CN108169274A - A kind of hot melt adhesive heat stability testing method and device - Google Patents
A kind of hot melt adhesive heat stability testing method and device Download PDFInfo
- Publication number
- CN108169274A CN108169274A CN201711468976.1A CN201711468976A CN108169274A CN 108169274 A CN108169274 A CN 108169274A CN 201711468976 A CN201711468976 A CN 201711468976A CN 108169274 A CN108169274 A CN 108169274A
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- hot melt
- melt adhesive
- heat stability
- stability testing
- softening point
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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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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of hot melt adhesive heat stability testing methods, include the following steps：1) prepare hot melt adhesive to be tested；2) hot melt adhesive is heated to melting, observes the color and luster of hot melt adhesive and the variation of appearance；3) under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered；4) hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.The step of present invention increases filtering before dilute consistency, softening point is tested, eliminates the influence of carbide in hot melt adhesive, effectively reduces the error of test result；Filter process can detach the carbide in hot melt adhesive, collect the amount that carbide can be accurately obtained after weighing, quantization is facilitated to compare the thermal stability of hot melt adhesive；This method is easy to operate, overcomes the subjective error brought due to different people is observed in existing method, and test result can be quantified, and precision is high.
Description
Technical field
The present invention relates to the physical property measurements of hot melt adhesive, and in particular to a kind of hot melt adhesive heat stability testing method and device.
Background technology
Hot melt adhesive is a kind of adhesive of plasticity, and in certain temperature range, physical state changes with temperature and changed,
Therefore hot melt adhesive thermal stability is an important indicator of hot melt adhesive quality testing, and the thermosol heat generally used at present is steady
Qualitative determination method but there are many deficiencies part, such as：After being heated at high temperature for a long time, it will appear in the glue sample test process of part
Situations such as gel, skinning, carbonization, if without filtration treatment, dilute consistency, softening point test will appear very big test and miss
Difference, so as to influence the accuracy of test；Test process is mainly observed, and can not be quantified test result, such as can not quantify height
The amount of sediment after temperature heating, it is more difficult to the variation after accurate observation hot melt adhesive high-temperature heating inside glue, therefore can not be accurately
Measure the stability of hot melt adhesive.
In order to improve the deficiencies in the prior art, it is necessary to which research and development are a kind of accurate, the hot melt adhesive that can quantify test result
Heat stability testing method, this method can solve the problems, such as dilute consistency, softening point test error, and sediment can be carried out
Quantization test effectively can accurately test out the thermal stability of hot melt adhesive.
Invention content
In view of the deficiencies of the prior art, dilute consistency, softening point test mistake are reduced it is an object of the present invention to provide a kind of
Difference, precision is high, the hot melt adhesive heat stability testing method that can quantify test result.
Another object of the present invention is to provide the device of hot melt adhesive heat stability testing, which includes strainer, eliminates
The influence of sediment effectively reduces the error of test result, test result is quantified.
To achieve these goals, the technical solution adopted by the present invention is：A kind of hot melt adhesive heat stability testing method, packet
Include following steps：
1) material prepares：Prepare 3-30g hot melt adhesive to be tested；
2) heating observation：Hot melt adhesive is heated to melting, observes the color and luster of hot melt adhesive and the variation of appearance；
3) it filters：Under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered, the thermal stability
Test device includes strainer；The hot melt adhesive on strainer, the weight of carbide as in hot melt adhesive are weighed after cooling；
4) it tests：Hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.
Preferably, the concrete operations of heating observation are in step 2)：Hot melt adhesive is placed in glass container at 160-200 DEG C
To melting, the skinning on observation hot melt adhesive surface darkens and carbonization phenomenon lower continuous heating 22-26h.
More specifically, the concrete operations of heating observation are in step 2)：(1) 15g hot melt adhesive samples are weighed；(2) prepare high
Spend the cylindrical glass container for 2cm, a diameter of 4cm；(3) glue sample is put in glass container, and places it in 180 DEG C of bakings
Case, heating and continuous observation；(4) after 24h, observed under the conditions of high-temperature fusion, hot melt adhesive surface whether occur apparent skinning,
It darkens and carbonization phenomenon.
Preferably, the strainer of heat stability testing device is stainless steel filtering net, and the mesh number of strainer is 80-120 mesh.More preferably
, strainer is replaceable stainless steel filtering net, and the mesh number of strainer is 100 mesh.
Preferably, the concrete operation step of softening point test is in step 4)：
1) the hot melt adhesive heating melting after 4-5g is filtered, fills and leads up copper ring hollow space, then be placed under room temperature and cool down with it
2-3h；
2) after cooling down, an a diameter of 9.525mm is placed among the colloid of copper ring, weighs the steel ball of 3.5 ± 0.05g；
3) copper ring for placing steel ball is placed on softening point measuring device frame, is put in the centre bore of softening point measuring device
Enter the thermometer of 45cm long, then softening point measuring device is put in the glass equipped with glycerine；
4) glass is positioned on the heating furnace for stablizing heating, as temperature increases, hot melt adhesive can gradually soften, steel ball
It is fallen across hot melt colloid, touches the softening point of temperature during floor, as hot melt adhesive.
Preferably, in step 4), the heating rate of heating furnace is 4.5-5.5 DEG C/min.
Specifically, the specific test process of dilute consistency testing is as follows：
Using the CAP2000+ models of the dilute consistency special measurement equipment of rich power, units of measurement is centipoise cp.
(1) probe is set, for being less than dilute consistency of below 30000cps, using No. 4 probes；
(2) temperature is set, and directly utilizes the temperature spot tested required for digital key input, such as 150 DEG C；
(3) rotating speed is set, and directly utilizes the rotating speed tested required for digital key input, such as 50 turns；
(4) after corresponding parameter is set, glue sample will be tested and be put on center heating IC (glue amount is appropriate), not excessively
Overflow rotating probe；
(5) after the glue tested sample is placed, probe is depressed with elevating lever, waiting temperature stabilization is in required test temperature
When spending, start key is pressed；
(6) after probe rotation stops, in the dilute consistency data of reality that hot melt adhesive sample is read on LCD screen.
The present invention also provides a kind of hot melt adhesive heat stability testing device, the hot melt adhesive heat stability testing device packet
Stent is included, main body frame is provided on stent, replaceable strainer is provided in main body frame.
Preferably, the material of the strainer is stainless steel.
Preferably, the mesh number of the strainer is 80-120 mesh.It is furthermore preferred that strainer is replaceable stainless steel filtering net, filter
The mesh number of net is 100 mesh.Stainless steel filtering net can place the phenomenon that causing to get rusty using process, can be according to the feelings of actual use
The stainless steel filtering net of hot melt adhesive heat stability testing device is replaced in condition, timing.
Present inventor does not melt floccule or carbonization it is discovered by experiment that can be generated after hot melt adhesive carbonization
Grain, and these carbonized particles grain sizes are smaller, using the strainer filtering of 80-120 mesh, can effectively detach these carbide, it can
With the carbide weight that precise generates, subsequent dilute consistency result test will not be influenced, so as to cause error.And work as
When being less than the strainer filtering of 80 mesh using mesh number, it is impossible to detach carbide well, the smaller carbide of some particles can enter
In hot melt adhesive, so as to subsequent softening point and dilute consistency testing, bring larger error；It is more than 120 purposes when using mesh number
During strainer filtering, the aperture of strainer is smaller, and filtering is slower, in addition, some are also remained on strainer without the hot melt adhesive being carbonized, meeting
Larger error is caused to subsequent softening point and dilute consistency testing.
The hot melt adhesive heat stability testing method of the present invention can quantify test result, for example, by weighing separation carbonization
Object quantifies carbide weight, also can further quantify hot melt adhesive after continuous high temperature is tested, and dilute consistency, softening point be not compared to
Change rate before test makes measurement result more accurate.
The beneficial effects of the invention are as follows：The step of present invention increases filtering before dilute consistency, softening point is tested excludes
The influence of carbide in hot melt adhesive effectively reduces the error of test result；Filter process can to the carbide in hot melt adhesive into
Row separation, collects the amount that carbide can be accurately obtained after weighing, quantization is facilitated to compare the thermal stability of hot melt adhesive；This method is grasped
Make simply, to overcome the subjective error brought due to different people is observed in existing method, test result can be quantified, precision is high.
Description of the drawings
Fig. 1 is the schematic diagram of the hot melt adhesive heat stability testing device of the present invention, wherein, each symbolic significance in schematic diagram
It is as follows：1- main body frames, 2- strainers, 3- stents.
Specific embodiment
Embodiment 1
A kind of hot melt adhesive heat stability testing device including stent 3, is provided with main body frame 1 on stent, in main body frame
It is provided with the strainer 2 for the stainless steel that replaceable mesh number is 100 mesh.
Embodiment 2
A kind of hot melt adhesive heat stability testing method, includes the following steps：
1) material prepares：Prepare 10g hot melt adhesive to be tested；
2) heating observation：Hot melt adhesive is placed in glass container the continuous heating 26h at 160 DEG C, and, to melting, observation heats
The skinning on glue surface darkens and carbonization phenomenon；
3) it filters：Under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered, the thermal stability
Test device includes the mesh number strainer replaceable for 100 purposes；The hot melt adhesive on strainer, as carbon in hot melt adhesive are weighed after cooling
The weight of compound, carbide weight is 0.32 gram after filtering；
4) it tests：Hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.
Wherein, the concrete operation step of softening point test is：
1) the hot melt adhesive heating melting after 4g is filtered, fills and leads up copper ring hollow space, then be placed under room temperature and cool down 2h with it；
2) after cooling down, an a diameter of 9.525mm is placed among the colloid of copper ring, weighs the steel ball of 3.5 ± 0.05g；
3) copper ring for placing steel ball is placed on softening point measuring device frame, is put in the centre bore of softening point measuring device
Enter the thermometer of 45cm long, then softening point measuring device is put in the glass equipped with glycerine；
4) glass is positioned on the heating furnace for stablizing heating with the heating rate of 4.5 DEG C/min, as temperature increases,
Hot melt adhesive can gradually soften, and steel ball passes through hot melt colloid to fall, and touches the softening point of temperature during floor, as hot melt adhesive.
Wherein, the specific test process of dilute consistency testing is as follows：
Using the CAP2000+ models of the dilute consistency special measurement equipment of rich power, units of measurement is centipoise cp.
(1) probe is set, for being less than dilute consistency of below 30000cps, using No. 4 probes；
(2) temperature is set, and directly utilizes the temperature spot tested required for digital key input, such as 150 DEG C；
(3) rotating speed is set, and directly utilizes the rotating speed tested required for digital key input, such as 50 turns；
(4) after corresponding parameter is set, glue sample will be tested and be put on center heating IC (glue amount is appropriate), not excessively
Overflow rotating probe；
(5) after the glue tested sample is placed, probe is depressed with elevating lever, waiting temperature stabilization is in required test temperature
When spending, start key is pressed；
(6) after probe rotation stops, in the dilute consistency data of reality that hot melt adhesive sample is read on LCD screen.
Embodiment 3
A kind of hot melt adhesive heat stability testing method, includes the following steps：
1) material prepares：Prepare 15g hot melt adhesive to be tested；
2) heating observation：Hot melt adhesive is placed in glass container the continuous heating at 180 DEG C, and, for 24 hours to melting, observation heats
The skinning on glue surface darkens and carbonization phenomenon；
3) it filters：Under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered, the thermal stability
Test device includes the mesh number strainer replaceable for 100 purposes；The hot melt adhesive on strainer, as carbon in hot melt adhesive are weighed after cooling
The weight of compound, carbide weight is 0.51 gram after filtering；
4) it tests：Hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.
Wherein, the concrete operation step of softening point test is：
1) the hot melt adhesive heating melting after 5g is filtered, fills and leads up copper ring hollow space, then be placed under room temperature and cool down 3h with it；
2) after cooling down, an a diameter of 9.525mm is placed among the colloid of copper ring, weighs the steel ball of 3.5 ± 0.05g；
3) copper ring for placing steel ball is placed on softening point measuring device frame, is put in the centre bore of softening point measuring device
Enter the thermometer of 45cm long, then softening point measuring device is put in the glass equipped with glycerine；
4) glass is positioned on the heating furnace for stablizing heating with the heating rate of 5 DEG C/min, as temperature increases, heat
Melten gel can gradually soften, and steel ball passes through hot melt colloid to fall, and touches the softening point of temperature during floor, as hot melt adhesive.
Wherein, the method for dilute consistency testing is identical with dilute consistency testing method in embodiment 2.
Embodiment 4
A kind of hot melt adhesive heat stability testing method, includes the following steps：
1) material prepares：Prepare 18g hot melt adhesive to be tested；
2) heating observation：Hot melt adhesive is placed in glass container the continuous heating 22h at 200 DEG C, and, to melting, observation heats
The skinning on glue surface darkens and carbonization phenomenon；
3) it filters：Under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered, the thermal stability
Test device includes the mesh number strainer replaceable for 120 purposes；The hot melt adhesive on strainer, as carbon in hot melt adhesive are weighed after cooling
The weight of compound, carbide weight is 0.55 gram after filtering；
4) it tests：Hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.
Wherein, the concrete operation step of softening point test is：
1) the hot melt adhesive heating melting after 5g is filtered, fills and leads up copper ring hollow space, then be placed under room temperature and cool down 2h with it；
2) after cooling down, an a diameter of 9.525mm is placed among the colloid of copper ring, weighs the steel ball of 3.5 ± 0.05g；
3) copper ring for placing steel ball is placed on softening point measuring device frame, is put in the centre bore of softening point measuring device
Enter the thermometer of 45cm long, then softening point measuring device is put in the glass equipped with glycerine；
4) glass is positioned on the heating furnace for stablizing heating with the heating rate of 5.5 DEG C/min, as temperature increases,
Hot melt adhesive can gradually soften, and steel ball passes through hot melt colloid to fall, and touches the softening point of temperature during floor, as hot melt adhesive.
Wherein, the method for dilute consistency testing is identical with dilute consistency testing method in embodiment 2.
Comparative example 1
This is the traditional test methods of hot melt adhesive thermal stability.
A kind of hot melt adhesive heat stability testing method, includes the following steps：
1) material prepares：Prepare 10g hot melt adhesive to be tested；
2) heating observation：Hot melt adhesive is placed in glass container the continuous heating at 180 DEG C, and, for 24 hours to melting, observation heats
The skinning on glue surface darkens and carbonization phenomenon.
By embodiment 1-4 it is found that 1-5 of the embodiment of the present invention can be by hot melt adhesive thermal stability results compared with comparative example 1
Quantization, determines specific numerical value, and the method in comparative example 1, merely by the variation on subjective observation hot melt adhesive surface, no
One intuitive test result of comparison can be provided.
Claims (8)
- A kind of 1. hot melt adhesive heat stability testing method, which is characterized in that include the following steps：1) material prepares：Prepare 3-30g hot melt adhesive to be tested；2) heating observation：Hot melt adhesive is heated to melting, observes the color and luster of hot melt adhesive and the variation of appearance；3) it filters：Under melting condition, hot melt adhesive is placed in heat stability testing device and is filtered, the test of the thermal stability Device includes strainer；The hot melt adhesive on strainer, the weight of carbide as in hot melt adhesive are weighed after cooling；4) it tests：Hot melt adhesive after filtering is cooled down, then carries out softening point test and dilute consistency testing.
- 2. hot melt adhesive heat stability testing method according to claim 1, which is characterized in that heating observation in step 2) Concrete operations are：Hot melt adhesive is placed in glass container the continuous heating 22-26h at 160-200 DEG C and, to melting, observes hot melt adhesive The skinning on surface darkens and carbonization phenomenon.
- 3. hot melt adhesive heat stability testing method according to claim 1, which is characterized in that heat stability testing device Strainer is stainless steel filtering net, and the mesh number of strainer is 80-120 mesh.
- 4. hot melt adhesive heat stability testing method according to claim 1, which is characterized in that softening point is tested in step 4) Concrete operation step be：1) the hot melt adhesive heating melting after 4-5g is filtered, fills and leads up copper ring hollow space, then be placed under room temperature and cool down 2-3h with it；2) after cooling down, an a diameter of 9.525mm is placed among the colloid of copper ring, weighs the steel ball of 3.5 ± 0.05g；3) copper ring for placing steel ball is placed on softening point measuring device frame, is put into the centre bore of softening point measuring device The thermometer of 45cm long, then softening point measuring device is put in the glass equipped with glycerine；4) glass is positioned on the heating furnace for stablizing heating, as temperature increases, hot melt adhesive can gradually soften, and steel ball passes through Hot melt colloid is fallen, and touches the softening point of temperature during floor, as hot melt adhesive.
- 5. hot melt adhesive heat stability testing method according to claim 4, which is characterized in that in step 4), heating furnace Heating rate is 4.5-5.5 DEG C/min.
- 6. a kind of hot melt adhesive heat stability testing device, which is characterized in that the hot melt adhesive heat stability testing device includes branch Frame is provided with main body frame on stent, replaceable strainer is provided in main body frame.
- 7. hot melt adhesive heat stability testing device according to claim 6, which is characterized in that the material of the strainer is not Become rusty steel.
- 8. hot melt adhesive heat stability testing device according to claim 6, which is characterized in that the mesh number of the strainer is 80-120 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711468976.1A CN108169274B (en) | 2017-12-29 | 2017-12-29 | Hot melt adhesive thermal stability testing method and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711468976.1A CN108169274B (en) | 2017-12-29 | 2017-12-29 | Hot melt adhesive thermal stability testing method and device |
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| CN108169274A true CN108169274A (en) | 2018-06-15 |
| CN108169274B CN108169274B (en) | 2020-12-01 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204685414U (en) * | 2015-05-29 | 2015-10-07 | 泰马克精密铸造（苏州）有限公司 | Point gum machine filter mechanism |
-
2017
- 2017-12-29 CN CN201711468976.1A patent/CN108169274B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204685414U (en) * | 2015-05-29 | 2015-10-07 | 泰马克精密铸造（苏州）有限公司 | Point gum machine filter mechanism |
Non-Patent Citations (4)
| Title |
|---|
| 中国石油化工总公司: "《SH/T 0209-92 液压油热稳定性测定法》", 20 May 1992, 中国石化出版社 * |
| 国家技术监督局: "《GB/T 15332-94 热熔胶粘剂软化点的测定 环球法》", 22 December 1994, 中国标准出版社 * |
| 国家技术监督局: "《GB/T 16998-1997 热熔胶粘剂热稳定性测定》", 26 September 1997, 中国标准出版社 * |
| 龚建贤 等: "《聚酰胺热熔胶抗氧化研究》", 《粘接》 * |
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