CN113970545B - Method for detecting performance of heat stabilizer in PVC product processing process - Google Patents
Method for detecting performance of heat stabilizer in PVC product processing process Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 66
- 238000012545 processing Methods 0.000 title claims abstract description 38
- 230000008569 process Effects 0.000 title claims abstract description 32
- 239000012760 heat stabilizer Substances 0.000 title claims abstract description 27
- 238000012360 testing method Methods 0.000 claims abstract description 61
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 claims abstract description 48
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000005070 sampling Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000010008 shearing Methods 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 10
- 230000008859 change Effects 0.000 claims description 18
- 230000014759 maintenance of location Effects 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 11
- 239000000945 filler Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000011056 performance test Methods 0.000 abstract description 4
- 238000010094 polymer processing Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 96
- 229920000915 polyvinyl chloride Polymers 0.000 description 65
- FCSHMCFRCYZTRQ-UHFFFAOYSA-N N,N'-diphenylthiourea Chemical compound C=1C=CC=CC=1NC(=S)NC1=CC=CC=C1 FCSHMCFRCYZTRQ-UHFFFAOYSA-N 0.000 description 5
- 239000012496 blank sample Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229930184510 Mallotus Natural products 0.000 description 1
- 241001060384 Mallotus <angiosperm> Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 description 1
- 238000007033 dehydrochlorination reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N2021/786—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour with auxiliary heating for reaction
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Abstract
The invention belongs to the technical field of polymer processing, and particularly relates to a method for detecting the performance of a heat stabilizer in the processing process of PVC products. According to the method, an actual production and processing process is simulated by means of a small single-screw extruder, a uniformly mixed PVC compound is poured into a hopper of the small single-screw extruder, and the PVC heat stabilizer performance is evaluated by means of screw conveying of the extruder, extrusion, barrel heating and melting, screw shearing and mixing, machine head extrusion sampling, sample taking, sample strip color difference testing of different residence time in the extruder and congo red test color changing time testing. The invention fills the blank of the performance test method of the heat stabilizer in the processing process of the PVC product, and has the advantages of simple operation, high accuracy of experimental results and good repeatability.
Description
Technical Field
The invention belongs to the technical field of polymer processing, and particularly relates to a method for detecting the performance of a heat stabilizer in the processing process of PVC products.
Background
The PVC heat stabilizer is an indispensable processing aid in the PVC product production and processing process, and the performance determines the heat stability in the PVC product processing process. Extrusion and injection molding are the most common production and processing modes of PVC products, and the principle is as follows: under the action of external transmission power, the PVC compound is conveyed by a screw, extruded, heated and melted by a machine barrel, sheared and mixed by the screw, and extruded by a machine head or injection molded by a mold. Because the extrusion and injection molding processes are accompanied by the characteristics of high temperature, high pressure and high shearing force, in order to ensure smooth production and processing of PVC products, the PVC heat stabilizer in the raw materials is required to have certain processing heat stability.
The existing laboratory method for verifying the performance of the PVC heat stabilizer comprises a static method and a dynamic method, wherein the static method evaluates the heat stability performance through the discoloration and dehydrochlorination of the PVC product under the high temperature condition, the dynamic method simulates the processing process of the PVC compound in actual production by means of a torque rheometer and a double-roller machine, and evaluates the dynamic heat stability through the color change of the PVC material, but in the actual production process, the extrusion and injection molding processes are complicated, the time is long, the characteristics of high temperature, high pressure and high shearing force are accompanied, and the temperature difference of each section of the heating machine barrel is large, so that the difference between the heat stability in the processing process of the finished product and the laboratory test result is large.
Disclosure of Invention
The invention solves the technical problems that: in order to solve the technical problems, the invention provides a method for detecting the performance of a heat stabilizer in the processing process of a PVC product, which simulates the actual production and processing process by means of a small single-screw extruder, and the method is characterized in that a uniformly mixed PVC compound is poured into a hopper of the small single-screw extruder, conveyed by a screw of the extruder, extruded, heated and melted by a machine barrel, sheared and mixed by the screw, extruded and sampled by a machine head, and the color difference of a sample strip with different residence time in the extruder and the congo red test color change time are tested to evaluate the performance of the PVC heat stabilizer. The method fills the blank of the performance test method of the heat stabilizer in the processing process of the PVC product, and has the advantages of simple operation, high accuracy of experimental results and good repeatability.
The specific technical scheme of the invention is as follows:
the invention provides a method for detecting the performance of a heat stabilizer in the processing process of PVC products, which comprises the following steps:
(1) And (3) batching: weighing PVC resin powder, a heat stabilizer and other raw materials according to the formula proportion;
(2) Mixing: mixing and stirring the weighed PVC resin powder, filler, processing aid and heat stabilizer by a high-speed mixer, controlling the mixing temperature of the high-speed mixer by combining a PLC heating and cooling program, and taking out the PVC mixture from the high-speed mixer after the mixing is completed;
(3) Starting the extruder: opening an extruder power supply, starting an extruder control program, opening an extruder barrel heating switch, and setting the temperature of each heating section of the extruder barrel to be: the method comprises the steps of starting an extruder screw motor after the extruder barrel is heated, turning on the extruder screw motor to 40r/min, pouring PVC mixture into a feed hopper of an extruder, and preparing for extrusion sampling after the extruder screw torque is stable;
(4) Sampling for the first time: after the extruder head discharges evenly, cutting out extruded sample strips with the length of 10cm, flattening the extruded sample strips on an air pressure slicer, placing the extruded sample strips and cooling the extruded sample strips to room temperature, reserving the extruded sample strips as blank groups, and marking serial numbers;
(5) Sampling for the nth time: after the last sampling is finished, the screw motor of the extruder is closed, the extruded spline part is cut off, the extruded spline part is discarded, and the PVC material which enters the extruder stays in the heating cylinder of the extruder for t n After the time, starting a screw motor of the extruder, cutting out a 50-60 cm section part of an extruded spline, flattening on an air pressure slicer, placing and cooling to room temperature, and marking a serial number;
(6) Congo red test: testing stability of each sampled sample by using Congo red method for multiple times, and recording average value of color change time of Congo red test paper;
(7) And (3) color difference meter analysis: observing and measuring the color of each sample by means of a color difference meter, recording measurement data L, a, b and YI, and calculating delta E values of each spline and the blank group spline, wherein
(8) Drawing analysis: and drawing a retention time-Congo red color change time line graph and a retention time-delta E value line graph, analyzing experimental data, and judging the stability performance of the PVC heat stabilizer in the processing process.
In the step (1), the other raw materials include a filler and a processing aid. The filler is one or more of calcium powder filler and titanium dioxide filler, and the processing aid is one or more of processing aid 10F and processing aid CPE.
In the step (2), the mixing and stirring process by a high-speed mixer is as follows: firstly, adjusting the rotating speed to 600r/min, stirring for 5min, then adjusting the rotating speed to 1500r/min, stirring until the temperature of the PVC mixture reaches 60 ℃, adjusting the rotating speed to 3000r/min, and reducing the rotating speed to zero after the temperature of the PVC mixture in the mixer is raised to 90 ℃; then, the PLC temperature raising-lowering program is opened, and the program is set as follows: firstly, increasing the rotating speed to 3000r/min, introducing condensed water after detecting that the temperature reaches 120 ℃, reducing the rotating speed to 600r/min, and reducing the rotating speed to zero after detecting that the temperature is reduced to 60 ℃;
in the step (3), preparation work before extrusion is needed, namely, before the PVC mixture is poured into a feed hopper of the extruder, the extruder is cleaned, and the method specifically comprises the following steps: and pouring a proper amount of clear machine material into a feeding hopper of the extruder, and cleaning the screw of the extruder until the cleaning of the screw is completed.
In the step (5), N is an integer of 1 or more, t n Respectively 5min, 10min and 20min.
In the step (6), the congo red method test specifically comprises the following steps: opening a heating power button of a Congo red thermostat, keeping the temperature of a standby device constant for 30min after the temperature of the standby device rises to 200 ℃, respectively shearing each sample into small test tubes of Congo red glass, shearing 3 parts of each sample, marking a sequence number, shearing the Congo red test paper with the length of 20mm and the width of 3mm, hanging the cut congo red test paper at the upper end of the glass tube after being folded in half, sequentially placing the small test tubes into a Congo red tester for testing, starting timing, gradually changing the red Congo red test paper into blue, recording the time when the test paper changes the blue, and calculating the color change time average value of the test paper.
According to the method for detecting the performance of the heat stabilizer in the processing process of the PVC product, the residence time of the sampled PVC mixture in the extruder is different, and the relation between the processing time of the PVC product and the stability of the heat stabilizer is determined in sequence. Two ways of determining the steady state are used, one is the common congo red method and the other is the color difference analysis. The color difference analysis tests a plurality of change values, and in order to comprehensively reflect the stable state, the geometric average value of a plurality of indexes is taken so as to more accurately reflect the comprehensive change of the stable state.
The invention has the following beneficial effects:
1. the problem that the performance of the heat stabilizer in the processing process of the PVC product cannot be directly tested is effectively solved, and the performance test of the heat stabilizer in the processing process is realized by simulating the actual production process.
2. The purpose of high accuracy and good repeatability of the thermal stability test result in the PVC heat stabilizer processing process is achieved.
3. The experimental method is simple and effective.
Drawings
FIG. 1 is a plot of residence time versus Congo red time for example 1 of the present invention;
FIG. 2 is a plot of residence time versus delta E for example 1 of the present invention.
Detailed Description
In order to more clearly illustrate the technical solutions of the present invention, it will be apparent that the embodiments described below are only some embodiments of the present invention, and other examples can be obtained according to these embodiments without inventive effort for a person skilled in the art.
Example 1
The apparatus employed in this embodiment includes: plasmec brand turbine mixer (TRL-10/FV/R), dr.colin single screw extruder, model E30M, hychtech brand air pressure slicer, model RS-8021B, liebish Congo red thermostat, model S-210,Mettler Toleto analytical balance, model MS 204S, kenicam Neodler color difference meter, model CM-5, stainless steel small medicine spoon, PE material bag, congo red test paper.
The raw materials in this embodiment include: zhongtai chemical resin powder, brands SG5, 10F (Baerlocher), chloride process titanium dioxide powder (Mallotus You Ke), calcium carbonate powder (Anhua), CPE (Shandong subsp.), PVC heat stabilizer-A (Baerlocher brand: R9374R), PVC heat stabilizer-B (Baerlocher brand: R9375R), PVC heat stabilizer-C (Baerlocher brand: R618R).
The method for verifying the performance test of the heat stabilizer in the processing process of the PVC product in the embodiment comprises the following steps:
(1) Sample preparation
Preparing three dry and clean PE material bags, respectively marking 1, 2 and 3, accurately weighing samples 1, 2 and 3 into PE material bags with corresponding serial numbers according to the formula shown in the following table 1, pouring each prepared PVC compound into a mixing pot of a dry and clean small high-speed mixer, covering a pot cover of the high-speed mixer, locking a locking device, starting a main power supply of the small high-speed mixer, opening a motor power supply button, adjusting a motor rotating speed knob to 600r/min, stirring for 5min, adjusting the motor rotating speed knob to 1500r/min after the PVC compound is uniformly stirred, adjusting the motor rotating speed knob to 3000r/min after the temperature of the PVC compound in the mixing pot reaches 60 ℃, reducing the motor rotating speed to zero after the PVC compound in the mixing pot is continuously heated to 90 ℃, starting a PLC heating-cooling program, and setting the PLC heating-cooling program of the small high-speed mixer as follows: the rotating speed is 3000r/min, the condensed water is introduced into the mixing pot after the temperature reaches 120 ℃, the rotating speed is reduced to 600r/min, the discharging valve is opened to discharge after the temperature is reduced to 60 ℃, after the heating-cooling procedure is finished, the prepared PVC compound is sequentially filled into PE material bags with serial numbers of 1, 2 and 3, a PVC compound sample 1 containing a PVC heat stabilizer-A, a PVC compound sample 2 containing a PVC heat stabilizer-B and a PVC compound sample 3 containing a PVC heat stabilizer-C are sequentially prepared.
Table 1 sample formulation in example 1
(2) Preparation of samples
Opening a general power button of the small extruder, starting control software of a host computer, opening a heating button of a machine barrel of the extruder, and setting the temperature of each heating section of the machine barrel of the small extruder to be: the method comprises the steps of starting an extruder screw motor after the extruder barrel is heated, turning on the extruder screw motor to 40r/min, pouring a proper amount of clear material into a feed hopper of a small extruder, cleaning the extruder screw, pouring a PVC compound sample 1 containing a PVC heat stabilizer-A into the feed hopper of the extruder after the screw is cleaned, and starting extrusion sampling after the torque of the extruder screw is displayed steadily.
Sampling for the first time: after the extruder head discharges evenly, cutting out extruded sample strips with the length of 10cm, flattening the extruded sample strips on an air pressure slicer, placing and cooling the extruded sample strips to room temperature, and marking the extruded sample strips with the serial numbers of 1-1.
Sampling for the second time: after the first sampling is finished, the screw motor of the extruder is closed, the extruded sample strip part is cut off, the extruded sample strip part is discarded, after the PVC material which enters the extruder stays in the heating cylinder of the extruder for 5min, the screw motor of the extruder is started, the extruded sample strip part with the length of 50-60 cm is cut off, the extruded sample strip part is flattened on the air pressure slicer, and the extruded sample strip part is placed and cooled to the room temperature, and the sequence number of the extruded sample strip part is marked as sample strip 1-2.
Third sampling: after the second sampling is finished, the screw motor of the extruder is closed, the extruded sample strip part is cut off, the extruded sample strip part is discarded, after the PVC material which enters the extruder stays in the heating cylinder of the extruder for 10min, the screw motor of the extruder is started, the extruded sample strip part with the length of 50-60 cm is cut off, the extruded sample strip part is flattened on an air pressure slicer, and is placed and cooled to the room temperature, and the sequence number of the extruded sample strip part is marked as sample strip 1-3.
Fourth sampling: after the third sampling is finished, the screw motor of the extruder is closed, the extruded sample strip part is cut off, the extruded sample strip part is discarded, after the PVC material which enters the extruder stays in the heating cylinder of the extruder for 20min, the screw motor of the extruder is started, the extruded sample strip part with the length of 50-60 cm is cut off, the extruded sample strip part is flattened on an air pressure slicer, and is placed and cooled to the room temperature, and the sequence number of the extruded sample strip part is 1-4.
According to the operation, blank sample bars 2-1, sample bars 2-2, sample bars 2-3, sample bars 2-4 of the PVC compound sample 2, sample bar blank 3-1, sample bars 3-2, sample bars 3-3 and sample bars 3-4 of the PVC compound sample 3 are sequentially prepared.
(3) Congo red test
Opening a heating power button of a Congo red thermostat, keeping the temperature of the standby device constant for 30min after the temperature of the standby device is increased to 200 ℃, respectively shearing a blank sample 1-1, a sample 1-2, a sample 1-3 and a sample 1-4 which are prepared from a sample 1 into small test tubes of Congo red glass, weighing 3 parts of each sample, marking a serial number, shearing a Congo red test paper with the length of 20mm and the width of 3mm, hanging the cut congo red test paper on the upper end of the glass tube after the cut Congo red test paper is folded in half, sequentially placing the small test tubes into a Congo red tester for testing, starting timing, recording the time when the red Congo red test paper becomes blue, calculating the test paper color change time average value, and recording data as shown in the following table 2.
Table 2 example 1 congo red test time data for each spline of sample 1
And cutting the sample strips 2-1, 2-2, 2-3 and 2-4 prepared by the sample 2 into small test tubes of Congo red glass, weighing 3 parts of each sample, marking a sequence number, cutting the small test tubes of Congo red with the length of 20mm and the width of 3mm, doubling the test tubes, hanging the test tubes on the upper ends of the glass tubes, sequentially placing the small test tubes into a Congo red tester for testing, starting timing, gradually changing the red Congo red test paper into blue, recording the time for changing the test paper, calculating the time average value for changing the test paper, and recording the data as shown in the following table 3.
TABLE 3 Congo red test time data for each of sample 2 strips of example 1
And respectively shearing a blank sample strip 3-1, a sample strip 3-2, a sample strip 3-3 and a sample strip 3-4 which are prepared from a sample 3 into small congo red test tubes of 0.05+/-0.005 g, weighing 3 parts of each sample, marking with a sequence number, shearing the congo red test paper with the length of 20mm and the width of 3mm, doubling the test paper, hanging the test paper at the upper end of the glass tube, sequentially placing the small test tubes into a congo red tester for testing, starting timing, gradually changing the red congo red test paper into blue, recording the time for changing the test paper, calculating the time average value for changing the test paper, and recording the data as shown in the following table 4.
Table 4 congo red test time data for each spline of example 1 sample 3
(4) Color measurement
Starting the color difference meter, adjusting the measurement type of the color difference meter to be reflection measurement, measuring the aperture to be 8mm, measuring the test aperture to be SCI, performing zero correction and whiteboard correction, respectively placing spline blank splines 1-1, spline 1-2, spline 1-3 and spline 1-4 prepared by the sample 1 on the color difference meter for measurement, and recording measurement data L, a, b, YI and delta E as shown in the following table 5.
Table 5 example 1 sample 1 produced spline color measurement values
The blank bars 2-1, 2-2, 2-3 and 2-4 prepared by the sample 2 are respectively measured on a color difference meter, and measured data L, a, b, YI and delta E are recorded as shown in the following table 6.
TABLE 6 sample 2 preparation of sample color measurement values
The blank bars 3-1, 3-2, 3-3, and 3-4 prepared by sample 3 were measured on a color difference meter, and the measured data L, a, b, YI, and Δe were recorded as shown in table 7 below.
Table 7 sample 3 example 1 sample color measurement values
(5) The residence time-Congo red color change time line diagram is shown in figure 1
(5) The residence time-delta E value time line diagram is shown in FIG. 2
(7) Analysis of experimental data
As can be seen from the above-described figure 1 example 1 residence time-Congo red time line graph, when the residence time of the sample in the extruder is zero, the Congo red times of sample 1-1, sample 2-1 and sample 3-1 of the three groups of samples are respectively 20min, 21min and 22min, and the Congo red experimental results are not greatly different, which means that the thermal stability performance of three PVC heat stabilizers is close, but as the experiment proceeds, when the residence time of the sample in the extruder reaches 20min, the Congo time of sample 1-4 of sample one suddenly drops to 1min, sample 1-4 is almost decomposed, the thermal stability performance is completely lost, which means that the processing thermal stability performance of PVC heat stabilizer-A is poor, and the Congo red times of sample 2-4 of sample two and sample 3-4 of sample three are respectively 6min and 8min, the sample still has a certain thermal stability performance, which means that PVC heat stabilizer-B, PVC-C has a good processing thermal stability performance.
Analysis of the example 1 retention time- ΔE value line graph of FIG. 2 above, when the retention time of the sample in the extruder was 5min, 10min, and 20min, respectively, sample one, sample 1-2, sample 1-3, and sample 1-4, respectively, were compared with sample 1-1, with a large change in ΔE value, which indicated a large change in color of the sample, indicating poor processing heat stability of PVC heat stabilizer-A, and sample two and sample three, which indicated a small change in ΔE value, indicating a small change in color of the sample, indicating that the sample still had some heat stability, indicating good processing heat stability of PVC heat stabilizer-B, PVC heat stabilizer-C.
In addition, we can also see from the YI of the extruded bars for each sample in tables 5, 6, and 7 that during the experiment, PVC heat stabilizer-a had better initial color retention, but poor long-term color retention, PVC heat stabilizer-B had poor initial color retention, but good long-term color retention, and PVC heat stabilizer-C had both excellent initial color retention and long-term color retention.
(8) Determination result
The PVC heat stabilizer-A has poor processing heat stability, is easy to decompose and change color in the processing process, is suitable for the product process with simple processing process and short time, has good processing heat stability, is difficult to decompose in the processing process, but is suitable for the product process with low color requirement due to poor initial color retention performance, and the PVC heat stabilizer-C has excellent processing heat stability, is difficult to decompose and change color in the processing process, and is suitable for the product process with complex processing process, long time and high color requirement.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A method for detecting the performance of a heat stabilizer in the processing of a PVC article, comprising the steps of:
(1) And (3) batching: weighing PVC resin powder, a heat stabilizer and other raw materials according to the formula proportion;
(2) Mixing: mixing and stirring the weighed PVC resin powder, filler, processing aid and heat stabilizer by a high-speed mixer, controlling the mixing temperature of the high-speed mixer by combining a PLC heating and cooling program, and taking out the PVC mixture from the high-speed mixer after the mixing is completed;
(3) Starting the extruder: opening an extruder power supply, starting an extruder control program, opening an extruder barrel heating switch, and setting the temperature of each heating section of the extruder barrel to be: the method comprises the steps of starting an extruder screw motor after the extruder barrel is heated, turning on the extruder screw motor to 40r/min, pouring PVC mixture into a feed hopper of an extruder, and preparing for extrusion sampling after the extruder screw torque is stable;
(4) Sampling for the first time: after the extruder head discharges evenly, cutting out extruded sample strips with the length of 10cm, flattening the extruded sample strips on an air pressure slicer, placing the extruded sample strips and cooling the extruded sample strips to room temperature, reserving the extruded sample strips as blank groups, and marking serial numbers;
(5) Sampling for the nth time: after the last sampling is finished, the screw motor of the extruder is closed, the extruded spline part is cut off, the extruded spline part is discarded, and the PVC material which enters the extruder stays in the heating cylinder of the extruder for t n After the time, starting a screw motor of the extruder, cutting out a 50-60 cm section part of an extruded spline, flattening on an air pressure slicer, placing and cooling to room temperature, and marking a serial number;
(6) Congo red test: testing stability of each sampled sample by using Congo red method for multiple times, and recording average value of color change time of Congo red test paper;
(7) And (3) color difference meter analysis: observing and measuring the color of each sample by means of a color difference meter, recording measurement data L, a, b and YI, and calculating delta E values of each spline and the blank group spline, wherein
(8) Drawing analysis: and drawing a retention time-Congo red color change time line graph and a retention time-delta E value line graph, analyzing experimental data, and judging the stability performance of the PVC heat stabilizer in the processing process.
2. The method of claim 1, wherein in step (1), the other raw materials include a filler, a processing aid.
3. The method of claim 2, wherein the filler is one or more of a calcium powder filler and a titanium dioxide filler, and the processing aid is one or more of a processing aid 10F and a processing aid CPE.
4. The method according to claim 1, wherein in the step (2), the mixing and stirring process by a high-speed mixer is as follows: firstly, adjusting the rotating speed to 600r/min, stirring for 5min, then adjusting the rotating speed to 1500r/min, stirring until the temperature of the PVC mixture reaches 60 ℃, adjusting the rotating speed to 3000r/min, and reducing the rotating speed to zero after the temperature of the PVC mixture in the mixer is raised to 90 ℃; then, the PLC temperature raising-lowering program is opened, and the program is set as follows: firstly, the rotating speed is increased to 3000r/min, condensed water is led in after the temperature is detected to be 120 ℃, the rotating speed is reduced to 600r/min, and then, the rotating speed is reduced to zero after the temperature is detected to be reduced to 60 ℃.
5. The method according to claim 1, wherein in the step (3), preparation before extrusion is required, i.e. purging the extruder before the PVC mixture is poured into the extruder hopper, specifically comprising: and pouring a proper amount of clear machine material into a feeding hopper of the extruder, and cleaning the screw of the extruder until the cleaning of the screw is completed.
6. The method according to claim 1, wherein in the step (5), N is an integer of 1 or more, t n Respectively 5min, 10min and 20min.
7. The method of claim 1, wherein in the step (6), the congo red method test is performed by: opening a heating power button of a Congo red thermostat, keeping the temperature of a standby device constant for 30min after the temperature of the standby device rises to 200 ℃, respectively shearing each sample into small test tubes of Congo red glass, shearing 3 parts of each sample, marking a sequence number, shearing the Congo red test paper with the length of 20mm and the width of 3mm, hanging the cut congo red test paper at the upper end of the glass tube after being folded in half, sequentially placing the small test tubes into a Congo red tester for testing, starting timing, gradually changing the red Congo red test paper into blue, recording the time when the test paper changes the blue, and calculating the color change time average value of the test paper.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590029A (en) * | 2011-12-23 | 2012-07-18 | 湖北犇星化工有限责任公司 | Method for determining stability of PVC heat stabilizer |
| CN102731934A (en) * | 2012-07-10 | 2012-10-17 | 苏州宝津塑业有限公司 | Method for preparing PVC (Polyvinyl Chloride) heat stabilizing agent by using liquid-state Ca/Zn |
| WO2014044160A1 (en) * | 2012-09-21 | 2014-03-27 | 中国林业科学研究院林产化学工业研究所 | Method for preparing grease/turpentine base liquid calcium-zinc composite thermal stabilizer for pvc use |
| CN112444482A (en) * | 2020-11-26 | 2021-03-05 | 百尔罗赫塑料添加剂（江苏）有限公司 | Method for testing amine resistance of PVC heat stabilizer and application |
-
2021
- 2021-10-22 CN CN202111237353.XA patent/CN113970545B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590029A (en) * | 2011-12-23 | 2012-07-18 | 湖北犇星化工有限责任公司 | Method for determining stability of PVC heat stabilizer |
| CN102731934A (en) * | 2012-07-10 | 2012-10-17 | 苏州宝津塑业有限公司 | Method for preparing PVC (Polyvinyl Chloride) heat stabilizing agent by using liquid-state Ca/Zn |
| WO2014044160A1 (en) * | 2012-09-21 | 2014-03-27 | 中国林业科学研究院林产化学工业研究所 | Method for preparing grease/turpentine base liquid calcium-zinc composite thermal stabilizer for pvc use |
| CN112444482A (en) * | 2020-11-26 | 2021-03-05 | 百尔罗赫塑料添加剂（江苏）有限公司 | Method for testing amine resistance of PVC heat stabilizer and application |
Non-Patent Citations (1)
| Title |
|---|
| 于培静 ; 钱荧辉 ; 赵长森 ; .PVC树脂热稳定性的评价方法.聚氯乙烯.2020,(06),全文. * |
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