Preparation method of gylcol ester type surfactant
By optimizing the esterification reaction process of ethylene glycol ester surfactants and using environmentally friendly processes and equipment, the problems of inefficiency, high cost and environmental pollution in traditional production methods are solved, and efficient, environmentally friendly and economical production results are achieved.
Patent Information
- Application Number
- CN202411633176.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-02-25
AI Technical Summary
The production methods of traditional glycol ester surfactants have problems such as inefficiency, high cost and environmental pollution, including long-term esterification reactions, high-energy-consuming separation processes and environmentally harmful emissions.
By optimizing the esterification reaction process, using an external circulating slurry reactor, controlling the reaction temperature and time, using an environmentally friendly catalyst, and purifying the treatment through reduced pressure distillation and activated carbon adsorption, reducing by-products and energy consumption.
It improves productivity and selectivity, reduces energy consumption and waste emissions, improves economic benefits and product quality, and meets the efficiency, environmental protection and economic requirements of industrial production.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of surfactant preparation, in particular to a method for preparing an ethylene glycol ester type surfactant. Background Art
[0002] Surfactant is a kind of compound with special molecular structure, which can accumulate on the surface of liquid and change the properties of interface. Ethylene glycol ester surfactant has become an important component of many industries such as daily chemical, pharmaceutical, agriculture, oil extraction, etc. due to its excellent surface activity, hydrophilic-hydrophobic balance and environmental friendliness. With the development of industry and the improvement of requirements for environmental protection, developing a method for preparing ethylene glycol ester surfactant that is both economical and efficient and environmentally friendly has become a hot spot in research and industry. Therefore, the present invention focuses on achieving efficient, low-cost and environmentally friendly production of ethylene glycol ester surfactant through innovative chemical processes and engineering technologies.
[0003] Traditional methods for producing glycol ester surfactants usually involve long esterification reactions, energy-intensive separation processes, and the emission of environmentally harmful byproducts. Although traditional production methods have supported the commercial production of surfactants in the past few decades, they are now facing problems such as low efficiency, high costs, and environmental pollution. For example, the traditional esterification process requires a large amount of solvent and energy consumption, and the reaction time is long, which not only increases production costs but also burdens the environment. In addition, the handling of byproducts and insufficient conversion of raw materials are also major problems in traditional methods.
[0004] These problems have prompted researchers and the industry to seek more efficient and environmentally friendly alternative technologies. Therefore, developing a new method for preparing glycol ester-based surfactants that can not only improve yield and selectivity, but also reduce energy consumption and waste emissions is of great significance to meet the needs of sustainable development of modern industry. Summary of the invention
[0005] The object of the present invention is to provide a method for preparing an ethylene glycol ester type surfactant, which optimizes the esterification reaction process, reduces energy consumption, and reduces adverse effects on the environment.
[0006] The present invention is achieved in that:
[0007] A method for preparing an ethylene glycol ester surfactant comprises the following steps:
[0008] S100, adding ethylene glycol, fatty acid and catalyst into a reactor according to the process setting ratio;
[0009] S200, heating the material put in step S100 to 140-170°C;
[0010] S300, stirring and reacting at 140-170°C for 4-6 hours;
[0011] S400, removing byproduct water under reduced pressure conditions of 10-100 mmHg;
[0012] S500, purifying the reactants.
[0013] Preferably, before adding materials into the reactor, an inert gas is first introduced into the reactor to remove oxygen and water vapor in the reactor.
[0014] Preferably, the inert gas is nitrogen or helium.
[0015] Preferably, the ethylene glycol is dehydrated before being fed into the reactor, and the fatty acid is purified before being fed into the reactor.
[0016] Preferably, the feed ratio of ethylene glycol to fatty acid is 1.2:1 to 1.5:1.
[0017] Preferably, the added amount of the catalyst is 0.01-0.1% of the total mass of ethylene glycol and fatty acid.
[0018] Preferably, the catalyst uses tributyltin oxide or sulfuric acid or p-toluenesulfonic acid.
[0019] Preferably, the reactor is a paddle reactor with an external circulation system.
[0020] Preferably, in step S500, vacuum distillation and activated carbon adsorption are used for purification.
[0021] Compared with the prior art, the beneficial effects of the present invention are: the preparation method of the ethylene glycol ester type surfactant provided by the present invention improves economic benefits, reduces energy consumption, and reduces adverse effects on the environment, has significant advantages both technically and economically, can meet the high efficiency, environmental protection and economic requirements of industrial production, and has broad market prospects and application value. DETAILED DESCRIPTION
[0022] A method for preparing an ethylene glycol ester surfactant comprises the following steps:
[0023] S100, ethylene glycol and fatty acids are added to a slurry reactor with an external circulation system in a mass ratio of 1.2:1 to 1.5:1. At the same time, a catalyst of 0.01-0.1% of the total mass of ethylene glycol and fatty acids is added to the reactor. In the esterification reaction of ethylene glycol, the ratio of ethylene glycol to fatty acids directly affects the conversion rate of the reaction and the purity of the product. Through experimental research and simulation optimization, it is found that the ratio of ethylene glycol to fatty acids of 1.2:1 to 1.5:1 can effectively improve the reaction conversion rate while ensuring the high purity of the product. Excess ethylene glycol can promote the transfer of the reaction to the product, but the impact of excess ethylene glycol on the subsequent purification process and the balance of cost-effectiveness also need to be considered. Ethylene glycol needs to be dehydrated before being added to the reactor to ensure its purity and reactivity. Fatty acids need to be purified to remove possible impurities and moisture to ensure the smooth progress of the esterification reaction.
[0024] The type and amount of catalyst have an important influence on the efficiency and product quality of the esterification reaction. Selecting a catalyst with high catalytic activity and low environmental impact, such as tributyltin oxide or a specific acid catalyst, such as sulfuric acid or p-toluenesulfonic acid, can accelerate the reaction process and improve the selectivity and purity of the product. Through reaction kinetics research, it is determined that the optimal amount of catalyst is between 0.01-0.1% of the total mass of ethylene glycol and fatty acids, which can achieve efficient conversion and facilitate post-processing.
[0025] The design of the reactor is crucial to ensure sufficient mixing and effective mass transfer of the reaction materials. An external circulation paddle reactor, that is, a paddle reactor with an external circulation system, is mainly composed of a reactor and an external circulation system, and there is a stirring device in the reactor. The external circulation system extracts part of the material in the reactor through pipes, pumps and other equipment, and then returns it to the reactor after passing through external heat exchangers and other equipment to achieve better heat transfer and material mixing. Therefore, the use of an external circulation paddle reactor can enhance the contact and mixing between the reactants and improve the reaction efficiency. At the same time, the stirring device of the reactor can ensure the uniform reaction of the reaction materials, reduce dead zones and local overheating, and ensure the consistency of product quality. Before adding materials to the reactor, an inert gas is first introduced into the reactor. The inert gas can be nitrogen, helium, etc., so that oxygen and water vapor in the reactor can be removed to prevent possible side reactions and hydrolysis reactions.
[0026] S200, heating the materials added in step S100 to 140-170°C.
[0027] S300, stir and react at 140-170°C for 4-6 hours.
[0028] Reaction temperature and reaction time have a significant impact on the progress of ethylene glycol esterification reaction and product quality. By accurately controlling the reaction temperature within the range of 140-170°C and the reaction time within 4-6 hours, the reaction can be effectively promoted while avoiding side reactions or product degradation caused by excessively high temperatures. A real-time monitoring system can be used to track the reaction progress to ensure that it is carried out under optimal reaction conditions.
[0029] S400, removing by-product water under reduced pressure conditions of 10-100 mmHg helps to promote reaction balance and improve product yield.
[0030] S500, purifying the reactants. After the esterification reaction is completed, it is necessary to remove the unreacted ethylene glycol, fatty acids and other impurities through purification and separation steps to obtain high-purity ethylene glycol ester surfactants. The products can be effectively separated and purified by methods such as vacuum distillation and activated carbon adsorption. During the vacuum distillation process, by precisely controlling the temperature and pressure, the different components can be effectively separated, while reducing the risk of thermal decomposition of heat-sensitive substances. Activated carbon adsorption can further remove pigments, odors and trace impurities, and improve the purity and quality of the product.
[0031] The preparation method of the ethylene glycol ester surfactant provided by the present invention has the following significant advantages:
[0032] 1. Improved yield, selectivity and economic benefits: The present invention significantly improves the yield of the target product by optimizing the reaction material ratio and accurately controlling the reaction conditions. The use of a specific high-efficiency catalyst can accelerate the esterification reaction, reduce the generation of by-products, and thus improve the selectivity of the product. This high conversion rate means that more target products can be obtained from the same amount of raw materials, thereby improving the economic benefits of production.
[0033] 2. Mild reaction conditions, few side reactions, and safe operation: Through carefully designed reaction conditions (such as temperature controlled at 140-170°C and reaction time controlled at 4-6 hours), side reactions that may be caused by excessively high temperatures are avoided, ensuring the quality and purity of the product. Mild reaction conditions help maintain the stability of raw materials, reduce energy consumption, and are also conducive to safe operation.
[0034] 3. Energy saving and environmental protection, reducing waste emissions: In the preparation process, environmentally friendly catalysts and optimized process flows are used to reduce energy consumption and waste emissions. Post-processing steps such as vacuum distillation and activated carbon adsorption effectively remove by-products and unreacted raw materials, reducing waste emissions. These environmental protection measures are in line with the current trend of greening and sustainable development of the industry.
[0035] 4. Reasonable process flow and high degree of automation: The preparation process flow of the present invention has been optimized, and the connection between each step is tight and efficient, which can realize the automation and scale of production, improve production efficiency and product consistency. The improvement of automation also helps to reduce human errors and ensure the stability and reliability of the production process.
[0036] 5. Excellent product quality and performance: The glycol ester surfactant prepared by the present invention has high purity and good chemical stability, so that the product exhibits excellent surface activity and emulsification properties in application. Good product performance enables the surfactant to be widely used in daily chemicals, metal processing, oil extraction and other fields, meeting the high-end needs of the market.
[0037] 6. The raw materials are widely available and the cost is relatively low: the ethylene glycol and fatty acid raw materials used in the present invention are widely available and relatively cheap, which helps to reduce the production cost. At the same time, by improving the reaction yield and optimizing the production process, the production cost per unit product is further reduced, and the market competitiveness is improved.
[0038] In summary, the method for preparing ethylene glycol ester surfactant provided by the present invention has significant advantages both technically and economically, can meet the requirements of high efficiency, environmental protection and economy of industrial production, and has broad market prospects and application value.
[0039] Although the present invention has been described in detail according to the previous embodiments, those skilled in the art should understand that they can still modify the technical solutions in the described embodiments, or replace some or all of the technical features therein with equivalents. These modifications or replacements will not change the essence of the relevant technical solutions and make them exceed the technical scope defined by the various embodiments of the present invention. Except for the technical features described in the specification, all other technical features are known to those skilled in the art.
Claims
1. A method for preparing an ethylene glycol ester type surfactant, characterized in that: The following steps are involved: S100, adding ethylene glycol, fatty acid and catalyst into a reactor according to the process setting ratio; S200, heating the material put into step S100 to 140-170°C; S300, stirring and reacting at 140-170°C for 4-6 hours; S400, removing byproduct water under reduced pressure conditions of 10-100 mmHg; S500, purifying the reactants.
2. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: Before adding materials into the reactor, an inert gas is first introduced into the reactor to remove oxygen and water vapor in the reactor.
3. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The inert gas is nitrogen or helium.
4. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The feed ratio of ethylene glycol to fatty acid is 1.2:1 to 1.5:
1.
5. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The ethylene glycol is dehydrated before being fed into the reactor, and the fatty acid is purified before being fed into the reactor.
6. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The added amount of the catalyst is 0.01-0.1% of the total mass of ethylene glycol and fatty acid.
7. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The catalyst used is tributyltin oxide, sulfuric acid or p-toluenesulfonic acid.
8. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: The reactor used was a paddle reactor having an external circulation system.
9. The method for preparing an ethylene glycol ester type surfactant according to claim 1, characterized in that: In the step S500, the purification process is performed by vacuum distillation and activated carbon adsorption.