# US 4,392,983 A · Transition metal composition, production and use > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,392,983 A - Document ID: US4392983A - Status: Granted - Kind: A - Application number: 06/285,526 - Filed: 1981-07-21 - Granted: 1983-07-12 - Earliest claimed: 1980-07-21 - Assignees: Imperial Chemical Industries PLC - Inventors: Angus J. Hartshorn; Eric Jones - Web page: https://patentgrep.com/patent/US4392983A ## CPC - C08F 10/00: Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond - C08F 4/022: {Magnesium halide as support anhydrous or hydrated or complexed by means of a Lewis base for Ziegler-type catalysts} - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS ## Abstract A transition metal composition has the composition M.sub.m,X.sub.p,TYn'Z where M is a metal of Groups Ib, IIa, IIIb, VIIa or VIII of the Periodic Table, X is an anion, T is a transition metal of Groups IVA--VIA of the Periodic Table, Y is an anion, Z is a melt-producing compound, m' is greater than zero and less than 100, n' is greater than zero and less than 8 (m'+1), and p' is m' x(valency of M)/(valency of X). The compositions of this type may be transformed into a liquid by heating and the hot liquid sprayed and the spray cooled. The sprayed material has a useful particle form and may be used as a component of a polymerization catalyst to polymerize an unsaturated monomer such as ethylene. ## Claims ### Claim 1 A process for the production of a transition metal composition which process comprises spraying a material which comprises a hot single phase liquid and cooling the spray so formed so as to obtain essentially spheroidal particles characterised in that the said single phase liquid has a composition represented by the general formula: M.sub.m X.sub.p TY.nZ (I) where M, where present, represents at least one metal of Groups Ib, IIa, IIIb, VIIa, VIII or the lanthanide series of the Periodic Table, X, where present, represents at least one anion, T represents at least one transition metal of Groups IVA, VA or VIA of the Periodic Table, Y represents at least one of the following atoms or groups: halide, oxyhalide, amino, alkoxide, thioalkoxide, carboxylate or sulphonate in an amount to satisfy the valency which T has in the composition, Z, where present, represents at least one melt-producing compound which, on heating with the transition metal compound TY, forms a single phase liquid, m is zero or a number less than 100; n is zero or a number less than 8 (m+one); and ##EQU3## ### Claim 2 (depends on 1) A process as claimed in claim 1 wherein the hot single phase liquid is formed by heating a mixture of at least one transition metal compound, at least one metal M compound and at least one melt-producing compound in the ratio to give a composition of formula (I). ### Claim 3 (depends on 1) A process as claimed in claim 1 wherein the hot single phase liquid is at a temperature in the range 30.degree. C. up to 400.degree. C. ### Claim 4 (depends on 1) A process as claimed in claim 1 where the hot single phase liquid is a melt and is at a temperature in the range from the melting point of the melt to 100.degree. C. above the said melting point. ### Claim 5 (depends on 1) A process as claimed in claim 1 wherein the material which is sprayed comprises the hot single phase liquid together with an inert diluent which is a liquid, a solid which is meltable at the temperature of the hot single phase liquid or a solid which remains unmolten and undissolved at the temperature of the hot single phase liquid. ### Claim 6 (depends on 1) A process as claimed in claim 1 wherein spraying is effected using a spray nozzle, pneumatic atomisation or a spinning disc. ### Claim 7 (depends on 1, 2, 3, 4, 5, 6) A process as claimed in any one of claims 1 to 6 wherein spraying is effected using an elevated pressure of from 5 to 100 kg/cm.sup.2 to generate the spray. ### Claim 8 (depends on 1) A process as claimed in claim 1 wherein the melt-producing compound is an alcohol and the essentially spheroidal particles are treated with a halogen-containing compound; or the essentially spheroidal particles are heated to at least partially remove the alcohol therefrom; or the essentially spheroidal particles are heated to at least partially remove the alcohol therefrom and simultaneously or subsequently are treated with a halogen containing compound. ### Claim 9 A magnesium chloride/titanium chloride/methanol adduct of the general formula: m.sup.2 MgCl.sub.2.TiCl.sub.x n.sup.2 CH.sub.3 OH wherein: m.sup.2 is a number which is in the range from 5 up to 50; n.sup.2 is a number which is greater than zero and less than 8 (m.sup.2 +one); and x is 3 or 4. ### Claim 10 A magnesium chloride/titanium chloride/methanol adduct which incorporates at least one further metal halide selected from zirconium chloride, vanadium chloride, manganous chloride, a chloride of iron, nickel, chloride and copper chloride. ### Claim 11 A metal halide adduct of the general formula: m.sup.2 MgCl.sub.2.aM.sup.1 Cl.sub.y cTiCl.sub.x bT.sup.1 Cl.sub.z.n.sup.3 CH.sub.3 OH wherein M.sup.1 is at least one metal selected from manganese, iron, nickel and copper; T.sup.1 is at least one metal selected from vanadium and zirconium; a is zero or a number having a value less than the value of m.sup.2 ; b is zero or a number having a value of less than 5c; c is a number which is greater than zero and does not exceed one; m.sup.2 is a number which is in the range from 5 up to 50; n.sup.3 is a number which is greater than zero and less than 8 (m.sup.2 +a+one); x is 3 or 4; y is equal to the valency of M.sup.1 ; z is 3 or 4; (m.sup.2 +a) has a value of from 5 up to 50; and (b+c) has a value of one; with the proviso that at least one of a and b has a value of greater than zero. ### Claim 12 (depends on 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11) A polymerisation catalyst which comprises (a) a transition metal composition obtained by the process of any one of claims 1 to 8 or a solid product or adduct as claimed in any one of claims 9 to 11; and (b) a Ziegler activator.