I Have a Research Support System

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

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

"Hello, Teacher Wei?" Xu Qiu was a little puzzled. Wei Xingsi usually sent messages or emails when he had something to do. What kind of things did he have to call to explain?

"The review comments for that EES article are back, minor corrections." Wei Xingsi's voice came from the receiver.

"Hey, I didn't receive the email." Xu Qiu exited the background of the call and glanced at the notification bar of the phone, but there was no new email notification.

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

"Hmm..." Xu Qiu understood a little bit. Teacher Wei probably wanted to train Han Jiaying, and this EES article was supposed to be the first in the joint work, so it was indeed more appropriate for her to write it.

He looked at the school girl next to him, and saw that she moved her mouth and mouthed silently: "I-didn't-ask-question-", she had no intention of revealing the relationship between the two to Teacher Wei .

Han Jiaying felt that this kind of thing was acceptable to the friends or students in the research group, but if it was reported to the teacher, she always felt a little weird. In the student days, there is a certain sense of antagonism between students and teachers, which is similar to the generation gap between children and parents. Many things can be told to peers around them, but they are not necessarily willing to tell their parents.

Xu Qiu understood, gestured "OK" to the school girl, and replied to Teacher Wei: "Yes, then let her do it. When she finishes writing, I will help her read it and make changes. "

"That's fine, just this matter, I'll forward the email to her later, and then copy you." Wei Xingsi finished speaking and hung up the phone.

Xu Qiu and Han Jiaying looked at each other, and the school girl said, "It seems that I'm going to stay in Handan to revise the article today, and Zhang Jiang will leave the post-experiment processing to senior brother."

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

"That's right." Han Jiaying nodded.

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

This time EES has only two reviewers. It seems that one is a domestic colleague and the other is a foreigner. This time I did not encounter any brainless ones. After all, the efficiency of the device is there, and they all gave suggestions for minor changes. Need to answer a few questions, add a small experiment, and cite a few literatures.

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, it can't be made into a tool. Xu Qiu's old-fashioned Chaohan Jiaying said: "I will entrust you with the heavy responsibility of **, and you must not disappoint the expectations of the organization."

Afterwards, he patted the junior girl on the shoulder again, and said, "You have been strengthened."

Han Jiaying rested her chin with one hand, and gave Xu Qiu a look of caring.

After leaving the cafeteria, the two walked to the school bus stop, picked up Wu Shengnan, and parted ways.

Xu Qiu brought Wu Shengnan to Zhangjiang, first went to the drug warehouse to get the drugs ordered before, and then received some laboratory consumables, rubber stoppers, cable ties, disposable droppers, etc.

Today, Xu Qiu plans to synthesize IDTT and ICIN-2F. The D unit structure he arranged for his senior is BDT-2TT, which is a conjugated fused ring unit with a linear conjugate length of 9. The A unit structure is ICIN-DM, which is also It is ICIN substituted with di(D)methyl(M). At the same time, they also need to help Xuemei process her two reactions, H21 and H22, which have been aggregated and need to be post-processed and Soxhlet extraction.

When they came to the microelectronics building, the two first put down their schoolbags 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 acted like she was ordered, and she didn't have the airs of a postdoctoral fellow. She has been engaged in scientific research for more than six years. The difference is actually very limited.

As far as the experimental level of professors and even academicians is concerned, it may not be as good as doctoral students who are active in the front line. The gap between ordinary scientific researchers and those big shots lies mainly in the proposal and realization of scientific research ideas, and whether they can grasp the next breakthrough.

Wu Shengnan has studied the publication of articles in Wei Xingsi's group in recent days, and found that Xu Qiu is the kind of scientific research idea that can be accurately grasped, so that in just one year, he led the group to publish a total of more than ten articles in the field of organic photovoltaics. It doesn't matter whether he passed metaphysics or has real strength, as long as he can bring himself to eat meat, the result speaks for itself.

Xu Qiu didn't know what the new postdoctorate senior was thinking. He looked at Han Jiaying's two reaction devices, and tentatively said, "Sister Wu Shengnan, you should be able to post-process the Stille polymerization reaction. There are two reactions here. How about one of us?"

"Okay." Wu Shengnan thought for a while, and added: "You should tell me again, I am afraid that the method I used before is not the same as here, and there will be deviations."

"Okay," Xu Qiu agreed. He didn't have much communication with Wu Shengnan before, and now he is "one of his own", so he should be flexible, so he introduced while operating: "Use a disposable dropper to drop the reaction product. into methanol solution..."

The two carried out the post-reaction treatment simultaneously. The polymer product was precipitated, filtered, wrapped with filter paper, loaded into a Soxhlet extractor, and started Soxhlet extraction with a mixed solvent of methanol, acetone, and n-hexane.

Now Jiaying Han has more experience in synthesis, and the reaction is bolder. A large amount can be injected at one time, and about 200 mg of the product can be obtained in one pot reaction, which is in place in one step, so that there is no need to conduct multiple experiments.

After the post-processing, 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 "hmm" and explained: "The solubility of the polymerization product we obtained was too poor before, so we had to use this method as a last resort. Later, we found that this method is very useful and can significantly improve the quality of the product, so we persisted. "

During the filtration, Xu Qiu took the time to build a device for re-distilling toluene. Now the indicator in the reaction bottle has changed color, indicating that it has become anhydrous toluene. Xu Qiu is collecting toluene while preparing for the next reaction.

Xu Qiu has no intention of using a microwave reactor for the reaction this time. Although theoretically using a microwave reactor will increase the speed of the reaction, the reaction conditions need to be explored, which will increase the time cost.

Xu Qiu's idea is to wait for himself to operate all the reactions involved, and then let the simulation laboratory do it for him to help find out the conditions, including which reactions are suitable for microwave reactions, and how long the reaction time should be.

The first step in the synthesis of IDTT involves the reaction of ethyl terephthalate (B) substituted with dibromo at the 2,5 positions and monothiophene (TT) units substituted with monotrimethyltin 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, distill toluene, which is what we did just now, and use sodium strips to absorb water. Benzophenone was used as an indicator to obtain anhydrous toluene with very little impurity content, and then..."

Wu Shengnan said: "It is generally the same, but my research group used double-row tubes for vacuuming before, and now you are directly using mechanical pumps, which are more vigorous."

Xu Qiu shrugged and explained with a smile: "Theoretically, it is more convenient to use double-row pipes, and it can prevent the solution from being directly sucked into the mechanical pump, but it is troublesome to install pipes, and it is always a direct pumping method." , I got used to smoking, but I didn’t change it.”

After chatting for a few more words, the two responded 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 obtained in Handan Sample preparation was done in the glove box.

Therefore, the four fume hoods are renamed "organic" now, and the other two fume hoods for liquid chromatography and rotary evaporator are also related to the organic field. Zhangjiang has completely turned into an organic world and has become an organic laboratory.

Wash and dry glass instruments and make nitrogen balloons.

In the two-neck flask, put the weighed medicine, dissolve it with toluene, and add a polytetrafluoroethylene shuttle-shaped magnetic stirring bar.

Set up the reaction device, from bottom to top are two-necked flasks, a condenser pipe connected to a condensate pipe, and a nitrogen balloon.

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

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

Rapidly raise the temperature to 120 degrees Celsius, turn on the condensate, and wrap the outside of the two-neck flask with aluminum foil.

Similar to the polymerization reaction, this Stille reaction needs to last for 12-48 hours, and there are almost no by-products. The longer the duration, the higher the yield of the reaction. Xu Qiu tentatively reacts for 24 hours.

After finishing, Xu Qiu glanced at the progress of Wu Shengnan next door, who was only a little slower than him, which meant that the postdoctoral senior sister's synthesis skills were not bad, and she was a skilled worker.

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

This reaction requires the use of acetic anhydride. Xu Qiu briefly checked 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 taking off a molecule of water. It is flammable. Its vapor and air can form explosive mixtures. It can cause combustion and explosion when exposed to open flames and high heat energy. It can undergo chemical reactions when it contacts with strong oxidants. It can be slowly dissolved in water. Turn into acetic acid, or react with alcohols to generate acetate.

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

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

This reminded him that when he was a child, whenever the flu season came, vinegar would be smoked at home, saying that it could kill the virus. Now it seems that, from a scientific point of view, because the concentration of acetic acid is too low, The sterilizing effect is very poor, this method is of no use other than finding guilt for yourself...

Fortunately, it is not smoked at home now...

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

Next, add a stirring bar in the reaction bottle, connect the condenser tube and the balloon, and finally raise the temperature to 160 degrees Celsius to allow the acetic anhydride to reflux.

Several raw materials are commercialized and relatively cheap. Xu Qiu injected 0.1 mole of raw materials at one time, that is, 23.5 grams of reactant A. The reaction lasted for about 6 hours.

Wu Shengnan also voted for ICIN-DM's first response at the same time.

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

PS: I wish all book lovers a happy New Year's Day, and all wishes come true in the new year!

PS2: A new month has begun, ask for a wave of monthly tickets...