Preparation method of heat-resistant rubber plasticizer

Abstract

The invention belongs to the field of rubber plasticizers, and particularly relates to a preparation method of a heat-resistant rubber plasticizer, aiming at the problem of poor heat resistance of the existing rubber plasticizer, the invention provides the following scheme: the preparation method comprises the following steps: S1, measuring an antioxidant, dioctyl phthalate, tricresyl phosphate and epoxidized fatty acid methyl ester; the composition is prepared from the following components in parts by weight: 1-5 parts of an antioxidant, 5-10 parts of dioctyl phthalate, 5-10 parts of tricresyl phosphate and 1-5 parts of epoxidized fatty acid methyl ester. S2, adding an antioxidant and dioctyl phthalate into the reaction kettle, and stirring and mixing to obtain a mixture; s3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester into the mixture, stirring and mixing, and carrying out polyesterification reaction to obtain a mixture; s4, the mixture is subjected to reduced pressure distillation, and a heat-resistant rubber plasticizer to-be-tested product is obtained.The heat-resistant rubber plasticizer has the good heat resistance, and the using effect is improved.

Description

Technical Field

[0001] The invention relates to the technical field of rubber plasticizers, and in particular to a method for preparing a heat-resistant rubber plasticizer. Background Art

[0002] Rubber plasticizer is a reagent. Rubber plasticization refers to adding certain substances to rubber to reduce the interaction between rubber molecules, thereby reducing the glass transition temperature of rubber, making the rubber plastic and fluid, and facilitating molding operations such as calendering and extrusion. At the same time, it can also improve certain physical and mechanical properties of vulcanized rubber, such as reducing hardness and tensile stress, giving higher elasticity and lower heat generation, and improving cold resistance.

[0003] The existing rubber plasticizers have poor heat resistance, so we propose a preparation method of a heat-resistant rubber plasticizer to solve the above problems. Summary of the invention

[0004] The purpose of the present invention is to solve the disadvantage of poor heat resistance of rubber plasticizer in the prior art, and to propose a preparation method of heat-resistant rubber plasticizer.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A method for preparing a heat-resistant rubber plasticizer comprises the following steps:

[0007] S1. Measure antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester. The specific weight parts are as follows: 1-5 parts of antioxidant, 5-10 parts of dioctyl phthalate, 5-10 parts of tricresyl phosphate, and 1-5 parts of epoxy fatty acid methyl ester;

[0008] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0009] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0010] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0011] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0012] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0013] Preferably, in S1, antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 2-4 parts of antioxidant, 6-9 parts of dioctyl phthalate, 6-9 parts of tricresyl phosphate, and 2-4 parts of epoxy fatty acid methyl ester.

[0014] Preferably, in S1, antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 3 parts of antioxidant, 7 parts of dioctyl phthalate, 7 parts of tricresyl phosphate, and 3 parts of epoxy fatty acid methyl ester.

[0015] Preferably, in S2, the antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 5-10 min and the stirring speed is 200-300 r / min to obtain a mixture.

[0016] Preferably, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, and the mixture is stirred for 10-15 min at a stirring speed of 200-300 r / min to carry out polyesterification reaction to obtain a mixture.

[0017] Preferably, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0018] Preferably, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling and testing is performed, the number of sampling points is 3-5, and the test data is recorded.

[0019] Preferably, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0020] Preferably, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterified, and then filtered to obtain a mixture.

[0021] Preferably, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0022] In the present invention, the preparation method of the heat-resistant rubber plasticizer has the following beneficial effects:

[0023] The use of dioctyl phthalate has good comprehensive performance, good compatibility with rubber, cold resistance, heat resistance, and good electrical insulation. The use of tricresyl phosphate has good flame resistance, heat resistance, oil resistance, and electrical insulation. The use of epoxy fatty acid methyl ester has plasticization and stability, and further improves thermal stability.

[0024] The invention has good heat resistance and improves the use effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The present invention is a flow chart of a method for preparing a heat-resistant rubber plasticizer. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0027] Embodiment 1

[0028] Reference Figure 1 , a method for preparing a heat-resistant rubber plasticizer, comprising the following steps:

[0029] S1. Measure antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester. The specific weight parts are as follows: 1 part of antioxidant, 5 parts of dioctyl phthalate, 5 parts of tricresyl phosphate, and 1 part of epoxy fatty acid methyl ester;

[0030] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0031] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0032] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0033] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0034] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0035] In this embodiment, in S2, an antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 5 minutes and the stirring speed is 200 r / min to obtain a mixture.

[0036] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are added to the mixture in sequence, and the mixture is stirred for 10 minutes at a stirring speed of 200 r / min to carry out polyesterification reaction to obtain a mixture.

[0037] In this embodiment, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0038] In this embodiment, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling and testing is performed, the number of sampling points is 3, and the test data is recorded.

[0039] In this embodiment, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0040] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterification reaction is carried out, and then filter pressing is carried out to obtain a mixture.

[0041] In this embodiment, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0042] Embodiment 2

[0043] A method for preparing a heat-resistant rubber plasticizer comprises the following steps:

[0044] S1, antioxidant, dioctyl phthalate, tricresyl phosphate, epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 2 parts of antioxidant, 6 parts of dioctyl phthalate, 6 parts of tricresyl phosphate, and 2 parts of epoxy fatty acid methyl ester;

[0045] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0046] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0047] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0048] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0049] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0050] In this embodiment, in S2, an antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 6 minutes and the stirring speed is 220 r / min to obtain a mixture.

[0051] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are added to the mixture in sequence, and the mixture is stirred for 11 minutes at a stirring speed of 220 r / min to carry out polyesterification reaction to obtain a mixture.

[0052] In this embodiment, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0053] In this embodiment, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling detection is performed, the number of sampling points is 4, and the detection data is recorded.

[0054] In this embodiment, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0055] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterification reaction is carried out, and then filter pressing is carried out to obtain a mixture.

[0056] In this embodiment, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0057] Embodiment 3

[0058] A method for preparing a heat-resistant rubber plasticizer comprises the following steps:

[0059] S1, antioxidant, dioctyl phthalate, tricresyl phosphate, epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 3 parts of antioxidant, 7 parts of dioctyl phthalate, 7 parts of tricresyl phosphate, and 3 parts of epoxy fatty acid methyl ester;

[0060] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0061] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0062] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0063] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0064] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0065] In this embodiment, in S2, an antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 7 minutes and the stirring speed is 240 r / min to obtain a mixture.

[0066] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are added to the mixture in sequence, and the mixture is stirred for 12 minutes at a stirring speed of 240 r / min to carry out polyesterification reaction to obtain a mixture.

[0067] In this embodiment, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0068] In this embodiment, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling detection is performed, the number of sampling points is 4, and the detection data is recorded.

[0069] In this embodiment, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0070] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterification reaction is carried out, and then filter pressing is carried out to obtain a mixture.

[0071] In this embodiment, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0072] Embodiment 4

[0073] A method for preparing a heat-resistant rubber plasticizer comprises the following steps:

[0074] S1, antioxidant, dioctyl phthalate, tricresyl phosphate, epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 4 parts of antioxidant, 9 parts of dioctyl phthalate, 9 parts of tricresyl phosphate, and 4 parts of epoxy fatty acid methyl ester;

[0075] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0076] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0077] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0078] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0079] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0080] In this embodiment, in S2, an antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 9 minutes and the stirring speed is 280 r / min to obtain a mixture.

[0081] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are added to the mixture in sequence, and the mixture is stirred for 14 minutes at a stirring speed of 280 r / min to carry out polyesterification reaction to obtain a mixture.

[0082] In this embodiment, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0083] In this embodiment, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling and testing is performed, the number of sampling points is 5, and the test data is recorded.

[0084] In this embodiment, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0085] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterification reaction is carried out, and then filter pressing is carried out to obtain a mixture.

[0086] In this embodiment, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0087] Embodiment 5

[0088] A method for preparing a heat-resistant rubber plasticizer comprises the following steps:

[0089] S1. Measure antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester. The specific weight parts are as follows: 5 parts of antioxidant, 10 parts of dioctyl phthalate, 10 parts of tricresyl phosphate, and 5 parts of epoxy fatty acid methyl ester;

[0090] S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture;

[0091] S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture;

[0092] S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested;

[0093] S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data;

[0094] S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

[0095] In this embodiment, in S2, an antioxidant and dioctyl phthalate are added into a reaction kettle and stirred for mixing. The stirring time is 10 min and the stirring speed is 300 r / min to obtain a mixture.

[0096] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are added to the mixture in sequence, and the mixture is stirred for 15 minutes at a stirring speed of 300 r / min to carry out polyesterification reaction to obtain a mixture.

[0097] In this embodiment, in S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

[0098] In this embodiment, in S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling and testing is performed, the number of sampling points is 5, and the test data is recorded.

[0099] In this embodiment, in S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

[0100] In this embodiment, in S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterification reaction is carried out, and then filter pressing is carried out to obtain a mixture.

[0101] In this embodiment, in S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

[0102] Experimental example

[0103] The heat-resistant rubber plasticizers prepared in Examples 1 to 5 were tested for heat resistance, and the specific data are shown in the following table:

[0104]

[0105] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing a heat-resistant rubber plasticizer, characterized in that: The following steps are involved: S1. Measure antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester. The specific weight parts are as follows: 1-5 parts of antioxidant, 5-10 parts of dioctyl phthalate, 5-10 parts of tricresyl phosphate, and 1-5 parts of epoxy fatty acid methyl ester; S2, adding an antioxidant and dioctyl phthalate into a reaction kettle, stirring and mixing to obtain a mixture; S3, sequentially adding tricresyl phosphate and epoxy fatty acid methyl ester to the mixture, stirring and mixing, and performing polyesterification reaction to obtain a mixture; S4, the mixture is subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested; S5. Put the heat-resistant rubber plasticizer to be tested into a collection bucket, conduct multi-point sampling and testing, and record the test data; S6. Compare the test data and analyze whether the data from multiple point tests are consistent. If they are consistent, conduct a heat resistance test. If they are qualified, the heat-resistant rubber plasticizer product is obtained. If they are inconsistent, issue a warning.

2. The method for preparing a heat-resistant rubber plasticizer according to claim 1, characterized in that: In the S1, antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 2-4 parts of antioxidant, 6-9 parts of dioctyl phthalate, 6-9 parts of tricresyl phosphate, and 2-4 parts of epoxy fatty acid methyl ester.

3. The method for preparing a heat-resistant rubber plasticizer according to claim 2, characterized in that: In the S1, antioxidant, dioctyl phthalate, tricresyl phosphate, and epoxy fatty acid methyl ester are measured, and the specific weight parts are as follows: 3 parts of antioxidant, 7 parts of dioctyl phthalate, 7 parts of tricresyl phosphate, and 3 parts of epoxy fatty acid methyl ester.

4. The method for preparing a heat-resistant rubber plasticizer according to claim 3, characterized in that: In S2, an antioxidant and dioctyl phthalate are added into a reaction kettle, and stirred and mixed. The stirring time is 5-10 minutes and the stirring speed is 200-300 r / min to obtain a mixture.

5. The method for preparing a heat-resistant rubber plasticizer according to claim 4, characterized in that: In S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, and the mixture is stirred for 10-15 minutes at a stirring speed of 200-300 r / min to carry out polyesterification reaction to obtain a mixture.

6. The method for preparing a heat-resistant rubber plasticizer according to claim 5, characterized in that: In the S4, the mixture is added into a distillation device, heated, decompressed, and subjected to reduced pressure distillation to obtain a heat-resistant rubber plasticizer to be tested.

7. The method for preparing a heat-resistant rubber plasticizer according to claim 6, characterized in that: In S5, the heat-resistant rubber plasticizer to be tested is placed in a collection bucket, and multi-point sampling and testing is performed, with the number of sampling points being 3-5, and the test data is recorded.

8. The method for preparing a heat-resistant rubber plasticizer according to claim 7, characterized in that: In S6, the heat-resistant rubber plasticizer is heated to test the heat resistance.

9. The method for preparing a heat-resistant rubber plasticizer according to claim 8, characterized in that: In S3, tricresyl phosphate and epoxy fatty acid methyl ester are sequentially added to the mixture, stirred and mixed, polyesterified, and then filtered to obtain a mixture.

10. The method for preparing a heat-resistant rubber plasticizer according to claim 9, characterized in that: In the S4, the mixture is measured, and the measured mixture is added to a vacuum distillation process, and vacuum distillation is performed to obtain a heat-resistant rubber plasticizer to be tested.

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