Plasticizer production and preparation method

A composite environmentally friendly plasticizer was prepared by vacuum pump decompression, polycondensation reaction and esterification treatment. This solved the problems of poor affinity and high cost of plasticizers in the existing technology, and realized the safety, environmental protection and degradability of plasticizers, thus promoting their widespread use.

CN120944187APending Publication Date: 2025-11-14河南顺泓环保材料有限公司
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Patent Information

Application Number
CN202511055895.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-30
Publication Date
2025-11-14

AI Technical Summary

Technical Problem

Existing plasticizers suffer from poor affinity and high cost during preparation, which limits their widespread use.

Method used

The process involves vacuum pump decompression dehydration, polycondensation reaction, esterification reaction, and sterilization. The ratio of fatty acids, glycerol, chlorinated paraffin, and bio-ester plasticizer is combined. The decompression dehydration reaction is carried out by vacuum pump, followed by the addition of a catalyst for polycondensation reaction, esterification reaction, and sterilization treatment, ultimately producing a composite environmentally friendly plasticizer.

Benefits of technology

This improved the plasticizer's compatibility and biodegradability, reduced preparation costs, and enabled the plasticizer to be safe, environmentally friendly, and widely used.

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Abstract

The invention relates to the technical field of chemistry, and discloses a plasticizer production and preparation method which comprises the following steps: weighing raw materials of a plasticizer according to a ratio, respectively putting the raw materials into a reaction kettle, adding an efficient solid catalyst from a kettle opening according to the mass of the materials, and simultaneously starting to carry out decompression dehydration reaction by using a vacuum pump; starting a heating device and a stirrer in the reaction kettle, stirring, adding a second catalyst after the gas mixture is completely dissolved, heating, carrying out condensation polymerization, reducing the vacuum degree in the reaction container to 0.15 kpa, and carrying out separation and purification after the reaction is finished. According to the production and preparation method of the plasticizer, through cold resistance of chlorinated paraffin, high intermiscibility of a bio-ester plasticizer and the like, the overall safety and environment-friendly effect of the plasticizer are guaranteed, the compounding capacity of the plasticizer is overall improved, meanwhile, the degradable effect of the plasticizer is guaranteed, the cost range of the plasticizer is guaranteed, and the plasticizer is suitable for industrial production. Further, the plasticizer is popularized and used, and the social value is greatly improved.
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Description

Technical Field

[0001] This invention relates to the field of chemical technology, specifically to a method for producing and preparing a plasticizer. Background Technology

[0002] Plasticizers are an indispensable fine chemical additive in the production of plastics. They are among the plastic additives with the largest production and consumption in the world. Because plasticizers have the advantages of lowering the glass transition temperature of polymer materials and improving the plasticity of materials, they are widely used in plastic and rubber products, medical materials, building materials and other fields.

[0003] Plasticizers are additives added to polymers to increase their plasticity, flexibility, and flowability during processing. Vegetable oil-based plasticizers modify the main component of natural vegetable oils, glycerol fatty acid esters, through functional group reactions, which can improve the compatibility of natural vegetable oils with PVC. However, some plasticizers have relatively simple internal structures, resulting in poor affinity during preparation and high preparation costs, which hinders their subsequent promotion and use. Summary of the Invention

[0004] (a) Technical problems to be solved

[0005] To address the shortcomings of existing technologies, this invention provides a method for producing plasticizers that has advantages such as good applicability, safety and environmental protection, and high biodegradability and composite properties. It solves the problems of poor affinity during preparation and high preparation costs.

[0006] (II) Technical Solution

[0007] To achieve the above-mentioned objectives, the present invention provides the following technical solution: a method for producing and preparing a plasticizer, comprising the following steps:

[0008] Step 1: Weigh each plasticizer raw material according to the formula and place them in the reaction vessel. Then, add a high-efficiency solid catalyst from the vessel opening according to the material mass, and simultaneously start the vacuum dehydration reaction using a vacuum pump.

[0009] Step 2: Start the heating device and stirrer in the reactor to stir it. After the gas mixture is completely miscible, add the second catalyst, raise the temperature to carry out the polycondensation reaction and lower the vacuum degree in the reaction vessel to 0.15 kPa. After the reaction is completed, separate and purify to obtain an environmentally friendly plasticizer.

[0010] Step 3: Continue the esterification reaction of the environmentally friendly plasticizer;

[0011] Step 4: Sterilization treatment, setting up sterilization pipelines and ultraviolet lamp beads;

[0012] Step 5: Finally, add the bio-ester plasticizer according to the formula, and continue stirring with the stirring motor for 80-100 minutes to obtain the composite environmentally friendly plasticizer.

[0013] Preferably, the plasticizer raw materials in step one are fatty acids, glycerol, chlorinated paraffin, bio-ester plasticizer and catalyst, and the mass ratio of fatty acids, glycerol, chlorinated paraffin and bio-ester plasticizer is 33:1:59:2.

[0014] Preferably, in step two, the stirring motor continues stirring for 20 to 70 minutes, and the temperature is controlled at 200-260℃.

[0015] Preferably, in step three, a high-temperature treatment of 260-300°C is used, and a protective gas is added for epoxy treatment.

[0016] Preferably, after the oxygen exchange treatment is completed in step three, the negative pressure reaction is stopped, and neutralization washing is performed to remove the catalyst and obtain crude ester.

[0017] Preferably, the first catalyst comprises a strong acidic inorganic or organic protic acid, the second catalyst comprises one of the types such as sulfuric acid or methanesulfonic acid, and the protective gas is nitrogen.

[0018] Preferably, the sterilization pipe in step four is installed in a curved manner, thus increasing the exhaust volume of the sterilization pipe during use.

[0019] (III) Beneficial Effects

[0020] Compared with the prior art, the present invention provides a method for producing and preparing plasticizers, which has the following beneficial effects:

[0021] 1. This plasticizer production and preparation method, through the cold resistance of chlorinated paraffin and the high compatibility of bio-ester plasticizers, ensures the overall safety and environmental protection of the plasticizer, improves the overall compounding ability of the plasticizer, ensures the biodegradability of the plasticizer, and keeps the cost range of the plasticizer, thereby realizing the promotion and use of the plasticizer and greatly improving its social value. Detailed Implementation

[0022] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] A method for producing a plasticizer includes the following steps:

[0024] First, the plasticizer raw materials are weighed according to the specified ratio. The plasticizer raw materials are fatty acids, glycerol, chlorinated paraffin, bio-ester plasticizer and catalyst. The mass ratio of fatty acids, glycerol, chlorinated paraffin and bio-ester plasticizer is 33:1:59:2. Then, they are placed in the reaction vessel. Then, a high-efficiency solid catalyst is added from the vessel opening according to the mass of the materials. At the same time, a vacuum pump is used to start the dehydration reaction under reduced pressure. The catalyst is a strong acidic inorganic or organic protic acid.

[0025] Next, start the heating device and stirrer in the reactor to make it stir. The stirring motor continues to stir for 20-70 minutes, and the temperature is controlled at 200-260℃. After the mixture is completely miscible, add the second catalyst, including one of the types such as sulfuric acid or methanesulfonic acid. Raise the temperature to carry out the polycondensation reaction and reduce the vacuum degree in the reaction vessel to 0.15 kPa. After the reaction is completed, separate and purify to obtain the environmentally friendly plasticizer.

[0026] Then, the environmentally friendly plasticizer is subjected to esterification reaction. The reaction is carried out at a high temperature of 260-300℃, and a protective gas is added for epoxy treatment for 2-3 hours. After the oxygen exchange treatment is completed, the negative pressure reaction is stopped, and neutralization and washing are performed to remove the catalyst and obtain crude ester. The crude ester is then sterilized by setting up sterilization pipes and ultraviolet lamps. The sterilization pipes are set up in a curved manner to increase the exhaust volume when the sterilization pipes are in use.

[0027] Finally, add the bio-ester plasticizer according to the formula, and continue stirring with the stirring motor for 80-100 minutes to obtain the composite environmentally friendly plasticizer.

[0028] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for producing and preparing a plasticizer, characterized in that, Includes the following steps: Step 1: Weigh each plasticizer raw material according to the formula and place them in the reaction vessel. Then, add a high-efficiency solid catalyst from the vessel opening according to the material mass, and simultaneously start the vacuum dehydration reaction using a vacuum pump. Step 2: Start the heating device and stirrer in the reactor to stir it. After the gas mixture is completely miscible, add the second catalyst, raise the temperature to carry out the polycondensation reaction and lower the vacuum degree in the reaction vessel to 0.15 kPa. After the reaction is completed, separate and purify to obtain an environmentally friendly plasticizer. Step 3: Continue the esterification reaction of the environmentally friendly plasticizer; Step 4: Sterilization treatment, setting up sterilization pipelines and ultraviolet lamp beads; Step 5: Finally, add the bio-ester plasticizer according to the formula, and continue stirring with the stirring motor for 80-100 minutes to obtain the composite environmentally friendly plasticizer.

2. The method for producing a plasticizer according to claim 1, characterized in that: In step one, the plasticizer raw materials are fatty acids, glycerol, chlorinated paraffin, bio-ester plasticizer and catalyst, and the mass ratio of fatty acids, glycerol, chlorinated paraffin and bio-ester plasticizer is 33:1:59:

2.

3. The method for producing a plasticizer according to claim 1, characterized in that: In step two, the stirring motor continues stirring for 20 to 70 minutes, with the temperature controlled at 200-260℃.

4. The method for producing a plasticizer according to claim 1, characterized in that: In step three, a high-temperature treatment of 260-300℃ is used, and a protective gas is added for epoxy treatment.

5. The method for producing a plasticizer according to claim 4, characterized in that: After the oxygen exchange treatment is completed in step three, the negative pressure reaction is stopped, and neutralization and washing are performed to remove the catalyst and obtain crude ester.

6. The method for producing a plasticizer according to claim 1, characterized in that: The first catalyst includes a strong acidic inorganic or organic protic acid, the second catalyst includes one of the types such as sulfuric acid or methanesulfonic acid, and the protective gas is nitrogen.

7. The method for producing a plasticizer according to claim 1, characterized in that: In step four, the sterilization pipe is installed in a curved manner, which increases the exhaust volume of the sterilization pipe during use.