Powders, alcohol ether sulfate

Sodium dodecylbenzenesulfonate is undoubtedly the anionic surfactant used in the greatest amount because it is the basic component in almost all laundry and dishwashing detergents in powder and liquid forms. However, alcohol and alcohol ether sulfates are the more versatile anionic surfactants because their properties vary, with the alkyl chain, with the number of moles of ethylene oxide added to the base alcohol and with the cation. Consequently, alcohol and alcohol ether sulfates are used in almost all scientific, consumer, and industrial applications. 

Alcohol ether sulfates (R0(CH2CH20)S03"Na-") - alcohol ethoxy-late reacted with sulfur trioxide and then neutralized in NaOH. Application s include dishwashing liquids and shampoos, home laundry powders, and personal care products. 

Natural C12-C16 fatty alcohols or C10-C15 synthetic fatty alcohols with >4 moles ofEO. Alcohol ethoxylates with 5-11 moles of EO are used in liquid and powdered laundry detergents as coactives with LAS and fatty alcohol ethers sulfate (FAES) in hard surface-cleaning formulations and in a host of industrial applications. Alcohol ethoxylates with 12-50 moles of EO and their respective sulfated and phosphated derivatives find use in emulsion polymerization and other select applications. 

The classical method for making tert-butyl esters involves mineral acid-catalysed addition of the carboxylic acid to isobutene but it is a rather harsh procedure for use in any but the most insensitive of substrates [Scheme 6.33].80-82 Moreover, the method is hazardous because a sealed apparatus is needed to prevent evaporation of the volatile isobutene. A simpler procedure [Scheme 6.34] involves use of tert-butyl alcohol in the presence of a heterogeneous acid catalyst — concentrated sulfuric acid dispersed on powdered anhydrous magnesium sulfate. 3 No interna] pressure is developed during the reaction and the method is successful for various aromatic, aliphatic, olefinic, heteroaromatic, and protected amino acids. Also primary and secondary alcohols can be converted into the corresponding /erf-butyl ethers using essentially the same procedure (with the exception of alcohols particularly prone to carbonium ion formation (e.g. p-... 

White, odorless, tasteless, heavy powder slowly dec by sunlight into mercuric chloride and metallic mercury sublimes at 400-500 without melting, d 7.15. Practically insol in water (0-00020g/]00 ml H20 at 25 ) HCI or alkali and alkaline earth chlorides increase soly in water. Insol in alcohol. ether. Dec by solns of alkali iodides, bromides or cya -nides into the mercuric salt and metallic mecury solns of alkali chlorides act similarly but slowly. It is blackened by ammonia, caustic alkali and alkaline earth solns. Protect from light. Incompat Bromides, iodides, alkali chlorides, sulfates, sulfites, carbonates, hydroxides, lime water, acacia, ammonia, golden antimony sulfide, cocaine, cyanides, copper salts, hydrogen peroxide, iodine, iodoform, lead salts, silver salts, soap, sulfides. 

PHYSICAL PROPERTIES (nickel chloride) yellow or brown scales nickel chloride hexahydrate appears as green, deliquescent crystals or crystal powder anhydrous salt is golden yellow odorless solid soluble in ethanol and ammonium hydroxide soluble in water insoluble in ammonia MP (1,001°C, 1834°F) DN (3.55 g/cm at 20°C) SG (3.55) VD (NA) VP (1 mmHg at 671°C). (nickel sulfate) yellow cubes nickel sulfate hexahydrate appears as blue to blue-green tetragonal crystals of green transparent crystals becomes blue and opaque at room temperature odorless soluble in water, ethanol, and methanol insoluble in alcohol, ether, and acetone MP (840°C, 1544°F loses SOj) DN (3.68 g/cm at 20°C) SG (3.68) VD (NA). 

Traditionally, powdered and liqnid laundry detergents contained linear alkyl benzene sulfonates, ether sulfates, and alcohol ethoxylates as surfactants, along with builders, enzymes, polymers, and possibly bleaches as additional active ingredients. These formulations dealt weU with different types of dirt and stains under a variety of water conditions. 

Alkyl ether sulfates, also called alcohol ethoxysulfates, are prepared by addition of one to four oxyethylene groups to an alcohol which is then sulfated. Oxyethylation enhances water solubility and foaming over the analogous alcohol sulfate, giving a product useful in shampoos and in liquid and powdered detergents. The raw material for these products can be either natural fatty alcohols or primary or secondary synthetic alcohols, usually of C12-C18 chain length. The analogous alkylphenol ether sulfates are found in industrial applications. Ether sulfates are not as sensitive to water hardness as are other anionic surfactants. 

Monohydroxyaluminum distearate, (HO)Al(OOC(CH2) gCH2)2, used to be the largest selling aluminum carboxylate (1). Although stiU sold, the product is no longer Hsted in the U.S. International Trade Commission Report (1) because of low volume or confidentiahty constraints because of too few supphers. Aluminum distearate is a white powder that is insoluble in water, alcohol, and ether. A key property is its abiUty to gel vegetable oils and hydrocarbons. Aluminum distearate is prepared by the reaction of aqueous sodium stearate with aqueous aluminum sulfate or chloride at pH 7.3. Aluminum monostearate is formed if the sodium stearate solution is held at pH 9.5 (44). 

Zinc. Next to sodium, zinc is the most used reductant. It is available in powder, dust, and granular (mossy) forms. Zinc gets coated by a l er of zinc oxide which must be removed to activate it before it can reduce effectively. It can easily be activated by shaking 3 to 4 min. in a 1% to 2% hydrochloric acid solution. This means for every 98 ml of water volume, add 2 ml of coned hydrochloric acid. Then wash this solution with water, ethatiol, acetone, and ether. Ot activation can be accomplished by washing zinc in a solution of anhydrous zinc chloride (a very small amount) in ether, alcohol, or tetrahydrofuran. Another way is to stir 180 g of zinc in a solution of 1 g copper sulfate pentahydrate. Personally, I like the HCl acid method. 

Chloride gas. Magnesium metal turnings, Arsenic trichloride, Tetrahydrofuran, Pentane, Sodium sulfate Diethyl ether, Dichloromethylphosphine, Ethyl alcohol, N,N-Diethylamine, 2-Diisopropylaminoethanol, Rhombic sulfur Hexachloroethane, Zinc powder... 

Ammonia, Picric acid. Water Picric acid. Ammonia, benzene Ammonia, Iodine crystals Ammonium nitrate. Charcoal powder Potassium dinitramide. Ammonium sulfate. Isopropyl alcohol. Petroleum ether... 

Add 30 mL of alcohol if the sample is liquid, or 23 mL of alcohol and 7 mL of glycerin if the sample is solid, followed by 3 mL of a 9 10 potassium hydroxide solution. Reflux under an all-glass condenser for 30 min. Cool the solution, add 30 mL of water, and transfer into a separator. Add 2 g of finely powdered sodium sulfate. Extract by shaking for 2 min with one 150-mL portion of ether and if an emulsion forms, with three additional 25-mL portions of ether. Combine the ether extracts, if necessary, and wash by swirling gently with 50 mL of water. Wash more vigorously with three additional 50-mL portions of water. Transfer the washed ether extract into a 250-mL volumetric flask, and add ether to volume. 

Morphine Sulfate, U5P. Morphine sulfate is prepared in the same manner as the hydrochloride (i.e.. by neutralizing morphine with diluted sulfuric acid). It occurs as feathery, silky, while crystals, as cubical masses of cry.slals, or as a white crystalline powder. Although it is a fairly stable salt, it loses water of hydration and darkens on exposure to air and light. It is soluble in water (1 16. 1 1 at 80°), poorly soluble in alcohol 11 570. 1 240 at 60°), and insoluble in chloroform or ether. Aqueous solutions have a pH of about 4.8 and may be. sterilized by healing in an autoclave. 

It iK dirs as levorotatory. colorless, efflorescent crystals orasawhitc crystalline powder. It is light sensitive. Codeine U slightly soluble in water (1 120) and sparingly soluble in ether (1 50). It is freely soluble in alcohol (1 2) and very soluble in chloroform (1 0.5). Codeine is a monoacidic base and readily forms salts with acids, with the most important being the sulfate and the phosphate. The acetate and methyl-bntniide derivatives have been used to a limited extent in tough preparations. 

Codeine Sulfate, USP. Ctxleine sulfate is prepared by neutralizing an aqueous suspension of codeine with diluted sulfuric acid and then effecting crystallization. It cK Curs us white cry.stals. usually needle-like, or as a white cry.stalline powder. The salt is efflorescent and light sensitive. It is. soluble in water (1 30. 1 6.S at 80°). much less soluble in alcohol (1 1.280). and insoluble in ether or chloroform. This salt of codeine is prescribed frequently but is not as suitable os the pho.sphate for liquid preparations. Solutions of the sulfate and the phosphate are incompatible with alkaloidal reagents and alkaline sub.stances. 

A solution of (7 ,7 )-diisopropyltartrate (E)-crotylboronate (46.Og, 0.152 mol) in dry toluene (1 L) was treated with powdered 4 A molecular sieves (6 g) at -78 °C. A solution of the aldehyde (13.1 g, 0.076 mol) in dry toluene (50 mL) was cooled to -78 °C and added dropwise into the suspension via a cannula. The resultant mixture was stirred at -78 °C for 1 h before an aqueous solution of sodium hydroxide (2 N, 70 mL) was added. The mixture was warmed to 0 °C, stirred for 30 min, and filtered through a pad of Celite. The aqueous layer was extracted with ether (3 x 250 mL) and the combined organic phases were washed with brine (200 mL), dried over magnesium sulfate, hltered, and concentrated in vacuo. The crude product was purihed via hash chromatography eluting with hexanes EtOAc (7 1) to afford 15.2 g (88%, 90% d.e.) of the alcohol as a colorless oil. 

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