Production process of bio-based plasticizer

By using a bio-based plasticizer production process, the health risks of phthalic plasticizers entering the human body have been eliminated, resulting in the production of high-quality, environmentally friendly bio-based plasticizers, which improves production efficiency and compatibility.

CN120944188APending 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
CN202511055899.1
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 phthalate plasticizers can enter the human body through various pathways, posing health risks and failing to meet environmental protection requirements.

Method used

The bio-based plasticizer production process includes steps such as esterification, refining, and distillation. Catalysts such as monobutyltin oxide or tetrabutyl titanate are used, combined with supplemental lighting and heating, and temperature and vacuum control are performed for mixing, filtration, and purification.

Benefits of technology

The production of green and environmentally friendly bio-based plasticizers has improved compatibility with polymer materials, enhanced product quality, reduced processing time, and increased production efficiency.

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Abstract

The invention relates to the technical field of chemistry, and discloses a bio-based plasticizer production process which comprises the following steps: weighing bio-based plasticizer raw materials according to a weight ratio, and adding into a reactor for processing; esterification treatment: adaptively adding a catalyst; refining treatment, mixing and filtering processing; the invention discloses a bio-based plasticizer production process, which comprises the following steps: S1, pretreatment, distillation treatment, stirring and purification treatment, in the step S1, a bio-based plasticizer raw material processing mode adopts stirring, materials are added in batches until all bio-based plasticizer raw materials are added, and the bio-based plasticizer production process has the characteristics of simple process, energy conservation, environmental protection and stable and excellent product quality; the plasticizer is environment-friendly and does not pollute the environment, magnesium oxide or activated carbon is added in the preparation process of the plasticizer, the compatibility of the plasticizer and a high polymer material is increased, meanwhile, the plasticizer is good in uniformity effect, and the production and processing efficiency of the bio-based plasticizer can be more effectively improved by adopting a light source for supplementary lighting and heating.
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Description

Technical Field

[0001] This invention relates to the field of chemical technology, specifically to a process for producing bio-based plasticizers. Background Technology

[0002] Plastic products are closely related to our lives. Most of these products are used in close proximity to us, while some come into contact with drinking water, food, or blood, causing certain additives in the plastic to be released into the atmosphere or even directly into the human body.

[0003] Trace amounts of plasticizers in the environment are pollutants that disrupt the ecological balance and harm human health. Currently, the most commonly used plasticizers are phthalates. However, research has confirmed that phthalate plasticizers can enter the human body through multiple routes, including oral, respiratory, intravenous, and skin absorption, and can have toxic effects on multiple systems of the body. Therefore, countries around the world are accelerating the development of non-toxic and pollution-free fresh plasticizers to replace phthalate plasticizers and meet increasingly stringent environmental protection requirements. Summary of the Invention

[0004] (a) Technical problems to be solved

[0005] To address the shortcomings of existing technologies, this invention provides a bio-based plasticizer production process that is simple, energy-saving, environmentally friendly, and produces stable and excellent product quality. It solves the problem that phthalate plasticizers can enter the human body through multiple routes, such as oral, respiratory, intravenous infusion, and skin absorption, and can cause toxicity to multiple systems of the body.

[0006] (II) Technical Solution

[0007] To achieve the above-mentioned objectives, the present invention provides the following technical solution: a bio-based plasticizer production process, comprising the following steps:

[0008] S1: Weigh the bio-based plasticizer raw materials according to the weight ratio and add them to the reactor for processing;

[0009] S2: Esterification treatment, with appropriate addition of catalyst;

[0010] S3: Refining, mixing, and filtration processes;

[0011] S4: Distillation, stirring, and purification processes.

[0012] Preferably, the bio-based plasticizer raw material in S1 is processed by stirring, and the material is added in batches until all the bio-based plasticizer raw material is added, and heating treatment is carried out simultaneously at a temperature of 170-260℃.

[0013] Preferably, the bio-based plasticizer raw material in S1 is stirred at a speed of 400-2200 r / min for a duration of 1-3 h, and the water produced by the reaction is continuously discharged using a water separator during the process.

[0014] Preferably, the temperature is controlled during the S2 process, with the temperature maintained at 200-240℃ and continuously stirred while adding nitrogen gas in real time for protective stirring. Then, a negative pressure reaction is carried out to ensure that the test acid value is ≤0.2mgKOH / g, and then a catalyst is added.

[0015] Preferably, in step S3, sodium hydroxide or sodium carbonate is added to the mixture, and then neutralized for 200-1000 seconds. The mixture is then heated to 175-225°C, ensuring a vacuum of ≥-0.09 MPa. After the heat treatment, the acid value is controlled to ≤0.2 mg KOH / g. The mixture is then cooled to 100°C and held at that temperature for 1.5-2.5 hours.

[0016] Preferably, in step S4, the above-mentioned mixture is added to a distillation apparatus, and during the distillation of the bio-based plasticizer mixture, a flow rate of 0.1-0.5 cubic meters and a temperature of 240-300℃ are used for continuous stirring for 20-75 minutes. Then, after controlling the temperature to reach 50-70℃, the bio-based plasticizer mixture is purified into plasticizer raw material for discharge and packaging.

[0017] Preferably, in step S3, the prepared bio-based plasticizer mixture is added to a vacuum filter and circulated for filtration under a pressure of 0.2-0.8 MPa until all impurities are discharged.

[0018] Preferably, the catalyst in S2 is monobutyltin oxide or tetrabutyl titanate.

[0019] Preferably, the gas inside the mixture is released based on S3, the reaction solution is cooled to room temperature, and magnesium oxide or activated carbon is added and mixed evenly.

[0020] Preferably, the bio-based plasticizer can be processed using a light source for supplemental lighting and heating. The light source can be ultraviolet light or fluorescent lamp with a power of 50-700W.

[0021] (III) Beneficial Effects

[0022] Compared with the prior art, the present invention provides a bio-based plasticizer production process, which has the following characteristics:

[0023] Beneficial effects:

[0024] 1. This bio-based plasticizer production process is characterized by its simplicity, energy efficiency, environmental friendliness, and stable and excellent product quality. It is also green and environmentally friendly, causing no pollution to the environment. Furthermore, the addition of magnesium oxide or activated carbon during the preparation process increases the compatibility of the plasticizer with polymer materials. At the same time, the plasticizer exhibits good uniformity. Moreover, the use of a light source for supplemental lighting and heating can more effectively improve the efficiency of bio-based plasticizer production and processing, thereby increasing the overall production speed. Detailed Implementation

[0025] 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.

[0026] Example 1:

[0027] A bio-based plasticizer production process involves weighing the bio-based plasticizer raw materials according to a weight ratio and adding them to a reactor for processing. The materials are added in batches until all the bio-based plasticizer raw materials are added, and simultaneous heating is performed at a temperature of 208°C. This achieves higher mixing efficiency for the bio-based plasticizer raw materials, thus reducing the overall processing time. Furthermore, the bio-based plasticizer raw materials are stirred at a speed of 1660 r / min for a duration of 1.55 h. During the process, a water separator continuously removes the water produced in the reaction. For heating, in addition to electric heating, a light source can be used for supplemental heating; the light source can be ultraviolet light or a fluorescent lamp with a power of 355W.

[0028] Furthermore, after the bio-based plasticizer has been stirred for a predetermined time, a temperature-controlled treatment is performed, with the temperature maintained at 220℃ and continuously stirred while adding nitrogen gas in real time for protective stirring. Then, a negative pressure reaction is carried out to ensure that the test acid value is ≤0.2mgKOH / g. Then, a catalyst is added, which is monobutyltin oxide or tetrabutyl titanate. At the same time, sodium hydroxide or sodium carbonate is added to the mixture, and after neutralization for 600 seconds, the temperature is raised to 205℃, ensuring that the vacuum degree is ≥-0.09MPa. After heat treatment, the acid value is controlled to ≤0.2mgKOH / g. Then, the mixture is cooled to 100℃ and held at that temperature for 1.8 hours. Then, the bio-based plasticizer mixture is added to a vacuum filter and circulated for filtration under a pressure of 0.6MPa until all impurities are discharged.

[0029] Furthermore, the final mixture is added to a distillation apparatus, and the bio-based plasticizer mixture is distilled at a flow rate of 0.3 cubic meters and a temperature of 275°C with continuous stirring for 45 minutes. Then, the temperature is controlled to reach 63°C to obtain the bio-based plasticizer mixture purified into plasticizer raw material for discharge and packaging.

[0030] Example 2:

[0031] A bio-based plasticizer production process involves weighing the bio-based plasticizer raw materials according to a weight ratio and adding them to a reactor for processing. The materials are added in batches until all the bio-based plasticizer raw materials are added, and simultaneous heating is performed at a temperature of 170℃. This achieves higher mixing efficiency for the bio-based plasticizer raw materials, thus reducing the overall processing time. The bio-based plasticizer raw materials are stirred at a speed of 2200 r / min for a duration of 3 hours. During the process, a water separator continuously discharges the water produced in the reaction. For heating, in addition to electric heating, a light source can be used for supplemental heating; the light source can be ultraviolet light or a fluorescent lamp with a power of 700W.

[0032] Furthermore, after the bio-based plasticizer has been stirred for a predetermined time, a temperature-controlled treatment is performed, with the temperature maintained at 200℃ and continuously stirred while adding nitrogen gas in real time for protective stirring. Then, a negative pressure reaction is carried out to ensure that the test acid value is ≤0.2mgKOH / g. Then, a catalyst is added, which is monobutyltin oxide or tetrabutyl titanate. At the same time, sodium hydroxide or sodium carbonate is added to the mixture. After neutralization for 1000 seconds, the temperature is raised to 225℃, ensuring a vacuum degree of ≥-0.09MPa. After heat treatment, the acid value is controlled to ≤0.2mgKOH / g. Then, the mixture is cooled to 100℃ and held at that temperature for 2.5 hours. The bio-based plasticizer mixture is then added to a vacuum filter and circulated for filtration under a pressure of 0.8MPa until all impurities are discharged.

[0033] Furthermore, the final mixture is added to a distillation apparatus, and the bio-based plasticizer mixture is distilled at a flow rate of 0.1 cubic meters and a temperature of 240°C with continuous stirring for 75 minutes. Then, the temperature is controlled to reach 50°C, and the bio-based plasticizer mixture is purified into plasticizer raw material for discharge and packaging.

[0034] 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 process for producing bio-based plasticizers, characterized in that: The process includes the following steps: S1: Weigh the bio-based plasticizer raw materials according to the weight ratio and add them to the reactor for processing; S2: Esterification treatment, with appropriate addition of catalyst; S3: Refining, mixing, and filtration processes; S4: Distillation, stirring, and purification processes.

2. The bio-based plasticizer production process according to claim 1, characterized in that: The bio-based plasticizer raw material in S1 is processed by stirring, and the material is added in batches until all the bio-based plasticizer raw material is added, while heating is carried out simultaneously at a temperature of 170-260℃.

3. The bio-based plasticizer production process according to claim 1, characterized in that: The bio-based plasticizer raw material in S1 is stirred at a speed of 400-2200 r / min for 1-3 hours, with the water produced during the reaction continuously discharged using a water separator.

4. The bio-based plasticizer production process according to claim 1, characterized in that: The process is based on S2, where temperature is controlled at 200-240℃ with continuous stirring and nitrogen added in real time for protective stirring. Then, a negative pressure reaction is carried out to make the test acid value ≤0.2mgKOH / g, and then a catalyst is added.

5. The bio-based plasticizer production process according to claim 1, characterized in that: In step S3, sodium hydroxide or sodium carbonate is added to the mixture, and then neutralized for 200-1000 seconds. The mixture is then heated to 175-225°C, ensuring a vacuum of ≥-0.09MPa. After the heat treatment, the acid value is controlled to ≤0.2mgKOH / g. The mixture is then cooled to 100°C and held at that temperature for 1.5-2.5 hours.

6. The bio-based plasticizer production process according to claim 1, characterized in that: In step S4, the above-mentioned mixture is added to a distillation apparatus, and during the distillation of the bio-based plasticizer mixture, a flow rate of 0.1-0.5 cubic meters and a temperature of 240-300℃ are used for continuous stirring for 20-75 minutes. Then, after controlling the temperature to reach 50-70℃, the bio-based plasticizer mixture is purified into plasticizer raw material for discharge and packaging.

7. The bio-based plasticizer production process according to claim 5, characterized in that: The bio-based plasticizer mixture prepared in step S3 is added to a vacuum filter and circulated for filtration under a pressure of 0.2-0.8 MPa until all impurities are discharged.

8. The bio-based plasticizer production process according to claim 4, characterized in that: The catalyst in S2 is either monobutyltin oxide or tetrabutyl titanate.

9. The bio-based plasticizer production process according to claim 5, characterized in that: The gas inside the mixture is released based on S3, the reaction solution is cooled to room temperature and magnesium oxide or activated carbon is added and mixed evenly.

10. The bio-based plasticizer production process according to claim 1, characterized in that: When processing the bio-based plasticizer, a light source can be used for supplemental lighting and heating. The light source can be ultraviolet light or fluorescent lamp with a power of 50-700W.