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Author: Subject: Chemical synthesis through the timeline of chemistry
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smile.gif posted on 31-7-2020 at 00:41
Chemical synthesis through the timeline of chemistry

Chemistry would not have came about without the fire building
Caveman Age - controlling fire

Bronze age - 3500 BC
Certain metals can be recovered from their ores by simply heating the rocks in a fire:

mercury, tin, lead, antimony, bismuth and (at a higher temperature) copper. This process is known as smelting
**Sodium dithionite is a reducing agent of sulfate**
**Thiourea dioxide**Persulfate**

These first metals were single elements, or else combinations as naturally occurred. By combining copper and tin, a superior metal could be made, an alloy called bronze.

Glass making -
Late bronze age/ Glass age
there was a rapid growth in glassmaking technology. The alkali of Syrian and Egyptian glass was soda ash (sodium carbonate), which can be extracted from the ashes of many plants. The latest vessels were 'core-formed', produced by winding a ductile rope of glass around a shaped core of sand and clay over a metal rod, then fusing it by reheating it several times.

Zinc (same with tin)
Zinc oxide smelted with carbon
Electrolysis of zinc sulfate
Electrolysis of sodium zincate
Single displacement magnesium with zinc chloride

Iron Age - 1200 BC - iron wrought iron and carbon steel
Many applications, practices, and devices associated with or involved in metallurgy were established in ancient China, such as the innovation of the blast furnace, cast iron, hydraulic-powered trip hammers, and double-acting piston bellows

Medieval alchemy
Abu Musa Jabir ibn Hayyan (aka Geber) Alchemist
"father of chemistry"
hydrochloric acid, nitric acid, aqua regia.

Hydrochloric acid
>>Free hydrochloric acid 16th century by Libavius, who prepared it by heating salt in clay crucibles i(I don't believe this)
>>Some claim pure hydrochloric acid first made by Basil Valentine in 15th century, by heating sodium chloride and green vitriol (iron sulfate)
>>17th century Johann Rudolf Glauber used sodium chloride salt and sulfuric acid to form hydrochloric acid.

Nitric acid
>> calcining potassium nitrate, (aluminum sulfate <200F>. low melting point flux) alum and copper sulfate.
>>1776 Glauber devised a process to obtain it by distilling potassium nitrate with sulfuric acid.
>>The industrial production of nitric acid from atmospheric air began in 1905 with the Birkeland–Eyde process,
>> Oswalt process by oxidation of ammonia to nitric acid

Synthesis of sulfuric acid
>>Roasting "green vitriol" (iron(II) sulfate) in an iron retort to form sulfuric acid
>> 18th century, from Pyrite (iron disulfide, heated in air to yield iron(II) sulfate, which was oxidized by further heating in air to form iron(III) sulfate, Fe2(SO4)3, which, when heated to 480 °C, decomposed to iron(III) oxide and sulfur trioxide, which could be passed through water to yield sulfuric acid in any concentration.
>>1736 Johann Glauber prepared sulfuric acid by burning sulfur together with potassium nitrate, in the presence of steam. As potassium nitrate decomposes, it oxidizes sulfur to SO3, which combines with water to produce sulfuric acid.
>>1746 John Roebuck adapted this method to produce sulfuric acid in lead-lined chambers, which were stronger, less expensive, and could be made larger than the previously used glass containers. Known as the lead chamber process
Sulfuric acid created by John Roebuck's process approached a 65% concentration.
John Glover improved concentration to 78%.
>> 1831, Peregrine Phillips created the contact process, which was a far more economical process for producing sulfur trioxide and concentrated sulfuric acid.

Aqua regia-
Desolving ammonium chloride in nitric acid
Hydrochloric acid and nitric acid mixture

1669 H. Brand - Phosphorus
>>Ammonium sodium phosphate(urine) silicon dioxide and carbon(activated)
>>calcium phosphate from bones/ phosphorus from bone ash.
**Hypophosphorous acid reduces chromium(III) oxide to chromium(II) oxide**
**Potassium Perphosphate**

The Retort
An early method for producing phosphorus starts by roasting bones, and uses clay retorts encased in a very hot brick furnace to distill out the phosphorus.

1735 G. Brandt - Cobalt
Isolation from the ore then smelting with carbon

1751 F. Cronstedt - Nickel
Isolation from the ore then smelting with carbon

1766 Henry Cavendish - Hydrogen
Iron or zinc on dilute acids (HCl)
>>François Isaac de Rivaz built the de Rivaz engine, powered by a mixture of hydrogen and oxygen in 1806. Edward Daniel Clarke invented the hydrogen gas blowpipe in 1819. The Döbereiner's lamp and limelight were invented in 1823

1771 Carl Wilhelm Scheele - Oxygen
produced oxygen gas by heating with focused sunlight mercuric oxide and various nitrates contained in a glass tube, which liberated oxygen

1772 D. Rutherford - Nitrogen
Reaction of ammonium chloride with sodium nitrite
By Oxidation of ammonia to Nitrogen gas
NEVER ammonium sulfate and sodium/calcium hypochlorite
Forms hydrazine / nitrogen trichloride depending on conditions
**nitrite and sodium metal = hyponitrite peroxohyponitrite**

Selenium oxidizer
*oxidation of selenium in water with chlorine yields selenic acid
Selenium dioxide and hydrogen peroxide yields selenic acid

1774 Scheele - Manganese
>>reducing the manganese dioxide with carbon.
>> Manganese dioxide added to sulfuric acid and ferrous sulfate in a 1.6:1 ratio. The iron reacts with the manganese dioxide to form iron hydroxide and elemental manganese.
>>Electrolysis of manganese sulfate to manganese metal

1774 Scheele - Chlorine
>>Reacting MnO2 with hydrochloric acid
>>electrolysis of sodium chloride the chloralkali process
Oxone (persulfate) and sodium chloride

1781 Peter Jacob Hjelm - Molybdenum
>Reduction of molybdenum oxide using carbon and linseed oil
>Reduction of Molybdenum trioxide with hydrogen gas
>Molybdenum trioxide reduction by aluminothermic reaction
>**Molybdenum trioxide sublimation at 1,100C (2,010F)**

1781 Scheele - Tungsten*****
>>Reduction of tungsten oxide with hydrogen or carbon
>> hydrogen reaction with tungsten hexafluoride to tungsten
>> decomp. of tungsten hexafluoride to fluorine and tungsten
Titanium hexachloride and Bismuth yield Tungsten (2) chloride

1794 Louis Vauquelin - Chromium
>> chromium oxide reduction with carbon
>>Silicothermic /aluminothermic reaction with chromium oxide
>>Electrolysis of chromium sulfate
**Chromous (II) ion is able to reduce acids to hydrogen,
Hypophosphorous acid and Chromium (III) Oxide > CrO
1784 Citric acid was first isolated by Carl Wilhelm Scheele, who crystallized it from lemon juice. The anhydrous form crystallizes from hot water, while the monohydrate forms when citric acid is crystallized from cold water. The monohydrate can be converted to the anhydrous form at about 78 °C. Citric acid also dissolves in absolute (anhydrous) ethanol.

>>>>>> materials science, the Citrate-gel method is a process similar to the sol-gel method, which is a method for producing solid materials from small molecules. During the synthetic process, metal salts or alkoxides are introduced into a citric acid solution. better distribution of ions and prevents the separation of components. The polycondensation of ethylene glycol and citric acid starts above 100 °С, resulting in polymer citrate gel formation.
1800 Alessandro Volta devises the first chemical battery, thereby founding the discipline of electrochemistry.

1807 Sir Humphry Davy - Potassium
electrolysis of molten KOH with the voltaic pile. Potassium was the first metal that was isolated by electrolysis. Later in the same year, Davy reported extraction of the metal sodium
>> thermal method reacting sodium with potassium chloride
>>reaction of potassium fluoride with calcium carbide Griesheimer process. **another use for calcium carbide**

1807 Sir Humphry Davy - Sodium
>>electrolysis of molten sodium hydroxide to sodium metal
>> carbothermal reduction of sodium carbonate at 1100 °C
>> electrolysis of molten sodium chloride with mixed in calcium chloride for a melting point below 700 °C

1808 Sir Humphry Davy - Boron
>>Potassium reacts with boric acid to form boron.
>>Iron and boric acid react at high temperatures forming boron
>> reduction of boric oxide with magnesium or aluminium.
>> reducing boron halides with hydrogen at high temperatures.

1808 Sir Humphry Davy - Magnesium
>>electrolysis mixture of magnesium oxide and mercuric oxide.
>>reductant preparation of finely divided metals from their salts by Rieke method.magnesium chloride and potassium forms finely divided magnesium metal
>> silicothermic Pidgeon process in the reduction of magnesium oxide and silicon, provided by a ferrosilicon alloy >> The process magnesium oxide with carbon at 2300 °C:
>>The Dow process electrolysis of molten magnesium chloride
>>solid oxide membrane technology, involves the electrolytic reduction of MgO. The electrolyte is yttria-stabilized zirconia The anode is silver. layer of graphite by the liquid silver anode.

1808 Sir Humphry Davy - Calcium
Pure calcium was isolated in 1808 via electrolysis of calcium oxide with Mercury(II) oxide on a platinum plate which was used as the anode, the cathode being a platinum wire partially submerged into mercury. Electrolysis then gave calcium–mercury amalgam distilling off the mercury gave calcium
>>electrolysis of molten calcium chloride to calcium metal
>>Reaction of calcium oxide with aluminum forms calcium

1808 Sir Humphry Davy - Strontium
>>electrolysis of strontium chloride and mercuric oxide,
>> reducing strontium oxide with aluminium. The strontium is distilled from the mixture.
>>Strontium metal can be prepared by electrolysis of a solution of strontium chloride in molten potassium chloride

1808 Sir Humphry Davy - Barium
>> electrolysis of barium chloride and mercuric oxide producing Barium metal
>> electrolysis of molten mixture of barium chloride and ammonium chloride
>> aluminium reacts with barium oxide at 1,100 °C (2,010 °F). The intermetallic compound BaAl4 is produced first
BaAl4 is an intermediate reacted with barium oxide to produce the barium metal. Barium vapor is condensed in an atmosphere of argon.
>>Barium oxide reacts with silicon at 1,200 °C (2,190 °F) yields barium metal and barium metasilicate.Electrolysis is not used because barium readily dissolves in molten barium chloride.

1811 Bernard Courtois - Iodine
Sodium iodide and sulfuric acid
Oxidizing sodium iodide with chlorine gas to iodine
Oxone (persulfate) and sodium iodine

1825 Antoine Jérôme Balard - Bromine
Sodium bromide and concentrated sulfuric acid
Oxidizing sodium bromide with chlorine gas to bromine
Oxone (persulfate) and sodium bromide

1821 William Thomas Brande - Lithium
it by electrolysis of lithium oxide, a process that had previously been employed by the chemist Sir Humphry Davy to isolate the alkali metals potassium and sodium.

1823 Berzelius - Silicon
>> reducing potassium fluorosilicate with molten potassium
>> potassium metal with silicon tetrafluoride to Silicon
>>electrolyzing sodium chloride and aluminium chloride with containing 10% silicon
>>carbothermal reduction of silicon dioxide to silicon
>>aluminothermal reduction of silicon dioxide to silicon
>>reduction of tetrachlorosilane (silicon tetrachloride) or trichlorosilane with zinc metal.
>>Thermal decomposition of silane or tetraiodosilane
> reduction of sodium hexafluorosilicate with metallic sodium.

1824 Hans Christian Ørsted - Aluminum
>Reacting anhydrous aluminium chloride and potassium metal
>>aluminium trichloride reacted with sodium
>>Aluminum oxide electrolysis with molten (980 °C , 1,800 °F) mixture of cryolite (Na3AlF6) with calcium fluoride as flux

1828 Friedrich Wöhler and Antoine Bussy - Beryllium
>>Reaction of metallic potassium with beryllium chloride
>> electrolysis of molten beryllium fluoride and sodium fluoride
>>thermal decomposition of beryllium iodide similar to production of zirconium.
>>react beryllium fluoride with magnesium at 900C (1,650 °F) with magnesium forms finely divided beryllium, and additional heating to 1,300 °C (2,370 °F) creates the compact metal
Electrolysis of molten beryllium chloride is then used to obtain the metal.

1828 Fiedrich Wöhler - Yttrium
>>reacting a volatile yttrium chloride and potassium

Lanthanum (All Lanthinides)
La2O3 + 6 NH4Cl → 2 LaCl3 + 6 NH3 + 3 H2O
LaCl3 reduction with lithium or calcium in argon
electrolysis of molten mixture of anhydrous LaCl3 and NaCl

Friedrich Wöhler synthesizes urea, thereby establishing that organic compounds could be produced from inorganic starting materials, disproving the theory of vitalism.
Crystal bar process/kroll process
titanium, zirconium, hafnium, vanadium, thorium, protactinium can be refined using their respected metal iodide
Metal tetrachloride and calcium/magnesium (Kroll process)
cheaper processes (e.g., FFC Cambridge, Armstrong)
**Titanium(II) chloride strong reducing agent**
*zirconium tetrachloride w/ Al metal to zirconium (3) chloride*

1830 Nils Sefström - Vandium
>>Reduction of vanadium(II) chloride, VCl2, with hydrogen.
>>vanadium pentoxide or sodium vanadate with calcium redox
>>vanadium pentoxide reducing with hydrogen or magnesium.
>>Decomposition of vanadium(III) iodide to vanadium metal


1841 Péligot - Uranium
Reduction of uranium tetrachloride with potassium to uranium

Hermann Kolbe obtains acetic acid from completely inorganic sources, further disproving vitalism

Benjamin Silliman, Jr. pioneers methods of petroleum cracking, which makes the entire modern petrochemical industry possible

William Henry Perkin synthesizes Perkin's mauve, the first synthetic dye. Created as an accidental byproduct of an attempt to create quinine from coal tar. This discovery is the foundation of the dye synthesis industry, one of the earliest successful chemical industries

1861 Bunsen - Rubidium
Heating charred rubidium tartrate to rubidium

Alexander Parkes exhibits Parkesine, one of the earliest synthetic polymers, at the International Exhibition in London. This discovery formed the foundation of the modern plastics industry

1864 Richter - Indium
Carbon reduction of Indium oxide
Electrolysis of Indium chloride
Electrolysis of sodium inadate
Indium(I) Bromide -sulfur lamp *magnatron/microwave*
Molten InCl3 conducts electricity whereas AlCl3 does not
***indium(I) compounds are powerful reducing agents***
** Indium Trichloride and lithium hydride react (in diethyl ether) forming Lithium Indium Hydride decomposes below 0C
Reacted "in situ" in organic synthesis as a reducing agent and to prepare tertiary amine and phosphine complexes of InH3.

1864 Christian Blomstrand - Niobium
>>Reaction of niobium chloride and hydrogen or carbon
>The electrolysis of molten of K2[NbOF5] and sodium chloride >>Reduction of Niobium fluoride with sodium.
>>Reaction thermite mixture of niobium oxide and aluminium

1864 De Marignac - Tantalum
>>reduced tantalum chloride by heating it in hydrogen gas
>>K2[TaF7] and sodium, at approximately 800 °C in molten salt
>>cheaper processes (e.g., FFC Cambridge, Armstrong)

Adolf von Baeyer begins work on indigo dye, a milestone in modern industrial organic chemistry which revolutionizes the dye industry

1875 Lecoq - Gallium
>> electrolysis of galium and potassium hydroxide solution
**Galium suboxide is a very strongreducing agent able to reduce Sulfuric acid to Hydrogen Sulfide**
Lithium tetrahydridogallate(lithium gallium Hydride) was first r It is prepared by the reaction of lithium hydride and an ethereal solution of gallium trichloride.

1879 Lars Nilson - Scandium
>>Electrolysis of a eutectic mixture of potassium, lithium, and scandium chlorides, at 700–800 °C
>> Reaction of scandium fluoride and calcium to Scandium

1882 Carl Setterberg/Bunsen - Caesium
>>electrolysing caesium cyanide to Caesium metal

1886 Henri Moissan - Flourine
electrolysis of potassium bifluoride and dry hydrogen fluoride . To prevent rapid corrosion of the platinum in his electrochemical cells, he cooled the reaction to extremely low temperatures in a special bath and forged cells from a more resistant mixture of platinum and iridium, and used fluorite stoppers

Fritz Haber and Carl Bosch develop the Haber process for making ammonia from its elements, a milestone in industrial chemistry with deep consequences in agriculture

Leo Hendrik Baekeland invents bakelite, one of the first commercially successful plastics

1910 Marie Curie - Radium
>>Isolated radium metal through electrolysis of radium chloride solution using a mercury cathode, producing a radium mercury amalgam.This amalgam was then heated in an atmosphere of hydrogen gas to remove the mercury, leaving pure radium metal.
>> isolated radium by thermal decomposition of its azide, Ra(N3)2 to radium metal
>>The metal is isolated by reducing radium oxide with aluminium metal in a vacuum at 1200 °C.

Harold Urey discovers deuterium by fractionally distilling liquid hydrogen

James Chadwick discovers the neutron

Wallace Carothers leads a team of chemists at DuPont who invent nylon, one of the most commercially successful synthetic polymers in history

Neil Bartlett synthesizes xenon hexafluoroplatinate, showing for the first time that the noble gases can form chemical compounds

What year of chemical skill can you reach
Mine is probably around 1750 excluding phosphorus]

[Edited on 1-8-2020 by symboom]

[Edited on 1-8-2020 by symboom]
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International Hazard

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[*] posted on 31-7-2020 at 00:52

I've always wondered did they master the art of glassware making, distillation and other things back in the historic times?
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Eddie Current
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[*] posted on 31-7-2020 at 04:30

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[*] posted on 31-7-2020 at 09:30

Soap, ethanol (via distillation in copper stills), candle making, pottery and glaze colorants, gunpowder, nitroglycerin, dynamite, perfumery and dye making (partially covered).
The economic aspects of these things far outweighed the scientific level.
Nor does the timeline provided correspond to the difficulty level.
Nylon is relatively easy, Ammonia is very hard to make via the Haber-Bosch process.
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