阅读说明：本技术 一种1-乙烯咪唑、其合成方法及合成装置 (1-vinyl imidazole, and synthesis method and synthesis device thereof ) 是由 沈健 吴天平 谢韦 邱欣欣 祁刚 于 2019-07-02 设计创作，主要内容包括：本发明涉及一种1-乙烯咪唑,由以下重量百分比原料构成：咪唑20%—40%、氢氧化钾15%—35%、乙炔15%—21%,余量为甲苯。其合成工艺包括反应釜预处理,物料混合,合成及减压蒸馏等四个步骤。本发明与现有技术相比,具有通用性好,操作简便的优势,一方面可极大的提高1-乙烯咪唑生产作业效率,降低物料损耗,另一方面可有效的提高生产产品纯度,降低杂质污染风险,从而在极大的提高了1-乙烯咪唑产品的生产效率和产品品质的同时,有效的降低了1-乙烯咪唑生产成本和物料损耗。(The invention relates to 1-vinylimidazole which is prepared from the following raw materials in percentage by weight: 20-40% of imidazole, 15-35% of potassium hydroxide, 15-21% of acetylene and the balance of toluene. The synthesis process comprises four steps of reaction kettle pretreatment, material mixing, synthesis, reduced pressure distillation and the like. Compared with the prior art, the method has the advantages of good universality and simple and convenient operation, can greatly improve the production operation efficiency of the 1-vinylimidazole and reduce the material loss on the one hand, and can effectively improve the purity of the produced product and reduce the impurity pollution risk on the other hand, thereby effectively reducing the production cost and the material loss of the 1-vinylimidazole while greatly improving the production efficiency and the product quality of the 1-vinylimidazole product.)

1. 1-vinylimidazole characterized in that: the 1-vinylimidazole is prepared from the following raw materials in percentage by weight: 20-40% of imidazole, 15-35% of potassium hydroxide, 15-21% of acetylene and the balance of toluene.

2. A 1-vinylimidazole according to claim 1 wherein: the purity of the imidazole, the potassium hydroxide, the acetylene and the toluene is not lower than 95 percent.

3. A1-vinyl imidazole synthesis process is characterized in that: the synthesis process of the 1-vinyl imidazole comprises the following steps:

s1, pretreating a reaction kettle, namely firstly introducing inert gas into the reaction kettle to ensure that the air pressure in the reaction kettle is 0.5-1.5 times of standard atmospheric pressure and the oxygen content is not more than 3%, then uniformly heating to 40-60 ℃ at a speed of 10-25 ℃/min under the condition of ensuring the air pressure in the reaction kettle to be stable, and preserving heat for 1-5 minutes;

s2, mixing the materials, after the step S1 is finished, firstly adding toluene into the reaction kettle under the condition that the temperature and the pressure of the reaction kettle are kept constant, then sequentially adding imidazole and potassium hydroxide into the reaction kettle, mixing the imidazole and the potassium hydroxide with the toluene, then unidirectionally stirring the mixture in the reaction kettle at a constant speed, simultaneously heating the mixture to 75-85 ℃ at a constant speed of 10-25 ℃/min, and keeping the stirring state and the temperature constant;

s3, synthesizing, after the step S2 is completed, firstly discharging inert gas in the reaction kettle, then adding acetylene gas into the reaction kettle, mixing the acetylene gas with the mixed materials in the reaction kettle and the reaction kettle, after the acetylene is mixed, preserving the heat of the mixture in the reaction kettle for 15-35 hours under the condition of keeping the stirring state unchanged, and then naturally cooling the mixture in the reaction kettle to 45-60 ℃ along with the reaction kettle;

and S4, carrying out reduced pressure distillation on the mixture obtained in the step S3, firstly separating the toluene from the mixture, and after the toluene is separated, continuing carrying out reduced pressure distillation on the mixture in the reaction kettle to obtain a finished product.

4. The process according to claim 3, wherein the inert gas in the step S1 is any one of nitrogen and carbon dioxide.

5. The process of claim 3, wherein the step S1 to S4 are performed by stirring the materials in the reaction kettle at constant speed and ultrasonic stirring at 50-300 rpm.

6. The process according to claim 3, wherein in the step S3, when acetylene is introduced into the reaction kettle, acetylene gas is introduced into the reaction kettle from the upper surface of the mixture in the reaction kettle and the interior of the mixed solution at the same time and is mixed with the mixture in the reaction kettle.

7. A process as claimed in claim 6, wherein the amount of acetylene introduced directly into the mixture is 2.5 to 5 times the amount of acetylene introduced onto the upper surface of the mixture.

8. The reaction kettle of claim 3, wherein the reaction kettle comprises a kettle body, at least one ultrasonic stirring device, at least three aeration pipes and air guide nozzles, wherein the ultrasonic stirring device is embedded in the kettle body and coaxially distributed with the kettle body, the aeration pipes are all positioned in the kettle body, one aeration pipe is connected with the lower end surface of the kettle body and is spirally distributed around the axis of the kettle body, the other two aeration pipes are embedded in the inner surface of the side wall of the kettle body and are distributed in parallel with the axis of the kettle body, the aeration pipes embedded in the inner surface of the side wall of the kettle body are all uniformly distributed around the axis of the kettle body, the air guide nozzles are at least three and are positioned in the kettle body and are mutually connected with the upper end surface of the kettle body, the air guide nozzles are uniformly distributed around the axis of the kettle body, and the axes of the air guide nozzles intersect with the axis of the kettle body and form an included angle of 45-15 degrees, and the distance between the intersection of the axis of the gas guide nozzle and the axis of the kettle body and the bottom of the kettle body is not more than the height 1/2 of the kettle body.

9. The reactor of claim 8, wherein the aeration pipe is uniformly provided with a plurality of aeration ports, the diameter of each aeration port is not more than 3 mm, and the total area of the aeration ports is 10-40% of the total area of the outer surface of the aeration pipe.

Technical Field

The invention relates to a preparation process of 1-vinylimidazole, belonging to the field of chemical industry.

Background

1-vinyl imidazole has extremely wide application in the fields of polymer resin materials, photosensitive reagents, petrochemical industry and the like, the prior preparation process and equipment which are usually adopted when 1-vinyl imidazole is produced and prepared can meet the requirement on the production and preparation of 1-vinyl imidazole, but in the preparation process, on one hand, the defects of low material mixing and synthesizing operation efficiency, serious material waste, poor finished product purity, easy pollution by external impurities and the like exist, so the production quality and efficiency of 1-vinyl imidazole products are seriously influenced, and on the other hand, the defects of relatively high production cost of 1-vinyl imidazole, serious material waste and the like also exist, so aiming at the problem, the development of a brand new 1-vinyl imidazole production process and equipment matched with the production process is urgently needed, to meet the requirements of production and use.

Disclosure of Invention

The invention aims to overcome the defects and provide a preparation process of 1-vinylimidazole. The technical scheme adopted by the invention for solving the technical problems is as follows:

in order to realize the purpose, the invention is realized by the following technical scheme:

1-vinylimidazole which is prepared from the following raw materials in percentage by weight: 20-40% of imidazole, 15-35% of potassium hydroxide, 15-21% of acetylene and the balance of toluene.

Furthermore, the purity of the imidazole, the potassium hydroxide, the acetylene and the toluene is not lower than 95%.

A1-vinyl imidazole synthesis process comprises the following steps:

s1, pretreating a reaction kettle, namely firstly introducing inert gas into the reaction kettle to ensure that the air pressure in the reaction kettle is 0.5-1.5 times of standard atmospheric pressure and the oxygen content is not more than 3%, then uniformly heating to 40-60 ℃ at a speed of 10-25 ℃/min under the condition of ensuring the air pressure in the reaction kettle to be stable, and preserving heat for 1-5 minutes;

s2, mixing the materials, after the step S1 is finished, firstly adding toluene into the reaction kettle under the condition that the temperature and the pressure of the reaction kettle are kept constant, then sequentially adding imidazole and potassium hydroxide into the reaction kettle, mixing the imidazole and the potassium hydroxide with the toluene, then unidirectionally stirring the mixture in the reaction kettle at a constant speed, simultaneously heating the mixture to 75-85 ℃ at a constant speed of 10-25 ℃/min, and keeping the stirring state and the temperature constant;

s3, synthesizing, after the step S2 is completed, firstly discharging inert gas in the reaction kettle, then adding acetylene gas into the reaction kettle, mixing the acetylene gas with the mixed materials in the reaction kettle and the reaction kettle, after the acetylene is mixed, preserving the heat of the mixture in the reaction kettle for 15-35 hours under the condition of keeping the stirring state unchanged, and then naturally cooling the mixture in the reaction kettle to 45-60 ℃ along with the reaction kettle;

and S4, carrying out reduced pressure distillation on the mixture obtained in the step S3, firstly separating the toluene from the mixture, and after the toluene is separated, continuing carrying out reduced pressure distillation on the mixture in the reaction kettle to obtain a finished product.

Further, the inert gas in the step S1 is any one of nitrogen and carbon dioxide.

Further, the materials in the reaction kettle are continuously stirred at a constant speed in the steps from S1 to S4, and ultrasonic stirring is adopted during stirring operation, wherein the stirring speed is 50-300 r/min.

Further, in the step S3, when acetylene is introduced into the reaction kettle, acetylene gas is simultaneously introduced into the reaction kettle from the upper surface of the mixture in the reaction kettle and the interior of the mixed solution, and is mixed with the mixture in the reaction kettle.

Further, the amount of acetylene directly introduced into the mixture is 2.5 to 5 times the amount of acetylene introduced onto the upper surface of the mixture.

A reaction kettle for a 1-vinyl imidazole preparation process, which comprises a kettle body, an ultrasonic stirring device, an aeration pipe and an air guide nozzle, wherein at least one ultrasonic stirring device is embedded in the kettle body and is coaxially distributed with the kettle body, at least three aeration pipes are arranged in the kettle body, one of the aeration pipes is connected with the lower end surface of the kettle body and distributed in a spiral structure around the axis of the kettle body, and at least two other aeration pipes are embedded on the inner surface of the side wall of the kettle body and distributed in parallel with the axis of the kettle body, and all the aeration pipes embedded on the inner surface of the side wall of the kettle body are uniformly distributed around the axis of the kettle body, at least three air guide nozzles are arranged in the kettle body and are mutually connected with the upper end surface of the kettle body, the air guide nozzles are uniformly distributed around the axis of the kettle body, and the axes of the air guide nozzles are intersected with the axis of the kettle body and form an included angle of 45-15 degrees, and the distance between the intersection of the axes of the air guide nozzles and the axis of the kettle body and the bottom of the kettle body is not more than the height 1/2 of the kettle body.

Furthermore, a plurality of aeration openings are uniformly distributed on the aeration pipe, the diameters of the aeration openings are not more than 3 mm, and the total area of the aeration openings is 10% -40% of the total area of the outer surface of the aeration pipe.

Compared with the prior art, the method has the advantages of good universality and simple and convenient operation, can greatly improve the production operation efficiency of the 1-vinylimidazole and reduce the material loss on the one hand, and can effectively improve the purity of the produced product and reduce the impurity pollution risk on the other hand, thereby effectively reducing the production cost and the material loss of the 1-vinylimidazole while greatly improving the production efficiency and the product quality of the 1-vinylimidazole product.

Drawings

FIG. 1 is a flow chart of the method of the present invention;

FIG. 2 is a schematic view of the reaction vessel structure.

Detailed Description