CN112646287A - PVC material and preparation method thereof - Google Patents

PVC material and preparation method thereof Download PDF

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CN112646287A
CN112646287A CN202011440571.9A CN202011440571A CN112646287A CN 112646287 A CN112646287 A CN 112646287A CN 202011440571 A CN202011440571 A CN 202011440571A CN 112646287 A CN112646287 A CN 112646287A
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pvc material
parts
stabilizer
plasticizer
pvc
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CN112646287B (en
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王超
薛晓琳
郑冉
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Changchun Jetty Automotive Parts Co Ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K3/2279—Oxides; Hydroxides of metals of antimony
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract

The invention provides a PVC material and a preparation method thereof. The PVC material comprises the following raw materials in parts by weight: 90-120 parts of PVC resin, 20-50 parts of plasticizer, 5-10 parts of stabilizer, 2-8 parts of flame retardant and 5-30 parts of filler; the plasticizer is trioctyl trimellitate, the filler is heavy calcium carbonate, and the stabilizer is a calcium-zinc stabilizer. The invention also provides a preparation method of the PVC material. The PVC material provided by the invention is environment-friendly and pollution-free, and has excellent high-temperature thermal stability and low-temperature impact resistance, the lowest low-temperature impact resistance temperature can reach-70 ℃, and the low-temperature impact resistance temperature is far better than the common level of the low-temperature impact resistance of the conventional PVC material.

Description

PVC material and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-performance, environment-friendly and low-temperature impact-resistant PVC material and a preparation method thereof.
Background
The PVC material opens up wide application prospect along with the development of the communication industry. The PVC material is a cable material prepared by taking polyvinyl chloride as a raw material, introducing various additives such as a plasticizer, a stabilizer, a flame retardant, a filler and the like, and performing processes such as blending, extrusion, granulation and the like, along with the continuous development of global marketization, the requirements on the performance of the cable are higher and higher, especially the cable can be entered only when the requirements of European Union ROHS and the like are met, the conventional cable material contains various additives, so that the production procedures are increased, the production cost is increased, the production efficiency is reduced, and the harmful additives can cause harm to the health of a producer.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a PVC material and a preparation method thereof. The PVC material has excellent high-temperature thermal stability and low-temperature impact resistance.
In order to achieve the purpose, the invention provides a PVC material which comprises the following raw materials in parts by weight: 90-120 parts of PVC resin, 20-50 parts of plasticizer, 5-10 parts of stabilizer, 2-8 parts of flame retardant and 5-30 parts of filler; the plasticizer is trioctyl trimellitate, the filler is heavy calcium carbonate, and the stabilizer is a calcium-zinc stabilizer.
In the PVC material, the PVC material can have good low-temperature impact resistance by selecting proper types of plasticizers, stabilizers and fillers and controlling the proportion of the components in the raw materials.
In the PVC material, the plasticizer and the stabilizer can improve the thermal stability of the PVC material, and the volatilization of the plasticizer can be slowed down by adding a proper amount of the stabilizer, so that the stability of the prepared PVC material is improved. The mass ratio of the plasticizer to the stabilizer can be controlled to be (4-6): (1-2), for example, the mass ratio of the plasticizer to the stabilizer can be controlled to 5: 1.
In the PVC material, the hardness and rheological property of the PVC material can be improved by controlling the effective ratio of the plasticizer to the filler, so that the low-temperature impact resistance of the PVC material is improved. In some embodiments, the mass ratio of the plasticizer to the filler may be controlled to be 8 (1-3).
In the PVC material, the plasticizer is preferably environment-friendly trimellitic acid trioctyl ester (TOTM), and the trioctyl trimellitate plasticizer is favorable for improving the low-temperature impact resistance of the PVC material. In addition, compared with the dioctyl phthalate plasticizer which is commonly used at present but does not meet the European Union standard, the trioctyl trimellitate adopted by the invention meets the European Union standard, is environment-friendly and pollution-free, and is beneficial to expanding the market and application range of PVC materials.
In the PVC material, the stabilizer plays a role in internal lubrication in the PVC material. The calcium zinc stabilizer is selected as the stabilizer, so that the low-temperature impact resistance of the PVC material can be improved, and the processability and the thermal stability of the PVC material can also be improved. The calcium zinc stabilizer generally comprises a zinc stearate calcium zinc stabilizer, and the mass content of zinc stearate in the zinc stearate calcium zinc stabilizer is at least 10%.
In the PVC material, the ground limestone is selected as the filler, so that the mechanical strength of the PVC material is enhanced, the material cost is reduced, and the low-temperature impact resistance of the PVC material is improved. The particle size of the heavy calcium carbonate can be 2500-3000 meshes (preferably 2800 meshes), and the mass ratio of calcium carbonate in the heavy calcium carbonate is generally more than 80%.
In the PVC material, under the condition that the dosage of other components of the raw material is kept unchanged, the dosage of the heavy calcium carbonate in the raw material is properly reduced, so that the low-temperature impact resistance of the PVC material can be further improved. For example, the raw materials of the PVC material may include: 90-120 parts of PVC resin, 20-50 parts (such as 30-50 parts) of plasticizer, 5-10 parts of stabilizer, 2-8 parts of flame retardant and 5 parts of filler.
In the above-mentioned PVC material, the average degree of polymerization of the PVC resin is preferably 1250-1350.
In the PVC material, the flame retardant is preferably Sb2O3The flame retardant comprises more than 82% of effective components by mass. In some embodiments, the flame retardant may be a flame retardant comprisingSb2O3The flame retardant of (1), the Sb2O3The mass ratio of (A) is generally more than 55%, and the flame retardant property is better.
The invention also provides a preparation method of the PVC material, which comprises the following steps:
step one, blending PVC resin and a plasticizer to obtain a first mixture;
adding a stabilizer, a flame retardant and a filler into the first mixture and blending to obtain a second mixture;
and step three, extruding and granulating the second mixture to obtain the PVC material.
In a specific embodiment of the present invention, in step one, the blending time is generally controlled to be 2min to 6min (e.g., 2min) to increase the compatibility between the PVC resin and the plasticizer.
In the second embodiment of the present invention, the blending time can be controlled to be 2min to 6min (for example, 2min) in order to increase the compatibility between the raw materials.
In the embodiment of the present invention, in the third step, the temperature of the extrusion can be controlled to 140-.
In a specific embodiment of the present invention, when the performance test of the PVC material is required, the third step may include cutting the PVC material after the compression molding into standard test bars.
In a specific embodiment of the present invention, the preparation method of the PVC material may include:
step one, blending PVC resin and the plasticizer for 2-6 min to obtain a first mixture;
adding a stabilizer, a flame retardant and a filler into the first mixture, and blending for 2-6 min to obtain a second mixture;
step three, putting the second mixture into a double-screw extruder, extruding and granulating at 140-180 ℃ (for example, 140 ℃, 170 ℃ and 180 ℃), and then obtaining the PVC material; and when the performance test is required, cutting the PVC material subjected to compression molding into a standard experimental sample strip.
The invention has the beneficial effects that:
according to the preparation method provided by the invention, the proper raw material components are selected, and the proportion of the components is controlled, so that the prepared PVC material has excellent high-temperature thermal stability and low-temperature impact resistance, the lowest low-temperature impact resistance temperature can reach-70 ℃, and the low-temperature impact resistance temperature is far better than that of the conventional PVC material.
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FIG. 1 is a photograph of the PVC material prepared in example 1.
FIG. 2 is a photograph of a PVC material prepared in comparative example 8.
FIG. 3 is a photograph of a PVC material prepared in comparative example 9.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
The manufacturer of the heavy calcium carbonate used in the following experiments is Guangzhou banyou powder Co.
Example 1
The embodiment provides a preparation method of a PVC material, which comprises the following steps:
1. weighing the following raw materials in parts by weight: 100 parts of PVC resin, 40 parts of TOTM plasticizer, 8 parts of calcium-zinc stabilizer, 5 parts of flame retardant and 5 parts of ground calcium carbonate.
2. Adding PVC resin and TOTM plasticizer into a high-speed mixer, blending for 2min, adding calcium zinc stabilizer, flame retardant and ground calcium carbonate, and blending for 2min to obtain a mixture;
3. and (3) placing the mixture into a double-screw extruder for granulation, wherein the extrusion temperature is 140-. The PVC material sample was cut with a standard cutter into standard test strips for testing and designated sample A.
Example 2
This example provides a process for the preparation of a PVC material which is essentially the same as the process of example 1 except that in this example 2 the weight parts of ground calcium carbonate are increased to 15 parts and the resulting PVC material is designated as sample B.
Example 3
This example provides a process for the preparation of a PVC material, which is essentially the same as the process of example 1, except that the weight fraction of ground calcium carbonate in this example was increased to 17 parts, and the resulting PVC material was designated as sample C.
Example 4
This example provides a process for the preparation of a PVC material, which is substantially the same as the process of example 1 except that the weight portion of ground calcium carbonate in this example is increased to 20 parts, and the resulting PVC material is designated as sample D.
Comparative example 1
This comparative example provides a process for the preparation of a PVC material that is substantially the same as the process of example 1 except that no filler is added to the comparative example and the resulting PVC material is designated sample E.
Comparative example 2
This comparative example provides a process for the preparation of a PVC material that is essentially the same as that of example 1 except that the comparative example employs 5 parts kaolin instead of 5 parts ground calcium carbonate as the filler, and the resulting PVC material is designated as sample F.
Comparative example 3
This comparative example provides a process for the preparation of a PVC material that is essentially the same as that of example 1 except that the comparative example uses 5 parts calcined kaolin instead of 5 parts ground calcium carbonate as the filler and the resulting PVC material is designated sample G.
Comparative example 4
This comparative example provides a process for the preparation of a PVC material that is essentially the same as the process of example 1 except that the comparative example uses 8 parts of barium zinc stabilizer instead of 8 parts of calcium zinc stabilizer as the stabilizer and the resulting PVC material is designated as sample H.
Comparative example 5
This comparative example provides a process for the preparation of a PVC material that is substantially the same as the process of example 4 except that the comparative example uses 8 parts of barium zinc stabilizer instead of 8 parts of calcium zinc stabilizer as the stabilizer and the resulting PVC material is designated as sample I.
Comparative example 6
This comparative example provides a process for the preparation of a PVC material that is substantially the same as that of example 2 except that the comparative example uses 40 parts epoxidized soybean oil instead of 40 parts TOTM as the plasticizer and the resulting PVC material is designated as sample J.
Comparative example 7
This comparative example provides a process for the preparation of a PVC material that is essentially the same as the process for the preparation of example 2, except that this comparative example replaces 40 parts of TOTM used in example 2 with 25 parts of TOTM and 15 parts of epoxidized soybean oil as plasticizers, and the resulting PVC material is designated as sample K.
The raw material compositions of the PVC stock used in examples 1-4 and comparative examples 1-7 are summarized in table 1.
All the PVC material samples are subjected to a thermal stability test and a low-temperature impact test. Wherein the thermal stability test is carried out according to the ISO 182-1 standard, and specifically comprises the following steps; 5mg of the granular sample was placed in a test tube to the lower level of the mark, a pH test paper 5mm wide was placed in the test tube, and the test tube was stoppered with cotton. Putting into a beaker filled with silicone oil with the temperature of 200 ℃, and starting timing to accurately divide. The time elapsed when the lower edge of the test paper begins to change color is the thermal stability time.
The low-temperature impact test was carried out according to the test method specified in GBT5470 "determination of brittle temperature by Plastic impact method", using the apparatus A of GBT 5470. The thermal stability and low temperature impact test results are summarized in table 1.
TABLE 1
Figure BDA0002830299990000051
Figure BDA0002830299990000061
The test results of table 1 were analyzed as follows:
(1) comparing the performance results of comparative examples 1-3 with those of example 1, it can be seen that the PVC material prepared by adding ground calcium carbonate as filler has excellent low-temperature impact resistance, and the low-temperature impact resistance temperature can reach-70 ℃, compared with the PVC material prepared by adding kaolin and calcined kaolin as filler and without filler; meanwhile, the thermal stability can be improved by adding the heavy calcium carbonate, so that the thermal stability of the PVC material can reach up to 310 ℃. This result demonstrates that the selection of a particular type of filler is beneficial for improving the thermal stability and low temperature impact resistance of the PVC material.
(2) Comparing the performance results of example 1 with comparative example 4, and example 4 with comparative example 5, it can be seen that the PVC material prepared with the calcium zinc stabilizer has a lower low temperature impact temperature compared to the barium zinc stabilizer. This result demonstrates that the selection of a particular class of calcium zinc stabilizers is beneficial for improving the low temperature impact resistance of the PVC material.
(3) Comparing the performance results of example 2, comparative example 6 and comparative example 7, it can be seen that the PVC material prepared using TOTM alone as the plasticizer has a lower low temperature impact temperature than the PVC material prepared using epoxidized soybean oil as the plasticizer and a mixture of epoxidized soybean oil and TOTM as the plasticizer. This result demonstrates that the selection of a specific type of plasticizer is advantageous for improving the low temperature impact resistance of the PVC material.
(4) As can be seen from the results of comparing the properties of examples 1 to 4, the low temperature impact resistance of the PVC material showed a significant decrease as the specific gravity of the ground calcium carbonate in the raw material was gradually increased from 5 parts to 20 parts. This result indicates that the proper reduction of the amount of ground calcium carbonate in the PVC raw material is beneficial for improving the thermal stability and low temperature impact resistance of the PVC material while maintaining the other basic properties (e.g., mechanical properties) of the PVC material without significant degradation.
The analysis shows that the preparation method of the PVC material provided by the invention can obtain excellent thermal stability and low temperature resistance by controlling the type selection and the dosage of each component in the raw materials, and the low temperature impact resistance temperature of the PVC material can reach-55 ℃ to-70 ℃, which is far better than the low temperature impact resistance of the conventional PVC material at present.
Comparative example 8
The comparative example provides a preparation method of a PVC material, wherein the PVC material comprises the following raw materials in parts by weight: 100 parts of PVC resin, 8 parts of calcium-zinc stabilizer, 5 parts of flame retardant, and 45 parts of TOTM plasticizer and heavy calcium carbonate, wherein the mass ratio of the TOTM plasticizer to the heavy calcium carbonate is 2: 1.
the procedure for preparing a processed PVC material from the above-mentioned starting materials was the same as in example 1, and the PVC material was designated as sample L.
The samples L were tested for thermal stability and low temperature impact in the same manner as samples A-K. Finally, the thermal stability of sample L was determined to be 220min, and low temperature impact resistance was shown to break at-40 ℃.
Comparing the test results of example 1 with those of comparative example 8, it can be seen that when the mass ratio of plasticizer to filler is less than or exceeds 8: in the range of (1-3), the thermal stability and low-temperature impact resistance of the PVC material are obviously reduced, which shows that the thermal stability and low-temperature impact resistance of the PVC material can be improved by controlling the proportion of the plasticizer and the filler.
Comparative example 9
The comparative example provides a preparation method of a PVC material, wherein the PVC material comprises the following raw materials in parts by weight: 100 parts of PVC resin, 8 parts of calcium-zinc stabilizer, 5 parts of flame retardant, 5 parts of ground calcium carbonate, and 48 parts of TOTM plasticizer and calcium-zinc stabilizer, wherein the mass ratio of the TOTM plasticizer to the calcium-zinc stabilizer is 15: 1.
the procedure for the preparation of the PVC material from the above-mentioned starting materials was the same as in example 1, giving the PVC material designated as sample M.
Sample M was tested for thermal stability and low temperature impact in the same manner as samples A-K. Finally, the thermal stability of sample M was determined to be 37min and the low temperature impact temperature was-45 ℃.
Comparing the test results of example 1 and this comparative example, it can be seen that when the mass ratio of plasticizer to calcium zinc stabilizer is less than or exceeds 5:1, the thermal stability and low-temperature impact resistance of the PVC material are obviously reduced, which shows that the thermal stability and low-temperature impact resistance of the PVC material can be improved by controlling the proportion of the plasticizer and the calcium-zinc stabilizer.
Fig. 1-fig. 3 are photographs of PVC materials processed in example 1, comparative example 8 and comparative example 9, respectively, and it can be seen by comparison that sample a processed in example 1 has a flat and smooth surface, and sample L and sample M processed in comparative example 8 and comparative example 9 have wrinkles and uneven surface distribution after the same processing procedure. This comparison result demonstrates that: according to the invention, by controlling the components of the raw materials in the PVC material and the effective proportion among the components, the processing performance of the PVC material can be improved, the obtained PVC material has a smooth and uniform surface, and the effective function of the PVC material in practical application can be exerted.

Claims (15)

1. The PVC material comprises the following raw materials in parts by weight: 90-120 parts of PVC resin, 20-50 parts of plasticizer, 5-10 parts of stabilizer, 2-8 parts of flame retardant and 5-30 parts of filler;
the plasticizer is trioctyl trimellitate, the filler is heavy calcium carbonate, and the stabilizer is a calcium-zinc stabilizer.
2. The PVC material according to claim 1, wherein the mass ratio of the plasticizer to the stabilizer is (4-6): (1-2), wherein the mass ratio of the plasticizer to the filler is 8 (1-3).
3. The PVC material according to claim 1 or 2, wherein the mass ratio of the plasticizer to the stabilizer is 5: 1.
4. The PVC material according to any one of claims 1 to 3, wherein the PVC material comprises the following raw materials in parts by weight: 90-120 parts of PVC resin, 20-50 parts of plasticizer, 5-10 parts of stabilizer, 2-8 parts of flame retardant and 5 parts of filler.
5. PVC material according to any of claims 1 to 4, wherein the calcium zinc stabilizer comprises a zinc stearate based calcium zinc stabilizer.
6. The PVC material according to claim 5, wherein the mass content of zinc stearate in the zinc stearate calcium-zinc stabilizer is greater than or equal to 10%.
7. The PVC material according to any one of claims 1 to 4, wherein the particle size of the heavy calcium carbonate is 2500-3000 meshes, and the mass proportion of the calcium carbonate in the heavy calcium carbonate is more than 80%.
8. The PVC material according to any one of claims 1 to 4 and 7, wherein the heavy calcium carbonate has a particle size of 2800 meshes.
9. The PVC material according to claim 1 or 4, wherein the average degree of polymerization of the PVC resin is 1250-1350.
10. PVC material according to claim 1 or 4, wherein the flame retardant comprises Sb2O3The flame retardant comprises active ingredients, wherein the mass ratio of the active ingredients in the flame retardant is more than 82%.
11. PVC material according to any of claims 1, 4, 10, wherein the flame retardant comprises Sb2O3In the flame retardant, Sb2O3Is more than 55 percent.
12. A process for the preparation of a PVC material as claimed in any one of claims 1 to 11, which comprises:
step one, blending PVC resin and the plasticizer to obtain a first mixture;
adding a stabilizer, a flame retardant and a filler into the first mixture and blending to obtain a second mixture;
and step three, extruding and granulating the second mixture to obtain the PVC material.
13. The preparation method of claim 12, wherein in the first step, the blending time is 2min to 6 min; in the second step, the blending time is 2min-6 min.
14. The preparation method of claim 13, wherein in the first step, the blending time is 2 min; in the second step, the blending time is 2 min.
15. The preparation method according to any one of claims 12 to 14, wherein the temperature of the extrusion in step three is 140-180 ℃.
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