Chemplex Company

Norchem, Inc.

Enron Chemical Corporation

Robert A Dombro

Yu-Tang Hwang

William Kirch

Thomas J Pullukat

Raymond E Hoff

Lloyd Pebsworth

A method of preparing a high pore volume, high surface area zirconia-titania-silica tergel useful as an olefin polymerization or copolymerization catalyst support comprises the steps of coprecipitating hydrous zirconia, hydrous titania and hydrous silica, aging and washing the resulting hydrotergel, removing water from the washed hydrotergel and optionally calcining the resulting xerotergel. Resins with predetermined properties such as high melt index, broad molecular weight distribution, high weight swell, etc. can be produced from catalysts of the chromium or Ziegler type based on these supports.

Zirconia-titania-silica tergels and their use as catalyst supports

An improved method of terminating ethylene polymerization and interpolymerization reactions by deactivating the Ziegler-type catalyst used in the reaction comprises the step of injecting a selected deactivating agent into the molten polymer solution in the polymerization reactor prior to degassing of the polymer solution. The deactivating agent is selected from the group consisting of:

Method of catalyst deactivation

A method of polymerizing olefins comprising contacting an olefin or mixture of olefins with a catalyst prepared with large pore volume zirconia-silica catalyst supports. The supports are prepared by reacting a zirconium compound of the formula M.sub.4 Zr(C.sub.2 O.sub.4).sub.4.nH.sub.2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A.sub.2 SiO.sub.3, where A is an alkali metal, in an aqueous solution at a pH equal to at least 11, then adding an acidic solution to a pH of about 5-9 to produce a hydrocogel. The hydrocogel is then aged and washed free of soluble by-products with an aqueous washing agent. Water is removed from the washed hydrocogel by azeotropic distillation or by washing with a water miscible solvent and then calcining the resulting xerocogel.

Method of polymerizing olefins

A catalyst and method in which the catalyst is active with a cocatalyst in the polymerization and copolymerization of 1-olefins and is prepared by reacting together one or more of a specific class of organic silicon compounds, a porous support or a silicon compound treated porous support, a Group IIA organometallic compound, and a Group IVB, VB transition metal compound or mixture thereof.

Polymerization method

Polymerization catalysts and methods

Catalysts prepared from large pore volume zirconia-silica catalyst supports and a method of polymerizing olefins comprising contacting an olefin or mixture of olefins with the catalysts. The supports are prepared by reacting a zirconium compound of the formula M.sub.4 Zr(C.sub.2 O.sub.4).sub.4.nH.sub.2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A.sub.2 SiO.sub.3, where A is an alkali metal, in an aqueous solution at a pH equal to at least 11, then adding an acidic solution to a pH of about 5-9 to produce a hydrocogel. The hydrocogel is then aged and washed free of soluble by-products with an aqueous liquid. Water is removed from the washed hydrocogel by azeotropic distillation or by washing with a water miscible solvent, then residual water is removed by chemically reacting this water with a ketal of the formula RC(OR).sub.2 R where R is the same or different and is an alkyl group of 1-5 carbon atoms, and then calcining the resulting xerocogel.

Olefin polymerization catalyst and catalyst support

A catalyst, a method of preparing a catalyst and method of polymerizing olefins with the catalyst in which the catalyst is prepared by reacting a support with a Group IIA organometallic compound essentially free of aluminum alkyls and reacting this product with water or a hydrocarbyl alcohol, then reacting this product with, for example, titanium tetrachloride, followed if necessary by removing unreacted ingredients and finally activating by contacting with a cocatalyst in the absence of oxygen and moisture.

Catalyst and methods

A new catalyst, method of making the catalyst and method of making polymers and copolymers therewith in which a porous support is reacted with an alkyl magnesium compound, the product of this is then reacted with a hydrocarbylhydrocarbyloxysilane and the product of this reacted with a titanium compound that contains halide. The resulting catalyst is activated with a cocatalyst that may be hydrogen or an alkyl derivative of lithium, magnesium, aluminum, aluminum halide or zinc.

Catalyst and method

A method of preparing large pore volume zirconia-silica catalyst supports, the resulting supports and a method of polymerizing olefins comprising contacting an olefin or mixture of olefins with a catalyst prepared with these supports. The supports are prepared by reacting a zirconium compound of the formula M.sub.4 Zr(C.sub.2 O.sub.4).sub.4.nH.sub.2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A.sub.2 SiO.sub.3, where A is an alkali metal, in an aqueous solution at a pH equal to at least 11, then adding an acidic solution to a pH of about 5-9 to produce a hydrocogel. The hydrocogel is then aged and washed free of soluble by-products first with water, then with aqueous ammonium nitrate and again with water. The water is removed from the washed hydrocogel by azeotropic distillation or by washing with a water miscible solvent, then residual water is removed by chemically reacting this water with a ketal of the formula RC(OR).sub.2 R where R is the same or different and is an alkyl group of 1-5 carbon atoms, and then calcining the resulting xerocogel.

Method of preparing catalyst supports

A method of preparing large pore volume zirconia-silica catalyst supports, the resulting supports and a method of polymerizing olefins comprising contacting an olefin or mixture of olefins with a catalyst prepared with these supports. The supports are prepared by reacting a zirconium compound of the formula M.sub.4 Zr(C.sub.2 O.sub.4).sub.4.nH.sub.2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A.sub.2 SiO.sub.3, where A is an alkali metal, in an aqueous solution at a pH equal to at least 11, then adding an acidic solution to a pH of about 5-9 to produce a hydrocogel. The hydrocogel is then aged and washed free of soluble by-products first with water, then with aqueous ammonium nitrate and again with water. The water is removed from the washed hydrocogel by azeotropic distillation or by washing with a water miscible solvent and then calcining the resulting xerocogel.

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Clinton, IA, United States of America

Robert A Dombro