阅读说明：本技术 一种n-氰乙基-n-苄基苯胺的制备方法 (Preparation method of N-cyanoethyl-N-benzylaniline ) 是由 阮煜翔 王凯 于 2019-09-23 设计创作，主要内容包括：本发明公开了一种N-氰乙基-N-苄基苯胺的制备方法,具体步骤包括：在处理桶内加入水和N-氰乙基苯胺,随后往处理桶内同时滴入氯化苄和碳酸钠溶液,滴加完毕后加入冰醋酸,搅拌,析出白色固体,过滤,水洗得到成品。(The invention discloses a preparation method of N-cyanoethyl-N-benzylaniline, which comprises the following specific steps: adding water and N-cyanoethylaniline into a treatment barrel, then simultaneously dripping benzyl chloride and sodium carbonate solution into the treatment barrel, adding glacial acetic acid after dripping is finished, stirring, separating out white solid, filtering, and washing with water to obtain a finished product.)

1. A preparation method of N-cyanoethyl-N-benzylaniline is characterized by comprising the following steps: the method comprises the following specific steps: adding water and N-cyanoethylaniline into a treatment barrel, then simultaneously dripping benzyl chloride and a sodium carbonate solution into the treatment barrel, adding glacial acetic acid after dripping is finished, stirring, separating out a white solid, filtering, and washing with water to obtain a finished product;

A treatment cavity is arranged in the treatment barrel (1), a through groove is arranged on the side wall of the treatment box (1), a first mounting plate (4) penetrates through the through groove, a partition plate (41) is arranged on the first mounting plate (4), the processing cavity is divided into an upper cavity and a lower cavity by the partition plate (41), the side wall of the lower cavity is provided with an opening, a material receiving box (3) is arranged in the lower cavity in a penetrating way, a stirring component is arranged in the upper cavity, a second mounting plate (13) is arranged at the top of the treatment barrel (1), a storage barrel (5) is arranged on the second mounting plate (13), a push plate (55) is arranged in the storage barrel (5), a heating block is also arranged in the upper chamber, a support rod is arranged at the top of the treatment barrel (1), a third mounting plate (2) is arranged on the support rod, the third mounting plate (2) is provided with a first air cylinder (22) for pushing the push plate (55) to move downwards; benzyl chloride and sodium carbonate solution are respectively placed in different storage barrels (5), water and N-cyanoethylaniline are placed in an upper chamber, a heating block works to increase the temperature in the upper chamber, a stirring assembly stirs the solution to heat the solution to a specified temperature, then a first air cylinder (22) pushes a push plate (55) to move downwards, reaction liquid in the storage barrels (5) is pushed out from the storage barrels (5) to be dripped into the upper chamber, and the reaction liquid flows together with the liquid in the upper chamber after being dripped into the upper chamber, so that the two reaction liquids are contacted and react to complete the preparation of the N-cyanoethyl-N-benzylaniline; after the product is prepared, the partition plate (41) is drawn out from the through groove, so that the upper chamber is communicated with the lower chamber, the reaction liquid in the upper chamber directly falls into the material receiving box (3), and the reaction liquid is discharged from the treatment cavity.

2. the process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: after water and N-cyanoethylaniline are added into the upper chamber, the solution is heated to 90-100 ℃ by the heating block, and then benzyl chloride and sodium carbonate solution are dripped into the solution.

3. The process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: after the dropwise addition of the benzyl chloride and sodium carbonate solution is completed, the benzyl chloride and the sodium carbonate solution are reacted for 3 hours at the temperature of 90-100 ℃.

4. The process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: after glacial acetic acid was added to the solution, the solution was cooled to 30 ℃ while stirring the solution.

5. The process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: the concentration of the sodium carbonate solution is 20%.

6. The process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: the support rod is provided with a first connecting plate and a second connecting plate, the first connecting plate and the second connecting plate are respectively arranged on two sides of the treatment barrel (1), the third mounting plate (2) is provided with a first sliding block, the first connecting plate is provided with a first sliding groove matched with the first sliding block, the second connecting plate is provided with a connecting groove, the third mounting plate (2) is provided with a first through hole matched with the connecting groove, a fixed block (241) penetrates through the first through hole, the side wall of the fixed block (241) is provided with a third connecting plate (243), the inner wall of the first through hole is provided with a first movable groove matched with the third connecting plate (243), the third connecting plate (243) is provided with a connecting spring, and the top of the fixed block (241) is provided with a fourth connecting plate (24); after adding benzyl chloride and sodium carbonate solution into storage vat (5), up pulling fourth connecting plate (24), pull out fixed block (241) from the spread groove, promote third mounting panel (2) along first spout, promote third mounting panel (2) to processing barrel (1) one side, place storage vat (5) in the assigned position on second mounting panel (13) after, promote third mounting panel (2) again along first spout, third mounting panel (2) remove to processing barrel (1) top, make fixed block (241) remove to the spread groove top, push fixed block (241) in the spread groove, it is fixed with third mounting panel (2), make first cylinder (22) and push pedal (55) form the cooperation, in order to drop the reaction liquid in storage vat (5) into the processing chamber make the reaction normally go on.

7. The process for producing N-cyanoethyl-N-benzylaniline according to claim 1, wherein: a groove is formed in the second mounting plate (13), a cover plate (51) matched with the groove is arranged at one end of the storage barrel (5), a rubber film is arranged on the inner wall of the groove, and the cover plate (51) is connected to the storage barrel (5) through threads; a second chute is arranged on the inner wall of the storage barrel (5), a second sliding block matched with the second chute is arranged on the side wall of the push plate (55), and a first supporting spring (551) is arranged on the second sliding block; a discharge hole is formed in the bottom of the storage barrel (5), a connecting ring matched with the discharge hole is arranged at the bottom of the storage barrel (5), a discharge pipe (56) is connected onto the connecting ring through threads, a second through hole matched with the discharge pipe (56) is formed in the bottom of the groove, and a first baffle (52) is rotatably connected into the discharge hole; when reaction liquid is added into the storage barrel (5), the storage barrel (5) is taken out from the second mounting plate (13), the cover plate (51) is rotated out from the storage barrel (5), the push plate (55) is arranged at the bottom of the storage barrel (5), so that the reaction liquid is added into the storage barrel (5), after the reaction liquid is filled, the cover plate (51) is rotated into the storage barrel (5), the discharge pipe (56) is rotated into the cover plate (51), the storage barrel (5) is inverted, the discharge pipe (56) is inserted into the second through hole, the cover plate (51) is embedded into the groove to fix the storage barrel (5), and the storage barrel (5) is arranged above the processing cavity to enable the reaction liquid to be dripped into the processing cavity.

Technical Field

The invention belongs to the technical field of dye preparation, and particularly relates to a preparation method of N-cyanoethyl-N-benzylaniline.

Background

The cyanoethyl-N-benzylaniline is a white powder with a melting point of 97.2-102.3 ℃. N-cyanoethyl-N-benzylaniline is an important organic intermediate which is widely applied to synthesis of pesticides, dyes and the like, the demand in China is large at present, the national enterprises in south such as Shanghai Wenzhou mainly produce the N-cyanoethyl-N-benzylaniline, and the product supply is insufficient. The production factories in China are few, and the N-cyanoethylbenzylaniline mainly depends on import from countries such as America, Japan and the like, so that the N-cyanoethylbenzylaniline has good prospect and great economic benefit in China.

The preparation of the N-cyanoethyl-N-benzylaniline relates to a plurality of processes, reaction liquid raw materials need to be carried for a plurality of times in the existing preparation of the N-cyanoethyl-N-benzylaniline, the reaction steps are complicated, and the output rate of the N-cyanoethyl-N-benzylaniline is influenced.

Disclosure of Invention

The invention provides a preparation method of N-cyanoethyl-N-benzylaniline, aiming at overcoming the defects of the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of N-cyanoethyl-N-benzylaniline comprises the following specific steps: adding water and N-cyanoethylaniline into a treatment barrel, then simultaneously dripping benzyl chloride and a sodium carbonate solution into the treatment barrel, adding glacial acetic acid after dripping is finished, stirring, separating out a white solid, filtering, and washing with water to obtain a finished product;

A treatment cavity is arranged in the treatment barrel, a through groove is formed in the side wall of the treatment box, a first mounting plate is arranged in the through groove in a penetrating manner, a partition plate is arranged on the first mounting plate and divides the treatment cavity into an upper chamber and a lower chamber, an opening is formed in the side wall of the lower chamber, a material receiving box is arranged in the lower chamber in a penetrating manner, a stirring assembly is arranged in the upper chamber, a second mounting plate is arranged at the top of the treatment barrel, a storage barrel is arranged on the second plate, a push plate is arranged in the storage barrel, a heating block is further arranged in the upper chamber, a support rod is arranged at the top of the treatment barrel, a third mounting plate is arranged on the support rod, and a first air cylinder for pushing the push; benzyl chloride and sodium carbonate solution are respectively placed in different storage barrels, water and N-cyanoethylaniline are placed in an upper chamber, a heating block works to raise the temperature in the upper chamber, a stirring assembly stirs the solution, the solution is heated to a specified temperature, then a first air cylinder pushes a push plate to move downwards, reaction liquid in the storage barrels is pushed out from the storage barrels, the reaction liquid is dripped into the upper chamber and flows together with the liquid in the upper chamber after being dripped into the upper chamber, and the two reaction liquids are contacted to react, so that the preparation of the N-cyanoethyl-N-benzylaniline is completed; after the product is manufactured, the partition plate is pulled out from the through groove, so that the upper chamber is communicated with the lower chamber, the reaction liquid in the upper chamber directly falls into the material receiving box, and the reaction liquid is discharged from the treatment cavity.

The treatment cavity is divided into an upper cavity and a lower cavity under the action of the partition plate, so that reaction liquid is directly discharged into a material receiving box in the lower cavity after reaction in the upper cavity, the waste liquid after the reaction is collected conveniently, the preparation of the N-cyanoethyl-N-benzylaniline is smoothly carried out, the collection treatment of the waste liquid is conveniently carried out, and the preparation efficiency of the N-cyanoethyl-N-benzylaniline is improved; the reaction of various reaction liquids can be completed in the upper chamber to generate the N-cyanoethyl-N-benzylaniline, the reaction liquids do not need to be carried, the waste of the reaction liquids in the carrying process is reduced, and the yield of the N-cyanoethyl-N-benzylaniline product is improved; the first cylinder is utilized to control the dripping amount of the benzyl chloride and sodium carbonate solution, so that the control precision of the benzyl chloride and sodium carbonate solution is improved, a proper amount of benzyl chloride and sodium carbonate solution is added into the upper chamber, the reaction is normally carried out, and the stability of the reaction is ensured; under the mutual cooperation of the storage vat and the second mounting plate, the storage vat is directly taken down from the second mounting plate, so that reaction liquid can be conveniently added into the storage vat, and the difficulty in preparing the N-cyanoethyl-N-benzylaniline is reduced.

After water and N-cyanoethylaniline are added into the upper chamber, the solution is heated to 90-100 ℃ by the heating block, and then benzyl chloride and sodium carbonate solution are dripped into the solution.

After the dropwise addition of the benzyl chloride and sodium carbonate solution is completed, the benzyl chloride and the sodium carbonate solution are reacted for 3 hours at the temperature of 90-100 ℃.

After glacial acetic acid was added to the solution, the solution was cooled to 30 ℃ while stirring the solution.

The concentration of the sodium carbonate solution is 20%.

The support rod is provided with a first connecting plate and a second connecting plate, the first connecting plate and the second connecting plate are respectively arranged on two sides of the treatment barrel, the third mounting plate is provided with a first sliding block, the first connecting plate is provided with a first sliding groove matched with the first sliding block, the second connecting plate is provided with a connecting groove, the third mounting plate is provided with a first through hole matched with the connecting groove, a fixed block penetrates through the first through hole, the side wall of the fixed block is provided with a third connecting plate, the inner wall of the first through hole is provided with a first movable groove matched with the third connecting plate, the third connecting plate is provided with a connecting spring, and the top of the fixed block is provided with a fourth connecting plate; after benzyl chloride and sodium carbonate solution are added into a storage vat, a fourth connecting plate is pulled upwards, a fixed block is pulled out from a connecting groove, a third mounting plate is pushed along a first sliding groove, the third mounting plate is pushed to one side of a treatment vat, the storage vat is placed at a designated position on the first mounting plate, the third mounting plate is pushed again along the first sliding groove, the third mounting plate moves to the position above the treatment vat, the fixed block moves to the position above the connecting groove, the fixed block is pushed into the connecting groove, the third mounting plate is fixed, a first air cylinder is matched with a push plate, and reaction liquid in the storage vat is dripped into a treatment cavity to enable the reaction to be normally carried out; under the mutual matching of the fixing block and the connecting groove as well as the sliding block and the sliding groove, the third mounting plate is fixed, so that the first cylinder is positioned above the storage barrel, the push plate in the storage barrel is pushed downwards under the action of the first cylinder, the benzyl chloride and the sodium carbonate solution are continuously and normally added into the upper chamber, and the reaction is normally carried out; the third connecting plate is pressed at the bottom of the first movable groove under the action of the connecting spring, so that the connecting effect of the fixing block and the connecting groove is improved, and the fixing effect of the third mounting plate is ensured; under the setting of fourth connecting plate, pulling fixed block that can be convenient removes to it does the installation to the storage vat to move the third mounting panel.

a groove is formed in the second mounting plate, a cover plate matched with the groove is arranged at one end of the storage barrel, a rubber film is arranged on the inner wall of the groove, and the cover plate is connected to the storage barrel through threads; a second chute is arranged on the inner wall of the storage barrel, a second sliding block matched with the second chute is arranged on the side wall of the push plate, and a first supporting spring is arranged on the second sliding block; the bottom of the storage barrel is provided with a discharge hole, the bottom of the storage barrel is provided with a connecting ring matched with the discharge hole, the connecting ring is connected with a discharge pipe through threads, the bottom of the groove is provided with a second through hole matched with the discharge pipe, and a first baffle plate is rotatably connected in the discharge hole; when reaction liquid is added into the storage barrel, the storage barrel is taken out of the second mounting plate, the cover plate is rotated out of the storage barrel, the push plate is arranged at the bottom of the storage barrel so that the reaction liquid can be added into the storage barrel, after the reaction liquid is filled, the cover plate is rotated onto the storage barrel, the discharging pipe is rotated onto the cover plate, the storage barrel is inverted, the discharging pipe is inserted into the second through hole, the cover plate is embedded into the groove to fix the storage barrel, and the storage barrel is arranged above the treatment cavity so that the reaction liquid can be dripped into the treatment cavity; under the threaded connection of the cover plate and the storage barrel, the storage barrel is opened to add the reaction liquid into the storage barrel, so that the adding difficulty of the reaction liquid is reduced; after the first air cylinder pushes the push plate to move downwards, the first air cylinder drives the piston rod to move upwards, the first supporting spring pushes the push plate to move upwards, and automatic resetting of the push plate is completed so that reaction liquid can be added into the storage barrel; the proper discharge pipes can be selected to be connected according to the required discharge amount, so that the discharge amounts in different storage barrels are different, different reaction liquids are added into the upper chamber according to proper proportion to be subjected to reaction treatment, and the waste of the reaction liquids is reduced; the friction force between the cover plate and the inner wall of the groove is increased under the action of the rubber film, and the matching effect of the cover plate and the groove is improved, so that the connecting effect of the storage barrel and the second mounting plate is improved; first baffle plays sealed effect to the discharge gate, prevents that the reaction liquid in the storage vat from spilling in the discharge gate, makes first baffle and push pedal mutually support to do accurate control to the reaction liquid.

The invention has the following advantages: the reaction of various reaction liquids can be completed in the upper chamber to generate the N-cyanoethyl-N-benzylaniline, the reaction liquids do not need to be carried, the waste of the reaction liquids in the carrying process is reduced, and the yield of the N-cyanoethyl-N-benzylaniline product is improved.

Drawings

FIG. 1 is a schematic view of a barrel according to the present invention.

FIG. 2 is a first cross-sectional view of the barrel of the present invention.

FIG. 3 is a schematic sectional view of a second exemplary embodiment of a barrel of the present invention.

Fig. 4 is an enlarged view of a portion a in fig. 3.

Fig. 5 is an enlarged view of fig. 3 at B.

FIG. 6 is a third schematic sectional view of the barrel of the present invention.

Fig. 7 is an enlarged view of fig. 6 at C.

Fig. 8 is an enlarged view of fig. 6 at D.

Fig. 9 is an enlarged view of fig. 6 at E.

Fig. 10 is an enlarged view of fig. 6 at F.

Fig. 11 is a fourth schematic cross-sectional view of the present invention.

Fig. 12 is an enlarged view at G in fig. 11.

Fig. 13 is an enlarged view of fig. 11 at H.

Detailed Description