High-temperature-resistant water test paste and preparation method thereof

Abstract

The invention relates to a high-temperature-resistant water test paste and a preparation method thereof, and belongs to the technical field of preparation of fine chemical products. The water testing paste is prepared by chemical modification and addition of an auxiliary carrier, solves the problems of viscosity reduction, dispersion and unstable color development of the existing water testing paste under a high-temperature condition, realizes clear display of a water level boundary line under a high-temperature environment, and has the capability of detecting the water content in an oil phase. The high-temperature-resistant water test paste is prepared through the coupling effect of a silane coupling agent and graft polymerization of modified phenolphthalein with olefin groups and a carrier. The water test paste shows excellent viscosity stability and color development performance in a high-temperature environment, can accurately detect the position of a water layer in liquid, and is expanded to detection of the water content in an oil phase. Experiments show that the water test paste is suitable for a high-temperature scene of 120 DEG C or above, and has wide industrial application value and application prospect.

Description

Technical Field

[0001] The present invention relates to a reagent for liquid detection, in particular a water test paste used under high temperature conditions, and belongs to the technical field of the preparation of fine chemical products. Background Art

[0002] The water test paste is a paste-like reagent used to detect the position of the water layer and the water content in a liquid, and is widely used in industries such as petroleum, chemical engineering, and shipping, for scenarios such as oil tanks and storage containers. However, the current water test paste is mainly applicable to normal temperature environments. Under high temperature conditions, its viscosity decreases significantly, and it is prone to dispersion, resulting in unclear color development or even failure.

[0003] In the prior art, Patent CN103173206A (Water test paste that changes color when encountering water): discloses a water test paste that changes color rapidly when encountering water, with the advantages of rapid color change and clear boundaries. However, its viscosity drops severely under high temperature conditions and it cannot be used stably.

[0004] Patent CN1066729A (Composition of water detection paste): proposes a reagent suitable for detecting the water level at the bottom of a petroleum container, with rapid color development, but there is a problem of insufficient stability in a high temperature environment.

[0005] Patent Application No. 201510030428.5 (A dual-purpose oil and water test paste): discloses a multi-functional reagent that can detect both the oil level and the water level, but is mainly applicable to normal temperature environments and lacks research on high temperature stability.

[0006] The main limitations of the current technology are as follows: Under high temperature conditions, the viscosity of the water test paste decreases significantly, it is prone to dispersion, and the color development is unstable. To address these problems, developing a high temperature resistant water test paste and its preparation method, which can maintain stable viscosity and color development performance in a high temperature environment, while expanding the detection function of the water content in the oil phase, has important application value.

[0007] The present invention provides a high temperature resistant water test paste and its preparation method, which solves the problems of viscosity reduction, dispersion, and unstable color development of the existing water test paste under high temperature conditions, realizes clear display of the water level boundary in a high temperature environment, and at the same time has the ability to detect the water content in the oil phase. Summary of the Invention

[0008] To achieve the above object, the present invention provides a high temperature resistant water test paste and its preparation method: The high temperature resistant water test paste of the present invention is composed of the following components in parts by weight: Polyethylene glycol: 50 - 70 parts, used as a liquid carrier to provide appropriate viscosity and ductility; Modified phenolphthalein: 5 - 15 parts, used as a color developer, grafted with a silane coupling agent to improve thermal stability; Calcium oxide: 10 - 20 parts, used as a solid carrier to enhance adhesion ability and adsorption; Nano-silica: 5 - 15 parts, providing physical reinforcement and enhancing high-temperature stability; Silane coupling agent A - 151: 1 - 5 parts, as a coupling agent to chemically couple the carrier and the chromogenic agent to form a stable structure; Glycerol: 0.1 - 5 parts, glycerol is used as an auxiliary material to improve viscosity; Silicone oil: 0.1 - 10 parts, improving the heat resistance and viscosity retention ability of the leak detection paste.

[0009] Furthermore, the preparation method of the modified phenolphthalein includes the following steps: At room temperature, put nitrobenzene into the reaction kettle and stir at a speed of 70 - 90 r / min. After stirring for 5 min, add phenolphthalein, acrylic anhydride and aluminum trichloride and continue stirring. React for 0.5 - 1 h to obtain modified phenolphthalein.

[0010] Furthermore, the weight parts composition of the modified phenolphthalein: nitrobenzene 70 - 80; phenolphthalein 10 - 20 parts; acrylic anhydride: 5 - 10 parts; aluminum trichloride 1 - 2 parts.

[0011] Furthermore, the particle size D of the nano-silica 50 10 - 20 nm, D 100 30 - 50 nm, which can improve the physical stability and high-temperature resistance of the leak detection paste.

[0012] Furthermore, the molecular weight of the polyethylene glycol is 400 - 1000, used as a liquid carrier to provide the fluidity and viscosity of the paste.

[0013] Furthermore, the calcium oxide has a calcium oxide content of more than 98% and is in the form of uniform powder. Calcium oxide not only acts as a solid carrier in the leak detection paste, but also can adsorb trace moisture, further improving the detection accuracy.

[0014] Furthermore, the preparation method of the high-temperature resistant leak detection paste includes the following steps: Put polyethylene glycol into the reaction kettle, and successively add glycerol, silicone oil, calcium oxide and nano-silica, stir until uniform, heat up to 70 - 90 °C, add modified phenolphthalein silane coupling agent, stir evenly, and continue to react for 1 - 2 h. After the reaction is completed, cool to room temperature to obtain the high-temperature resistant leak detection paste.

[0015] Furthermore, the leak detection paste can be stably used in a high-temperature environment of 120 °C to 150 °C, and will not disperse due to a decrease in viscosity when detecting liquids.

[0016] Furthermore, the leak detection paste has a clear color change boundary, can accurately detect the position of the water layer in the liquid, and can also be used for the detection of water content in the oil phase.

[0017] The advantages of the present invention are as follows: Through the coupling effect of silane coupling agent A-151, its siloxane groups react with polyethylene glycol, calcium oxide and silica, endowing the carrier with grafting activity. At the same time, its olefin groups polymerize with the olefin-based phenolphthalein color-developing agent, grafting phenolphthalein onto the carrier. This grafting structure significantly improves the thermal stability and solvent stability of the water detection paste, enabling it to maintain stable viscosity and clear color development under high-temperature environments. Meanwhile, the physical reinforcement effect of nano-silica further enhances the overall performance. In addition, the addition of auxiliary material glycerol improves the viscosity of the water detection paste, making the paste have better ductility and adhesion, and the introduction of silicone oil significantly improves the heat resistance and viscosity retention ability of the water detection paste.

[0018] Advantages: 1. It has excellent viscosity stability and color development performance in high-temperature environments above 120°C; 2. The color development boundary is clear, and it can quickly detect the position of the water layer in the liquid; 3. It is applicable to the detection of water content in the oil phase, expanding the application scenarios of the water detection paste; 4. It overcomes the problems of viscosity reduction and color development performance failure caused by high temperature in the prior art. Specific Embodiments

[0019] The synthesis route of the high-temperature resistant water detection paste of the present invention is as follows: To facilitate the understanding of the present invention, the present invention will be further described below in conjunction with examples and comparative examples. The following examples are only for better understanding of the present invention, and do not mean that the present invention is limited to the following examples. The present invention will be further described in detail below in conjunction with examples and comparative examples.

[0020] Example 1: Preparation of High-Temperature Resistant Water Detection Paste with Basic Formula Preparation of Modified Phenolphthalein: At room temperature, 70 g of nitrobenzene is placed in a reaction kettle and stirred at a rotation speed of 70 r / min. After stirring for 5 min, 20 g of phenolphthalein, 8 g of acrylic anhydride and 2 g of aluminum trichloride are added and stirred continuously for 0.5 h to obtain modified phenolphthalein.

[0021] Preparation of High-Temperature Resistant Water Detection Paste: 50 g of polyethylene glycol with a molecular weight of 600, 0.1 g of glycerol, and 0.1 g of silicone oil are placed in a reaction kettle and stirred at a rotation speed of 80 r / min. After stirring for 5 min, 10 g of uniform powdery calcium oxide with a calcium oxide content of 98.13% and D 50 10.33 nm, D 10010 g of nano-silica with a size of 30.48 nm was heated to 80 °C, and 10 g of modified phenolphthalein and 2 g of silane coupling agent A-151 were added successively and stirred evenly. After reacting for 1 h and cooling to room temperature, a high-temperature resistant water test paste was obtained.

[0022] Performance tests showed that the water test paste had a clear color change boundary and no dispersion phenomenon at a high temperature of 120 °C, and could be stably used for the detection of the water layer in liquids.

[0023] Example 2: Formula of water test paste with increased calcium oxide content Preparation of modified phenolphthalein: At room temperature, 70 g of nitrobenzene was placed in a reaction kettle and stirred at a speed of 70 r / min. After stirring for 5 min, 18 g of phenolphthalein, 10 g of acrylic anhydride and 2 g of aluminum trichloride were added and stirred continuously. After reacting for 0.5 h, modified phenolphthalein was obtained.

[0024] Preparation of high-temperature resistant water test paste: 60 g of polyethylene glycol with a molecular weight of 800, 0.1 g of glycerol and 0.1 g of silicone oil were placed in a reaction kettle and stirred at a speed of 80 r / min. After stirring for 5 min, 20 g of uniform powdered calcium oxide with a calcium oxide content of 98.22% and D 50 10.19 nm, D 100 8 g of nano-silica with sizes of 31.44 nm were heated to 80 °C, and 12 g of modified phenolphthalein and 3 g of silane coupling agent A-151 were added successively and stirred evenly. After reacting for 1 h and cooling to room temperature, a high-temperature resistant water test paste was obtained.

[0025] Tests showed that the water test paste still had good viscosity and color change performance at an environment of 150 °C, and at the same time, the adsorption ability of calcium oxide significantly improved the detection sensitivity to moisture.

[0026] Example 3: Preparation of water test paste with different carrier combinations Preparation of modified phenolphthalein: At room temperature, 70 g of nitrobenzene was placed in a reaction kettle and stirred at a speed of 75 r / min. After stirring for 5 min, 18 g of phenolphthalein, 10 g of acrylic anhydride and 2 g of aluminum trichloride were added and stirred continuously. After reacting for 0.7 h, modified phenolphthalein was obtained.

[0027] Preparation of high-temperature resistant water test paste: 70 g of polyethylene glycol with a molecular weight of 1000, 5 g of glycerol and 0.1 g of silicone oil were placed in a reaction kettle and stirred at a speed of 90 r / min. After stirring for 5 min, 20 g of uniform powdered calcium oxide with a calcium oxide content of 98.25% and D 50 13.39 nm, D 10012 g of nano-silica with a size of 31.75 nm was heated to 85 °C, and 8 g of modified phenolphthalein and 2 g of silane coupling agent A-151 were added successively and stirred evenly. After reacting for 1.2 h and cooling to room temperature, a high-temperature resistant water test paste was obtained.

[0028] The experimental results showed that the paste had stable performance in a high-temperature environment of 125 °C, demonstrating the effect of glycerol as an auxiliary material to improve viscosity. The paste had better ductility and adhesion.

[0029] Example 4: Preparation of a water test paste for enhancing color development sensitivity Preparation of modified phenolphthalein: At room temperature, 70 g of nitrobenzene was placed in a reaction kettle and stirred at a speed of 75 r / min. After stirring for 5 min, 20 g of phenolphthalein, 10 g of acrylic anhydride and 2 g of aluminum trichloride were added and stirring was continued. After reacting for 0.8 h, modified phenolphthalein was obtained.

[0030] Preparation of high-temperature resistant water test paste: 55 g of polyethylene glycol with a molecular weight of 400, 0.1 g of glycerol, and 0.1 g of silicone oil were placed in a reaction kettle and stirred at a speed of 80 r / min. After stirring for 5 min, 12 g of uniform powdered calcium oxide with a calcium oxide content of 98.27% and D 50 11.66 nm, D 100 10 g of nano-silica with sizes of 31.47 nm were heated to 85 °C, and 15 g of modified phenolphthalein and 4 g of silane coupling agent A-151 were added successively and stirred evenly. After reacting for 1.5 h and cooling to room temperature, a high-temperature resistant water test paste was obtained.

[0031] Tests showed that the color development boundary of the paste was clearer, it had higher sensitivity to changes in trace moisture, and showed higher detection accuracy in the detection of water content in the oil phase.

[0032] Example 5: Preparation of a water test paste under high-temperature extreme environments Preparation of modified phenolphthalein: At room temperature, 75 g of nitrobenzene was placed in a reaction kettle and stirred at a speed of 75 r / min. After stirring for 5 min, 18 g of phenolphthalein, 8 g of acrylic anhydride and 1 g of aluminum trichloride were added and stirring was continued. After reacting for 1 h, modified phenolphthalein was obtained.

[0033] Preparation of high-temperature resistant water test paste: 65 g of polyethylene glycol with a molecular weight of 600, 5 g of silicone oil and 0.1 g of glycerol were placed in a reaction kettle and stirred at a speed of 80 r / min. After stirring for 5 min, 15 g of uniform powdered calcium oxide with a calcium oxide content of 98.73% and D 50 11.66 nm, D 10010 g of nano-silica with a size of 31.47 nm was heated to 90 °C, and 10 g of modified phenolphthalein and 3 g of silane coupling agent A-151 were added successively and stirred evenly. After continuing the reaction for 1.5 h and cooling to room temperature, a high-temperature resistant water test paste was obtained.

[0034] Experiments showed that this formulation could maintain good stability at 160 °C, with a clear color boundary line, and the introduction of silicone oil significantly improved the heat resistance and viscosity retention ability of the water test paste.

[0035] Comparative Example 1: Preparation of ordinary phenolphthalein water test paste 50 g of polyethylene glycol with a molecular weight of 600, 0.1 g of glycerol, and 0.1 g of silicone oil were placed in a reaction kettle, stirred at a speed of 80 r / min for 5 min, and then 10 g of uniform powdery calcium oxide with a calcium oxide content of 98.13% and D 50 10.33 nm, D 100 10 g of nano-silica with sizes of 10.33 nm and 30.48 nm was heated to 80 °C, 10 g of ordinary phenolphthalein and 2 g of silane coupling agent A-151 were added successively and stirred evenly. After continuing the reaction for 1 h and cooling to room temperature, an ordinary water test paste was obtained.

[0036] Performance tests showed that this water test paste had no obvious color boundary line at 80 °C, no dispersion phenomenon occurred, and it could not be used for detecting the water layer in liquids.

[0037] Comparative Example 2: Preparation of ordinary calcium oxide water test paste 50 g of polyethylene glycol with a molecular weight of 600, 0.1 g of glycerol, and 0.1 g of silicone oil were placed in a reaction kettle, stirred at a speed of 80 r / min for 5 min, and then 10 g of powdery and granular mixed calcium oxide with a content of 78.62% and D 50 10.33 nm, D 100 10 g of nano-silica with sizes of 10.33 nm and 30.48 nm was heated to 80 °C, 10 g of ordinary phenolphthalein and 2 g of silane coupling agent A-151 were added successively and stirred evenly. After continuing the reaction for 1 h and cooling to room temperature, an ordinary water test paste was obtained.

[0038] Performance tests showed that this water test paste had no obvious color boundary line at 70 °C and dispersion phenomenon occurred, and it could not be used for detecting the water layer in liquids.

[0039] Comparative Example 3: Preparation of ordinary silica water test paste Place 50 g of polyethylene glycol with a molecular weight of 600, 0.1 g of glycerol, and 0.1 g of silicone oil in a reaction kettle, with a rotation speed of 80 r / min, stir for 5 min, then add 10 g of powdery and granular mixed calcium oxide with a content of 78.62% and 10 g of ordinary silica, heat to 80 °C, and sequentially add 10 g of ordinary phenolphthalein and 2 g of silane coupling agent A-151, and stir evenly. Continue to react for 1 h, and obtain an ordinary water test paste after cooling to room temperature.

[0040] Performance tests show that the water test paste has an obvious color boundary line at room temperature, but dispersion occurs and it cannot be used for the detection of the water layer in liquids.

Claims

1. A high temperature resistant water testing paste and a preparation method thereof, characterized in that: The invention comprises the following components in parts by weight: 50-70 parts of polyethylene glycol; 5-15 parts of modified phenolphthalein; Calcium oxide: 10-20 parts; Nano silicon dioxide: 5-15 parts; Silane coupling agent A-151: 1-5 parts; Glycerin: 0.1-5 parts; Silicone oil: 0.1-10 parts.

2. A high temperature resistant water testing paste and a preparation method thereof according to claim 1, characterized in that: The preparation method of the modified phenolphthalein comprises the following steps: Put nitrobenzene into a reaction kettle at room temperature and stir at a speed of 70-90 r / min. After stirring for 5 minutes, add phenolphthalein, acrylic anhydride and aluminum chloride and continue stirring. React for 0.5-1 hour to obtain modified phenolphthalein.

3. A high temperature resistant water testing paste and a preparation method thereof according to claim 2, characterized in that: The modified phenolphthalein is composed of: 70-80 parts by weight of nitrobenzene; 10-20 parts by weight of phenolphthalein; 5-10 parts by weight of acrylic anhydride; and 1-2 parts by weight of aluminum chloride.

4. A high temperature resistant water testing paste and a preparation method thereof according to claim 3, characterized in that: The nano-silicon dioxide particle size D 50 10-20nm, D 100 30-50nm.

5. A high temperature resistant water testing paste and a preparation method thereof according to claim 4, characterized in that: The molecular weight of the polyethylene glycol is 400-1000.

6. A high temperature resistant water testing paste and a preparation method thereof according to claim 5, characterized in that: The calcium oxide has a calcium oxide content of more than 98% and is in a uniform powdery state.

7. A high temperature resistant water testing paste and a preparation method thereof according to claim 6, characterized in that: The method for preparing the high temperature resistant water testing paste comprises the following steps: Place polyethylene glycol in a reaction kettle, add glycerol, silicone oil, calcium oxide and nano-silicon dioxide in sequence, stir until uniform, heat to 70-90°C, add modified phenolphthalein and silane coupling agent, stir evenly, continue to react for 1-2 hours, and after the reaction is completed, cool to room temperature to obtain a high temperature resistant water test paste.

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