CN112432877A - Method for measuring content of glue in heat-insulating material - Google Patents
Method for measuring content of glue in heat-insulating material Download PDFInfo
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- CN112432877A CN112432877A CN202011445247.6A CN202011445247A CN112432877A CN 112432877 A CN112432877 A CN 112432877A CN 202011445247 A CN202011445247 A CN 202011445247A CN 112432877 A CN112432877 A CN 112432877A
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The invention discloses a method for measuring the content of glue in a heat-insulating material, which comprises the steps of accurately weighing a heat-insulating material sample to be measured, placing the heat-insulating material sample in a container with constant weight, adding a mixed solvent into the container to fully disperse the sample in the solvent, standing and precipitating, pouring out liquid in the container, and keeping insoluble substances in the container; drying the container filled with the insoluble substances to volatilize the solution in the container completely, and weighing the mass of the container and the insoluble substances; and finally, calculating the content of the heat-insulating material glue according to the reduced mass of the sample. The test method is simple and efficient, the test process and the test result are easy to judge and control, and the result with better accuracy and consistency can be obtained.
Description
Technical Field
The invention relates to the technical field of solid rocket engine testing, in particular to a method for measuring the glue content of a T-1 heat-insulating material.
Background
The heat insulating layer is an important part of a heat-proof structure in the solid rocket engine and plays a role in preventing the temperature in the engine combustion chamber shell from damaging the structural integrity of the engine combustion chamber shell and resisting high temperature, high fuel gas flow and particle erosion.
The carbon fiber reinforced heat-insulating material (T-1 heat-insulating material) is prepared by adopting carbon fiber woven fabric to impregnate phenolic resin and nitrile rubber glue solution, and has good heat insulation, ablation resistance, scouring resistance and other performances. The glue solution content of the phenolic resin and the nitrile rubber in the T-1 heat-insulating material is enough to ensure that the carbon fiber framework can be fully filled under the action of process pressure, and the enough interlayer bonding strength is ensured. When the content of the glue solution is insufficient, the glue solution formed by the phenolic resin and the nitrile rubber is insufficient to completely fill the carbon fiber framework, so that the bonding area between T-1 heat-insulating materials is influenced, the bonding performance of the heat-insulating materials cannot meet the standard requirement, and the heat-insulating materials cannot be effectively adhered to the inner wall of the combustion chamber, so that the contact part of the combustion chamber shell and gas is burnt out.
The T-1 heat-insulating material is influenced by production equipment, control instruments, technological processes and other factors in the actual production process, the gum dipping amount of the upper layer and the gum dipping amount of the lower layer are greatly different during multilayer gum dipping, so that the actual gum content and the set amount of the upper layer and the lower layer are greatly different, the distribution uniformity of the gum material in the heat-insulating material is fluctuated to a certain extent, and the factors directly influence the quality of the produced product. A TG (glass transition temperature) ignition weightlessness analysis method is a method for measuring the glue content in the T-1 heat-insulating material in the current industrial production, but the method has the disadvantages of complicated test process, high cost and small test sampling amount, so that the real content of the glue in a sample is too much different from the detected content, the test result is inaccurate and the discreteness is large.
Therefore, establishing a simple, reliable and accurate method for determining the glue content distribution in the thermal insulation material is of great significance to the production and research of T-1 thermal insulation materials.
Disclosure of Invention
The invention provides a method for measuring the content of heat-insulating material glue, which is simple and efficient, is easy to judge and control the test process and the test result, and can obtain the result with better accuracy and consistency.
The invention has the technical scheme that the method for measuring the content of the heat-insulating material glue comprises the following steps:
s1, accurately weighing a thermal insulation material sample m to be measured, placing the thermal insulation material sample m in a container with constant weight, and weighing the sample and the container to obtain the mass m1Adding a mixed solvent into a container to fully disperse the sample in the mixed solvent, standing for precipitation, pouring out liquid in the container, and keeping insoluble substances in the container;
s2, drying the container filled with the insoluble substances to evaporate the solution in the container to be dry, and weighing the mass m of the container and the insoluble substances2；
S3, calculating the content of the heat-insulating material glue according to the reduced mass of the sample, wherein the specific formula is as follows:
in the formula:
ω: insulation material glue content,%;
m: sample mass, g;
m1: dissolving the total mass g of the sample and the container before cleaning;
m2: total mass of insoluble matter and container, g after dissolution and cleaning.
Furthermore, the heat insulating material is prepared by impregnating carbon fiber woven fabrics with glue solution of phenolic resin and nitrile rubber.
Furthermore, the mixed solvent in S1 is prepared by mixing acetone and ethyl acetate according to the mass ratio of 1: 2-4.
Further, the mixed solvent in S1 is prepared by mixing acetone and ethyl acetate according to the mass ratio of 1: 3.
Further, when the solution is dissolved in S1, the container is heated in a water bath, and the heating temperature is controlled to be 30-40 ℃.
Further, when heating in water bath, stirring for 1-2 min, standing for 1-2 min, and pouring out the liquid.
Further, the insoluble matter obtained in S1 is again added with the solvent in the container for dissolution, standing and separation; the solvent is added for 1-6 times.
More preferably, the test is performed 4 times with the solvent.
Further, the drying temperature in S2 is 130-150 ℃.
Further, the drying time in S2 is 0.5-1 h.
The invention has the following beneficial effects:
1. the invention adopts the mixed solvent for dissolution, can quickly and effectively resolve the phenolic resin and the nitrile rubber glue solution from the carbon insulation fiber material, has high detection result accuracy, and provides technical support for the quality control of the heat insulation layer of the solid rocket engine.
2. In the solvent dissolving process, a heating environment of water bath with a certain temperature is provided, so that on one hand, the rapid and sufficient dissolution of the sample is facilitated, the testing time is shortened, and the accuracy of the testing result is improved. On the other hand, the water bath heating mode enables the change process to be easily observed, and violent reaction caused by direct heating and uncontrollable temperature are avoided.
3. In the process of testing the glue content, complete dissolution of glue and complete volatilization of a solvent are important factors influencing the accuracy of the test, when the dissolution times are insufficient, the glue in the T-1 heat-insulating material cannot be completely dissolved in a reagent, so that the test result is smaller, and if the solvent is not completely volatilized, the test result is larger. Through the control of solvent dissolution and solvent volatilization conditions for many times, the rapid and sufficient dissolution of the glue in the sample and the safe and complete volatilization of the solvent are ensured, and the accuracy of the test result is ensured.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
weighing 2g of T-1 heat-insulating material sample, accurately weighing the sample to 0.0001g, wherein the mass is 2.0968g, placing the sample and the beaker in a 150mL beaker with constant weight, weighing 86.2641g of the total mass of the sample and the beaker, adding 40mL of mixed solvent prepared from acetone and ethyl acetate according to the weight ratio of 1:3 into the beaker with the sample, heating the mixture in a 35 ℃ water bath, stirring for 1min to fully disperse the sample in the beaker, standing for 1min for slight precipitation, pouring out turbid liquid, leaving black floccule (carbon fiber braided fabric) in the beaker, repeatedly adding the mixed solvent for dissolving for 4 times, stirring and dissolving, then clearing and brightening the mixed solvent solution, finally pouring out the liquid, placing the beaker and insoluble substances in the beaker in a 130 ℃ oven for drying for 0.5h, completely drying the solution in the beaker, transferring the beaker into a dryer for cooling to room temperature, and weighing 85.3520g of the mixed solvent. The gum content was calculated as the mass reduction of the sample and is expressed by equation (1):
in the formula:
ω: t-1 insulation material glue content,%;
m: sample mass, g;
m1: dissolving the total mass g of the sample and the beaker before cleaning;
m2: total mass of insoluble matter and beaker after dissolution and washing, g.
Specifically, the glue content of the T-1 insulation was measured to be 43.50%.
Example 2:
weighing 2g of T-1 heat-insulating material sample, accurately weighing the sample to 0.0001g, wherein the mass is 2.2282g, placing the sample and the beaker in a 150mL beaker with constant weight, weighing 85.0760g of the total mass of the sample and the beaker, adding 40mL of mixed solvent prepared from acetone and ethyl acetate according to the weight ratio of 1:2 into the beaker with the sample, heating the mixture in a water bath at 40 ℃, stirring for 2min to fully disperse the sample in the beaker, standing for 2min for slight precipitation, pouring out turbid liquid, leaving black floccule (carbon fiber braided fabric) in the beaker, repeatedly adding the mixed solvent for dissolving for 5 times, stirring and dissolving, then clearing and brightening the mixed solvent, pouring out the liquid, placing the beaker and insoluble substances in the beaker in an oven at 150 ℃ for drying for 0.5h until the solution in the beaker is completely dried, moving the beaker to a dryer for cooling to room temperature, and weighing 84.1212g of the mixed solvent. The gum content was calculated as the reduced mass of the sample,
specifically, the glue content of the T-1 insulation was measured to be 42.85%.
Example 3:
weighing 2.0132g of T-1 heat-insulating material sample, placing the sample in a 150mL beaker with constant weight, weighing the total mass of the sample and the beaker, wherein the total mass is 84.7808g, adding 40mL of mixed solvent prepared from acetone and ethyl acetate according to the weight ratio of 1:2 into the beaker with the sample, heating the beaker in water bath at 40 ℃, stirring for 2min to fully disperse the sample in the beaker, standing for 1min for slight precipitation, pouring out turbid liquid, leaving black floccule (carbon fiber woven fabric) in the beaker, repeatedly adding the mixed solvent for dissolving for 4 times until the mixed solvent is transparent after stirring and dissolving, pouring out the liquid, placing the beaker and insoluble substances in the beaker into an oven at 130 ℃ for drying for 1h until the solution in the beaker is completely dried, transferring the beaker into a dryer for cooling to room temperature, and weighing 83.9143 g. The gum content was calculated as the reduced mass of the sample,
specifically, the glue content of the T-1 insulation was measured to be 43.04%.
Example 4:
acetone, ethyl acetate, mixed solvents prepared from acetone and ethyl acetate according to the weight ratio of 1:2, 1:3 and 1:4 and 6 different organic reagents of trichloromethane are respectively selected as solvents to test the content of the T-1 heat-insulating material glue in a certain batch. During the dissolving process, the sample is rapidly dispersed in the mixed solvent of acetone and ethyl acetate, the solvent becomes very turbid, and the mixed solvent in the beaker is gradually clear and bright after being dissolved by stirring for a plurality of times. When acetone, ethyl acetate and chloroform alone were used as the solvent, the sample dispersed slowly and the solvent became slightly cloudy. The specific test results are shown in table 1.
TABLE 1
Different solvents have great influence on the test result, analytically pure acetone and ethyl acetate are selected to be mixed according to the mass ratio of 1:3 to be used as the solvent, and the standard deviation of the content of the T-1 heat-insulating material glue is measured to be 0.02, so that the solution of the analytically pure acetone and the ethyl acetate according to the mass ratio of 1:3 is preferably used as the solvent of the T-1 heat-insulating material.
Example 5: in the solvent dissolving process, a certain heating environment is provided, so that the sample can be quickly and fully dissolved, the testing time is shortened, and the accuracy of the testing result is improved. Considering that the solvent is an organic reagent, the solvent is flammable and volatile, the water bath heating temperature can be controlled within a proper range, the water bath heating avoids the direct heating to cause over-intensity and uncontrollable temperature, and the change process is easy to observe. In the experiment, a solvent dissolution test is carried out in a water bath environment at the temperature of 30-40 ℃.
When the dissolution frequency is not enough, the glue in the T-1 heat-insulating material can not be completely dissolved in the reagent, so that the test result is smaller. Placing the sample beaker in a water bath at 30-40 ℃ for stirring for 1-2 min each time for fully dispersing the sample in the beaker, standing for 1-2 min, pouring out turbid liquid after slight precipitation, and leaving black floccule in the beaker. The dissolution step was repeated 1-6 times to measure the gum content in the T-1 insulation, the test results are shown in Table 2.
TABLE 2
As can be seen from the above table, when the number of times of dissolution is less than 4, the experimental result is significantly smaller, and the solvent is observed to be in a turbid state after the last dissolution. When the dissolving time is more than 4 times, the test result tends to be stable, and the solvent is clear and bright after the last dissolving in the dissolving process, which indicates that the glue in the sample is completely dissolved, so the dissolving time is preferably 4 times.
Example 6:
accuracy verification
After the test conditions are selected and optimized, a T-1 thermal insulation material standard sample with the glue content of 42% -49% is adopted, namely during manufacturing, the fiber content and the glue content are known, and the weight ratio of acetone: ethyl acetate mass ratio 1: and 3, repeatedly dissolving the mixture in a water bath for 4 times, standing and precipitating, pouring out turbid liquid, putting black floccules in a beaker, putting the beaker in an oven at the temperature of 130 ℃ for drying for 0.5h, and weighing the mass. The gum content was calculated as the reduced mass of the sample and the test results are shown in table 3.
TABLE 3 determination of the gum content of T-1 insulating material by solvent dissolution method
Because the glue content in the standard sample slowly volatilizes, the test results are all less than the theoretical value. The relative error between the test value and the theoretical value is less than 2 percent, namely the test accuracy of the method provided by the invention meets the requirement.
Example 7:
precision verification
A batch of T-1 insulation material was weighed as 2g, and the weight ratio of acetone: ethyl acetate mass ratio 1: and 3, repeatedly dissolving the mixture in a water bath for 4 times, standing and precipitating, pouring out turbid liquid, putting black floccules in a beaker, putting the beaker in an oven at the temperature of 130 ℃ for drying for 1 hour, and weighing the mass. The gum content was calculated as the mass reduction of the sample and tested in parallel 5 times with the test results shown in table 4.
TABLE 4 determination of the gum content of T-1 insulating material by solvent dissolution method
As can be seen from the above table, the relative standard deviation of the gum content is 0.51% and less than 2% after 5 parallel tests, and the experimental results prove that the testing precision of the solvent dissolution method meets the requirements.
Claims (10)
1. A method for measuring the content of heat-insulating material glue comprises the following steps:
s1, accurately weighing a thermal insulation material sample m to be measured, placing the thermal insulation material sample m in a container with constant weight, and weighing the sample and the container to obtain the mass m1Adding a mixed solvent into a container to fully disperse the sample in the mixed solvent, standing for precipitation, pouring out liquid in the container, and keeping insoluble substances in the container;
s2, drying the container filled with the insoluble substances to evaporate the solution in the container to be dry, and weighing the mass m of the container and the insoluble substances2；
S3, calculating the content of the heat-insulating material glue according to the reduced mass of the sample, wherein the specific formula is as follows:
in the formula:
ω: insulation material glue content,%;
m: sample mass, g;
m1: dissolving the total mass g of the sample and the container before cleaning;
m2: total mass of insoluble matter and container, g after dissolution and cleaning.
2. The method of claim 1, wherein: the heat insulating material is prepared by impregnating carbon fiber woven fabric with phenolic resin and nitrile rubber.
3. The method of claim 1, wherein: the mixed solvent in the S1 is prepared by mixing acetone and ethyl acetate according to the mass ratio of 1: 2-4.
4. The method of claim 1, wherein: the mixed solvent in the S1 is formed by mixing acetone and ethyl acetate according to the mass ratio of 1: 3.
5. The method of claim 1, wherein: and when the materials are dissolved in S1, heating the container in water bath at the temperature of 30-40 ℃.
6. The method of claim 5, wherein: when heating in water bath, stirring for 1-2 min, standing for 1-2 min, and pouring out the liquid.
7. The method of claim 1, wherein: adding the solvent into the insoluble substance obtained in the S1 again for dissolving, standing and separating; the solvent is added for 1-6 times.
8. The method of claim 7, wherein: the test was carried out 4 times using a solvent.
9. The method of claim 1, wherein: and the drying temperature in S2 is 130-150 ℃.
10. The method of claim 1, wherein: and the drying time in S2 is 0.5-1 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110940609A (en) * | 2019-10-31 | 2020-03-31 | 江南工业集团有限公司 | Method for measuring gum content of gum-dipped cloth |
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2020
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| CN103940698A (en) * | 2014-05-06 | 2014-07-23 | 湖北三江航天江河化工科技有限公司 | HMX content assaying method |
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| CN110940609A (en) * | 2019-10-31 | 2020-03-31 | 江南工业集团有限公司 | Method for measuring gum content of gum-dipped cloth |
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