CN201848257U - Novel circulating hydrolyzing device - Google Patents

Novel circulating hydrolyzing device Download PDF

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Publication number
CN201848257U
CN201848257U CN2010206042293U CN201020604229U CN201848257U CN 201848257 U CN201848257 U CN 201848257U CN 2010206042293 U CN2010206042293 U CN 2010206042293U CN 201020604229 U CN201020604229 U CN 201020604229U CN 201848257 U CN201848257 U CN 201848257U
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necked flask
piston
pipe
path
oil bath
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单永奎
孙卓东
丁永杰
张恒强
申欢欢
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East China Normal University
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East China Normal University
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Abstract

本实用新型公开了一种新型循环水解装置,其特点包括恒温磁力搅拌器、油浴锅、三颈烧瓶,支架,所述恒温磁力搅拌器设于支架的底部,油浴锅设于恒温磁力搅拌器的上方,三颈烧瓶设于支架的中部且三颈烧瓶的瓶体位于油浴锅内;所述三颈烧瓶上分别设有分馏管、进样器及溢流管,分馏管上连接储液管,储液管分为三路,第一路连接回流冷凝管、第二路连接第一活塞、第三路连接第二活塞,第二活塞通过橡胶管与溢流管连接。本实用新型采用循环反应的方式,打破了可逆反应的平衡,具有可连续进样、产物分离彻底、水解产率高,易于操控的优点。

Figure 201020604229

The utility model discloses a novel circulating hydrolysis device, which is characterized in that it comprises a constant temperature magnetic stirrer, an oil bath, a three-necked flask, and a bracket. Above the device, the three-necked flask is located in the middle of the support and the bottle body of the three-necked flask is located in the oil bath; The liquid pipe and the liquid storage pipe are divided into three paths, the first path is connected to the return condensing pipe, the second path is connected to the first piston, the third path is connected to the second piston, and the second piston is connected to the overflow pipe through a rubber tube. The utility model adopts a circular reaction mode, which breaks the balance of the reversible reaction, and has the advantages of continuous sample injection, complete product separation, high hydrolysis yield and easy control.

Figure 201020604229

Description

新型循环水解装置 New circulating hydrolysis device

技术领域technical field

本实用新型涉及化学合成与分解技术领域对有机物质实施水解的装置,尤其是一种新型循环水解装置。The utility model relates to a device for hydrolyzing organic substances in the technical field of chemical synthesis and decomposition, in particular to a novel circulating hydrolysis device.

背景技术Background technique

 现有技术的实验室进行水解实验所使用的水解装置一般为回流装置。由于有机化学物质的水解反应一般为可逆反应,在普通的回流装置中,底物、溶剂、催化剂、反应产物混在一起,使可逆反应迅速达到平衡,受反应平衡的限制,水解产率无法提高,不能达到反应产物彻底水解的目的,导致水解产率低,造成原料和催化剂的浪费,有悖绿色化学要求,为提高水解产率,不得不增加产物分离的操作程序。The hydrolysis device that the laboratory of prior art carries out hydrolysis test is generally reflux device. Since the hydrolysis reaction of organic chemical substances is generally a reversible reaction, in an ordinary reflux device, the substrate, solvent, catalyst, and reaction product are mixed together, so that the reversible reaction can quickly reach equilibrium. Limited by the reaction balance, the hydrolysis yield cannot be increased. The purpose of complete hydrolysis of the reaction product cannot be achieved, resulting in low hydrolysis yield, resulting in waste of raw materials and catalysts, which is contrary to the requirements of green chemistry. In order to improve the hydrolysis yield, the operating procedure of product separation has to be increased.

实用新型内容Utility model content

本实用新型的目的是针对现有技术的不足而设计的一种循环水解装置,它采用循环反应的方式,打破了可逆反应的平衡,具有可连续进样、产物分离彻底、水解产率高,易于操控的优点。The purpose of this utility model is a kind of circulation hydrolysis device designed for the deficiencies in the prior art, it adopts the mode of circulation reaction, has broken the balance of reversible reaction, has continuous sampling, product separation is complete, hydrolysis yield is high, The advantage of being easy to handle.

实现本实用新型目的的具体技术方案是:The concrete technical scheme that realizes the utility model purpose is:

一种新型循环水解装置,其特点包括恒温磁力搅拌器、油浴锅、三颈烧瓶,支架,所述恒温磁力搅拌器设于支架的底部,油浴锅设于恒温磁力搅拌器的上方,三颈烧瓶设于支架的中部且三颈烧瓶的瓶体位于油浴锅内;所述三颈烧瓶上分别设有分馏管、进样器及溢流管,分馏管上连接储液管,储液管分为三路,第一路连接回流冷凝管、第二路连接第一活塞、第三路连接第二活塞,第二活塞通过橡胶管与溢流管连接。A new type of circulating hydrolysis device, which features a constant temperature magnetic stirrer, an oil bath, a three-necked flask, and a bracket. The constant temperature magnetic stirrer is arranged at the bottom of the bracket, and the oil bath is arranged above the constant temperature magnetic stirrer. The neck flask is arranged in the middle part of the support and the bottle body of the three-necked flask is located in the oil bath; the three-necked flask is respectively provided with a fractionation tube, a sample injector and an overflow tube, and the fractionation tube is connected with a liquid storage pipe, and the liquid storage The pipe is divided into three paths, the first path is connected to the return condensing pipe, the second path is connected to the first piston, the third path is connected to the second piston, and the second piston is connected to the overflow pipe through a rubber tube.

本实用新型采用循环反应的方式,打破了可逆反应的平衡,具有可连续进样、产物分离彻底、水解产率高,易于操控的优点。The utility model adopts a circular reaction method, which breaks the balance of the reversible reaction, and has the advantages of continuous sample injection, complete product separation, high hydrolysis yield and easy control.

附图说明Description of drawings

    图1为本实用新型的结构示意图。Figure 1 is a schematic structural view of the utility model.

具体实施方式Detailed ways

参阅图1,本实用新型包括恒温磁力搅拌器1、油浴锅2、三颈烧瓶3,支架4,所述恒温磁力搅拌器1设于支架4的底部,油浴锅2设于恒温磁力搅拌器1的上方,三颈烧瓶3设于支架4的中部且三颈烧瓶3的瓶体位于油浴锅2内;所述三颈烧瓶3上分别设有分馏管5、进样器6及溢流管8,分馏管5上连接储液管7,储液管7分为三路,第一路连接回流冷凝管12、第二路连接第一活塞11、第三路连接第二活塞10,第二活塞10通过橡胶管9与溢流管8连接。Referring to Fig. 1, the utility model comprises constant temperature magnetic stirrer 1, oil bath 2, three-necked flask 3, support 4, and described constant temperature magnetic stirrer 1 is located at the bottom of support 4, and oil bath 2 is located at constant temperature magnetic stirrer Above the device 1, the three-necked flask 3 is located in the middle of the support 4 and the bottle body of the three-necked flask 3 is located in the oil bath 2; The flow pipe 8 and the fractionating pipe 5 are connected to the liquid storage pipe 7, and the liquid storage pipe 7 is divided into three paths, the first path is connected to the reflux condensation pipe 12, the second path is connected to the first piston 11, and the third path is connected to the second piston 10. The second piston 10 is connected with the overflow pipe 8 through the rubber tube 9 .

本实用新型是这样使用的:The utility model is used like this:

参阅图1,以缩醛水解为例说明本实用新型的工作过程,通过进样器6给三颈烧瓶3内装入底物缩醛、水和催化剂,经恒温磁力搅拌器1控制油浴锅2的加热温度,给三颈烧瓶3油浴加热,使底物缩醛,水和催化剂在三颈烧瓶3内反应一段时后生成相应的醇和醛,且使水和醇发生共沸,由于缩醛的沸点远高于水和醇,故共沸组分中缩醛的含量极低,醇和水经分馏管5、储液管7及回流冷凝管12,经回流冷凝管12冷凝后储存在储液管7中,由于醇的密度小于水的密度,醇在储液管7的上部,水在储液管7的下部,根据储液体积和密度差额调解溢流管8的高度,水和生成的醛可以通过活塞10循环至三颈烧瓶3中,生成的醇可以通过活塞11由反应体系中分离出,通过进样器6的连续进样,实现缩醛的彻底水解和反应产物的连续分离。Referring to Fig. 1, take acetal hydrolysis as example to illustrate the working process of the present utility model, fill substrate acetal, water and catalyst in the three-necked flask 3 by sample injector 6, control oil bath 2 through constant temperature magnetic stirrer 1 The heating temperature is to heat the oil bath of the three-necked flask 3, so that the substrate acetal, water and catalyst react in the three-necked flask 3 for a period of time to generate corresponding alcohol and aldehyde, and make the water and alcohol azeotrope, due to the acetal The boiling point of alcohol is much higher than that of water and alcohol, so the content of acetal in the azeotropic component is extremely low. Alcohol and water pass through fractionation tube 5, liquid storage tube 7 and reflux condenser tube 12, and are stored in the storage liquid after being condensed by reflux condenser tube 12. In the pipe 7, since the density of alcohol is less than that of water, the alcohol is at the top of the liquid storage pipe 7, and the water is at the bottom of the liquid storage pipe 7. The height of the overflow pipe 8 is adjusted according to the liquid storage volume and density difference, and the water and the generated The aldehyde can be circulated to the three-necked flask 3 through the piston 10, and the generated alcohol can be separated from the reaction system through the piston 11, and the continuous injection of the sampler 6 can realize the complete hydrolysis of the acetal and the continuous separation of the reaction product.

本实用新型适用于水解产物与溶剂能共沸、密度有一定差距且各水解产物在溶剂中的溶解量有明显差异的反应体系,特别适用于缩醛的水解。The utility model is suitable for a reaction system in which a hydrolyzate and a solvent can azeotrope, have a certain density difference, and have obvious differences in the dissolving amount of each hydrolyzate in the solvent, and is especially suitable for the hydrolysis of acetal.

Claims (1)

1.一种新型循环水解装置,其特征在于它包括恒温磁力搅拌器(1)、油浴锅(2)、三颈烧瓶(3),支架(4),所述恒温磁力搅拌器(1)设于支架(4)的底部,油浴锅(2)设于恒温磁力搅拌器(1)的上方,三颈烧瓶(3)设于支架(4)的中部且三颈烧瓶(3)的瓶体位于油浴锅(2)内;所述三颈烧瓶(3)上分别设有分馏管(5)、进样器(6)及溢流管(8),分馏管(5)上连接储液管(7),储液管(7)分为三路,其中,第一路连接回流冷凝管(12)、第二路连接第一活塞(11)、第三路连接第二活塞(10),第二活塞(10)通过橡胶管(9)与溢流管(8)连接。1. A novel circulating hydrolysis device is characterized in that it comprises a constant temperature magnetic stirrer (1), an oil bath (2), a three-necked flask (3), a support (4), and the constant temperature magnetic stirrer (1) Set at the bottom of the bracket (4), the oil bath (2) is set above the constant temperature magnetic stirrer (1), the three-necked flask (3) is set in the middle of the bracket (4) and the bottle of the three-necked flask (3) The body is located in the oil bath (2); the three-necked flask (3) is respectively provided with a fractionation tube (5), a sampler (6) and an overflow tube (8), and the fractionation tube (5) is connected to the storage The liquid pipe (7) and the liquid storage pipe (7) are divided into three paths, wherein the first path is connected to the reflux condensation pipe (12), the second path is connected to the first piston (11), and the third path is connected to the second piston (10 ), the second piston (10) is connected with the overflow pipe (8) through the rubber tube (9).
CN2010206042293U 2010-11-12 2010-11-12 Novel circulating hydrolyzing device Expired - Fee Related CN201848257U (en)

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Granted publication date: 20110601

Termination date: 20161112