CN108169274B - Hot melt adhesive thermal stability testing method and device - Google Patents
Hot melt adhesive thermal stability testing method and device Download PDFInfo
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- CN108169274B CN108169274B CN201711468976.1A CN201711468976A CN108169274B CN 108169274 B CN108169274 B CN 108169274B CN 201711468976 A CN201711468976 A CN 201711468976A CN 108169274 B CN108169274 B CN 108169274B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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Abstract
The invention discloses a hot melt adhesive thermal stability testing method, which comprises the following steps: 1) preparing a hot melt adhesive to be tested; 2) heating the hot melt adhesive to be molten, and observing the color and appearance changes of the hot melt adhesive; 3) under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering; 4) and cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test. The filtering step is added before the testing of the thin consistency and the softening point, so that the influence of carbide in the hot melt adhesive is eliminated, and the error of the testing result is effectively reduced; the carbide in the hot melt adhesive can be separated in the filtering process, and the carbide amount can be accurately obtained after collection and weighing, so that the thermal stability of the hot melt adhesive can be conveniently quantized and compared; the method is simple to operate, overcomes subjective errors caused by observation of different people in the existing method, quantifies the test result and has high precision.
Description
Technical Field
The invention relates to a physical property test of a hot melt adhesive, in particular to a method and a device for testing the thermal stability of the hot melt adhesive.
Background
The hot melt adhesive is a plastic adhesive, and the physical state of the hot melt adhesive changes along with the temperature change in a certain temperature range, so that the thermal stability of the hot melt adhesive is an important index for detecting the quality of the hot melt adhesive, and the currently generally adopted hot melt adhesive thermal stability determination method has many defects, such as: after long-time high-temperature heating, the conditions of gelation, skinning, carbonization and the like can occur in the testing process of part of the rubber sample, and if filtration treatment is not carried out, very large testing errors can occur in the tests of the thin consistency and the softening point, so that the testing accuracy is influenced; the test process is mainly observation, and the test result can not be quantized, for example, the amount of sediment after high-temperature heating can not be quantized, and the change of the inside of the glue solution after the high-temperature heating of the hot melt adhesive can not be accurately observed, so that the stability of the hot melt adhesive can not be accurately measured.
In order to overcome the defects in the prior art, it is necessary to develop an accurate hot melt adhesive thermal stability testing method capable of quantifying the testing result, which can solve the problems of testing errors of thin consistency and softening point, and can quantitatively test the precipitate, thereby effectively and accurately testing the thermal stability of the hot melt adhesive.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the hot melt adhesive thermal stability test method which reduces the test errors of the thin consistency and the softening point, has high precision and can quantify the test result.
The invention also aims to provide a hot melt adhesive thermal stability testing device which comprises a filter screen, thereby eliminating the influence of precipitates, effectively reducing the error of a test result and quantifying the test result.
In order to achieve the purpose, the invention adopts the technical scheme that: a hot melt adhesive thermal stability test method comprises the following steps:
1) preparing materials: preparing 3-30g of hot melt adhesive to be tested;
2) heating and observing: heating the hot melt adhesive to be molten, and observing the color and appearance changes of the hot melt adhesive;
3) and (3) filtering: under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering, wherein the thermal stability testing device comprises a filter screen; after cooling, weighing the hot melt adhesive on the filter screen, namely weighing the carbide in the hot melt adhesive;
4) and (3) testing: and cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test.
Preferably, the specific operation of heating observation in step 2) is: and (3) putting the hot melt adhesive into a glass container, continuously heating for 22-26h at 160-200 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color darkening and carbonization on the surface of the hot melt adhesive.
More specifically, the specific operation of heating observation in step 2) is as follows: (1) weighing a 15g hot melt adhesive sample; (2) preparing a cylindrical glass container with the height of 2cm and the diameter of 4 cm; (3) putting the glue sample in a glass container, putting the glass container in an oven at 180 ℃, and heating for continuous observation; (4) after 24 hours, observing under the condition of high-temperature melting, and judging whether obvious skinning, color deepening and carbonization phenomena appear on the surface of the hot melt adhesive.
Preferably, the filter screen of the thermal stability testing device is a stainless steel filter screen, and the mesh number of the filter screen is 80-120 meshes. More preferably, the filter screen is a replaceable stainless steel filter screen, and the mesh number of the filter screen is 100 meshes.
Preferably, the specific operation steps of the softening point test in the step 4) are as follows:
1) heating and melting 4-5g of filtered hot melt adhesive, filling the hollow part of the copper ring with the hot melt adhesive, and cooling for 2-3h at normal temperature;
2) after cooling, placing a steel ball with the diameter of 9.525mm and the weight of 3.5 +/-0.05 g in the middle of the colloid of the copper ring;
3) placing the copper ring with the steel balls on a softening point measuring device frame, placing a thermometer with the length of 45cm in a central hole of the softening point measuring device, and then placing the softening point measuring device in a glass cup filled with glycerol;
4) the glass cup is placed on a heating furnace with stable temperature rise, the hot melt adhesive can be gradually softened along with the temperature rise, and the steel balls fall through the hot melt adhesive body to reach the temperature of the floor, namely the softening point of the hot melt adhesive.
Preferably, in the step 4), the heating rate of the heating furnace is 4.5-5.5 ℃/min.
Specifically, the specific test procedure of the thin consistency test is as follows:
the CAP2000+ model of a special measuring device for the bolexu consistency is adopted, and the measurement unit is centipoise cp.
(1) Setting probes, wherein for the thin consistency below 30000cps, a No. 4 probe is adopted;
(2) setting the temperature, directly inputting a temperature point to be tested, such as 150 ℃, by using a number key;
(3) setting the rotating speed, directly inputting the rotating speed to be tested by using a number key, such as 50 revolutions;
(4) after setting corresponding parameters, putting a to-be-tested glue sample on a central heating IC (the glue amount is proper), and not overflowing the rotary probe too much;
(5) after the rubber sample to be tested is placed, the probe is pressed down by a lifting rod, and a start key is pressed down when the temperature is stabilized at the required testing temperature;
(6) and after the rotation of the probe is stopped, reading the actual thickness data of the hot melt adhesive sample on the liquid crystal screen.
The invention also provides a hot melt adhesive thermal stability testing device which comprises a support, wherein a main body frame is arranged on the support, and a replaceable filter screen is arranged in the main body frame.
Preferably, the filter screen is made of stainless steel.
Preferably, the mesh number of the filter screen is 80-120 meshes. More preferably, the filter screen is a replaceable stainless steel filter screen, and the mesh number of the filter screen is 100 meshes. Stainless steel filter screen can place the use and cause rusty phenomenon, can regularly change hot melt adhesive thermal stability testing arrangement's stainless steel filter screen according to the in-service use condition.
The inventor of the application discovers through experiments that after the hot melt adhesive is carbonized, infusible floccules or carbonized particles can be generated, the grain size of the carbonized particles is small, the 80-120-mesh filter screen is adopted for filtering, the carbides can be effectively separated, the weight of the generated carbides can be accurately weighed, and subsequent testing of a thin consistency result can not be influenced, so that errors are caused. When the filtering is carried out by adopting a filter screen with the mesh number smaller than 80 meshes, carbides cannot be well separated, and some carbides with smaller particles can enter the hot melt adhesive, so that a larger error is brought to the subsequent softening point and thin consistency test; when the filter screen with the mesh number larger than 120 is adopted for filtering, the aperture of the filter screen is small, the filtering is slow, and in addition, some hot melt adhesives without carbonization also remain on the filter screen, so that larger errors can be caused in subsequent tests of softening points and thin consistencies.
The hot melt adhesive thermal stability test method can quantify the test result, for example, the carbide is weighed and separated, the weight of the carbide is quantified, and the change rate of the thin consistency and the softening point of the hot melt adhesive after continuous high-temperature test can be further quantified compared with the change rate before test, so that the measurement result is more accurate.
The invention has the beneficial effects that: the filtering step is added before the testing of the thin consistency and the softening point, so that the influence of carbide in the hot melt adhesive is eliminated, and the error of the testing result is effectively reduced; the carbide in the hot melt adhesive can be separated in the filtering process, and the carbide amount can be accurately obtained after collection and weighing, so that the thermal stability of the hot melt adhesive can be conveniently quantized and compared; the method is simple to operate, overcomes subjective errors caused by observation of different people in the existing method, quantifies the test result and has high precision.
Drawings
Fig. 1 is a schematic view of a hot melt adhesive thermal stability testing device of the present invention, wherein the symbols in the schematic view have the following meanings: 1-main body frame, 2-filter screen, 3-support.
Detailed Description
Example 1
The utility model provides a hot melt adhesive thermal stability testing arrangement, includes support 3, is provided with main body frame 1 on the support, is provided with removable mesh in the main body frame and is 100 mesh stainless steel's filter screen 2.
Example 2
A hot melt adhesive thermal stability test method comprises the following steps:
1) preparing materials: preparing 10g of hot melt adhesive to be tested;
2) heating and observing: placing the hot melt adhesive in a glass container, continuously heating for 26h at 160 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color deepening and carbonization on the surface of the hot melt adhesive;
3) and (3) filtering: under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering, wherein the thermal stability testing device comprises a replaceable filter screen with the mesh number of 100; after cooling, weighing the hot melt adhesive on the filter screen, namely weighing the carbide in the hot melt adhesive, wherein the weight of the carbide after filtering is 0.32 g;
4) and (3) testing: and cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test.
The specific operation steps of the softening point test are as follows:
1) heating and melting 4g of filtered hot melt adhesive, filling the hollow part of the copper ring with the hot melt adhesive, and cooling for 2 hours at normal temperature;
2) after cooling, placing a steel ball with the diameter of 9.525mm and the weight of 3.5 +/-0.05 g in the middle of the colloid of the copper ring;
3) placing the copper ring with the steel balls on a softening point measuring device frame, placing a thermometer with the length of 45cm in a central hole of the softening point measuring device, and then placing the softening point measuring device in a glass cup filled with glycerol;
4) the glass cup is placed on a heating furnace which is stably heated at the heating rate of 4.5 ℃/min, the hot melt adhesive is gradually softened along with the temperature rise, and the steel balls fall through the hot melt adhesive body to contact the floor, namely the temperature of the hot melt adhesive is the softening point of the hot melt adhesive.
Wherein, the specific test process of the thin consistency test is as follows:
the CAP2000+ model of a special measuring device for the bolexu consistency is adopted, and the measurement unit is centipoise cp.
(1) Setting probes, wherein for the thin consistency below 30000cps, a No. 4 probe is adopted;
(2) setting the temperature, directly inputting a temperature point to be tested, such as 150 ℃, by using a number key;
(3) setting the rotating speed, directly inputting the rotating speed to be tested by using a number key, such as 50 revolutions;
(4) after setting corresponding parameters, putting a to-be-tested glue sample on a central heating IC (the glue amount is proper), and not overflowing the rotary probe too much;
(5) after the rubber sample to be tested is placed, the probe is pressed down by a lifting rod, and a start key is pressed down when the temperature is stabilized at the required testing temperature;
(6) and after the rotation of the probe is stopped, reading the actual thickness data of the hot melt adhesive sample on the liquid crystal screen.
Example 3
A hot melt adhesive thermal stability test method comprises the following steps:
1) preparing materials: preparing 15g of hot melt adhesive to be tested;
2) heating and observing: placing the hot melt adhesive in a glass container, continuously heating for 24h at 180 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color deepening and carbonization on the surface of the hot melt adhesive;
3) and (3) filtering: under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering, wherein the thermal stability testing device comprises a replaceable filter screen with the mesh number of 100; after cooling, weighing the hot melt adhesive on the filter screen, namely weighing the carbide in the hot melt adhesive, wherein the weight of the carbide after filtering is 0.51 g;
4) and (3) testing: and cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test.
The specific operation steps of the softening point test are as follows:
1) heating and melting 5g of filtered hot melt adhesive, filling the hollow part of the copper ring with the hot melt adhesive, and cooling for 3 hours at normal temperature;
2) after cooling, placing a steel ball with the diameter of 9.525mm and the weight of 3.5 +/-0.05 g in the middle of the colloid of the copper ring;
3) placing the copper ring with the steel balls on a softening point measuring device frame, placing a thermometer with the length of 45cm in a central hole of the softening point measuring device, and then placing the softening point measuring device in a glass cup filled with glycerol;
4) the glass cup is placed on a heating furnace which is stably heated at the heating rate of 5 ℃/min, the hot melt adhesive is gradually softened along with the temperature rise, and the steel balls fall through the hot melt adhesive body to contact the floor, namely the temperature of the steel balls is the softening point of the hot melt adhesive.
The method of the thin consistency test is the same as that of example 2.
Example 4
A hot melt adhesive thermal stability test method comprises the following steps:
1) preparing materials: preparing 18g of hot melt adhesive to be tested;
2) heating and observing: placing the hot melt adhesive in a glass container, continuously heating for 22h at 200 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color deepening and carbonization on the surface of the hot melt adhesive;
3) and (3) filtering: under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering, wherein the thermal stability testing device comprises a replaceable filter screen with 120 meshes; after cooling, weighing the hot melt adhesive on the filter screen, namely weighing the carbide in the hot melt adhesive, wherein the weight of the carbide after filtering is 0.55 g;
4) and (3) testing: and cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test.
The specific operation steps of the softening point test are as follows:
1) heating and melting 5g of filtered hot melt adhesive, filling the hollow part of the copper ring with the hot melt adhesive, and cooling for 2 hours at normal temperature;
2) after cooling, placing a steel ball with the diameter of 9.525mm and the weight of 3.5 +/-0.05 g in the middle of the colloid of the copper ring;
3) placing the copper ring with the steel balls on a softening point measuring device frame, placing a thermometer with the length of 45cm in a central hole of the softening point measuring device, and then placing the softening point measuring device in a glass cup filled with glycerol;
4) the glass cup is placed on a heating furnace which is stably heated at the heating rate of 5.5 ℃/min, the hot melt adhesive is gradually softened along with the temperature rise, and the steel balls fall through the hot melt adhesive body to contact the floor, namely the temperature of the hot melt adhesive is the softening point of the hot melt adhesive.
The method of the thin consistency test is the same as that of example 2.
Comparative example 1
This example is a conventional test method for the thermal stability of hot melt adhesives.
A hot melt adhesive thermal stability test method comprises the following steps:
1) preparing materials: preparing 10g of hot melt adhesive to be tested;
2) heating and observing: and (3) putting the hot melt adhesive into a glass container, continuously heating for 24h at 180 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color deepening and carbonization on the surface of the hot melt adhesive.
Comparing examples 1-4 with comparative example 1, it can be seen that examples 1-5 of the present invention can quantify the thermal stability results of the hot melt adhesive and determine specific values, whereas the method of comparative example 1, simply by subjectively observing the changes in the surface of the hot melt adhesive, does not provide a more intuitive test result.
Claims (3)
1. A hot melt adhesive thermal stability test method is characterized by comprising the following steps:
1) preparing materials: preparing 3-30g of hot melt adhesive to be tested;
2) heating and observing: heating the hot melt adhesive to be molten, and observing the color and appearance changes of the hot melt adhesive;
3) and (3) filtering: under the condition of melting, putting the hot melt adhesive into a thermal stability testing device for filtering, wherein the thermal stability testing device comprises a filter screen; after cooling, weighing the hot melt adhesive on the filter screen, namely weighing the carbide in the hot melt adhesive;
4) and (3) testing: cooling the filtered hot melt adhesive, and then performing a softening point test and a thin consistency test;
wherein, the specific operation of heating observation in the step 2) is as follows: placing the hot melt adhesive in a glass container, continuously heating for 22-26h at 160-200 ℃ until the hot melt adhesive is molten, and observing the phenomena of skinning, color darkening and carbonization on the surface of the hot melt adhesive;
wherein, the filter screen of the thermal stability testing device in the step 3) is a stainless steel filter screen, and the mesh number of the filter screen is 80-120 meshes.
2. The hot melt adhesive thermal stability test method according to claim 1, wherein the specific operation steps of the softening point test in the step 4) are as follows:
1) heating and melting 4-5g of filtered hot melt adhesive, filling the hollow part of the copper ring with the hot melt adhesive, and cooling for 2-3h at normal temperature;
2) after cooling, placing a steel ball with the diameter of 9.525mm and the weight of 3.5 +/-0.05 g in the middle of the colloid of the copper ring;
3) placing the copper ring with the steel balls on a softening point measuring device frame, placing a thermometer with the length of 45cm in a central hole of the softening point measuring device, and then placing the softening point measuring device in a glass cup filled with glycerol;
4) the glass cup is placed on a heating furnace with stable temperature rise, the hot melt adhesive can be gradually softened along with the temperature rise, and the steel balls fall through the hot melt adhesive body to reach the temperature of the floor, namely the softening point of the hot melt adhesive.
3. The hot melt adhesive thermal stability test method according to claim 2, wherein in the step 4), the heating rate of the heating furnace is 4.5-5.5 ℃/min.
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