Device for measuring hydrogen content of methyl high-hydrogen-content silicone oil

Abstract

The utility model discloses a device for measuring hydrogen content of methyl high-hydrogen-content silicone oil and relates to the technical field of detection devices. Comprising a sealing cover, a water bath constant-temperature oscillator, a condensation pipe, a gas measuring pipe, a leveling bottle and a three-way valve are arranged in the sealing cover, a reaction bottle with a sealed bottle opening is placed on an oscillation platform of the water bath constant-temperature oscillator and used for containing a mixed sample of n-butyl alcohol and silicone oil, and a reaction cup is placed in the reaction bottle and used for containing alkali liquor sodium hydroxide. The rim of the reaction cup is higher than the liquid level of the reaction bottle; the gas measuring pipe coaxially penetrates into the condensation pipe, and the two ends of the gas measuring pipe extend out of the condensation pipe. The sealing cover is additionally arranged to keep airflow stable, the constant-temperature effect is enhanced, and the influence of the external environment on the reaction process is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of detection devices, in particular to a device for determining the hydrogen content of methyl high-hydrogen silicone oil. Background Art

[0002] Hydrogenated silicone oil is an important class of organosilicon compounds with exceptionally good hydrophobicity. Under the action of metal salt catalysts, it can crosslink to form a film at low temperatures, forming a waterproof membrane on the surfaces of various materials. It can be used as a waterproofing agent for various materials such as fabrics, glass, leather, and metal. It can also undergo a hydrosilylation reaction with compounds containing unsaturated bonds, introducing different groups into the hydrogenated silicone oil to produce products with different uses. It is primarily used as an organosilicon surfactant and polyurethane foam leveling agent. Hydrogen content is a key indicator of hydrogenated silicone oil, directly affecting the performance of products produced using it as a raw material. Therefore, accurately measuring the hydrogen content of hydrogenated silicone oil to meet different production needs is of great significance.

[0003] HG / T4804-2015 "Methyl High Hydrogen Silicone Oil" discloses an indicator, detection method and detection device for determining the hydrogen content of methyl high hydrogen silicone oil by gas volumetric method. The method adopts Long's nitrogen measuring instrument device. According to the reaction between hydrogen silicone oil and alkaline solution, the volume of hydrogen is read through the gas tube, and the hydrogen content is calculated by the gas equation. There are areas that can be further optimized and improved in this method, specifically: first, the reaction bottle of this method is Y-shaped, which is inconvenient for sample weighing and reagent addition; second, during the reaction process, it is unstable when placed during the stabilization time and is easy to tip over. During the reaction process, the gas tube is placed in the air, and the temperature is easily affected by the external environment; in addition, the key to the gas volumetric method is to ensure that the analysis device is sealed and leak-proof. The data is often unstable due to poor sealing during the analysis process, and the gas equation requires that the sample needs to be kept at a constant temperature. Utility Model Content

[0004] The purpose of the utility model is to provide a device for measuring the hydrogen content of methyl high-hydrogen silicone oil to solve the problems raised in the above background technology.

[0005] To achieve the above objectives, the present invention provides the following technical solutions:

[0006] A device for determining the hydrogen content of methyl high-hydrogen silicone oil, characterized by comprising: a sealed cover, wherein a water bath constant-temperature oscillator, a condenser, a gas burette, a level bottle, and a three-way valve are arranged in the sealed cover; a reaction bottle with a sealed bottle mouth is placed on an oscillation platform of the water bath constant-temperature oscillator, the reaction bottle is used to hold a mixed sample of n-butanol and silicone oil; a reaction cup is placed in the reaction bottle, the reaction cup is used to hold alkaline solution sodium hydroxide, and the cup mouth of the reaction cup is higher than the liquid level of the reaction bottle;

[0007] The condenser is arranged vertically, the gas measuring tube is coaxially passed through the condenser and extends out of the condenser at both ends, the two ends of the condenser are sealedly connected to the gas measuring tube, and the inlet and outlet of the water pump in the water bath constant temperature oscillator are simultaneously connected to the condenser through pipes;

[0008] The first port of the three-way valve is connected to the gas measuring tube, the second port is connected to the internal cavity of the sealing cover, and the third port is connected to the reaction bottle. The lower end of the gas measuring tube is connected to the level bottle through a pipeline.

[0009] Furthermore, a hydrogen alarm device is installed on the top of the sealing cover.

[0010] Furthermore, the mouth of the reaction bottle is sealed by a sealing plug equipped with an air connection tube, and the reaction bottle is connected to the third port of the three-way valve through the air connection tube on the sealing plug.

[0011] Compared with the prior art, the utility model has the following advantages: the reaction bottle of the utility model adopts a flat-bottom flask, which makes it easy to weigh the sample, the reaction solvent is fully contacted for reaction, and the hydrogen preparation is more complete; the hydrogen alarm device can monitor hydrogen leakage in real time to ensure detection accuracy; the electric three-way valve can quickly adjust the liquid levels of the level bottle and the gas tube to be parallel; by adding a water bath constant temperature oscillator, the detection of hydrogen content achieves a constant temperature effect, reduces the influence of temperature changes on the volume of hydrogen, meets the requirements of the gas state equation, and the data is stable; the condenser is connected to the constant temperature water in the water bath constant temperature oscillator to ensure that the gas tube in the condenser is in a constant temperature state; adding a sealing cover to maintain airflow stability enhances the constant temperature effect and reduces the influence of the external environment on the reaction process. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 This is a schematic diagram of the detection device of the present utility model. DETAILED DESCRIPTION

[0013] In order to make the purpose, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings.

[0014] Reference Figure 1 As shown, the utility model discloses a device for measuring the hydrogen content of methyl high-hydrogen silicone oil, comprising a sealing cover 1, the sealing cover 1 comprising a sealing cover 1.1 with an upper opening and a cover 1.2 detachably and sealingly connected to the open end of the sealing cover 1.1, a hydrogen alarm device 2 is also installed on the top of the sealing cover 1, and a water bath constant temperature oscillator 3, a level bottle 11, a condenser 4, a gas measuring tube 5, and a three-way valve 6 are arranged in the sealing cover 1, and the three-way valve 6 is an electrically controlled three-way valve.

[0015] A reaction bottle 7 with a sealed mouth is placed on the oscillation platform of the water bath constant temperature oscillator 3. The reaction bottle 7 is a flat-bottom flask. The mouth of the reaction bottle 7 is sealed by a sealing plug 8. The reaction bottle 7 is used to place a mixed sample of n-butanol and silicone oil. A reaction cup 9 is placed in the reaction bottle 7. The reaction cup 9 is used to place alkaline sodium hydroxide. The mouth of the reaction cup 9 is higher than the liquid level of the reaction bottle 7.

[0016] The condenser 4 is arranged vertically, and the gas measuring tube 5 is coaxially passed through the condenser 4 and extends out of the condenser 4 at both ends. The two ends of the condenser 4 are sealed with the gas measuring tube 5, and the water pump inlet and outlet of the water bath constant temperature oscillator 3 are connected to the upper and lower ends of the condenser 4 through pipes at the same time.

[0017] The first port of the three-way valve 6 is connected to the gas measuring tube 5, and the second port is connected to the internal cavity of the sealing cover 1. The sealing plug 8 at the mouth of the reaction bottle 7 is provided with a gas connecting tube 10. The third port of the three-way valve 6 is connected to the gas connecting tube 10 on the sealing plug 8, and the lower end of the gas measuring tube 5 is connected to the level bottle 11 through a pipeline.

[0018] Example 1: According to an embodiment of a device for determining the hydrogen content of methyl high-hydrogen silicone oil of the utility model, 0.1 g of sample is weighed in a weighing bottle, 30 ml of n-butanol is added and mixed evenly, 15 ml of 20% sodium hydroxide solution is added to a reaction cup, the reaction cup is carefully placed in the reaction bottle, and then placed in a water bath constant temperature oscillator, the switch is turned on, the sodium hydroxide solution in the reaction cup should not contact the mixture of n-hexane and sample in the reaction bottle, check for air leakage, open the electric three-way valve to connect to the gas pipe, adjust the zero point, turn on the oscillator switch, tilt the reaction cup, and fully contact the sodium hydroxide solution with the sample. When the liquid level in the gas pipe no longer drops, turn off the oscillator, stabilize for 5 minutes, adjust the level, read and record the data.

[0019] Example 2: The steps of the method described in this example are the same as those in Example 1, except that the following parameters are different: 0.2 g of sample is weighed in a weighing bottle, 20 ml of n-butanol is added and mixed evenly, and 15 ml of 25% sodium hydroxide solution is added in a reaction cup.

[0020] Example 3: The steps of the method described in this example are the same as those in Example 1, except that the following parameters are different: 20 g of sample is weighed in a weighing bottle, 25 ml of n-butanol is added and mixed evenly, and 20 ml of 20% sodium hydroxide solution is added in a reaction cup.

[0021] Comparative Example 1: According to the example of HG / T4804-2015, 0.1 g was weighed and placed on one side of the reaction flask, 4 ml of n-butanol was poured into it, 4 ml of 20% sodium hydroxide solution was placed on the other side of the reaction flask, the device was connected and placed in a water bath, the zero point was adjusted and the leakage was checked, the reaction flask was removed and tilted left and right to allow the sodium hydroxide solution to react with the sample. When the liquid level in the measuring tube no longer dropped, the reaction flask was returned to the water bath and allowed to stand for 5 minutes. The level was adjusted and the data was read and recorded.

[0022] Comparative Example 2: According to the example of HG / T4804-2015, 0.2 g was weighed and placed on one side of the reaction flask, 5 ml of n-butanol was poured into it, and 5 ml of 15% sodium hydroxide solution was placed on the other side of the reaction flask.

[0023] Comparative Example 3: According to the example of HG / T4804-2015, 5 g was weighed and placed on one side of the reaction flask, 5 ml of n-butanol was poured into it, and 8 ml of 25% sodium hydroxide solution was placed on the other side of the reaction flask.

[0024] According to the formula

[0025]

[0026] Where: X-mass fraction of hydrogen content, expressed in %;

[0027] The value of the atmospheric pressure during the experiment, in Pa;

[0028] V-the value of the hydrogen volume reading, in ml;

[0029] T-water bath temperature in °C;

[0030] m-mass of the sample, in g.

[0031] The measured results are shown in Table 1:

[0032] Table 1 Test results of hydrogen content of methyl high hydrogen silicone oil

[0033]

[0034] As can be seen from Table 1, in Comparative Example 1, because the interlayer between the gas measuring tube and the sleeve is filled with air that cannot flow, its temperature is different from that of the water bath and is easily affected by the external temperature, resulting in poor accuracy of the results. In Example 1, because the interlayer between the gas measuring tube and the sleeve is filled with flowing circulating water, its temperature is consistent with that of the water bath and there is almost no temperature change, the effect on the hydrogen volume is negligible, and the detection results are highly accurate and precise.

[0035] It can be seen from the above scheme that the utility model has the following advantages: the utility model improves the reaction bottle, making it convenient to weigh the sample, the reaction solvent is fully contacted for reaction, and the hydrogen preparation is more complete; the hydrogen alarm device can monitor hydrogen leakage in real time to ensure detection accuracy; by adding a water bath constant temperature oscillator, the detection of hydrogen content achieves a constant temperature effect, reducing the influence of temperature changes on the volume of hydrogen, meeting the requirements of the gas state equation, and the data is stable.

Claims

1. A device for measuring the hydrogen content of methyl high hydrogen silicone oil, characterized in that: The invention comprises a sealing cover, wherein a water bath constant temperature oscillator, a condenser, a gas burette, a level bottle, and a three-way valve are arranged in the sealing cover; a reaction bottle with a sealed bottle mouth is placed on the oscillation platform of the water bath constant temperature oscillator, the reaction bottle is used to place a mixed sample of n-butanol and silicone oil, a reaction cup is placed in the reaction bottle, the reaction cup is used to place alkaline solution sodium hydroxide, and the cup mouth of the reaction cup is higher than the liquid level of the reaction bottle; The condenser is arranged vertically, the gas measuring tube is coaxially passed through the condenser and extends out of the condenser at both ends, the two ends of the condenser are sealedly connected to the gas measuring tube, and the inlet and outlet of the water pump in the water bath constant temperature oscillator are simultaneously connected to the condenser through pipes; The first port of the three-way valve is connected to the gas measuring tube, the second port is connected to the internal cavity of the sealing cover, and the third port is connected to the reaction bottle. The lower end of the gas measuring tube is connected to the level bottle through a pipeline.

2. A device for measuring the hydrogen content of methyl high hydrogen silicone oil according to claim 1, characterized in that: A hydrogen alarm device is also installed on the top of the sealing cover.

3. A device for measuring the hydrogen content of methyl high hydrogen silicone oil according to claim 1, characterized in that: The mouth of the reaction bottle is sealed by a sealing plug equipped with an air connection tube, and the reaction bottle is connected to the third port of the three-way valve through the air connection tube on the sealing plug.

4. A device for measuring the hydrogen content of methyl high hydrogen silicone oil according to claim 1, characterized in that: The three-way valve is an electrically controlled three-way valve.

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