Improved method of catalyst for producing n-butyl acetate
阅读说明：本技术 一种乙酸正丁酯生产用催化剂的改进方法 (Improved method of catalyst for producing n-butyl acetate ) 是由 郑铁江 马阳升 陶植 吴晓明 赵跃 王忠法 周国君 万鹏 邹淼 于 2020-06-22 设计创作，主要内容包括：本发明涉及绿色环保溶剂技术领域,具体公开了一种乙酸正丁酯生产用催化剂的改进方法,采用新型的固体超强酸催化剂来替代传统浓硫酸,将固体酸催化剂或组合作为填料分别放置于反应塔顶部和精馏塔入口处,待反应物基本都转化为乙酸丁酯后,再通过精馏得到理想的乙酸正丁酯产品。本发明通过采用固体超强酸催化剂和优化生产工艺,降低生产成本,提高产品的附加值及其质量,使乙酸正丁酯的生产过程变得更加环保无害,制得的产品乙酸正丁酯质量在国家标准的基础上得到进一步提高：质量百分含量：≥99.8％；酸度：≤0.005％,具有很大的经济效益和社会效益。(The invention relates to the technical field of green environment-friendly solvents, and particularly discloses an improved method of a catalyst for producing n-butyl acetate. The invention reduces the production cost and improves the added value and the quality of the product by adopting the solid super acidic catalyst and optimizing the production process, so that the production process of the n-butyl acetate becomes more environment-friendly and harmless, and the quality of the prepared n-butyl acetate product is further improved on the basis of national standards: the mass percentage content is as follows: not less than 99.8%; acidity: less than or equal to 0.005 percent, and has great economic and social benefits.)
1. An improved method of a catalyst for producing n-butyl acetate is characterized in that: the method comprises the following steps:
s1, mixing TiO2、Fe2O3ZrO, ZnO and Al2O3Dissolving one or more soluble salts with distilled water, and adjusting pH of the solution with ammonia water toAlkaline, precipitating, washing and drying;
s2, dissolving the solid obtained in S1 in H2SO4Concentrating the solution at 70-100 deg.C;
s3, transferring the concentrated thick liquid in the S2 to 500-800 ℃ below a muffle furnace for roasting for 3-6h to prepare SO4 2-A solid super acidic catalyst;
s4, adding SO4 2-The solid super acidic catalyst is a filler and is placed at the top of the reaction tower and the inlet of the rectifying tower, and after reactants are basically converted into n-butyl acetate in the production of the n-butyl acetate, an ideal n-butyl acetate product is obtained at the bottom of the tower through rectification.
2. The improvement of a catalyst for the production of n-butyl acetate as claimed in claim 1, wherein H in S22SO4The molar volume unit of the solution is 0.1-1 mol/L.
Technical Field
The invention relates to the technical field of green and environment-friendly solvents, in particular to an improved method of a catalyst for producing n-butyl acetate.
Background
The traditional industrial production mode of n-butyl acetate generally utilizes acetic acid and butanol to directly dehydrate and condense under the catalytic action of concentrated sulfuric acid to generate n-butyl acetate, and the catalyst of the method is concentrated sulfuric acid and has low cost. While the concentrated sulfuric acid is used as a catalyst, the concentrated sulfuric acid continuously absorbs water generated in the esterification reaction, so that the reaction is promoted to move to the right, and the ideal reaction efficiency is obtained. The traditional production process is widely applied to chemical industrial production in China at present, but the concentrated sulfuric acid causes corrosion to equipment and the like to a certain extent, increases the maintenance cost of the equipment, is complex in production process, wastes a large amount of manpower and material resources, increases the production cost, has low yield and cannot meet the market demand in time.
The n-butyl acetate is used as an environment-friendly industrial raw material and has wide market prospect. The research on n-butyl acetate is carried out at home and abroad, mainly focuses on the aspect of catalytic process, but has a plurality of defects from the implementation of production, and various manufacturers also actively optimize the process, particularly actively research on the aspect of energy consumption.
Disclosure of Invention
The invention aims to provide an improved method of a catalyst for producing n-butyl acetate, which replaces the traditional concentrated sulfuric acid with a novel solid super acidic catalyst, places the solid super acidic catalyst as a filler at the top of a reaction tower and the inlet of a rectifying tower, and rectifies after reactants are basically converted into n-butyl acetate, so that the quality of the prepared product n-butyl acetate is further improved on the basis of national standards: the mass percentage content is as follows: not less than 99.8%; acidity: less than or equal to 0.005 percent.
In order to realize the purpose, the technical scheme is as follows: an improved process for producing a catalyst for n-butyl acetate production comprising the steps of:
s1, mixing TiO2、Fe2O3ZrO, ZnO and Al2O3Dissolving one or more soluble salts corresponding to the combination with distilled water, adjusting the pH of the solution to be alkaline by ammonia water, precipitating, washing and drying;
s2, dissolving the solid obtained in S1 in H2SO4Concentrating the solution at 70-100 deg.C;
s3, transferring the concentrated thick liquid in the S2 to 500-800 ℃ below a muffle furnace for roasting for 3-6h to prepare SO4 2-A solid super acidic catalyst;
s4, adding SO4 2-The solid super acidic catalyst is a filler and is placed at the top of the reaction tower and the inlet of the rectifying tower, and after reactants are basically converted into n-butyl acetate in the production of the n-butyl acetate, an ideal n-butyl acetate product is obtained at the bottom of the tower through rectification.
Further, H in S22SO4The molar volume unit of the solution is 0.1-1 mol/L.
The invention has the beneficial effects that: the invention reduces the production cost and improves the added value and the quality of the product by adopting the solid super acidic catalyst and optimizing the production process, so that the production process of the n-butyl acetate becomes more environment-friendly and harmless, and the quality of the prepared n-butyl acetate product is further improved on the basis of national standards: the mass percentage content is as follows: not less than 99.8%; acidity: less than or equal to 0.005 percent.
Detailed Description
The following describes the specific embodiments of the present invention with reference to examples, so that the technical solutions and the advantages thereof are more clear and clear. The following described embodiments are exemplary and are intended to be illustrative of the invention, but are not to be construed as limiting the invention.
In the specific embodiment of the invention, the invention specifically discloses an improved method of a catalyst for producing n-butyl acetate, which comprises the following specific steps:
s1, mixing TiO2、Fe2O3ZrO, ZnO and Al2O3Dissolving one or more soluble salts corresponding to the combination with distilled water, adjusting the pH of the solution to be alkaline by ammonia water, precipitating, washing and drying;
s2, dissolving the solid obtained in S1 in 0.1-1mol/L H2SO4Concentrating the solution at 70-100 deg.C;
s3, transferring the concentrated thick liquid in the S2 to 500-800 ℃ below a muffle furnace for roasting for 3-6h to prepare SO4 2-A solid super acidic catalyst;
s4, adding SO4 2-The solid super acidic catalyst is a filler and is placed at the top of the reaction tower and the inlet of the rectifying tower, and after reactants are basically converted into n-butyl acetate in the production of the n-butyl acetate, an ideal n-butyl acetate product is obtained at the bottom of the tower through rectification.