Disclosure of Invention
In order to solve the defects in the prior art, the device and the method for testing the hairiness defect of the high-performance fiber provided by the invention realize quantitative detection of the hairiness defect of the high-performance fiber, provide exact reference data for production and evaluation of the high-performance fiber, reduce the research and development, production and application costs of the high-performance fiber, and have the advantages of simple, quick and convenient operation and higher testing precision.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, there is provided an apparatus for testing high performance fiber hairiness defects, comprising: a hot air field surrounded by the shell; a heat source mounted on the housing for heating the hot air field; an air inlet section connected with the shell and positioned at one end of the hot air field, wherein the air inlet section is communicated with the hot air field; the air inlet section is provided with an air inlet which is connected with an outlet of the circulating fan through a circulating air pipe; the high-performance fiber sample inlet is connected with the air inlet section and used for fixing high-performance fibers and enabling the high-performance fibers to hang in the hot air field; the sampling section is connected with the shell and positioned at the other end of the hot air field, the sampling section is communicated with the hot air field, and a plurality of sampling ports are arranged on the sampling section; and an exhaust section communicated with the sampling section and the inlet of the circulating fan, wherein the exhaust section is provided with an external air source interface.
Further, the air inlet comprises a first air inlet and a second air inlet with a poor opening; the air inlet section is also provided with an air speed adjusting plate for adjusting the air speed of the first air inlet and/or the second air inlet.
Further, the high-performance fiber sample inlet is connected with the air inlet section by a buckle.
Further, the sampling port comprises a first sampling port and a second sampling port, and the first sampling port and the second sampling port are respectively provided with a collecting filter screen with different meshes.
Further, the mesh number of the collecting filter screen is 2-50 meshes.
Further, the hot air field hot air circulating system further comprises an electric control console, wherein the electric control console is used for controlling the operation of the circulating fan and the temperature in the hot air field.
In a second aspect, there is provided a method for testing high performance fiber hairiness defect, using the apparatus for testing high performance fiber hairiness defect according to the first aspect, the method comprising: preparation before testing is carried out, and the initial mass m of the high-performance fiber to be tested is recorded 0-1 The method comprises the steps of carrying out a first treatment on the surface of the The method comprises the steps of feeding high-performance fibers to be tested into a hot air field through a high-performance fiber sample inlet, and starting a device for testing according to a set testing process; after the test is finished, collecting the fallen high-performance fibers from each sampling port, weighing the fibers, and recording the weight of the fibers as the weight of the fibers of the sampling ports; based on the initial mass m of the high-performance fiber 0-1 And the weight of the fiber at the sampling port, and calculating the defect ratio; and photographing the high-performance fibers collected from each sampling port, and analyzing and calculating image data through computer software to obtain relevant evaluation parameters of hairiness.
Further, pre-test preparation, comprising: fixing the device for testing the hairiness defect of the high-performance fiber on a horizontal tabletop in a room, and maintaining the indoor temperature and humidity constant; purging and cleaning the circulating air pipe and the hot air field through an external air source interface; the sampling port comprises a sampling port I and a sampling port II, wherein the sampling port I and the sampling port II are respectively provided with collecting filter screens with different meshes, and before the collecting filter screens are arranged, the weight of the collecting filter screens is recorded, wherein the weight of the collecting filter screen at the sampling port I is recorded as m 1-1 The weight of the collecting filter screen at the two positions of the sampling port is recorded as m 2-1 The method comprises the steps of carrying out a first treatment on the surface of the And (3) debugging the circulating fan, setting a test wind speed, and adjusting the output temperature of the heat source.
Further, according to the initial mass m of the high-performance fiber 0-1 And the weight of the fiber at the sampling port, and calculating the defect ratio, wherein the defect ratio is specifically as follows: the weight of the fiber of the sampling port comprises the weight of a collecting filter screen at one position of the sampling port after the test is finished, and is recorded as m 1-2 The weight of the collecting filter screen at the two positions of the sampling port is recorded as m 2-2 The method comprises the steps of carrying out a first treatment on the surface of the After the test is finished, the residual mass of the high-performance fiber at the high-performance fiber sample inlet is recorded as m 0-2 ;
The absolute mass of hairiness defect is the mass change before and after a sampling port collects a filter screen, and the defect ratio is as follows:
the absolute mass of the second hairiness defect is the front-back mass change of the collecting filter screen at the second sampling port (8), and the defect ratio is as follows:
the total reaction mass change, namely the material loss ratio is:
further, the image data is analyzed and calculated by computer software to obtain relevant evaluation parameters of hairiness, including but not limited to hairiness expansion size, diameter, number, hairiness frequency ratio, average value and CV value.
Compared with the prior art, the invention has the beneficial effects that: the invention tests the type and the quantity characteristic value of the hairiness defect of the high-performance fiber at a controllable temperature, collects the hairiness defect at different process stages through a variable temperature field, collects the hairiness defect with different sizes through different specification collecting filter screens, evaluates the absolute weight of the hairiness defect with different types through measuring the weight increment before and after the collecting filter screens, and automatically analyzes the hairiness defect type of the high-performance fiber through high-power digital camera auxiliary graphic software, and comprises the following steps: the hairiness shape and quantity ratio are high, the testing precision is high, and the operation is simple, convenient and quick. The invention can provide quantitative evaluation parameters for the production and application of the high-performance fiber, and reduce the cost of the development and application stage of the high-performance fiber.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
As shown in fig. 1 to 4, an apparatus for testing hairiness defects of high performance fibers, comprising:
a hot air field 5 surrounded by the shell;
a heat source 6 mounted on the housing for heating the hot air field 5;
an air inlet section connected with the shell and positioned at one end of the hot air field 5, wherein the air inlet section is communicated with the hot air field 5; the air inlet section is provided with an air inlet which is connected with the outlet of the circulating fan 2 through a circulating air pipe 3;
the high-performance fiber sample inlet 1 is connected with the air inlet section and is used for fixing high-performance fibers and enabling the high-performance fibers to hang in the hot air field 5;
the sampling section is connected with the shell and positioned at the other end of the hot air field 5, the sampling section is communicated with the hot air field 5, and the sampling section is provided with a plurality of sampling ports;
and an exhaust section communicated with the sampling section and the inlet of the circulating fan 2 is provided with an external air source interface 9.
The air inlets comprise a first air inlet 31 and a second air inlet 32 with opening differences, and the opening differences of the first air inlet 31 and the second air inlet 32 are used for realizing the difference of the wind speeds of the first air inlet 31 and the second air inlet 32; the air inlet section is also provided with an air speed adjusting plate 4 for adjusting the air speed of the first air inlet 31 and/or the second air inlet 32.
The sampling port comprises a first sampling port 7 and a second sampling port 8, and the first sampling port 7 and the second sampling port 8 are respectively provided with a collecting filter screen 11 with different meshes.
The high-performance fiber sample inlet 1 adopts a quick buckle to quickly place a bundle of high-performance fibers with fixed length in the hot air field 5 for heat treatment; the circulating fan 2 can be set by the electric control console 10 to realize the opening and closing of the hot air field, and the control of different circulating air volumes is realized through the rotation speed adjustment of the circulating fan 2; the circulating air pipe 3 realizes the left and right wind speed difference of a high-performance fiber sample in a hot air field through the opening difference of the structures of the air inlets (the first air inlet 31 and the second air inlet 32) at the left side and the right side, and the highest wind speed can reach 10m/s; the local wind speed is adjustable through the adjustment of the wind speed adjusting plate 4, and finally, the high-performance fiber sample shakes under the air flow wind speed difference to strip hairiness defects; the temperature control of the hot air field is realized through the heat sources 6 around the hot air field 5 under the TIC monitoring setting of the electric control desk 10, and the highest temperature can reach 1000 ℃ with the precision of 0.5 ℃. The slurry applied on the surface of the fiber has a protective effect or the fiber has a chemical reaction at a certain processing temperature, so that the hairiness condition of a sample of the high-performance fiber can not be completely fed back only by normal-temperature air flow, and the state under various conditions can be comprehensively simulated through different process temperature adjustment.
The first sampling port 7 and the second sampling port 8 can be used for quickly installing and collecting metal collecting filter screens 11 with different meshes, wherein the meshes are 2-50 meshes, and the metal collecting filter screens are used for collecting hairiness defects with different sizes; the external air source interface 9 can be externally connected with other air sources, such as nitrogen, and the like, can perform targeted heat treatment according to the performance of the high-performance fiber sample, and can thoroughly clean the air pipe.
The method for testing the high-performance fiber hairiness defect by adopting the device for testing the high-performance fiber hairiness defect comprises the following steps:
preparation before testing is carried out, and the initial mass m of the high-performance fiber to be tested is recorded 0-1 ;
The high-performance fiber to be tested is sent into a hot air field 5 through a high-performance fiber sample inlet 1, and a device is started to test according to a set test process;
after the test is finished, collecting the fallen high-performance fibers from each sampling port, weighing the fibers, and recording the weight of the fibers as the weight of the fibers of the sampling ports;
based on the initial mass m of the high-performance fiber 0-1 And the weight of the fiber at the sampling port, and calculating the defect ratio;
and photographing the high-performance fibers collected from each sampling port, and analyzing and calculating image data through computer software to obtain relevant evaluation parameters of hairiness.
1. Preparation before testing
1. Before testing, fixing the device for testing the hairiness defect of the high-performance fiber on a horizontal table top in a room, and keeping the temperature and humidity of a testing room constant, wherein the room temperature is 20+/-2 ℃, and the relative humidity is 45+/-3%.
2. Opening an electrical control console 10, debugging the circulating fan 2, and thoroughly cleaning the circulating air pipe 3 and the hot air field 5 through an external air source interface 9;
3. the invention is characterized in that a first sampling port 7 and a second sampling port 8 are respectively provided with metal collecting filter screens 11 with different meshes, wherein the first sampling port 7 is provided with the collecting filter screens 11 with about 2-5 meshes, and the second sampling port 8 is provided with the collecting filter screens 11 with about 50 meshes, so that the collecting of different hairiness defects is realized. Before placing the collection screen 11, the weight of the collection screen 11 was weighed and recorded, and the weight of the collection screen at the first 7 sampling ports was recorded as m 1-1 The weight of the collecting filter screen at the second sampling port 8 is recorded as m 2-1 ;
4. Starting a debugging circulating fan 2 through an electrical control console 10, and setting a test wind speed;
5. the output temperature of the heat source 6 is regulated by the electrical console 10, and the temperature can be selected according to the material chemistry of the high performance fiber being tested.
2. Defect test
6. After the temperature is controlled to be stable through the electric control console 10, the circulating fan 2 is regulated to the minimum wind speed, a tested high-performance fiber sample is sent into a hot wind field through the high-performance fiber sample inlet 1, 10-50 fiber bundles with the length of about 1m are selected, and the initial mass m of the high-performance fiber to be tested is recorded 0-1 ;
7. After the circulating fan 2 is regulated to the process air speed, hot air flow hairiness stripping is carried out according to different high-performance fiber characteristics such as the decomposition time of the applied slurry or the thermal reaction time of the fiber. After a period of hot air flow treatment, the circulating fan 2 is adjusted to the minimum air speed, after the heat source 6 is closed, the collecting filter screens 11 of the sampling port I7 and the sampling port II 8 are taken out twice, and the treated high-performance fiber sample is placed in a dryer.
3. Defect analysis calculation
8. Measuring the weight of the treated high-performance fiber sample sampling port I7 and sampling port II 8 after heat treatment by an analytical balance, and recording the weight of the sampling port I7 after the test as m 1-2 The weight of the collecting filter screen at the second 8 part of the sampling port is recorded as m 2-2 The method comprises the steps of carrying out a first treatment on the surface of the After the test is finished, the residual mass of the high-performance fiber at the high-performance fiber sample inlet 1 is recorded as m 0-2 ;
The absolute mass of hairiness defect is the front and back mass change of a collecting filter screen at 7 positions of a sampling port, and the defect ratio is as follows:
the absolute mass of the second hairiness defect is the front and back mass change of the collecting filter screen at the second sampling port 8, and the defect ratio is as follows:
the total reaction mass change, i.e. the material loss (including chemical reaction) ratio is:
the three data reflect the factors of chemical reaction change, hairiness defect damage and the like of the high-performance fiber in a potential hot wind field, and can also be used for sub-sampling one type of hairiness defect under different heat treatment time according to the reaction speed.
9. And (3) shooting and orienting the metal filter screen with the hairiness defect collected at the 7-position sampling port by a high-definition digital camera, analyzing and calculating image data by computer software to obtain relevant statistical values of hairiness expansion size, diameter, quantity and the like, and calculating to obtain hairiness frequency ratio, average value, CV value and the like.
The apparatus and method for testing high performance fiber hairiness defects according to the present invention will be further described with reference to two specific examples.
Example 1 testing for hairiness defects in carbon fibers of certain type
1. Before testing, the device for testing the hairiness defect of the high-performance fiber is fixed on a horizontal tabletop, the temperature and humidity of a testing room are kept constant, the room temperature is 20+/-2 ℃, and the relative humidity is 45+/-3%. And finishing the earlier-stage equipment cleaning, filter screen measuring and installing work;
2. opening an electric control console, setting the temperature of a hot air field to be 350 ℃, and maintaining the temperature of the hot air field to be stable for 5 minutes in a state of circulating hot air flow for 3 m/s;
3. selecting 3 carbon fiber ingots of the same model and the same batch, wherein in the embodiment, T800-grade (12K) carbon fibers produced by Jiangsu Hengshen Co., ltd are selected, 40 sections of 1 m-long and smooth carbon fiber tows are taken from each ingot, and a sample is sent into a hot air field through a high-performance fiber sample inlet at the lowest wind speed (40 sections of carbon fiber tows are used as carbon fiber samples for one-time test);
4. the air flow is treated for 30min under the air flow state of circulating hot air flow of 3m/s at the temperature of 350 ℃ of a hot air field;
5. the hairiness defect weight of the first collecting filter screen of the sampling port and the second collecting filter screen of the sampling port is respectively 20mg and 0.5mg, and the hairiness defect loss rate of the first sampling port and the second sampling port is respectively 1.1% and 0.5 mill;
6. through high definition digital camera analysis, in the hairiness defect of filter screen department is collected to sampling port one place, initially can divide into: the number of filament bundles with the diameter exceeding 5mm is 2, the number of filament bundles with the length exceeding 5mm is 20, the number of filament bundles with the length exceeding 2-5mm is 50, and the number of filament bundles with the length exceeding 10mm is 4.
Implementation example 2, test of hairiness defect of certain carbon fiber precursor-PAN precursor
1. Before testing, the device for testing the hairiness defect of the high-performance fiber is fixed on a horizontal tabletop, the temperature and humidity of a testing room are kept constant, the room temperature is 20+/-2 ℃, and the relative humidity is 45+/-3%. And finishing the earlier-stage equipment cleaning, filter screen measuring and installing work;
2. opening an electric control console, setting the temperature of a hot air field to be 150 ℃, and maintaining the temperature of the hot air field to be stable for 5 minutes in a state of circulating hot air flow of 0.4 m/s;
3. selecting a certain carbon fiber precursor, namely PAN precursor 1 ingot, wherein the precursor is a T700 grade (12K) carbon fiber precursor produced by Jiangsu Hengshen Co., ltd, taking 40 sections of flat PAN precursor with the length of 1m, and sending a sample into a hot air field at the lowest wind speed through a high-performance fiber sample inlet;
4. the air flow is treated for 10min under the air flow state of 0.4m/s of circulating hot air flow at the temperature of 150 ℃ of a hot air field;
5. the hairiness defect weight of the first collecting filter screen at the first sampling port is 5mg respectively;
6. a second collecting filter screen is refilled at the first sampling port, the temperature of a hot air field is set to be 230 ℃,240 ℃,250 ℃ and 260 ℃ in the air flow state of circulating hot air flow of 0.4m/s, and the air flow treatment stage is carried out for 10min and 40min;
7. and by measuring a second collecting filter screen at the first sampling port, the hairiness defect weight of the second collecting filter screen at the second sampling port is 10mg and 1mg respectively.
8. Analysis by high definition digital camera:
in the hairiness defect of one part of the collecting filter screen, the method can be primarily divided into: 0 filament bundles with the diameter exceeding 5mm and the length exceeding 5mm are arranged at the position of 40 parallel filaments, 20 filament bundles with the length of 2-5mm are arranged at the position of 20 filament bundles with the length exceeding 10mm, and the number of filament filaments is 1;
among hairiness defects at two parts of the collecting filter screen, the hairiness defects can be primarily divided into: the number of filament bundles with the diameter exceeding 5mm is 1, the number of filament bundles with the length exceeding 5mm is 3, the number of filament bundles with the length being 2-5mm is 40, the number of filament bundles with the length exceeding 10mm is 5, and the number of tar and dust impurities is 15.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and variations could be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and variations should also be regarded as being within the scope of the invention.