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Electrospinning - pt.28, 29, 30


Chemist


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In my first experiment with polystyrene and DMF, I prepared a moderately concentrated solution (13.58%), as I was unsure whether the polymer would dissolve at all. I was even more doubtful that electrospinning this solution would produce fibrous material. Since a positive result was unexpectedly obtained, I decided to increase the polystyrene concentration.

I gradually added 2.560 g of expanded polystyrene to 10.085 g of dimethylformamide. The polymer dissolved, forming a white, turbid solution with a concentration of 20.2%. To my surprise, the viscosity of the liquid remained relatively low. I used the resulting solution for electrospinning.

Visually, the process was similar to the previous experiment using a 13.58% polystyrene solution. A cotton wool-like coating formed on the collector, and fibers were visible under a microscope. No splashing of the solution was observed this time. After using about 2 mL of the solution, I stopped the experiment, intending to further increase the polymer concentration.



Электроспиннинг: раствор полистирола в диметилформамиде - Часть 28
В первом эксперименте с полистиролом и DMF я приготовил раствор умеренной концентрации (13.58%), поскольку не был уверен, растворится ли полимер. Еще больше я сомневался, что электроспиннинг данного раствора приведет к образованию волокнистого материала. Неожиданно был получен положительный результат, поэтому я решил увеличить концентрацию полистирола.

К 10.085 г диметилформамида постепенно добавил 2.560 г вспененного полистирола. Полимер растворился, образовав белый мутный раствор с концентрацией 20.2%. К моему удивлению, вязкость жидкости оказалась сравнительно низкой. Полученный раствор я использовал для электроспиннинга.

Процесс визуально протекал аналогично предыдущему эксперименту, в котором был использован 13.58% раствор полистирола. На коллекторе образовалось покрытие, похожее на хлопковую вату, под микроскопом были видны волокна. Образование брызг в этот раз не наблюдалось. Использовав около 2 мл раствора, я прекратил эксперимент, намереваясь еще больше увеличить концентрацию полимера.


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Electrospinning: Solutions of Polystyrene in Dimethylformamide
Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide




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I prepared a new polystyrene solution by weighing 2.025 g of my existing 20.2% polystyrene solution and adding 0.225 g of expanded polystyrene. I was unsure whether the polymer would dissolve and whether the resulting solution would be suitable for electrospinning, so I deliberately used minimal amounts of the substances. Upon stirring, the polymer gradually dissolved, forming a 28.2% solution with a viscosity that proved to be perfectly acceptable.

I began electrospinning. It was a frosty, sunny day, and bright rays of sunlight fell on the needle from the side. The result was unexpected: streams of solution escaping from the needle resembled sparkling whips. These "whips" then disintegrated into bundles of streams that transformed into threads. Under different lighting conditions, this process remained invisible. However, the "formation of cotton wool in the air" was almost not observed.

A characteristic white coating of electrospun polystyrene formed on the collector. When the solution ran out, I decided to prepare a new solution and continue the process without separating the already formed coating from the collector.



Электроспиннинг: раствор полистирола в диметилформамиде - Часть 29
Новый раствор полистирола приготовил, взвесив 2.025 г имеющегося 20.2% раствора полистирола и добавив в него пенополистирол весом 0.225 г. Я не был уверен, растворится ли полимер и будет ли пригоден полученный раствор для электроспиннинга, поэтому использовал минимальные количества веществ. При перемешивании полимер постепенно растворился, образовав 28.2% раствор, который имел вполне приемлемую вязкость.

Начал электроспиннинг. День был морозный и солнечный. Яркие солнечные лучи падали сбоку на иглу. Результат оказался неожиданным - струи раствора, которые вырывались из иглы, были похожи на сверкающие кнуты. Затем эти "кнуты" распадались на пучки струй, которые превращались в нити. При другом освещении данный процесс оставался невидимым. Зато "образование ваты в воздухе" почти не наблюдалось.

На коллекторе образовалось характерное белое покрытие электроспиннингового полистирола. Когда раствор закончился, я решил приготовить новый раствор, чтобы продолжить процесс, не отделяя уже образовавшееся покрытие от коллектора.


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Electrospinning: Solutions of Polystyrene in Dimethylformamide
Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide


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To continue electrospinning, I needed to prepare a new polystyrene solution in DMF with a high polymer concentration. It turned out that, after numerous experiments, I had used up all the glass bottles available in the laboratory. As a result, I had to prepare the solution in a PET bottle, even though I was not certain whether this polymer was resistant to DMF.

I weighed out 10.120 g of dimethylformamide and 4.120 g of expanded polystyrene and gradually added the polymer to the solvent. Large pieces of polystyrene became highly electrified during breakage and stuck to my gloves. Under calmer circumstances, I could have filmed a video demonstrating electrostatic forces, but I had a different objective at the time.

Although the volume of expanded polystyrene was much greater than that of the DMF, the polymer dissolved. A white solution with a polystyrene concentration of 28.9% and moderate viscosity formed. I filled a syringe with the solution and continued electrospinning.

This time, I was able to observe the "formation of cotton wool in the air": a fibrous material was literally forming before my eyes. At a certain point, fiber formation suddenly stopped, even though some polystyrene solution still remained in the syringe. I assumed that the solution had hardened inside the needle, blocking the flow.

The syringe pump is designed for use with 20 ml syringes. When the plunger movement is blocked, or when the plunger reaches its maximum upper position (that is, when all the solution has been expelled), an audible alarm should sound. However, no alarm was triggered. This did not surprise me, as I had modified the pump's standard operating configuration. Instead of 20 ml syringes, I use 2 ml syringes together with a special rod that transfers force from the pump to the syringe plunger. When using 2 ml syringes, the alarm usually does not sound.

I turned off the high voltage, removed the syringe from the setup, and discovered that the rod was already in its maximum upper position. This position corresponds to the fully depressed syringe plunger - that is, to a state in which all the solution should have been expelled. However, some solution still remained in the syringe. The plunger movement had been blocked because the needle was clogged. The conclusion was clear: under pressure, the thin plastic plunger rod had begun to bend, allowing the pump rod to reach its uppermost position before the syringe was actually empty. With 20 ml syringes, the plunger rod is much thicker and more rigid, which reliably triggers the alarm.

I quickly replaced the needle and resumed electrospinning. Eventually, the solution in the syringe was completely exhausted, and the collector became coated with a thick layer of cotton-like material. It is worth noting that the solution used for electrospinning consisted of nearly one-third polymer by weight.



Электроспиннинг: раствор полистирола в диметилформамиде - Часть 30
Итак, необходимо было приготовить новый раствор полистирола в DMF с высокой концентрацией полимера, чтобы продолжить электроспиннинг. Оказалось, делая многочисленные эксперименты, я использовал все стеклянные бутылочки, которые были в лаборатории. Пришлось готовить раствор в PET бутылке, хотя я не был уверен, что данный полимер устойчив к действию DMF.

Взвесил 10.120 г диметилформамида и 4.120 г вспененного полистирола. Постепенно добавлял полимер в растворитель. Крупные кусочки полистирола сильно электризовались при измельчении, прилипая к перчаткам. В спокойной обстановке можно было бы снять наглядное видео, посвященное электростатическим силам, но передо мной стояла другая задача.

Объем пенополистирола намного превышал объем DMF, тем не менее, полимер растворился. Образовался белый раствор с концентрацией полистирола 28.9% и умеренной вязкостью. Набрал раствор в шприц и продолжил электроспиннинг.

В этот раз можно было наблюдать "образование ваты в воздухе" - волокнистый материал формировался буквально на глазах. В определенный момент образование волокон остановилось, хотя в шприце еще остался раствор полистирола. Я предположил, что раствор затвердел в игле, препятствуя потоку жидкости.

Данный шприцевой насос рассчитан на использование 20 мл шприцов. Когда движение поршня блокируется или поршень шприца достигает крайнего верхнего положения (весь раствор выдавлен), должна включаться звуковая сигнализация. Однако, сигнализация не включилась. Я не удивился, поскольку изменил стандартный порядок работы насоса. Вместо 20 мл шприцов, я использую 2 мл шприцы и специальный стержень, который передает усилие от насоса к поршню шприца. В случае 2 мл шприцов сигнализация, как правило, не срабатывала.

Отключил высокое напряжение, извлек шприц из установки и обнаружил, что стержень находился в крайнем верхнем положении. Такое положение стержня соответствует крайнему положению поршня шприца, когда поршень выдавил из шприца весь раствор. Однако, в шприце оставался раствор. Движение поршня было заблокировано, поскольку игла шприца забилась. Вывод: пластиковый шток поршня начал изгибаться под давлением стержня, что позволило стержню достигнуть крайнего верхнего положения, когда шприц еще не был пустым. В случае 20 мл шприцов шток поршня был толще и гнулся гораздо труднее, поэтому срабатывала сигнализация.

Быстро заменил иглу и продолжил электроспиннинг. Наконец, раствор в шприце израсходовался, коллектор покрылся толстым слоем материала, похожего на вату. Примечательно, что использованный для электроспиннинга полистирола раствор почти на 1/3 по весу состоял из полимера.


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Electrospinning: Solutions of Polystyrene in Dimethylformamide
Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide

Electrospinning: Solutions of Polystyrene in Dimethylformamide



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