CN112362532A - Gel temperature testing method for polyvinyl chloride paste resin - Google Patents
Gel temperature testing method for polyvinyl chloride paste resin Download PDFInfo
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- CN112362532A CN112362532A CN202011078879.3A CN202011078879A CN112362532A CN 112362532 A CN112362532 A CN 112362532A CN 202011078879 A CN202011078879 A CN 202011078879A CN 112362532 A CN112362532 A CN 112362532A
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- polyvinyl chloride
- temperature
- paste resin
- chloride paste
- viscosity
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- 239000011347 resin Substances 0.000 title claims abstract description 104
- 229920005989 resin Polymers 0.000 title claims abstract description 104
- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 77
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 77
- 238000012360 testing method Methods 0.000 title claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims description 20
- 239000004014 plasticizer Substances 0.000 claims description 16
- 238000010998 test method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000001879 gelation Methods 0.000 claims description 6
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 5
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 230000008030 elimination Effects 0.000 abstract description 3
- 238000003379 elimination reaction Methods 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract description 3
- 229920001944 Plastisol Polymers 0.000 description 5
- 239000004999 plastisol Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002649 leather substitute Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Images
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Abstract
The invention discloses a gel temperature testing method for polyvinyl chloride paste resin, which is characterized in that tangent lines of two curve segments with sharp changes on a viscosity-temperature curve graph corresponding to the polyvinyl chloride paste resin under the heating at a fixed heating rate are determined, and then the temperature corresponding to the intersection point of the two tangent lines is determined as the gel temperature of the polyvinyl chloride paste resin. The polyvinyl chloride paste resin gel temperature testing method provided by the invention has the advantages of simple operation, reliable result, stable testing process, elimination of human factor influence and the like, and further provides a convenient and credible testing means for research and development departments and paste resin downstream manufacturers.
Description
Technical Field
The invention relates to the technical field of polyvinyl chloride paste resin performance testing, in particular to a gel temperature testing method for polyvinyl chloride paste resin.
Background
Polyvinyl chloride paste resin is one of polyvinyl chloride resin varieties, and is applied by being mixed with a plasticizer under stirring to form a plastisol. At present, the main production processes of polyvinyl chloride paste resin comprise a micro-suspension method and an emulsion method, and the particle size range of the polyvinyl chloride paste resin is generally 0.1-2.0 mu m. The PVC paste resin is mainly applied to soft products such as artificial leather, floor leather, toys, wallpaper, automotive interior materials and the like.
Because, in the paste resin molding process, the plastisol undergoes a plasticizing process from gel to melt under the conditions of stress, heat and the like. The gel temperature is the temperature at which the resin particles begin to swell by absorbing the plasticizer during heating until the plasticizer continuously penetrates into the resin particles until the plasticizer is completely absorbed and the sol loses fluidity, at which time the plastisol assumes a gel structure without mechanical strength.
It follows that the gel temperature plays an important role in the application and processing of paste resins. For example, in the production of coated cloth and artificial leather by a coating method, when multi-layer coating and priming are carried out, the gelation temperature is required to be reached, plasticization is not required, and the dry state is required to be kept, so that the subsequent operation is prevented from being influenced by roll sticking when passing through rollers such as a guide roll, a calender roll, a cooling roll and the like; in addition, gel re-plasticizing process is required in the production of dipping gloves, rotary molded parts, slush molded shoes and boots, etc.
Since the gel temperature measurement has not been an ideal method, the measurement time is often expressed in practice as the time required for the viscosity of the plastisol to reach a set value, or as the time required for stirring while heating until the paste stringy does not adhere to the stirring rod. However, both methods indirectly characterize the gel speed and the gel temperature by time, and neither method is tested on the gel temperature.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the gel temperature testing method for the polyvinyl chloride paste resin, and the method has the advantages of accurate test, simple operation and small system error.
In order to solve the technical problems, the invention adopts the following technical scheme:
a gel temperature test method for a polyvinyl chloride paste resin, comprising:
testing the viscosity of the polyvinyl chloride paste resin under the heating at a fixed heating rate to obtain a corresponding viscosity-temperature curve chart;
determining tangents to two steeply changing curve segments on the viscosity-temperature profile;
the temperature corresponding to the intersection of the two tangent lines was determined as the gel temperature of the polyvinyl chloride paste resin.
Further, when the viscosity of the polyvinyl chloride paste resin under heating at a fixed temperature rising rate is tested, the method comprises the following steps:
grinding, stirring and defoaming the polyvinyl chloride paste resin and the plasticizer in a vacuum defoaming machine to obtain uniformly dispersed paste;
placing the paste in a constant-temperature water bath at 25 ℃ and keeping the temperature for 1-2 h;
the viscosity of the paste was tested by a rotary rheometer under heating at a fixed ramp rate.
Further, the mass ratio between the polyvinyl chloride paste resin and the plasticizer is 100: 60.
Further, the plasticizer is dioctyl phthalate.
Further, when the polyvinyl chloride paste resin is tested by the rotational rheometer, the rotational rheometer is set to a flat shear mode, a temperature sweep mode and a single-frequency vibration mode.
Further, the diameter of the flat plate in the flat plate shearing is set to 35mm, the plate gap is set to 0.5mm, and the vibration frequency in the single frequency vibration mode is set to 1 Hz.
Further, the deformation of the paste by the rotational rheometer was controlled to be 1%.
Further, when the viscosity of the polyvinyl chloride paste resin was measured under heating at a fixed temperature rising rate, the fixed temperature rising rate was 4 to 6 ℃/mi.
Further, when the viscosity of the polyvinyl chloride paste resin was measured under heating at a constant temperature rising rate, the temperature variation ranged from 25 to 130 ℃.
Further, the polyvinyl chloride paste resin is one of PSH-10 resin powder, PSM-31 resin powder, PSL-31 resin powder and PCMA-12 resin powder.
The invention provides a method for testing the gel temperature of polyvinyl chloride paste resin, which determines the tangent lines of two curve segments with sharp changes on a viscosity-temperature curve chart corresponding to the polyvinyl chloride paste resin under the heating at a fixed heating rate, and then determines the temperature corresponding to the intersection point of the two tangent lines as the gel temperature of the polyvinyl chloride paste resin. The polyvinyl chloride paste resin gel temperature testing method provided by the invention has the advantages of simple operation, reliable result, stable testing process, elimination of human factor influence and the like, and further provides a convenient and credible testing means for research and development departments and paste resin downstream manufacturers.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a graph of viscosity-temperature curves of a polyvinyl chloride paste resin according to an exemplary embodiment 1 of the present invention;
FIG. 2 is a graph of viscosity-temperature curves of polyvinyl chloride paste resin according to exemplary embodiment 2 of the present invention;
FIG. 3 is a graph of viscosity-temperature curves of polyvinyl chloride paste resin according to exemplary embodiment 3 of the present invention;
fig. 4 is a viscosity-temperature graph of a polyvinyl chloride paste resin according to exemplary embodiment 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A gel temperature test method for polyvinyl chloride paste resin, comprising the steps of:
s100, testing the viscosity of the polyvinyl chloride paste resin under heating at a fixed heating rate to obtain a corresponding viscosity-temperature curve chart;
s200, determining tangent lines of two curve segments with sharp changes on a viscosity-temperature curve graph;
s300, determining the temperature corresponding to the intersection point of the two tangent lines as the gel temperature of the polyvinyl chloride paste resin;
wherein the polyvinyl chloride paste resin is PSH-10 resin powder.
The gel temperature of the polyvinyl chloride paste resin is determined by determining tangent lines of two curve segments which are subjected to sharp changes on a viscosity-temperature curve graph corresponding to the polyvinyl chloride paste resin under the heating at a fixed heating rate, and then determining the temperature corresponding to the intersection point of the two tangent lines. The polyvinyl chloride paste resin gel temperature testing method provided by the invention has the advantages of simple operation, reliable result, stable testing process, elimination of human factor influence and the like, and further provides a convenient and credible testing means for research and development departments and paste resin downstream manufacturers.
In a preferred embodiment, the viscosity of the polyvinyl chloride paste resin when heated at a constant temperature rise rate is measured, and the method comprises:
s101, grinding, stirring and defoaming the polyvinyl chloride paste resin and the plasticizer in a vacuum defoaming machine to obtain uniformly dispersed paste;
s102, placing the paste in a constant-temperature water bath at 25 ℃ and keeping the temperature for 1-2 h;
s103, testing the viscosity of the paste under heating at a fixed heating rate by a rotary rheometer.
The vacuum defoaming machine used in this example was a japanese rock-type stirring and kneading machine, and the stirring and defoaming time was 20 min; the constant temperature water bath is low temperature constant temperature water bath HN-50 DC.
Preferably, the mass ratio between the polyvinyl chloride paste resin and the plasticizer is 100: 60. In this example, 50g of the polyvinyl chloride paste resin and 30g of the plasticizer were weighed.
Further, the plasticizer is dioctyl phthalate. The plasticizer is preferably dioctyl phthalate because dioctyl phthalate has good mixing properties and high plasticizing efficiency, and is also low in volatility.
Preferably, the rotational rheometer is set to a flat shear, temperature sweep, and single frequency vibration mode when the polyvinyl chloride paste resin is tested by the rotational rheometer. Wherein the rotational rheometer is HAAKE MARS 40.
Wherein the diameter of the flat plate in the flat plate shearing is set to 35mm, the plate gap is set to 0.5mm, and the vibration frequency in the single-frequency vibration mode is set to 1 Hz.
More specifically, the deformation of the paste by the rotational rheometer is controlled to be 1%.
In a preferred embodiment, the fixed temperature rise rate is 4 to 6 ℃/mi n when the viscosity of the polyvinyl chloride paste resin is measured under heating at the fixed temperature rise rate. Preferably, the fixed temperature rise rate in this embodiment is 5 ℃/min.
Preferably, the temperature variation range is 25 to 130 ℃ when the viscosity of the polyvinyl chloride paste resin is measured under heating at a fixed temperature rising rate.
Fig. 1 is a viscosity-temperature curve diagram of PSH-10 resin powder, and the gel temperature of PSH-10 resin powder is 93.4 ℃ as determined by the tangent line of two curve segments with sharp changes on the viscosity-temperature curve diagram.
Example 2
This example differs from the gel temperature test method for a polyvinyl chloride paste resin in example 1 in that: the polyvinyl chloride paste resin in this example was PSM-31 resin powder.
Fig. 2 is a viscosity-temperature graph of the PSM-31 resin powder, and it can be determined that the gel temperature of the PSM-31 resin powder is 87.3 ℃ by determining tangents to two curve segments with sharp changes on the viscosity-temperature graph.
Example 3
This example differs from the gel temperature test method for a polyvinyl chloride paste resin in example 1 in that: the polyvinyl chloride paste resin in this example was PSL-31 resin powder.
Fig. 3 is a viscosity-temperature graph of the PSL-31 resin powder, and the gel temperature of the PSL-31 resin powder can be found to be 83.9 ℃ by determining tangents to two curve segments with sharp changes on the viscosity-temperature graph.
Example 4
This example differs from the gel temperature test method for a polyvinyl chloride paste resin in example 1 in that: the polyvinyl chloride paste resin in this example was PCMA-12 resin powder.
FIG. 4 is a graph showing the viscosity-temperature curve of the PCMA-12 resin powder, and the gel temperature of the PCMA-12 resin powder was 77.4 ℃ as determined by cutting lines of two sharply changed curve segments on the viscosity-temperature curve.
Table 1 is a table of gel temperature data of the polyvinyl chloride paste resins of examples 1 to 4
From the test results, the gel temperature of each brand of paste resin tested basically conforms to the theoretical and practical conditions.
The test principle of the invention is as follows: since the gel temperature of the polyvinyl chloride paste resin is the temperature at which the network structure between polyvinyl chloride chains begins to form, rheological performance parameters such as the viscosity of the sol, the storage modulus G ', the loss modulus G ″ and the like all change significantly at this time, the viscosity increases sharply, a smaller G "means a weaker viscosity, and a larger G' means an increased elasticity. The gel temperature obtained by the invention is the temperature when the network structure between polyvinyl chloride chains begins to form, at the moment, rheological performance parameters of the sol such as viscosity, storage modulus G ', loss modulus G' and the like are remarkably changed, the viscosity is increased sharply, G 'is decreased, the viscosity is decreased, and G' is increased, so the elasticity is increased. Therefore, the calculation and analysis of these characteristic parameters can determine the gelation temperature, which means that the plastisol of the polyvinyl chloride paste resin changes from a "sticky" liquid into a solid with "elasticity", and plays an important role in the design of the processing technology. The invention also provides a gel temperature test method which can test the gel temperature of different paste resin pastes and can test pastes prepared by polyvinyl chloride paste resin and plasticizer with different mass ratios according to the purpose of a tester and the processing condition of a producer.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for testing gel temperature of a polyvinyl chloride paste resin, comprising:
testing the viscosity of the polyvinyl chloride paste resin under the heating at a fixed heating rate to obtain a corresponding viscosity-temperature curve chart;
determining tangents to two steeply changing curve segments on the viscosity-temperature profile;
the temperature corresponding to the intersection of the two tangent lines was determined as the gel temperature of the polyvinyl chloride paste resin.
2. The method for testing gel temperature of polyvinyl chloride paste resin according to claim 1, wherein the method for testing viscosity of polyvinyl chloride paste resin under heating at a fixed temperature rising rate comprises:
grinding, stirring and defoaming the polyvinyl chloride paste resin and the plasticizer in a vacuum defoaming machine to obtain uniformly dispersed paste;
placing the paste in a constant-temperature water bath at 25 ℃ and keeping the temperature for 1-2 h;
the viscosity of the paste was tested by a rotary rheometer under heating at a fixed ramp rate.
3. The gelation temperature test method for polyvinyl chloride paste resin according to claim 2, wherein the mass ratio between the polyvinyl chloride paste resin and the plasticizer is 100: 60.
4. The gel temperature test method for polyvinyl chloride paste resin according to claim 3, wherein the plasticizer is dioctyl phthalate.
5. The method for testing gel temperature of polyvinyl chloride paste resin according to claim 2, wherein the rotational rheometer is set to a flat shear, a temperature sweep and a single frequency vibration mode when the polyvinyl chloride paste resin is tested by the rotational rheometer.
6. The gelation temperature test method for polyvinyl chloride paste resin according to claim 5, wherein the plate diameter in plate shearing is set to 35mm, the plate gap is set to 0.5mm, and the vibration frequency in the mono-frequency vibration mode is set to 1 Hz.
7. The method for testing the gelation temperature of polyvinyl chloride paste resin according to claim 6, wherein the deformation of said paste by said rotational rheometer is controlled to 1%.
8. The method for testing gel temperature of polyvinyl chloride paste resin according to any one of claims 1 to 7, wherein the fixed ramp rate is 4-6 ℃/min when the viscosity of polyvinyl chloride paste resin is tested under heating at the fixed ramp rate.
9. The method for testing gel temperature of polyvinyl chloride paste resin according to claim 8, wherein the temperature variation range is 25-130 ℃ when the viscosity of polyvinyl chloride paste resin is tested under heating at a constant temperature rising rate.
10. The gelation temperature test method for polyvinyl chloride paste resin according to any one of claims 1 to 9, wherein said polyvinyl chloride paste resin is one of PSH-10 resin powder, PSM-31 resin powder, PSL-31 resin powder and PCMA-12 resin powder.
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| CN202011078879.3A CN112362532A (en) | 2020-10-10 | 2020-10-10 | Gel temperature testing method for polyvinyl chloride paste resin |
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| CN202011078879.3A CN112362532A (en) | 2020-10-10 | 2020-10-10 | Gel temperature testing method for polyvinyl chloride paste resin |
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