PRODUCTION

Europeans

Improve

Acetylene

Processes,

Focus

Attention ' . ' . · • , - : · : * • ' ^ • ' . ' · - . - · • · · .

ί^-ί^^^'ϊΓ ·̂? Other Products

T h e Burner · . y SJBA*—metallic burner and a sheet of wafer to reduce carbon de­position. ~A - > * BASF—ceramic burner and a spray of water to quench the flame. H oecht—water-cooled metallic burner. Flame is quenched ' w i t h water followed by oil .

a n d C h e a p e r Recovery System · · .

SBA^—anhydrous ' a m ­monia solvent system. Monfecatini-Fctuser— methanol solvent sys­tem.

More European Acetylene Processes Europeans continue to develop acetylene processes using natural gas and other hydrocarbons

J V l o S T PETROCHEMICAL ACETYLENE PLANTS in the United States use proc­esses developed in Europe a few years back. European development in this field hasn't slowed down. New plants are being built, and improved processes are being worked out.

Partial oxidation processes—like the Sachsse process developed at BASF in Germany—have been the basis for most U. S. plants. Their problems can be divided into two main groups: burner design; and separation of acetylene from the hydrogen and other sub­stances in the cracked gas stream.

Here's what's new in partial oxida­tion in Europe:

• Société Belge de l'Azote has come up with a new burner to ease the car­bon deposit problem, and a cheap solvent to cut acetylene recovery costs —liquid anhydrous ammonia. Raw material: either methane or higher hydrocarbons.

• T h e Fauser process, at Montecatini in Italy, uses another cheap solvent— methanol. The by-product carbon mon­oxide-hydrogen mixture—often used for synthesis gas for other products—is al­ready compressed to 13 atmospheres.

• In Germany, Farbwerke Hoechst's new process uses naphtha, with boiling points up to 200° C. Feed is not burned with oxygen directly. It is cracked in a flame of lean gas (from the recovery system) burning with oxygen.

In a partial oxidation process part of the feed is burned to supply energy for the cracking of the remainder of the hydrocarbon. In the cracking process hydrogen atoms are broken off and carbon-to-carbon bonds are broken. Under proper conditions the active molecular fragments combine to form acetylene and hydrogen. Acetylene is very unstable at high temperatures, so the reaction mixture must be cooled very rapidly.

In the BASF process methane and oxygen streams are preheated sepa­rately, passed into the mixing chamber of a ceramic burner and then through a perforated "burner block." The re­action takes place in a flame just be­yond the burner block. The gas stream is almost immediately quenched by a water spray.

Excessive carbon deposition has al­ways been a big problem in burners for

partial oxidation of hydrocarbons, es­pecially those higher than C l s and in particular unsaturated hydrocarbons. In the Société Belge de l'Azote burner, water is introduced as a sheet 'which surrounds the flame and flows parallel to the gases. In this way it carries off the carbon particles which otherwise accumulate on the walls of the burner.

Exactly how to keep the sheet in the proper form is one of the key points in Société Belge de l'Azote's know-how. The sheet must be thin and continuous. It must also remain parallel to the axis of the flame.

One way to obtain such a sheet is to force water through a slot around the edge of the burner. If the flame points downward, a cylindrical screen with water flowing over it can be used. The screen ensures good distribution of the water.

The burner is entirely metallic. Ac­cess for maintenance purposes is easy, although practically no maintenance is needed.

Hoechst's process uses a somewhat different approach. Instead of burn­ing part of the feed itself to get the temperatures needed for cracking, it burns a lean gas stream taken off at a point in the recovery process. The lean gas consists chiefly of hydrogen, with some methane. A number of other gases could be used just as well. The gas is burned with oxygen, and naphtha feed is introduced into the flame. The reaction is quenched with water fol­lowed by oil. This burner is also metallic and is water cooled.

• Acetylene Separa t ion . Acetylene is only one of the cracked gases leaving the burner in a partial oxidation proc­ess. In the BASF process, for example, the amount of acetylene in the cracked gas is only 8<fr. Carbon monoxide and hydrogen are also major components, but there are also some methane, carbon dioxide, nitrogen, ethylene, and other substances. In some processes, enough ethylene is formed that it is a s important a product as acetylene.

Selective absorption in a solvent is the usual method of separating acety­lene from impurities or co-products. In the BASF process cracked gas contacts a suitable solvent—say dimethylforma-mide or butyrolactone—in a tower. Acetylene dissolves. Heating the rich solvent and lowering the pressure re­lease the acetylene.

Of course, it isn't all that simple. The solvent is not absolutely selective for acetylene but dissolves other sub­stances as well. Carbon dioxide is one of these. I t , and other components less soluble than acetylene in the solvent, must be stripped off before acetylene is removed.

Other impurities are more, rather than less, soluble than acetylene in the solvent. They must be removed if the

7 6 C & E N J U N E 17, 1957

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-now available.. .anotlaer organic sulfuir aairxpoxxrxdi

Tr i ch l o rome thanesu l f ony l Ch lo r ide has highly reactive chlorine and S02 groups. Typi­cal of th is versatile molecule are reactions with olefins to increase chain length, with alkalies, ammonia and amines to form salts, and condensations with aromatics. All four chlorines are reactive; the S0 2 group can be retained, reduced or eliminated.

T r i c h l o r o m e t h a n e s u l f o n y l C h l o r i d e , C I 3 CS0 2 CI , M.W. 217.9 , is a lach rymato ry white solid» with a penetrating odor. It melts at 142°C and boils at 170°C. It is soluble in most organic solvents, almost insoluble in water. It i s stable at normal temperatures; unlike most sulfonyl chlorides it is not easily hydrolyzed.

It is reported to be of value for improving

Diesel fuels, in the vulcanization of rubber, in the manufacture of insecticides and complex organics, dyes and pharmaceuticals.

Trichloromethanesulfonyl Chloride is now available in development quantities.

Stauffer's Research in organic sulfur com­pounds is extensive; unmatched, we believe. For further information, write for technical bul­letins on Trichloromethanesulfonyl Chloride and any of the other organic sulfur compounds listed below.

Chlorodimethyl Sulfide bis-(Chloromethyl)Sulfide bis-(Phenyl)Sulfone bis-(Chlorophenyl)Sulfone Perchloromethyl Mercaptan Triphenylsulfonium Chloride

:M:';:: ;Μ·"&-:·>Μ'·;ΐΜ;ΐ·:':;νί^

, 636 Ca l i fo rn ia Street, Sa vy YoVk 1 T | N e w y o r k ; F ranc isco 8 i Ca l i fb rn i

J U N E 17, 1957 C & E N 77

Κ. W. Chemicals Ltd. offer t h e i r s e r v i c e s

t o

American Chemical

Manufacturers a s S a l e s C o n c e s s i o n a i r e s

of chemical and allied p r o d u c t s

possessing a sound sales p o t e n ­

t ia l in U . K. a n d Br i t i sh C o m ­

m o n w e a l t h m a r k e t s .

Communications to:—

41 K i n g s w a y ,

L O N D O N , W . C . 2 .

E N G L A N D

M a k e sure that you get the highest quality laboratory glassware for the lowest pos­sible price by making the "TWO-WAY" Test. STEP 1. Obtain samples of several ad­

vertised brands of laboratory glass­ware. Be sure to include a piece of Doerr Diamond D Blue Line. Devise the most rigid tests you can think

of and evaluate each brand on the basis of these tests. Tabulate the results.

STEP 2. Now, compare the prices. You will f ind that the Doerr Diamond D Blue Line is your best buy . offering the highest quality for the lowest possible price.

PRODUCTION

solvent is recycled. Higher acetylenes are the chief offenders here. If left in the system they polymerize and build up in the solvent. So, an additional, more drastic, stripping operation must also be included in the separation process.

Solvents like dimethylformamide or butyrolactone are expensive, and a lot of research has gone into finding cheaper ones. The Montecatini-Fauser process uses methanol. Cracked gas from the burner is compressed to 14 atmospheres and contacts methanol cooled to —70° C. Heating the rich solven* to 20° C. drives off the acety­lene, as well as the carbon dioxide. Washing the rnixtiire of gases with aqua ammonia removes the C 0 2 , leav­ing pure acetylene. Higher acetylenes

are removed from the methanol b y distillation.

The lean gas left after acetylene h a s been removed is fractionated to recover ethylene. Fur ther cooling to minus 160° C. removes methane, which is sent back to the cracking furnace. T h e carbon monoxide-hydrogen mixture which is left is already compressed to 13 atmospheres and is used for meth­anol synthesis.

The Société Belge de l'Azote proc­ess uses liquid anhydrous ammonia as a solvent. It is a cheap and highly specific solvent for acetylene. Gases from the burner a re first passed through two electrostatic filters to remove carbon particles and then they are washed in two columns for partial puri­fication. The first dissolves the carbon

One of the control panels at Chemische Werke Huels

European Petrochemical Acetylene Plaints While their scientists are busy improving processes, Europeans a re al­

ready operating many acetylene plants . Here is a quick run-down. • I taly, Italy already has three acetylene plants using natural gas as

a raw material, with a fourth on the way.

• SISAS, in Milan, and the Edison Group at its p lan t near Venice, bo th use the Sachsse partial oxidation process—developed a t BASF in Germany -

• Montecatini also uses a part ial oxidation process a t its 20-ton-per-day plant at Novara. This plant capacity is being doubled. A methanol p lan t , soon to be followed by an ammonia plant, uses by-product carbon mon­oxide and hydrogen for synthesis gas.

• Under construction is the fourth plant—for ANIC, at Ravenna. I t will be ready in the spring of 1958, and will be integrated with b u t a d i e n e / styrene rubber and nitrogen fertilizers plants. Opposing the previous trend, this plant will be designed by a U. S. company, Union Carb ide . The Italian plant will be similar to Carbide's at Texas City b u t will b e bigger.

• France and Belgium. Société Belge de l'Azote has a semicommercial plant at Liege, Belgium, and it is engineering a full-scale plant now under construction for Houillères du Bassin de Lorraine in France.

• Germany. Farbwerke Hoechst has recently announced that it h a s a pilot plant using a new process. Besides this and the BA.SF plant a t Ludwigshaven, Germany has a very large plant using the electric a r c process at Chemische Werke Huels. This went into operation in 1940. The arc process is economical a t this particular location because of t h e availability of cheap electricity and raw materials. Natural gas, refinery gases, and the so-called "hydrogénation off-gas" from coal a r e all used. Gases are passed through an arc chamber at high speed to give acetylene, hydrogen, and some minor products.

7 8 C & E N J U N E 17, 1957

ACID

WIDELY USED FOR BROMINATION and as an intermediate, Hydrobromic Acid has made a place for itself in the manufacture of dyes, drugs, perfumes, sedatives, photographic emulsions and in many other fields. Michigan Chemical Corporation assures a prompt and continuous supply of HBr of guaranteed purity at a reasonable price.

HYDROBROMIC ACID

ASSAY: 4 8 % TECHNICAL 6 2 % TECHNICAL

Molecular Weight: Specific Gravity at 2 0 / 4 ° C : Pounds per gallon at 20°C:

HC1, not more than: Vapor pressure at 30°C:

at 50°C:

80.924 1.488

12.4 0.10%

80.924 1.74

14.5 0.15%

85 mm 380 mm

C-56-12 •Reg. U.S. Pat. Off

Michigan Chemical Corporation, for more than twenty years a quality producer of chemicals, offers a series of pure bromine derivatives, among them Ethyl Bromide, Monobromobenzene, Cy-clopentyl Bromide and Hydrobromic Acid, specially made for use in pharmaceutical manufacturing. Write for further informa­tion or catalog.

M I C H I G A N C H E M I C A L C O R P O R A T I O N 536 Bankson Street, Saint Louis, Michigan

EASTERN SALES OFFICE: 230 Park Avenue. New York 17, New York

J U N E 17, 1 9 5 7 C & E N 7 9

Dowa Mining's Kosaka hydro-metallurgical plant where Dorrco FluoSolids System roasts 8 3 metric tons of complex copper-zinc concentrates per d a y .

One of two 2 0 ft. dia. FluoSolids Reactors roast­ing 2 3 5 metric tons per day of crushed pyrrhotite ore at Dowa's O k a y a m a Plant.

Flu id iza t ion— key to m a x i m u m

ut i l i za t ion in J a p a n Processing copper bear ing p y r r h o t i t e ore, t h e D o w a M i n i n g C o m p a n y a t t h e O k a y a m a , J a p a n p l a n t is producing . . . a n d a l l from the s ame raw mater ia l . . . s in tered i ron ore for blast furnace use , cement copper a n d sulphur ic acid. Of major impor t ance in this un ique instal lat ion is t h e Dor rco FluoSolids Sys t em. Util izing t he p r o v e n principles of fluidization, t he c rushed r a w ore is roas ted unde r control led condi t ions in t h e S y s t e m . . . providing S O 2 gas for con tac t acid m a n u f a c t u r e . . . Roas te r calc ine is acid leached for copper recovery a n d leach residue is sintered a s b las t furnace feed. Dorr-Oliver in conjunct ion with our associates in J a p a n , Sank i E n ­gineering Co . L t d . of T o k y o , h a v e collaborated wi th D o w a Engineers before. A t D o w a ' s hydro-meta l lu rg ica l p lan t in Kosaka , J a p a n , t he Dor rco FluoSolids Sys tem is a pr ime factor in the world ' s first success­ful roas t ing of copper and zinc wi th electro winning of b o t h meta l s . Fo r detai led informat ion o n D-O e q u i p m e n t and services involving the separa t ion of finely d iv ided solids in suspension or fluid techniques , d r o p a line t o Dorr-Oliver Inc . , S tamford , Connec t i cu t .

FluoSolids is α Trademark of Dorr-Oliver Inc. Reg. U. S. Pat. Off .

I N C O R P O R A T E D

$^|tiç ; 'dp^ F Ο Ε D C O N N E C T I C U

PRODUCTION

dioxide. The second—with methanol as the solvent—removes moisture, aro-matics, and heavier acetylenes.

The partially purified gas is then washed in cold, liquid anhydrous am­monia at atmospheric pressure. Acet­ylene dissolves and is separated from the ammonia by distillation.

When hydrocarbons higher than methane are used as feed, ethylene is formed in substantial quantities in ad­dition to acetylene. Ethylene does not dissolve in the ammonia. It is re­moved by fractionation of the gas stream leaving the ammonia* contactor. The residual gases contain carbon mon­oxide, hydrogen, and some methane, but no carbon dioxide.

• Still in t h e Lab. Besides these improved processes already in pilot-scale operation, there are some labora­tory processes with more daring in­novations.

In Great Britain, the National Re­search Development Corp. has obtained U. S. and British patents on two partial oxidation processes. In one, methane and oxygen are burned in a fuel-rich mixture in an internal combustion piston engine.

Quenching of the burning mixture takes place in the expansion stroke, so part of the heat of reaction can be re­covered as useful work. Process is controlled by varying engine speed, ignition timing, compression ratio, and the methane-oxygen ratio.

In the second method part of the cooling takes place in a gas turbine, which also makes it possible to recover useful work from the heat of reaction.

The electric arc is used in laboratory experiments at Knapsack-Griesheim, a subsidiary of Hoechst. The aim of this work—for which a Belgian patent has been granted—is to use the arc to convert molecular hydrogen into atomic hydrogen. Atomic hydrogen is very active and brings about a number of reactions with hydrocarbons.

In one experiment the atomic hydro­gen stream, moving at over 400 meters per second, impinges on preheated pro­pane. The reaction chamber tempera­ture is 1200° to 1600° C. The re­action is rapidly quenched by cold water. Yields as high as 85% acety­lene have been obtained, but there are many problems to be solved before the process can be put on a continuous large-scale basis.

• Process Selection. If a company does not want to invest the capital re­quired for a large, integrated project it may be better off getting its acetylene from calcium carbide. A petrochemi­cal acetylene plant may not be economi­cal if by-products cannot be put to work. Carbon monoxide and hydrogen can best be used as synthesis gas for

8 0 C & E N J U N E 17, 1957

CHEMISTRY— Physical, organic, colloid, analytic, biologi­cal, and radiation chemistry, in such areas as thin films, poly­mers, capsular phenomena, photographic systems, membranes, non-mechanical printing techniques, dyes and color studies, elastomers, adhesives, plastics, lubrication, electro-deposition.

PHYSICS · · · Challenging assignments in ferromagnetics and ferroelectrics, electroluminescence, phosphors, photoconductors, high-speed printing techniques, vacuum deposition, X-ray dif­fraction, crystal structure, low-temperature studies, powdered metal compaction, domain studies.

ELECTRONICS . . . Memory devices, access circuitry, input and output devices, computer components, advanced magnetic core devices and circuits, switching circuits, transistors, diodes, semi-conductors, logical design, experimental and prototype design, are among the challenges awaiting you at NCR.

METALLURGY · · · Alloys, brazing, ductile castings, pow­dered metals, precision casting, gas analysis, foundry processes. MA THEM A TICS- · · Numerical analysis, computation theory, Boolean algebra, computer logic, programming. CERAStfiCS . . . Ferrite electronic components, phosphors, dielectrics.

ATONE OF THE WORLD'S MOST SUCCESSFUL CORPORATIONB Choose your own area of research or development from those above. You may work at either basic studies or application phases. There is a University Extension in our own plant for graduate study to­ward Master's Degrees, with a tuition refund plan. NCR has regular seminars on scientific topics . . . a large technical library . . . pilot plant facilities. Let us tell you more about NCR! Write: Director of Scientific Personnel, Section No. E, The National Cash Register Company, Dayton 9, Ohio. THE NATIONAL CASH REGISTER COMPANY

J U N E 17, 1 9 5 7 C & E N 8 1

New Text

DIDYMIUM A plentiful and economical rare earth mixture

a report by LINDSAY

You have often watched a welder at work, watched briefly that is, because the intense glare, even at a safe dis­tance, forced you to t u rn your eyes awav. And you wondered perhaps how it is that a welder, even with protective goggles, can focus his eyes on a weld­ing spot for minutes at a time.

The secret, of course, is Didijmium. The lenses in the welder's goggles, and in the glass blower's goggles, too, are m a d e with d i d y m i u m which com­pletely absorbs yellow sodium light, thereby reducing glare and eye fatigue.

WHAT IS DIDYMIUM?

In 1842, a European chemist named Mosander separated from a crude rare earth mixture some material he called "didymium." He thought it was a new element. Actually it was a mixture of rare earths predominantly neodymium and praseodymium. Classically, didy­mium means a mixture of Nd and Pr. However, commercially, the name di­dymium is restricted to the cerium-free group of rare earths extracted from mo-nazite ore, since the composition of the mixture is reasonably constant.

Didymium is the basic material from which all the other rare earths except

Absorption Spectrum of

DIDYMIUM CHLORIDE SOLUTION

from monazite containing 1 g. rare earth

oxide/100 ml. compared with water in 5 cm. cells

cer ium are p roduced . L indsay p ro ­duces didymium in various forms for different applications. For example :

Didymium Carbonate—pink powder, insoluble in water, soluble in acids.

Didymium Oxide —brown powder, insoluble in alkalis, soluble in acids.

Didymium Chlor ide —pink lumps, soluble in water and acids.

TYPICAL APPROXIMATE COMPOSITION OF RARE EARTHS |

La203

Nd 2 0 3

Ρ Γ 6 0 , ! 1 Sma03

IN DIDYMIUM MATERIAL

1 Other rare earths and

4 5 % 3 8 % 11 %

4 %

2 %

Didymium is one of the most economi­cal forms of rare earth mixtures and is available for prompt shipments in car­load quantities. It is useful for the col­oring characteristics of Nd and Pr and for some of the other rare earth proper­ties where purity is of secondary im­portance.

In addition to its extensive applica­tion in the p r o d u c t i o n of lenses for

400 500 600

WAVELENGTH-MILLIMICRONS

PLEASE ADDRESS INQUIRIES TO

LINDSAY (HEMICAL ( P M P A N Y 266 ANN STREET · WEST CHICAGO, ILLINOIS

welders' and glass blowers' goggles, di­dymium has other important uses. In coloring and decolorizing of glass. As a porcelain coloring agent. In light filters for calibration of instruments. To con­trol the temperature coefficient of ca­pacitance in barium-titanate ceramic condensers for radio and electronic use (U.S. Pat. 2,398,008). In stainless steels w h i c h a r e f o r g e d h o t (U.S. Pa t . 2,553,330).

We'd like to t empt you to investigate didymium and o ther rare earth salts as possible materials for use in your chem­ical and manufacturing processes. T h e very fact that important companies in a w i d e c r o s s - s e c t i o n of i n d u s t r y , through their own research, have dis­covered profitable applications for the rare earths may intrigue your own re­search people.

We can be helpful to you and will b e pleased to supply any information we can. Please keep in mind that we p ro ­duce rare earths in purities up to 99.9% and higher in some cases (which is a n achievement in itself). Shipments, de ­pending on the salts you may need, can be made to fit your schedules in quan­tities from a gram to a carload.

8 2 C & E N J U N E 17, 1 9 5 7

PRODUCTION

products like ammonia or methanol. If higher hydrocarbons are used instead of methane as the starting material an outlet for ethylene must be found. Thus, the final choice of a process often depends largely upon the particular use to be made of the byproducts.

Cheaper Titanium? Armour Research Foundation finds w a y to make pure t i ­tanium tetrachloride f rom i l -menite

A R M O U R RESEARCH FOUNDATION has come up with a new process aimed a t making pure titanium tetrachloride from low grade ores at less cost. De­veloped by Friedric Schossberger, the process is based on an old-time quan­titative separation method for t i tanium —a method dating back to 1901.

The quantitative method uses TiCl4 . The TiCl4 is dissoved in HCl; KCl is added and potassium chlorotitanate, K2TiCle , precipitates. Schossberger starts with ilmenite—cheap ti tanium ore —dissolves it in sulfuric acid ra ther than HCl because ilmenite is more soluble in sulfuric. Iron content is re­duced by two controlled crystalliza­tion steps when its level is high enough to interfere.

sssrtSi "H?«P-,«-·

φ For Confident Shipping Hercules Powder has greatly reduced its problems of freight damage during rail shipment by using these Evans D F modified cars. Loads—be they palleted bags, cases, drums, or mixtures of these —are locked into position by "fences." In this way, material does not shift or topple as the car lurches and sways, according to Evans Products. Here, a workman at Hercules* Mansfield, Mass., plant loads pentaerythritol on pallets for shipment to Cleveland, Ohio.

Next, Schossberger t rea ts the sul­furic acid solution with gaseous HCl at about 0° C. He then saturates the mixture with KCl. Upon further cool­ing the chlorotitanate precipi tates out. After separating the chloroti tanate, he heats it to 330° to 400° C . Pure ti­tanium tetrachloride is evolved; iron stays behind with the KCl.

His process has three major advan­tages, Schossberger declares:

• Cheaper titanium ore—ilmenite, rather than rutile—can be used.

• Lower process temperatures are needed—around 400° compared to the 850° C. or so used in the present chlorination process.

• Resultant t i tanium tetrachloride is pure. I t shows no vanadium and iron chlorides, major impurities of the chlorination process.

Armour is still developing the proc­ess. However, it looks so good that the foundation expects it eventually to replace chlorination. •

in balances

the Right-Α- Weigh pays its way "That is what I hear from many of my customers. In some of t h e o t h e r laboratories they like the Ainsworth Right-A-Weigh so m u c h they don't care whether or not i t pays for itself.

"There is no question about t h e fact t h a t the one pan, subst i tut ion-weigh ing Right-A-Weigh is fast, accurate, easy to use, easy to r e a d . . . and saves a lot of time for chemis ts and technicians.

"These advantages plus the 'little th ings that count ' . . .sapphire bearings, built-in Brunton Metal Class S Weights, compensated beams, arc type beam arrestment, slideout side panels, good op t i c s . . . explain the fast growing popular i ty of the Right-A-Weigh balance."

IT'S THE LITTLE

THINGS THAT COUNT

Just call ï/our^laboratorj^suppl^ salesman7 .He^caiTgive yovi more' information about Ainsworth proved and improved balances and weights.^ "*&>&»*3$> „*-

J U N E 17. 1957 C & E N 83