Rapid detection method for carbon tetrachloride in water-based paraffin remover and inhibitor

Abstract

The invention discloses a rapid detection method for carbon tetrachloride in a water-based paraffin remover and inhibitor, the rapid detection method is suitable for rapid detection of the carbon tetrachloride in the paraffin remover and inhibitor, the rapid detection steps comprise sample preparation, reagent preparation, detection stage and result determination, and the method has the advantages of rapidness and high efficiency, and can be used for rapid screening of the carbon tetrachloride in the paraffin remover and inhibitor. The method comprises the following steps: adding a fresh aluminum bromide ethanol solution into a to-be-detected water-based paraffin remover and inhibitor, keeping a water bath at 100 DEG C, and continuously stirring; if white precipitates or flocculent insoluble substances appear in the sample to be detected, it is judged that the sample to be detected contains carbon tetrachloride, and if white precipitates or flocculent insoluble substances do not appear in the sample to be detected, it is judged that the sample to be detected does not contain carbon tetrachloride. According to the method, large instruments and equipment are not needed, and rapid detection of carbon tetrachloride in the water-based paraffin remover and inhibitor can be achieved in a simple and efficient mode.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of rapid detection of oil field chemicals, and particularly relates to a rapid detection method for carbon tetrachloride in water-based wax removal and inhibition agent. BACKGROUND

[0002] With the increasing use of oil field chemicals in oil field enterprises, the role of oil field chemicals is becoming more and more important, which can effectively solve the problems of thick oil, low permeability, high water content and the like, and improve the oil and gas exploitation efficiency. The main function of the water-based wax removal and inhibition agent is to dissolve organic wax and prevent wax crystallization, which can prevent and remove wax deposition in pipelines, and a large amount of organic solvents such as benzene, toluene, gasoline and diesel are often used as main components. Since carbon tetrachloride has the best wax removal and inhibition effect, a product with substandard quality is used as a component in the production of water-based wax removal and inhibition agent. However, carbon tetrachloride can introduce chlorine elements that corrode pipelines, causing equipment corrosion and other problems, and even causing failure accidents. In order to further do a good job in safety and health, it is necessary to strictly control the carbon tetrachloride component in the water-based wax removal and inhibition agent.

[0003] As an organic chlorine substance, carbon tetrachloride can be detected by using the existing organic chlorine detection method. The standard "SY-T6300-2009 Technical Conditions for Wax Removal and Inhibition Agent for Oil Production" clearly requires that the wax removal and inhibition agent cannot contain organic chlorine, that is, it cannot contain carbon tetrachloride. The standard also provides a corresponding detection method, i.e. oxygen bottle combustion method. This method calculates the total chlorine content in the water-based wax removal and inhibition agent by titration, and then subtracts the inorganic chlorine to obtain the content of carbon tetrachloride. The patent "Method for qualitatively and quantitatively determining organic chlorine in oil field chemicals" (application number 201810395561.4) uses a method combining solid-phase extraction, gas chromatography and mass spectrometry, which can process a large number of oil field chemicals and determine the content of organic chlorine therein. However, this method uses a variety of large instruments, which is difficult to apply to on-site rapid detection and has obvious limitations. When facing a large number of samples to be detected, this method has the problems of complicated steps and inability to rapidly detect, which cannot meet the current demand for rapid screening of carbon tetrachloride. SUMMARY

[0004] The purpose of the present application is to provide a rapid detection method for carbon tetrachloride in water-based wax removal and inhibition agent, which solves the problem of complicated detection steps and inability to rapidly detect carbon tetrachloride in the existing water-based wax removal and inhibition agent.

[0005] The technical solution adopted by the present application is a rapid detection method for carbon tetrachloride in water-based wax removal and inhibition agent, and the specific steps are as follows:

[0006] Step 1: Sample preparation: take a certain amount of water-based wax removal and inhibition agent, place it in a beaker, and place the beaker in a 100℃ water bath as a sample to be detected, and reserve it for use;

[0007] Step 2: Reagent preparation: take aluminum bromide, ethanol, mix them, stir at room temperature, prepare a fresh aluminum bromide ethanol solution, and reserve;

[0008] Step 3: Take the fresh aluminum bromide ethanol solution prepared in step 2, add it to the sample to be tested, keep the water bath at 100℃, and continue stirring;

[0009] Step 4: After stirring is complete, if white precipitate or flocculent insoluble matter appears in the sample to be tested, it is determined that the sample to be tested contains carbon tetrachloride, and if no white precipitate or flocculent insoluble matter appears in the sample to be tested, it is determined that the sample to be tested does not contain carbon tetrachloride.

[0010] The present application is also characterized in that,

[0011] Further, the ethanol of step 2 is anhydrous ethanol.

[0012] Further, the ratio of aluminum bromide to anhydrous ethanol is (5-10) g:(80-100) mL.

[0013] Further, the stirring time of step 3 is 5 min.

[0014] Further, the ratio of aluminum bromide ethanol solution to sample to be tested in step 3 is (5-10) mL:(80-100) g.

[0015] Compared with the prior art, the present application has the following beneficial effects:

[0016] Currently, the prior art includes oxygen bottle combustion method, oxidation microcoulometry method, which have many detection steps, use indirect method to determine carbon tetrachloride, and sodium biphenyl reduction method has the problem of large end point judgment error. These three methods still cannot achieve the purpose of rapid detection of carbon tetrachloride. The present application is a rapid detection method for carbon tetrachloride in water-based paraffin remover, which is suitable for rapid detection of carbon tetrachloride in paraffin remover and paraffin inhibitor, does not need to use large instruments and equipment, and can realize rapid detection of carbon tetrachloride in water-based paraffin remover through a simple and efficient way. The rapid detection steps include sample preparation, reagent preparation, detection stage, and result determination, and the method has the advantages of rapidness and efficiency, and can be used for rapid screening of carbon tetrachloride in paraffin remover and paraffin inhibitor. The present application will help to further improve the quality control of water-based paraffin remover, effectively protect property and personal safety, and has a broad application prospect. DETAILED DESCRIPTION

[0017] The present application will be described in detail below in conjunction with specific embodiments.

[0018] Example 1

[0019] The application provides a rapid detection method for carbon tetrachloride in water-based paraffin remover, which comprises the following steps:

[0020] (1) a certain amount of water-based paraffin remover is taken and placed in a beaker, and the beaker is placed in a 100 DEG C water bath as a sample to be tested, ready for use;

[0021] (2) a certain amount of aluminum bromide and anhydrous ethanol are taken and mixed, and the mixture is stirred at room temperature to prepare a fresh aluminum bromide ethanol solution, ready for use;

[0022] (3) a certain amount of the fresh aluminum bromide ethanol solution is taken and added to the sample to be tested, and the 100 DEG C water bath is kept and stirring is continued for 5 min;

[0023] (4) if white precipitate or flocculent insoluble matter appears in the sample to be tested, it is determined that the sample to be tested contains carbon tetrachloride, and if no white precipitate and flocculent insoluble matter appears in the sample to be tested, it is determined that the sample to be tested contains no carbon tetrachloride.

[0024] Example 2

[0025] This example is an example of rapid detection of carbon tetrachloride in water-based paraffin remover.

[0026] 100 g of water-based paraffin remover is taken and placed in a beaker, and the beaker is placed in a 100 DEG C water bath as a sample to be tested, ready for use; 10 g of aluminum bromide and 100 mL of anhydrous ethanol are taken and mixed, and the mixture is stirred at room temperature to prepare a fresh aluminum bromide ethanol solution, ready for use; 10 mL of the fresh aluminum bromide ethanol solution is taken and added to the sample to be tested, and the 100 DEG C water bath is kept and stirring is continued for 5 min; if white precipitate or flocculent insoluble matter appears in the sample to be tested, the sample to be tested is filtered, and the solid substance is taken and placed in anhydrous ethanol, and if the solid substance dissolves, it is determined that the sample to be tested contains carbon tetrachloride.

[0027] Example 3

[0028] This example is an example of rapid detection of carbon tetrachloride in water-based paraffin remover.

[0029] 80 g of water-based paraffin remover is taken and placed in a beaker, and the beaker is placed in a 100 DEG C water bath as a sample to be tested, ready for use; 5 g of aluminum bromide and 80 mL of anhydrous ethanol are taken and mixed, and the mixture is stirred at room temperature to prepare a fresh aluminum bromide ethanol solution, ready for use; 5 mL of the fresh aluminum bromide ethanol solution is taken and added to the sample to be tested, and the 100 DEG C water bath is kept and stirring is continued for 5 min; if white precipitate or flocculent insoluble matter appears in the sample to be tested, the sample to be tested is filtered, and the solid substance is taken and placed in anhydrous ethanol, and if the solid substance dissolves, it is determined that the sample to be tested contains carbon tetrachloride.

[0030] It can be seen that the method for rapidly detecting carbon tetrachloride in water-based paraffin cleaning and preventing agent provided by the application can realize rapid detection of carbon tetrachloride in water-based paraffin cleaning and preventing agent through a simple and efficient way without using large instruments and equipment. The rapid detection steps include sample preparation, reagent preparation, detection stage and result determination, and the method has the advantages of rapidness and efficiency and can be used for rapid screening of carbon tetrachloride in paraffin cleaning and preventing agent. The application will help to further improve the quality control of water-based paraffin cleaning and preventing agent, effectively protect property and personal safety, and has a wide application prospect.

[0031] The key innovation point of the application is that:

[0032] The aluminum bromide reacts with carbon tetrachloride in a 100℃ water bath to generate white crystals (precipitated tetrabromomethane, also known as carbon tetrabromide) that are insoluble in water. The precipitate is insoluble in water and soluble in ethanol, diethyl ether and chloroform. Therefore, the reaction and precipitation phenomenon can be used for qualitative detection of carbon tetrachloride in water-based paraffin cleaning and preventing agent.

[0033] Reaction equation: 4AlBr3+3CCl4→4AlCl3+3CBr4↓

[0034] The rapid detection of carbon tetrachloride in the application is only applicable to water-based paraffin cleaning and preventing agent, and cannot be used for detection of carbon tetrachloride in oil-based paraffin cleaning and preventing agent, because the organic solvent in the oil-based paraffin cleaning and preventing agent can dissolve tetrabromomethane, thereby causing the precipitation phenomenon.

[0035] In order to achieve the above-mentioned purposes, the main technical means adopted in the application is described clearly, completely and accurately, the essential content of the application is described, and the degree of disclosure is that the ordinary skilled person in the art can understand and implement.

Claims

1. A rapid detection method for carbon tetrachloride in water-based dewaxing and wax-preventing agents, characterized in that, The specific steps are as follows: Step 1: Sample preparation: Take a certain amount of water-based anti-wax agent, place it in a beaker, and put the beaker in a 100℃ water bath as the sample to be tested. Step 2: Reagent preparation: Take aluminum bromide and ethanol, mix them together, stir at room temperature, and prepare a fresh aluminum bromide ethanol solution for later use; Step 3: Detection stage: Take the fresh aluminum bromide ethanol solution prepared in step 2, add it to the sample to be tested, and keep it in a 100°C water bath with continuous stirring; Step 4: Result determination: If a white precipitate or flocculent insoluble matter appears in the sample after stirring, the sample is determined to contain carbon tetrachloride. If no white precipitate or flocculent insoluble matter appears in the sample, the sample is determined to be free of carbon tetrachloride.

2. The rapid detection method for carbon tetrachloride in water-based dewaxing agents according to claim 1, characterized in that, The ethanol mentioned in step 2 is anhydrous ethanol.

3. The rapid detection method for carbon tetrachloride in water-based dewaxing agents according to claim 2, characterized in that, The ratio of aluminum bromide to anhydrous ethanol is (5-10) g: (80-100) mL.

4. The rapid detection method for carbon tetrachloride in water-based dewaxing agents according to claim 1, characterized in that, The continuous stirring time in step 3 is 5 minutes.

5. The rapid detection method for carbon tetrachloride in water-based dewaxing agents according to claim 1, characterized in that, The ratio of aluminum bromide ethanol solution to the sample to be tested in step 3 is (5-10) mL: (80-100) g.