Oligomer synthesis and compounding method of vulcanized network stabilizer

Abstract

The invention relates to the technical field of manufacturing of functional nano materials for high polymer materials, and discloses an oligomer synthesis and compounding method of a vulcanized network stabilizer, which comprises the following steps: mixing phthalic anhydride and dihydric alcohol according to a molar ratio of (1.00-1.25): 1.00, adding concentrated sulfuric acid as a catalyst, carrying out esterification reaction at 130-155 DEG C for 4-6 hours, cooling to 80-100 DEG C after the reaction is finished, and discharging to obtain the vulcanized network stabilizer. The oligomer obtained in the step a is compounded and mixed with zinc stearate, monostearin, a silane coupling agent, PE wax and white carbon black to form a homogeneous solid finished product, and by optimizing esterification reaction conditions (the molar ratio of phthalic anhydride to dihydric alcohol and temperature control) and a compounding process, generation of by-products is remarkably reduced, and the uniformity and stability of the finished product are improved. The method is suitable for high-efficiency production of the rubber vulcanization aid.

Description

Technical Field

[0001] The present invention relates to the technical field of manufacturing functional nanomaterials for polymer materials, and specifically relates to a method for synthesizing oligomers through an esterification reaction and compounding to prepare a vulcanization network stabilizer. Background Art

[0002] Vulcanization network stabilizers are key additives used in the rubber industry to improve vulcanization efficiency and material properties. Traditional preparation methods mostly adopt single-component compounding or high-temperature and high-pressure synthesis processes, which have the following problems:

[0003] 1. Many reaction by-products: Low-boiling by-products are easily generated in the esterification reaction, requiring complex post-treatment and increasing costs;

[0004] 2. Poor compounding stability: The compatibility of each component in the existing compounding process is insufficient, resulting in easy stratification or uneven performance of the finished product;

[0005] 3. High energy consumption: The reaction temperature control is inaccurate, easily causing energy waste. Summary of the Invention

[0006] The purpose of the present invention is to provide a method for synthesizing and compounding oligomers of a vulcanization network stabilizer, which solves the problems of many current reaction by-products, poor compounding stability, and high energy consumption.

[0007] To achieve the above purpose, the present invention provides the following technical solution: A method for synthesizing and compounding oligomers of a vulcanization network stabilizer, and its reaction equation is as follows;

[0008]

[0009] The method for synthesizing and compounding oligomers of a vulcanization network stabilizer described above includes the following steps:

[0010] A. Raw material ratio: 300 kg of phthalic anhydride, 120 - 200 kg of diol (selected from at least one of ethylene glycol, propylene glycol, and butanediol), and the molar ratio of phthalic anhydride to diol is 1.00 - 1.25:1.00; The catalyst is 3 - 6 kg of concentrated sulfuric acid;

[0011] B. Add phthalic anhydride and diol to the reaction kettle, and slowly add concentrated sulfuric acid;

[0012] C. Seal the reaction kettle, connect the condensation device, and heat with steam to 130 - 155 °C, and stir and react for 4 - 6 hours;

[0013] D. Control the temperature to gradually rise to 150 - 155 °C by adjusting the backwater discharge amount, and cool to 80 - 100 °C for discharging after the reaction ends;

[0014] E. By-product treatment: The low-boiling point by-products (boiling point 100~150℃) produced in the reaction are condensed, collected and then burned for disposal.

[0015] F. Compound raw materials: oligomer, zinc stearate, monoglyceride, silane coupling agent, PE wax, white carbon black;

[0016] G. Mixing process: Add the oligomer and compound raw materials into the mixing pot according to the proportion, and stir them thoroughly until they become a homogeneous solid product.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] 1. There are few reaction by-products. Esterification reaction tends to generate many low-boiling point by-products. This production process has few by-products and the boiling point is between 100 and 150 ° C. It is not only highly safe, but also easy to recycle and burn;

[0019] 2. After compounding, the application can improve the dispersibility of the product and the stretching of the molecular chain, and can adjust the pH value to ensure that the vulcanization conditions remain unchanged;

[0020] 3. Compounding can also satisfy the synthetic monomers to better participate in vulcanization cross-linking and improve the vulcanization network structure;

[0021] 4. The synthesis process has low energy consumption. Since the raw materials have a high boiling point and cannot be evaporated, the reflux components are small (mainly water and by-products generated by the reaction), which reduces the energy consumed in the reflux process. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The schematic diagram of the synthesis process of the oligomer of the present invention;

[0023] Figure 2 This is a schematic diagram of the compounding process flow of the present invention. DETAILED DESCRIPTION

[0024] The present invention will be described in more detail below by way of examples, which are merely illustrative and do not in any way limit the scope of the present invention.

[0025] The present invention provides a technical solution: a method for synthesizing and compounding oligomers of a vulcanization network stabilizer, and the reaction equation is as follows:

[0026]

[0027] Embodiment 1:

[0028] A. Raw material ratio: 300 kg of phthalic anhydride, 150 kg of propylene glycol (molar ratio 1.2:1), and 4 kg of concentrated sulfuric acid as catalyst;

[0029] B. Add phthalic anhydride and diol into the reaction pot, and slowly add concentrated sulfuric acid;

[0030] C. Seal the reaction kettle, connect the condensation device, turn on the steam heating to 145 °C, and stir the reaction for 5 hours;

[0031] D. Control the temperature to gradually rise to 150 - 155 °C by adjusting the return water discharge amount, and cool to 80 - 100 °C for discharging after the reaction ends;

[0032] E. By - product treatment: The low - boiling - point by - products (boiling point 100 - 150 °C) generated during the reaction are collected by condensation and then disposed of by combustion.

[0033] F. Compound raw materials: oligomer 25%, zinc stearate 20%, silane coupling agent 20%, PE wax 10%, white carbon black 25%;

[0034] G. Mixing process: Put the oligomer and the compound raw materials into the mixing kettle according to the proportion, and stir fully until a homogeneous solid product is obtained.

[0035] Example 2:

[0036] A. Raw material ratio: phthalic anhydride 300 kg, ethylene glycol 120 kg (molar ratio 1.0:1), and the catalyst is concentrated sulfuric acid 5 kg;

[0037] B. Add phthalic anhydride and diol into the reaction kettle, and slowly add concentrated sulfuric acid;

[0038] C. Seal the reaction kettle, connect the condensation device, turn on the steam heating to 150 °C, and stir the reaction for 6 hours;

[0039] D. Control the temperature to gradually rise to 150 - 155 °C by adjusting the return water discharge amount, and cool to 80 - 100 °C for discharging after the reaction ends;

[0040] E. By - product treatment: The low - boiling - point by - products (boiling point 100 - 150 °C) generated during the reaction are collected by condensation and then disposed of by combustion.

[0041] F. Compound raw materials: oligomer 35%, monoglyceride 10%, zinc stearate 20%, PE wax 10%, white carbon black 20%, silane coupling agent 5%;

[0042] G. Mixing process: Put the oligomer and the compound raw materials into the mixing kettle according to the proportion, and stir fully until a homogeneous solid product is obtained, and the anti - delamination performance of the product is significantly improved.

[0043] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for synthesizing and compounding oligomers of a vulcanization network stabilizer, characterized in that: The reaction equation is as follows; The method for synthesizing and compounding the oligomer of a vulcanization network stabilizer comprises the following steps: A. Mix phthalic anhydride and diol in a molar ratio of 1.00~1.25:1.00, add concentrated sulfuric acid as a catalyst, and carry out an esterification reaction at 130~155°C for 4~6 hours. After the reaction is completed, cool to 80~100°C and discharge; B. Compound the oligomer obtained in step a with zinc stearate, monoglyceride, silane coupling agent, PE wax, and white carbon black, and mix to form a homogeneous solid product.

2. The method for synthesizing and compounding the oligomer of a vulcanization network stabilizer according to claim 1, characterized in that The diol is at least one of ethylene glycol, propylene glycol, or butanediol.

3. The method for synthesizing and compounding the oligomer of the vulcanization network stabilizer according to claim 1, characterized in that, During the reaction process, the temperature is gradually raised to 150~155°C by discharging the reflux water.

4. The oligomer synthesis and compounding method of a vulcanization network stabilizer according to claim 1, characterized in that, The mass percentages of the compounding raw materials are: zinc stearate 10~15%, monoglyceride 5~15%, silane coupling agent 10~15%, PE wax 5~10%, white carbon black 15~25%, and the rest is the oligomer.

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