Method for detecting curing degree of resin in casting sand template by differential scanning calorimeter
Technical Field
The invention relates to the technical field of resin performance detection, in particular to a method for detecting the curing degree of resin in a casting sand template by using a differential scanning calorimeter.
Background
The resin generally refers to an organic polymer which has a softening or melting range after being heated, tends to flow by an external force when softened, and is solid, semi-solid, or liquid at room temperature. In the casting process, resin is required to be filled in a cast sand mold plate for plasticity, and a mold is formed after the resin is cured. In order to understand the degree of curing of resin in a cast sand pattern plate (rock wool plate), it is necessary to detect the degree of curing of resin.
At present, the curing degree of resin in a casting sand template is tested by soaking the casting sand template in water for a certain time, taking out the casting sand template, adding reagents such as ammonium chloride, ammonia water, 4-aminoantipyrine, potassium ferricyanate and the like for color development, and searching for the corresponding curing degree through a colorimetric card. When the detection method is used, in the sample preparation process, the sample is polluted, so that the detection result is inaccurate, and the colorimetric judgment can be carried out by naked eye observation, so that a larger error exists.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the method for detecting the curing degree of the resin in the casting sand template by using the differential scanning calorimeter, has the advantages of avoiding the sample from being polluted, reducing the detection error and the like, and solves the problems that the sample is easily polluted and the error of visual colorimetry is larger in the existing detection method.
(II) technical scheme
The invention provides the following technical scheme: the method for detecting the curing degree of resin in the casting sand template by using a differential scanning calorimeter comprises the following steps:
weighing three groups of 10g rock wool board samples for later use, closing a door plate of a muffle furnace, opening a switch of the muffle furnace, heating the muffle furnace to raise the temperature to 550 ℃, opening the door plate of the muffle furnace, quickly placing the three groups of rock wool board samples into the muffle furnace for burning, and keeping the temperature of the muffle furnace constant at 550 ℃ for two hours;
step two, after constant-temperature firing is carried out on the three groups of rock wool board samples for two hours by using a muffle furnace, a switch of the muffle furnace is closed, a door plate of the muffle furnace is opened, the three groups of rock wool board samples are taken out and placed in a dryer for cooling, when the temperature of the three groups of rock wool board samples is cooled to room temperature, the three groups of rock wool board samples are placed on a weighing device for weighing, and the average value is calculated after weighing;
weighing three groups of 3g of resin samples for later use, closing a box door of a precision oven, opening a switch of the precision oven, heating the precision oven to raise the temperature to 135 ℃, opening the box door of the precision oven, putting the three groups of resin samples into the precision oven, keeping the precision oven at the constant temperature of 135 ℃ for two hours, drying the three groups of resin samples for two hours by using the precision oven, closing the switch of the precision oven, opening the box door of the precision oven, putting the three groups of resin samples into a dryer for cooling, weighing the three groups of resin samples by using a weighing device when the temperature of the three groups of resin samples is cooled to room temperature, and calculating an average value after weighing;
step four, weighing 10-15 mg of resin sample by using a weighing device, putting the 10-15 mg of resin sample into a DSC high-pressure sample tray, covering a cover, putting the DSC high-pressure sample tray into a DSC detection chamber, setting the initial temperature of 50 ℃, heating to 300 ℃ at 1min/10 ℃ on DSC, keeping the temperature at 300 ℃ for 1min, and setting the weight input value to be 'sample mass x solid content'; after the temperature rise is finished, calculating the heat a released by heat;
step five, weighing 15-20 mg of rock wool sample by using a weighing device, putting the 15-20 mg of rock wool sample into a DSC high-pressure sample tray, covering a cover, putting the DSC high-pressure sample tray into a DSC detection chamber, setting the initial temperature on DSC to be 50 ℃, heating to 300 ℃ at 1min/10 ℃, keeping the temperature at 300 ℃ for 1min, and setting the weight input value to be 'sample mass organic matter content'; when the temperature rise is finished, calculating the heat b released by heat release;
step six, calculating the curing degree according to a curing degree formula, wherein the curing degree formula is as follows: degree of cure 1- (b organic mass/a solid mass).
Preferably, three groups of rock wool board samples and three groups of resin samples are weighed according to the requirements in GB/T5480-2017.
Preferably, the rock wool board sample and the resin sample are both made of 218 resin.
Preferably, the heat a in the fourth step and the heat b in the fifth step are detected by scanning with a differential scanning calorimeter.
Preferably, the rock wool sample and the resin sample in the second step and the third step are subjected to real-time temperature detection by using an infrared thermometer when being cooled.
Preferably, the step one, the step two, the step three, the step four, the step five and the step six are repeated three times, and the average value of the calculation results of the step six is taken.
Preferably, the weigher is a high-precision molecular weighing scale.
(III) advantageous effects
Compared with the prior art, the invention provides a method for detecting the curing degree of resin in a casting sand template by using a differential scanning calorimeter, which has the following beneficial effects:
according to the method for detecting the degree of solidification of resin in the cast sand template by using the differential scanning calorimeter, through the steps of setting step one, step two, step three, step four, step five and step six, the national standard is adopted for sampling operation, so that the sample is not polluted, the heat release trend of the resin and the heat release trend of the rock wool board can be detected by DSC, the heat release quantity J/g is obtained, the solid content of the resin and the organic matter content of the rock wool board are measured according to the national standard, and therefore the degree of solidification of the resin in the cast sand template made of rock wool can be calculated according to a standard formula for calculating the degree of solidification.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The method for detecting the curing degree of resin in the casting sand template by using a differential scanning calorimeter comprises the following steps:
weighing three groups of 10g rock wool board samples for later use, closing a door plate of a muffle furnace, opening a switch of the muffle furnace, heating the muffle furnace to raise the temperature to 550 ℃, opening the door plate of the muffle furnace, quickly placing the three groups of rock wool board samples into the muffle furnace for burning, and keeping the temperature of the muffle furnace constant at 550 ℃ for two hours;
step two, after constant-temperature firing is carried out on the three groups of rock wool board samples for two hours by using a muffle furnace, a switch of the muffle furnace is closed, a door plate of the muffle furnace is opened, the three groups of rock wool board samples are taken out and placed in a dryer for cooling, when the temperature of the three groups of rock wool board samples is cooled to room temperature, the three groups of rock wool board samples are placed on a weighing device for weighing, and the average value is calculated after weighing;
weighing three groups of 3g of resin samples for later use, closing a box door of a precision oven, opening a switch of the precision oven, heating the precision oven to raise the temperature to 135 ℃, opening the box door of the precision oven, putting the three groups of resin samples into the precision oven, keeping the precision oven at the constant temperature of 135 ℃ for two hours, drying the three groups of resin samples for two hours by using the precision oven, closing the switch of the precision oven, opening the box door of the precision oven, putting the three groups of resin samples into a dryer for cooling, weighing the three groups of resin samples by using a weighing device when the temperature of the three groups of resin samples is cooled to room temperature, and calculating an average value after weighing;
step four, weighing 10-15 mg of resin sample by using a weighing device, putting the 10-15 mg of resin sample into a DSC high-pressure sample tray, covering a cover, putting the DSC high-pressure sample tray into a DSC detection chamber, setting the initial temperature of 50 ℃, heating to 300 ℃ at 1min/10 ℃ on DSC, keeping the temperature at 300 ℃ for 1min, and setting the weight input value to be 'sample mass x solid content'; after the temperature rise is finished, calculating the heat a released by heat;
step five, weighing 15-20 mg of rock wool sample by using a weighing device, putting the 15-20 mg of rock wool sample into a DSC high-pressure sample tray, covering a cover, putting the DSC high-pressure sample tray into a DSC detection chamber, setting the initial temperature on DSC to be 50 ℃, heating to 300 ℃ at 1min/10 ℃, keeping the temperature at 300 ℃ for 1min, and setting the weight input value to be 'sample mass organic matter content'; when the temperature rise is finished, calculating the heat b released by heat release;
step six, calculating the curing degree according to a curing degree formula, wherein the curing degree formula is as follows: the curing degree is 1- (b organic matter amount/a solid mass), through the steps of I, II, III, IV, V and VI, a heat release trend of the resin and the rock wool board can be detected through DSC, a heat release amount J/g is obtained, and then the solid content of the resin and the organic matter content of the rock wool board are measured according to national standards, so that the curing degree of the resin in the cast sand-type board made of the rock wool material can be calculated according to a standard formula for calculating the curing degree.
The three groups of rock wool board samples and the three groups of resin samples are weighed according to the requirements in GB/T5480-2017, so that the sampling accuracy is improved, and the samples are prevented from being polluted.
The rock wool board sample and the resin sample are both made of 218 resin.
And (4) scanning and detecting the heat a in the fourth step and the heat b in the fifth step by a differential scanning calorimeter, wherein the differential scanning calorimeter can accurately detect the heat.
And the rock wool sample and the resin sample in the second step and the third step are subjected to real-time temperature detection by using an infrared thermometer during cooling, and the infrared thermometer can be used for detecting the temperatures of the rock wool sample and the resin sample in real time and knowing the temperature conditions of the rock wool sample and the resin sample in real time.
The first step, the second step, the third step, the fourth step, the fifth step and the sixth step are repeated for three times, and the average value of the results calculated in the sixth step is taken, so that the error of the test result caused by a large error of data is avoided, and the accuracy of the test result is improved.
The weighing device is a high-precision molecular weighing scale, so that the measuring precision of the weighing device is ensured, the error of measured data is reduced, and the accuracy of the measured data is improved.
In summary, according to the method for detecting the degree of solidification of resin in the casting sand-shaped plate by using the differential scanning calorimeter, through the steps of the first step, the second step, the third step, the fourth step, the fifth step and the sixth step, the national standard is adopted for sampling operation, so that the sample is not polluted, the heat release trend of the resin and the rock wool plate can be detected through DSC, the heat release quantity J/g is obtained, the solid content of the resin and the organic matter content of the rock wool plate are measured according to the national standard, and therefore the degree of solidification of the resin in the casting sand-shaped plate made of rock wool can be calculated according to the standard formula for calculating the degree of solidification.
It should be noted that the term "comprises/comprising" when used in this specification is taken to specify the presence of stated elements, integers, steps, operations, elements, components, and/or groups thereof, but does not exclude the presence or addition of other elements, integers, steps, operations, elements, components, and/or groups thereof. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.