Oil field sludge multicomponent testing method

[0042] Example

[0043] like figure 1 As shown, extracting 5 parts of sludge samples with a quality of 8 grams from different regions of a certain oil field carries out the test of each component according to the oilfield sludge multi-component test method of the present invention, specifically including the following process:

[0044] (1) Put each sample into five non-adhesive filter cartridges with constant weight, and mark them as samples No. 1, 2, 3, 4 and 5 respectively, and package them with a mass of m 筒 In the rubber-free filter cartridges, the quality of each filter cartridge is as described in Table 1, and then the corresponding glue-free filter cartridges were placed in the extraction devices numbered 1, 2, 3, 4, and 5 from sample No. 1 , and respectively use petroleum ether extractant with a boiling range of 90-95°C to conduct heating and reflux extraction at 90±3°C until the extract is clear, and then continue to reflux for 1h. Wherein the extraction device structure in this step is as follows figure 2 As shown, there is an extraction bottle 1 for holding the extraction solvent at the bottom, a heating device (not shown) is arranged below the extraction bottle 1, a thermometer 3 is also arranged in the extraction bottle, and a thermometer 3 is arranged above the extraction bottle 1. There is an extraction tube 2 for containing solute, the bottom of the extraction tube 2 is closed and the upper part is open, and the bottom of the extraction tube 2 is connected laterally with a capillary 2B extending into the extraction bottle. The upper mouth of the extraction bottle 1 is connected to the extraction A bypass pipe 2A is provided between the upper parts of the pipes 2. The bypass pipe 2A extends upward to the upper end of the extraction pipe 2 and communicates with it laterally. A water separator 4 is connected above the extraction pipe 2. The water separator 4 includes a lower side The water-splitting measuring cylinder and the branch pipe 4A laterally bypassed above the water-separating measuring cylinder, the outlet below the branch pipe extends into the extraction pipe 2, the top of the water-separating measuring cylinder is connected to the condensation pipe 5, and the top of the condensation pipe 5 is provided with a dryer 6 , the drier 6 is filled with a desiccant for drying water vapor, and the net weight of the drier 6 together with the inner desiccant is m 干0. When adopting above-mentioned extraction device to carry out the sample extraction of the present invention, the glue-free filter cartridge after packaging is placed in extraction tube 2, and extraction bottle 1 is used to contain extraction agent, and bottom heating device heats extraction agent, The extractant is heated and evaporated upwards for cyclic extraction and purification, so that the organic solute easily soluble in the extractant in the filter cartridge is dissolved and returned to the extraction bottle 1 until it is completely dissolved, and the insoluble residue remains in the filter cartridge.

[0045] (2) Evacuate the extracts in the extraction bottles after extraction in step (1) separately to containers numbered 1, 2, 3, 4, and 5 for later use, and then add toluene to each extraction bottle Extracting agent, and heating to make the extracting agent at 110±3°C, heat and reflux until the extract is clear, continue to reflux for 1h, so that all the asphalt in the residue in the filter cartridge is dissolved in the toluene extract, and wait for the device After cooling for 2 hours, measure the volume of the water phase in each extraction device with a water dividing cylinder and record it as V 水 , and then take out the non-adhesive filter cartridge, dry it at 120±3°C, weigh the mass of the filter cartridge after drying, and record it as m 渣+筒;, finally take off the steam desiccant 6, weigh the mass of each desiccator respectively and record it as m 干1 , m 干1 with m 干0 The difference is the amount of water vapor collected by the dryer, which is converted into V 水 The amount of moisture in the sample can be accurately determined; record the above data in this step in Table 1.

[0046] (3) the toluene solution in each extraction bottle 1 in the step (2) is poured into the m 瓶1 In each Erlenmeyer flask, the solvent was rotatably evaporated at 120±3°C;

[0047] (4) No. 1-5 sherwood oil solution that step (2) is vented to obtain is loaded into respectively numbered as 1-5 such as image 3 In the alumina adsorption column 7 with the structure shown, the bottom is connected with an Erlenmeyer flask 8, and each column is tested with petroleum ether, toluene, and toluene-ethanol with a volume ratio of 1:1 in a water bath at 50±2°C. Wash the alumina chromatography column with mixed reagents, and collect the solution washed by petroleum ether into Erlenmeyer flasks numbered 1-5 with constant weight; In the third conical flask of 5, the solution washed by the toluene-ethanol test mixed reagent is collected respectively in the conical flask four with the number of 1-5 after constant weight, and the above washing process can separate dissolved saturated components, aromatic components and Colloid, the mass of each Erlenmeyer flask after constant weight is recorded as m 瓶2 、m 瓶3 and m 瓶4 , and then rotate and evaporate until the solvent is completely volatilized; specifically, when each sample is rinsed separately, the petroleum ether solution of each sample obtained by venting in step (2) is loaded into the chromatographic column numbered 1-5 respectively After neutralization, the bottoms are respectively connected with Erlenmeyer flasks numbered 1-5, and in a water bath at 50±2°C, first use a flask with a volume of V 1 The sherwood oil washes the alumina chromatographic column until the solution at the liquid end at the bottom is colorless and clear, and the volumetric consumption of sherwood oil is V 1 , Remove each Erlenmeyer flask II, and obtain a petroleum ether solution containing saturated components in the Erlenmeyer flask II. At the bottom of the chromatographic column, use three Erlenmeyer flasks numbered 1-5 to connect respectively, and wash the chromatographic column with benzyl to the bottom of the liquid end solution to be colorless and clear, and the volume consumption of toluene is V 2 , Move each Erlenmeyer flask three times to obtain a toluene solution containing aromatic components. Use conical flasks numbered 1-5 to connect at the bottom of each chromatography column, and use volume V 3 Wash the chromatography column with ethanol until the liquid at the bottom is clear, aiming to wash down the polar colloids of small molecules, and then use V 3 volume of toluene, designed to desorb macromolecular colloids, and then rinse with a volume of V 3 The toluene-ethanol solution washes to desorb the macromolecular colloid components in the layer plate column, and then washes the chromatographic column with ethanol solution to complete the washing of the macromolecular colloid, and finally obtains the macromolecular colloid in each Erlenmeyer flask four. quality toluene-ethanol solution. After rinsing, each Erlenmeyer flask was rotatably evaporated until the solvent was completely evaporated; wherein the amount of each rinsing solution V 1、2或3 =8*oil content of sludge*component coefficient, the unit is ml, the value of component coefficient, saturated fraction and aromatic fraction are taken as 80, colloid is taken as 40, wherein the oil content of sludge can be according to step (2) Substitute the measured data into formula (2) to get the calculation.

[0048] (5) Place each Erlenmeyer flask solution corresponding to each sample in steps (3) and (4) in a vacuum drying oven, vacuum dry at 105±3°C and 93kpa, and weigh the amount of the Erlenmeyer flask respectively. Mass, the mass of each sample Erlenmeyer flask is recorded as m 瓶1+沥青 , m 瓶2+饱和 , m 瓶3+芳香 , m 瓶4+胶质 , recorded in Table 1.

[0049] (6) Use 15mL volume ratio of 1:1 toluene- Mixed butanone reagents are combined and poured into conical flasks numbered 1-5 with constant weight five, and the mass of conical flask five is denoted as m 瓶5 , and then use 10mL of toluene-butanone mixed reagent with a volume ratio of 1:1 to wash the original Erlenmeyer flask 3 times, pour the washing solution into the corresponding Erlenmeyer flask 5, and place each Erlenmeyer flask 5 in a cold bath Frozen and crystallized at a cooling rate of 0.5K/min, and continued to age at a constant temperature for 1h when cooled to -20±0.1°C, and filtered under reduced pressure. The solid on the filter paper was crude wax crystals, and the temperature of the solution was 50±3°C Dissolve the wax crystals in petroleum ether, remove the solvent by rotary evaporation at 90±3°C, place in a vacuum drying oven, dry under reduced pressure at 105±3°C and 93kpa, weigh the mass of each conical flask, denoted as m 瓶5+石蜡 , recorded in Table 1, (7) According to the measurement data of each step above, calculate the water, oil, residue, asphalt, saturated content, aromatic content, colloid content in each oily sludge sample according to the formula (1)-(8) and paraffin content, as described in Table 1.

[0050] Table 1

[0051]

[0052] The relative standard deviation was calculated for the content results of each component measured in Table 1, and the results are shown in Table 2. The standard deviation of each test result was far less than 1%, and the measurement accuracy was high.

[0053] Table 2

[0054]

[0055] Verification example 1