organosilicon low-boiling substances ≥ 99.999%.

[0038] Example 4

[0039] For the adsorption separation evaluation device of an organosilicon low-boiling mixture system in Example 1, the vaporization chamber temperature is 70°C, the pressure is 0.6 MPa, the flow rate of the organosilicon low-boiling mixture system is 0.8 mL / min, the cooling medium of the condenser is ethanol, and the adsorbent inside the adsorption column is metal-organic framework material.

[0040] After running for 20 h as described above, the purity of the organosilicon low-boiling substances ≥ 99.999%.

[0041] Example 5

[0042] For the adsorption separation evaluation device of an organosilicon low-boiling mixture system in Example 1, the vaporization chamber temperature is 80°C, the pressure is 0 MPa, the flow rate of the organosilicon low-boiling mixture system is 1 mL / min, the cooling medium of the condenser is liquid nitrogen, and the adsorbent inside the adsorption column is metal-organic framework material.

[0043] After running for 15 h as described above, the purity of the organosilicon low-boiling substances ≥ 99.999%.

[0044] Unless otherwise specified, the terms used in this invention have the meanings commonly understood by those skilled in the art.

[0045] The embodiments described in this invention are for illustrative purposes only and are not intended to limit the scope of protection of this invention. Those skilled in the art can make various other substitutions, changes and improvements within the scope of this invention. Therefore, this invention is not limited to the above embodiments but is only defined by the claims.

Claims

1. An adsorption separation evaluation device for a low-boiling-point organic silicon mixed system, characterized in that: The raw material storage tank (1) is connected to the top inlet end of the vaporization chamber (3) via the feed pump (2), and the outlet pipeline of the vaporization chamber (3) is respectively connected to the top and bottom ends of the adsorption column (4); the upper and lower ends of the adsorption column (4) are sealed with glass wool for fixing the adsorbent; The outlet pipeline at the top of the adsorption column (4) is connected to the inlet end of the condenser (6); The bottom outlet end of the condenser (6) is connected to the inlet end of the collecting tank (7); A constant temperature box (5) is provided outside the vaporization chamber (3) and the adsorption column (4) for stabilizing the temperature of the vaporization chamber (3) and the adsorption column (4); A vacuum system is provided at the top of the adsorption column (4) for adjusting the vacuum degree in the adsorption column (4).

2. The organic silicon low boiling point mixed system adsorption separation evaluation device according to claim 1, characterized in that: The raw material storage tank is provided with a nitrogen inlet pipe for realizing nitrogen protection in the device.

3. The organic silicon low boiling point mixed system adsorption separation evaluation device according to claim 1, characterized in that: There is at least one adsorption column (4). When there are multiple adsorption columns, the adsorption columns are connected in series or in parallel for adsorption.

4. The organic silicon low boiling point mixed system adsorption separation evaluation device according to claim 1, characterized in that: The upper part of the collecting tank (7) is provided with a nitrogen inlet pipe and an exhaust pipe for realizing nitrogen protection in the device.

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