I Have a Research Support System

On Wednesday morning, it was originally planned that Xu Qiu and Han Jiaying took Wu Shengnan to Zhangjiang for a synthesis.

As a result, Xu Qiu received a call from Teacher Wei at around 8 o'clock in the morning. At this time, he was having breakfast with his school girl in the cafeteria and turned on the hands-free.

"Hey, Teacher Wei?" Xu Qiu was a little confused. Wei Xingsi usually sends messages or emails. What things must be called to explain?

"The review comments for that EES article are back, and make some changes." Wei Xingsi's voice came from the earpiece.

"Hey, I haven't received the email." Xu Qiu exited the call background and glanced at the notification bar of the phone. There was no new email notification.

"I haven't forwarded the email yet. I intend to let Han Jiaying write the reply file of the review comments. What do you think?" Wei Xingsi asked.

"Um..." Xu Qiu understood. Teacher Wei should have the idea of ​​training Han Jiaying, and nominally this EES article is the first in the joint work, so it is indeed appropriate for her to write it.

He looked at the school girl next to him and saw that she moved her mouth and said silently: "I—no—question—question—" without revealing the intention of the relationship between the two to Teacher Wei .

Han Jiaying thinks that this kind of thing is acceptable to the teammates or classmates. If it reaches the teacher, she always feels a little weird. In school days, there is a natural sense of opposition between students and teachers, similar to the generation gap between children and parents. Many things can be talked to their peers, but they are not necessarily willing to tell their parents.

Xu Qiu understood, Chao Xuemei gave an "OK" gesture and replied to Teacher Wei: "Yes, let her come. When she finishes writing, I will help her take a look and change it. "

"That's OK, for this matter, I will forward the email to her later, and then copy it to you." Wei Xingsi finished speaking and hung up the phone.

Xu Qiu and Han Jiaying glanced at each other, and the school girl said, "It seems that I am going to stay in Handan to change the article. Zhang Jiang's post-processing of the experiment will be handled by senior brother."

"No problem," Xu Qiu responded with a smile, and then confirmed to Han Jiaying: "Two Stille polymerization reactions, H21 and H22 synthesis, right."

"Right." Han Jiaying nodded.

Not long after, Xu Qiu received an email from Teacher Wei.

This time there are only two reviewers for EES. It seems that one is a domestic colleague, and the other is a foreigner. This time I didn’t encounter a brainless person. After all, the device efficiency is there, and they all gave suggestions for minor changes. Need to answer a few questions, add a small experiment, and cite a few documents.

It is not difficult for Xu Qiu to answer these opinions, but for Han Jiaying, it may be a certain test.

However, if jade is not carved, Xu Qiu's old-fashioned Chaohan Jiaying said: "The important task is left to you, and you must not disappoint the organization's expectations."

Then, he patted the school **** the shoulder again, and said, "You have been strengthened."

Han Jiaying put her cheek in one hand, and Xu Qiu cast a white look, revealing a caring look.

Leaving the canteen, the two walked to the school bus spot, picked up Wu Shengnan, and then parted ways.

Xu Qiu took Wu Shengnan to Zhangjiang, first went to the drug warehouse to get the medicines ordered before, and then used some laboratory consumables, such as rubber stoppers, cable ties, and disposable droppers.

Today, Xu Qiu plans to synthesize IDTT and ICIN-2F. The D unit structure he arranged for his senior sister is BDT-2TT, which is a conjugated fused ring unit with a linear conjugation length of 9, and the A unit structure is ICIN-DM. It is the ICIN substituted with two (D) methyl (M). At the same time, they have to help the school girl handle her two reactions, H21 and H22, which have been polymerized and need the next post-processing and Soxhlet extraction.

When they came to the microelectronics building, the two put down their school bags in the A501 office to complete the preparatory work before the experiment, including the quality of the reaction materials.

Afterwards, they entered the A502 laboratory. Wu Shengnan looked like she was ordered, but she had no post-doctoral post. She has been engaged in scientific research for more than six years. The longer she does scientific research, the more she knows about the operation of single experiments. The difference is actually very limited.

To say that the experimental level of professors and even academicians may not be as good as those of doctoral students who are active in the front line. The gap between ordinary scientific researchers and those big bosses lies mainly in the proposal and realization of scientific research ideas, and whether they can catch the next breakthrough.

In recent days, Wu Shengnan has studied the publication of articles in Wei Xingsi’s group, and found that Xu Qiu is the kind of scientific research idea. Once he grasped the accuracy, he led the group to publish more than ten articles in the field of organic photovoltaics in just one year. Regardless of whether he has passed metaphysics or really has the strength, these are not important, as long as he can eat meat with himself, the result shows everything.

Xu Qiu didn’t know the thoughts of the new post-doctorate sister. He looked at Han Jiaying’s two reaction devices and tentatively said: “Senior Wu Sheng, you should be able to post-process the Stille polymerization reaction. There are two reactions here. How about we all alone?"

"Okay." Wu Shengnan thought for a while and added: "You should tell me again. I'm afraid the method I used before is different from this one, and there will be deviations."

"Okay," Xu Qiu agreed. He didn't have much communication with Wu Shengnan before. Now he is a "owner" and he should be active. He said, "Drip the reaction product with a disposable dropper." Into the methanol solution..."

The two of them performed post-reaction treatment simultaneously. The polymer product was separated out, filtered, wrapped in filter paper, and put into a Soxhlet extractor, and started Soxhlet extraction with a mixed solvent of methanol, acetone and n-hexane.

Now Han Jiaying has rich synthesis experience, and the dosage reaction is bolder. With a relatively large amount of dosage at one time, about 200 mg of product can be obtained in one pot reaction, and it is done in one step, so there is no need to conduct multiple experiments.

After the post-processing was over, Wu Shengnan concluded: "These post-processing steps are similar to what I did before, but you have an extra step of chloroform Soxhlet extraction."

Xu Qiu let out a "huh" and explained: "The solubility of the polymer product we got before was too poor. This method was used as a last resort. Later I found that this method was very useful and could significantly improve the quality of the product, so I persisted. "

During the filtration, Xu Qiu took the time to build a toluene re-distillation equipment. Now the indicator in the reaction flask has changed color, indicating that it has become anhydrous toluene. Xu Qiu collected toluene while preparing for the next reaction.

This time, Xu Qiu did not plan to use a microwave reactor for the time being. Although in theory the use of a microwave reactor would increase the reaction speed, but the reaction conditions need to be explored, which will increase the time cost.

Xu Qiu's idea is to wait until he has done all the reactions involved personally, and then let the simulation laboratory do it for him to help explore the conditions, including what reaction is suitable for microwave reaction, and how long the reaction time is.

In the first step of the synthesis of IDTT, the dibromo-substituted ethyl terephthalate (B) at the 2,5 position reacts with the monotrimethyltin-substituted thiophene (TT) unit to form the structure of TT-B-TT.

This is a simple small molecule Stille reaction. Xu Qiu also introduced the Stille reaction steps summarized in the group and told Wu Shengnan: "First, re-vapor toluene, which we did just now. Use sodium bars to absorb water. Benzophenone was used as an indicator to obtain anhydrous toluene with minimal impurities, and then..."

Wu Shengnan said: "In general, it is the same, but my research group used double-row tubes for vacuuming. Now you are directly on the mechanical pump, which is more vigorous."

Xu Qiu shrugged and explained with a smile: "In theory, it is more convenient to use double-row pipes, and it can prevent the solution from being directly sucked into the mechanical pump. However, it is more troublesome to set up pipes, plus it is always pumped directly. I got used to smoking, but I didn’t change it."

After chatting for a few more words, the two reacted together. Wu Shengnan occupied Tian Qing’s fume hood. Now Tian Qing does not make perovskite quantum dot materials. Duan Yun also mainly makes organic-based thermoelectric materials, which can be used in Handan. Sample preparation is completed in the glove box.

Therefore, the four fume hoods are now renamed "organic", and the other two fume hoods for liquid chromatography and rotary evaporation are also related to the organic field. Zhang Jiang has become an organic world and an organic laboratory.

Cleaning and drying glass instruments, making nitrogen balls.

In a two-necked flask, put the weighed medicine, dissolve it with toluene, and add a Teflon spindle-shaped magnetic stir bar.

Set up the reaction device, from bottom to top, there are two-necked flasks, condenser tubes connected to condensate pipes, and nitrogen balloons.

Use a three-way valve, three pumps and three rows to ensure the nitrogen atmosphere in the reaction system.

Weigh, add catalyst, repeat the operation of three pumps and three rows.

The temperature is quickly increased to 120 degrees Celsius, the condensate is turned on, and the outside of the two-necked flask is covered with aluminum foil.

Similar to the polymerization reaction, this Stille reaction needs to last 12-48 hours with almost no by-products. The longer the duration, the higher the yield of the reaction. Xu Qiu will react for 24 hours temporarily.

After the completion, Xu Qiu glanced at the progress of Wu Shengnan next door, only a little bit slower than him, indicating that the postdoctoral sister's success is not bad, she is a skilled worker.

After Wu Shengnan finished, Xu Qiu continued the first step in the synthesis of ICIN-2F. Phthalic acid (reactant A) substituted by dichloro at the 3 and 4 positions on the benzene ring reacted with acetic anhydride to form 3 on the benzene ring. , Phthalic anhydride substituted by dichloro at the 4 position.

This reaction requires acetic anhydride. Xu Qiu briefly consulted the MSDS manual. Acetic anhydride is a colorless and transparent liquid with a boiling point of about 140 degrees Celsius. It is the product of two acetic acid molecules with one molecule of water removed. It is flammable. Its vapor and air can form an explosive mixture. It can cause combustion and explosion when exposed to open flames and high thermal energy. It can react chemically when it comes in contact with strong oxidants. It becomes acetic acid, or reacts with alcohols to generate acetate.

Acetic acid, also known as acetic acid, is the main component of edible vinegar.

Xu Qiu took out the acetic anhydride from the reagent cabinet, put it in the fume hood, opened the cap, and could smell the vinegar through the fume hood.

This reminded him that when he was a child, every time he was in the flu season, his family would smoke vinegar, saying that he could kill the virus or something. From a scientific point of view, it seems that the concentration of acetic acid is too low. The bactericidal effect is very poor. This method is of no use except to find a crime for yourself~www.ltnovel.com~...

Fortunately, I don’t smoke at home now...

Xu Qiu first filled the reaction flask with 50 ml of acetic anhydride, and then weighed the reactant A and poured it into the reaction flask. At room temperature, the reactant A was almost insoluble in acetic anhydride, showing a suspended state.

Then, add a stir bar to the reaction flask, connect the condenser tube and balloon, and finally raise the temperature to 160 degrees Celsius, and let the acetic anhydride reflux.

Several raw materials are commercialized and relatively cheap. Xu Qiu puts 0.1 mole of raw materials, which is 23.5 grams of Reactant A, and this reaction takes about 6 hours.

Wu Shengnan also voted for the first reaction of ICIN-DM.

The raw material she chose was the reaction of phthalic acid substituted with dimethyl at positions 3 and 4 on the benzene ring with acetic anhydride. The reaction conditions were similar.

PS: Happy New Year's Day to all book friends, and everything you want in the new year will come true!

PS2: A new month has begun, ask for a monthly pass...