A E Staley Manufacturing Company

Frank Verbanac

Austin Harry Young

Rolland W Short

The invention provides an improved cellulosic ester or ether product with a degree of ester or ether substitution of between 2.0 and about 2.9 which is derivatized or further reacted by reaction with an acrylamide reactant to provide pendant acrylamide functionality or substituents at a degree of substitution (D.S.) of at least about 0.05 (preferably from about 0.05 to about 0.5) and to thereby provide a polymerizable organic solvent-soluble product which is insoluble in water and copolymerizable with vinyl monomers. The product is conveniently prepared by reacting said cellulose ether or ester derivative with a catalyst and the acrylamide reactant at a pH of from between about 4.2 and about 4.5. The reaction is carried out at a temperature between 80.degree. C. and 120.degree. C. for from one-half to three hours, while removing the water of reaction. The resulting acrylamide functionality-containing cellulose ester or ether product typically contains unreacted, residual hydroxyl groups in an amount corresponding to a hydroxyl D.S. of from about 0.05 to about 0.95.

Cellulosic organic solvent soluble products

The invention provides an improved cellulosic ester or ether product with a degree of substitution of between 2.0 and about 2.9 which is derivatized or further reacted by reaction with an acrylamide reactant to substitute to a D.S. of from about 0.05 to about 0.5 and provide a hydroxyl D.S. of from about 0.05 to about 0.5, and thereby provide a polymerizable organic solvent-soluble product which is insoluble in water and copolymerizable with vinyl monomers. The product is prepared by reacting a cellulose derivative with a catalyst and the acrylamide reactant at a pH of from between about 4.2 and about 4.5. The reaction is carried out at a temperature between 80.degree. C. and 120.degree. C. for from one-half to three hours, while removing the water of reaction.

Water-absorbent, starch copolymerizates are prepared by copolymerizing an ethylenically unsaturated starch with other ethylenically unsaturated monomers which contain water-attractant groups or precursors of water-attractant groups. The water-absorbent starch copolymerizates may be easily prepared into the desired configuration for a particular end-use or combined with other substrates or carriers. The unpolymerized starch and monomers or precursors thereof may be applied or incorporated into a suitable carrier or substrate (e.g., cellulosic materials such as textiles, papers, etc.) and copolymerized in situ to provide a composite article of unitary construction with the water-absorbent starch copolymerizate permanently bonded or affixed thereto.

Water-absorbent starch copolymerizates

Preformed, homogeneous, non-linear starch copolymerizate articles may be prepared by copolymerizing a preformed, homogeneous mixture of water, ethylenically unsaturated starch and ethylenically unsaturated monomers to provide a labyrinth of copolymerized starch chains interconnected with each other by the copolymerized monomeric units. The invention is particularly suitable for preparing high-binder, aqueous coating compositions which may be applied to a variety of substrates and subsequently copolymerized with polymerization initiating systems. Improved water- and detergent-resistance may be obtained by incorporating film-forming additives, cross-linking reagents or polyunsaturated compounds into the copolymerizable starch composition.

Copolymerized starch composition

A free-flowing binder-disintegrant powder material consisting essentially of a precompacted-starch powder, especially adapted for use in direct compression tabletting machines to produce non-friable tablets having excellent disintegration properties. This precompacted-starch powder is also useful as a free-flowing filler for blending with dry powder ingredients in dry-dosage capsules. The precompacted-starch powder is obtained by subjecting an ungelatinized granular starch to physical compaction without supplementary thermal energy, but with sufficient mechanical energy input to obtain a precompacted-starch having birefringent granules and non-birefringent fragments of granules and some aggregates of granules and fragments, and then dried to a moisture content of 9-16% total weight basis. After precompacting, the starch is pulverized to form a free-flowing powder having a loose bulk density of 0.5 to about 0.7 grams per milliliter. The precompacted-starch powder is essentially free of +40 mesh particles, at least 90% of the particles are -80 mesh, at least about 10% is +270 mesh, and from about 30% to 90% is -270 mesh size on a total weight basis (U.S. Standard Sieve Series, A.S.T.M. Specifications). Cold water solubility of the precompacted-starch powder is in the range of from 4% to about 40% by weight, preferably about 10% to 20% by weight, and this powder is capable of being formed into a hard, non-friable tablet in combination with other active ingredients in a direct compression tabletting machine, the precompacted-starch powder being dually functional as both a binder and disintegrant. The resulting tablet has a hardness index of at least about 4 kilograms, preferably at least 8 kilograms, a friability loss of less than 1% by weight, a swelling power of 2.5 to about 12, preferably at least 8, and is capable of effectively disintegrating when placed in water.

Precompacted-starch binder-disintegrant-filler material for direct

The invention relates to starch acrylamides containing polymerizable pendant acrylamide groups. The hydrophilic or hydrophobic properties of the starch can be altered or modified by the acrylamide groups or the type of starch chain. The starch acrylamides can be homopolymerized or copolymerized with other ethylenically unsaturated monomers as well as other cross-linking reagents to provide water-resistant, clear, flexible coatings or shaped articles. The hydrophilic starch acrylamide hydrolyzates herein readily disperse into water at a high solids level to provide low-viscosity pastes which may be used as a vehicle to prepare flexible, water-insoluble starch-based coatings. The starch acrylamides may be prepared by etherifying a starch with N-methylol acrylamides in the presence of an acid catalyst and a polymerization inhibitor.

Starch acrylamides and the method for preparing the same

Starch hydrolyzates having a desired degree of polymerization are prepared by hydrolyzing derivatized starch esters with amylase and thereafter saponifying the starch ester hydrolyzates to obtain a hydrolyzate product essentially free from substitution. Amylolysis and saccharide distribution of the resultant saponified hydrolyzates are effectively accomplished by pre-selecting a starch ester having the appropriate degree of ester substitution.

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Decatur, IL, United States of America

Frank Verbanac