CN103048213A - Method for testing performance of mold pressing premixed material - Google Patents
Method for testing performance of mold pressing premixed material Download PDFInfo
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- CN103048213A CN103048213A CN2012105277312A CN201210527731A CN103048213A CN 103048213 A CN103048213 A CN 103048213A CN 2012105277312 A CN2012105277312 A CN 2012105277312A CN 201210527731 A CN201210527731 A CN 201210527731A CN 103048213 A CN103048213 A CN 103048213A
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Abstract
The invention discloses a method for testing performance of a mold pressing premixed material. The method comprises the following steps of: testing the mold pressing premixed material through the procedures of heating and heat retaining at different temperature sections by a thermal weight loss instrument particularly; reading the decreased amount of quality of the material at each stage respectively from a tested thermal weight loss analysis curve; comparing the decreased amount of the quality of the material at each stage with the quality of a sample, thereby obtaining volatile matters, resin content and fiber content; and finally calculating the cure degree of the material according to data of the volatile matters and the resin content obtained by a chemical method of soaking dissoluble resin on the mold pressing premixed material by acetone. The method provided by the invention makes up the defects of the conventional test method for testing the performance of the mold pressing premixed material, improves test items, guarantees the reliability of a mold pressing product as a main heat insulation material of a spaceflight solid rocket engine, provides accurate performance parameter basis for the production of the mold pressing product, improves production efficiency, lowers production costs, and guarantees the smooth operation of a lot production task.
Description
Technical field
The present invention relates to a kind of material performance test method, be specifically related to a kind of mold pressing premix performance test methods.
Background technology
Mold pressing premix is to be prepared from after being mixed by a certain percentage by chopped high silica fiber and phenolics, is the adiabatic main raw material(s) with pressing of rocket motor structure spare.Premix becomes pressing through the High Temperature High Pressure molded curing, and the mode of physics calcination in traditional acetone chemical immersion and the luxuriant good fortune stove is adopted in its performance test always, and the cycle that the limited and this method of testing of test event needs is long, and testing cost is high, and measuring accuracy is low.
Mold pressing premix performance test is a vital task that guarantees the pressing quality, therefore need to seek and improve the feasible effective new method of performance test for mold pressing premix.
Summary of the invention
The invention provides a kind of mold pressing premix performance test methods, adopt thermogravimetic analysis (TGA) and chemical combined test, can once record fugitive constituent, resin content, fiber content and four performance parameters of degree of cure, for the pressing production run provides accurately performance parameter foundation, can guarantee better the requirement of thermal insulation material product quality.
The technical solution used in the present invention is as follows:
1, sample preparation and weighing
Evenly take by weighing a small amount of mold pressing premix powdered sample, put into alumina crucible.
2, test fugitive constituent
Adopt hot weightless instrument, the alumina crucible that fills mold pressing premix powdered sample is placed on the central authorities of thermal weight loss sensor, the furnace body temperature of hot weightless instrument is elevated to 105 ℃ ± 2 ℃ from room temperature, then at 105 ℃ ± 2 ℃ insulation 5min, in this test process, can observe a step on the thermogravimetric curve, i.e. the minimizing of quality, can read the quality of minimizing from the curve, the quality of this minimizing and the ratio of sample quality are exactly fugitive constituent.
3, test resin content
To continue to be warmed up to 600 ℃ ± 2 ℃ at 105 ℃ ± 2 ℃ mold pressing premix samples that are incubated 5min, then at 600 ℃ ± 2 ℃ insulation 5min, in this process, can observe second step on the thermogravimetric curve, reduce the second time that is quality, can read the quality that reduces for the second time from curve, the quality of this minimizing and the ratio of sample quality are exactly resin content.
4, fiber content test
Curve can be tending towards level when the mold pressing premix sample behind 600 ℃ ± 2 ℃ insulation 5min continued insulation 5min, be that reducing no longer appears in quality, read the quality of residue this moment from test curve, the ratio of this residue quality and sample quality is exactly fiber content.
5, degree of cure test
Evenly take by weighing broken section of premix, its immersion is placed with in the glass beaker of acetone and soaks 15min, dries by the fire 30min after filtering under 105 ℃ ± 2 ℃ temperature, weigh after being cooled to room temperature, the fugitive constituent of then measuring according to thermal weight loss and the data of resin content are calculated degree of cure.
Preferably, in sample preparation and the step of weighing, described premix powdered sample takes by weighing quality control between 5-25mg.
Preferably, broken section of 1g～1.3g premix is placed with 100ml acetone with its immersion, and capacity is to soak in the glass beaker of 250ml.
Preferably, in air dry oven, dry after the quantitative filter paper of employing φ 12.5 filters.
Preferably, be connected with purge gas in the body of heater of hot weightless instrument.
Preferably, purge gas is nitrogen, and ventilation flow rate is controlled in the 40ml/min.
Preferably, in test volatile quantity content step, with the speed intensification of 10 ℃/min.
Preferably, in test resin content step, with the speed continuation intensification of 15 ℃/min.
Beneficial effect of the present invention:
The deficiency of conventional test methodologies when the present invention has remedied mold pressing premix performance test, perfect its test event has been guaranteed the reliability of pressing as the main thermal insulation material of solid space rocket engine simultaneously.The present invention for pressing production provides accurately performance parameter foundation, has further improved production efficiency, has reduced production cost, has guaranteed carrying out smoothly of batch production task by the performance of full test mold pressing premix.
Description of drawings
Fig. 1 has shown the thermogravimetric curve schematic diagram that mold pressing premix is carried out performance test.
Embodiment
The present invention will be further described below in conjunction with drawings and Examples:
See also Fig. 1.
The present invention adopts thermogravimetic analysis (TGA) and chemical combined method of testing (being called for short " heat-change method ").Heat-change method is a kind of physics and the efficient method of testing of planning as a whole combination of chemistry, and it comprises thermogravimetic analysis (TGA) stage and test chemical stage, and this method of testing has remedied the deficiency of conventional test methodologies, perfect mold pressing premix performance test project.The concrete hot weightless instrument that adopts, test by the program segment that under the different temperatures section, heats up and be incubated, and from the test the thermogravimetic analysis (TGA) curve on read respectively each stage quality reduction, then do ratio with sample quality respectively with the reduction of each stage quality, obtain fugitive constituent, resin content and fiber content, the chemical method that adopts at last acetone that soluble resin content in the mold pressing premix is soaked calculates degree of cure according to the fugitive constituent of thermal weight loss test and the data of resin content.
Operating process of the present invention is as follows:
The thermogravimetic analysis (TGA) stage: with tweezers and scissors mold pressing premix is torn apart first, and long filament shredded, then mold pressing premix powdered sample evenly takes a morsel, put into 40ul standard alumina crucible, adopt hot weightless instrument, the alumina crucible that is placed with mold pressing premix powdered sample is placed on the central authorities of thermal weight loss (TGA) sensor, the purge gas component of setting the hot weightless instrument body of heater is nitrogen, and ventilation flow rate is controlled in the 40ml/min.Speed with 10 ℃/min is warmed up to 105 ℃ ± 2 ℃ from room temperature, temperature-rise period needs 8min, and then at 105 ℃ ± 2 ℃ insulation 5min, 13min reads the minimizing m1 that corresponding ordinate is improved quality from first step flex point of thermogravimetric curve, then just compare with m0 with m1 and can draw fugitive constituent, namely
Speed with 15 ℃/min continues to be warmed up to 600 ℃ ± 2 ℃, temperature-rise period needs 33min, and then at 600 ℃ ± 2 ℃ insulation 5min, 51min reads the minimizing m2 that corresponding ordinate is improved quality from second step flex point of thermogravimetric curve, then just compare with m0 with m2 and can draw resin content, namely
Curve can be tending towards level when the sample behind 600 ℃ ± 2 ℃ insulation 5min continued insulation 5min, and namely reducing no longer appears in quality, reads the quality m3 of residue this moment from test curve, and the ratio of this residue quality m3 and sample quality m0 is exactly fiber content, namely
The test chemical stage: evenly take by weighing 1g～broken section M0 of 1.3g premix, its immersion is placed with 100ml acetone, capacity is to soak 15min in the glass beaker of 250ml, after filtering, the quantitative filter paper of employing φ 12.5 in 105 ℃ ± 2 ℃ air dry ovens, dries by the fire 30min, be cooled to the M1 that weighs after the room temperature, then the fugitive constituent V that measures according to thermal weight loss and the data of resin content R are calculated degree of cure C
Test period of the present invention is short, convenient test is quick, reaches 1 hour/batch.The present invention has also improved measuring accuracy, from ten thousand/bring up to 100,000/.Adopt the present invention, every batch of starting material have reduced by 5 grams, have reduced testing cost.Simultaneously, the present invention provides reliable and stable test result for process of producing product, better guarantees product quality, has guaranteed carrying out smoothly of batch production task.
Above-mentioned is to specify of the present invention, and the present invention is not limited to this.For example, indication mold pressing premix is not limited to high silica fiber and phenolics batch mixing among the present invention, also can comprise the fibre resin batch mixing of other type.In addition, purge gas also is not limited to nitrogen.Protection scope of the present invention is limited by its claim.
Claims (8)
1. mold pressing premix performance test methods, it is characterized in that: the method comprises the steps:
1) sample preparation and weighing
Evenly take by weighing a small amount of mold pressing premix powdered sample and put into alumina crucible;
2) test fugitive constituent
Adopt hot weightless instrument, the described alumina crucible that fills mold pressing premix powdered sample is placed on the central authorities of thermal weight loss sensor, the hot weightless instrument furnace body temperature is elevated to 105 ℃ ± 2 ℃ from room temperature, then at 105 ℃ ± 2 ℃ insulation 5min, then read the quality of minimizing from thermogravimetric curve, the ratio of the quality m1 of this minimizing and sample quality m0 is exactly fugitive constituent;
3) test resin content
To continue to be warmed up to 600 ℃ ± 2 ℃ at 105 ℃ ± 2 ℃ mold pressing premix powdered samples that are incubated 5min, then at 600 ℃ ± 2 ℃ insulation 5min, read the quality that reduces for the second time from thermogravimetric curve subsequently, the ratio of the quality m2 of this minimizing and sample quality m0 is exactly resin content;
4) test fiber content
Behind 600 ℃ ± 2 ℃ insulation 5min, mold pressing premix powdered sample is continued insulation 5min, read the quality m3 of residue this moment from thermogravimetric curve, the ratio of quality m3 and sample quality m0 is exactly fiber content;
5) test degree of cure
Evenly take by weighing broken section M0 of mold pressing premix, its immersion is placed with in the glass beaker of acetone and soaks 15min, under 105 ℃ ± 2 ℃ temperature, dries by the fire 30min after filtering, be cooled to the M1 that weighs after the room temperature, then calculate degree of cure according to the data of described fugitive constituent and resin content.
2. a kind of mold pressing premix performance test methods according to claim 1, it is characterized in that: in sample preparation and the step of weighing, described premix powdered sample takes by weighing quality m0 and is controlled between the 5-25mg.
3. a kind of mold pressing premix performance test methods according to claim 1 is characterized in that: in test degree of cure step, take by weighing broken section of 1g～1.3g premix, its immersion is placed with in the glass beaker that 100ml acetone, capacity are 250ml soaks.
4. according to claim 1 or 3 described a kind of mold pressing premix performance test methods, it is characterized in that: in test degree of cure step, in air dry oven, dry after adopting the Filter paper filtering of φ 12.5.
5. a kind of mold pressing premix performance test methods according to claim 1 is characterized in that: be connected with purge gas in the hot weightless instrument body of heater.
6. a kind of mold pressing premix performance test methods according to claim 5, it is characterized in that: described purge gas is nitrogen, and ventilation flow rate is controlled in the 40ml/min.
7. a kind of mold pressing premix performance test methods according to claim 1 is characterized in that: in test volatile quantity step, with the speed intensification of 10 ℃/min.
8. a kind of mold pressing premix performance test methods according to claim 1 is characterized in that: in test resin content step, with the speed continuation intensification of 15 ℃/min.
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| CN103743645A (en) * | 2013-07-19 | 2014-04-23 | 中国石油化工股份有限公司 | Method for controlling quality of polymer for reservoir oil displacement using thermal gravimetric analysis technology |
| CN104165860A (en) * | 2014-08-17 | 2014-11-26 | 江苏恒州特种玻璃纤维材料有限公司 | Online detection process for components of high-silica glass fiber mesh |
| CN107121353A (en) * | 2017-05-16 | 2017-09-01 | 国网河北省电力公司电力科学研究院 | A kind of equivalent run time decision method of silastic material based on thermogravimetic analysis (TGA) |
| 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 |
| CN111175342A (en) * | 2020-01-19 | 2020-05-19 | 太尔化工（南京）有限公司 | Method for detecting curing degree of resin in casting sand template by differential scanning calorimeter |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103743645A (en) * | 2013-07-19 | 2014-04-23 | 中国石油化工股份有限公司 | Method for controlling quality of polymer for reservoir oil displacement using thermal gravimetric analysis technology |
| CN104165860A (en) * | 2014-08-17 | 2014-11-26 | 江苏恒州特种玻璃纤维材料有限公司 | Online detection process for components of high-silica glass fiber mesh |
| CN107121353A (en) * | 2017-05-16 | 2017-09-01 | 国网河北省电力公司电力科学研究院 | A kind of equivalent run time decision method of silastic material based on thermogravimetic analysis (TGA) |
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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 |
| CN111175342A (en) * | 2020-01-19 | 2020-05-19 | 太尔化工（南京）有限公司 | Method for detecting curing degree of resin in casting sand template by differential scanning calorimeter |
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Application publication date: 20130417 |