Production of low molecular weight linear hydrogen siloxanes

Claim 2

A process for the production of hydrogen containing siloxanes of the formula: M'D.sub.x.sup.H D.sub.y M' where M'=R 3-i 1 H i SiO 1/2 with R 1 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals and the subscript i ranges from 0 to 3; D H =R 2 HSiO 2/2 with R 2 being independently selected from the group consisting of hydrogen and one to forty carbon atom monovalent hydrocarbon radicals; and D=R 2 3 SiO 2/2 where each R 3 is independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals; and the subscript x ranges from 1 to 20 and the subscript y ranges from 0 to 20; comprising: (a) mixing a hydrogen containing siloxane selected from the group consisting of: i) D z H where D H is as previously defined and z varies from 3 to 8; and ii) M'D xx H D yy M' where M', D H , and D are as previously defined and xx is greater than 20 and yy is either 0 or greater than 20; with (b) an M' rich silicone compound comprising M' where M' is as previously defined, wherein when said M' rich compound additionally comprises D, T, or Q groups, D is as previously defined, T=R 4 SiO 3/2 with R 4 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals, and Q=SiO 4/2 where the molar ratio of silicon atoms in the M' groups in said M' rich silicone compound to the sum of the silicone atoms in the M', D, T, and Q groups in said M' rich silicone compound is 0.04 or greater; in the presence of a catalyst selected from the group consisting of acid washed clays, zeolites, ion exchange resins and linear phosphonitrilic halides and (c) heating the mixture of said hydrogen containing siloxane and said M' rich silicone compound to a temperature ranging from 20° C. to 200° C.

Claim 3

The process of claim 1 wherein said catalyst is a solid catalyst selected from the group consisting of 1) acid washed clays, 2) zeolites, and 3) ion exchange resins.

Claim 4

The process of claim 2 where the temperature ranges from 40° C. to 180° C.

Claim 5

The process of claim 3 where the catalyst is an acid washed clay.

Claim 6

The process of claim 3 where the catalyst is a zeolite.

Claim 7

The process of claim 3 where the catalyst is an ion exchange resin.

Claim 8

The process of claim 1 where the catalyst is a linear phosphonitrilic halide.

Claim 9

The process of claim 7 where the temperature ranges from 20° C. to 140° C.

Claim 10

The process of claim 8 where the linear phosphonitrilic halide is selected from the group consisting of: i) (PX 3 (N(PX 2 )) k NPX 3 ) + (PX 6 )-- where X is halogen selected from the group consisting of fluorine, chlorine, bromine and iodine and k is an integer of one or greater; ii) Cl 3 P(NPCl 2 ) n NPCl 3 + PCl 6 -- where n is an integer of from 1 to 6; iii) Cl 3 P(NPCl 2 ) m NPCl 3 + ECl p -- where E is an element having an electronegativity value of from 1.2 to 2, m is an integer of from 0 to 9 and p is an integer of from 4 to 6; iv) O(X) 2-f Y f P(NPX 2 ) g NPX 3-h Y h where g is an integer ranging from 0 to 8, f is 0 or 1, h is 0 or 1, X is a halogen selected from the group consisting of fluorine, chlorine, bromine, and iodine, Y is selected from the group consisting of OH, OR' and R'CO 2 where R' is alkyl or aryl; and v) O(X) 2-r Y r P(NPX 2 ) s NP(O)X 2-t Y t where s is an integer ranging from 0 to 8, r is 0 or 1, t is 0 or 1, X is a halogen selected from the group consisting of fluorine, chlorine, bromine, and iodine, Y is selected from the group consisting of OH, OR' and R'CO 2 where R' is alkyl or aryl.

Claim 11

The process of claim 9 where the catalyst is (PX 3 (N(PX 2 )) k NPX 3 ) + (PX 6 ) - .

Claim 12

The process of claim 9 where the catalyst is Cl 3 P(NPCl 2 ) n NPCl 3 + PCl 6 - .

Claim 13

The process of claim 9 where the catalyst is Cl 3 P(NPCl 2 ) m NPCl 3 + ECl p - .

Claim 14

The process of claim 9 where the catalyst is O(X).sub.2-f Y.sub.f P(NPX.sub.2).sub.g NPX.sub.3-h Y.sub.h.

Claim 15

The process of claim 9 where the catalyst is O(X).sub.2-r Y.sub.r P(NPX.sub.2).sub.s NP(O)X.sub.2-t Y.sub.t.

Claim 16

The process of claim 9 further comprising deactivating said linear phosphonitrilic halide catalyst by heating to a temperature above 140° C.

Claim 17

The process of claim 15 where the amount of said linear phosphonitrilic halide catalyst ranges from 1 to 1,000 parts per million by weight of the reaction mixture.

Claim 18

The process of claim 1 where i=0 and R 1 , R 2 , R 3 and R 4 are each methyl.

Claim 19

The process of claim 1 where i=1 and R 1 , R 2 , R 3 and R 4 are each methyl.

Claim 20

The process of claim 1 where i=0, yy=0 and R 1 , R 2 , R 3 and R 4 are each methyl and the catalyst is an acid washed clay.

Claim 21

A process for the production of hydrogen containing siloxanes of the formula: M'D.sub.x.sup.H D.sub.y M' where M'=R 3-i 1 H i SiO 1/2 with R 1 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals and the subscript i ranges from 0 to 3; D H =R 2 3 SiO 2/2 with R 2 being independently selected from the group consisting of hydrogen and one to forty carbon atom monovalent hydrocarbon radicals; and D=R 2 3 SiO 2/2 where each R 3 is independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals; and the subscript x ranges from 1 to 20 and the subscript y ranges from 0 to 20; consisting essentially of: (a) mixing a hydrogen containing siloxane selected from the group consisting of: (i) D z H where D H is as previously defined and z varies from 3 to 8; and (ii) M'D xx H D yy M' where M', D H , and D are as previously defined and xx is greater than 20 and yy is either 0 or greater than 20; with (b) an M' rich silicone compound comprising M' where M' is as previously defined, wherein when said M' rich compound additionally comprises D, T, or Q groups, D is as previously defined, T=R 4 SiO 3/2 with R 4 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals, and Q=SiO 4/2 where the molar ratio of silicon atoms in the M' groups in said M' rich silicone compound to the sum of the silicone atoms in the M', D, T, and Q groups in said M' rich silicone compound is 0.04 or greater; in the presence of a catalyst selected from the group consisting of acid washed clays, zeolites, ion exchange resins and linear phosphonitrilic halides and (c) heating the mixture of said hydrogen containing siloxane and said M' rich silicone compound to a temperature ranging from 20° C. to 200° C.

Claim 22

A process for the production of hydrogen containing siloxanes of the formula: M'D.sub.x.sup.H D.sub.y M' where M'=R 3-i 1 H i SiO 1/2 with R 1 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals and the subscript i ranges from 0 to 3; D H =R 2 3 SiO 2/2 with R 2 being independently selected from the group consisting of hydrogen and one to forty carbon atom monovalent hydrocarbon radicals; and D=R 2 3 SiO 2/2 where each R 3 is independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals; and the subscript x ranges from 1 to 20 and the subscript y ranges from 0 to 20; consisting essentially of: (a) mixing a hydrogen containing siloxane selected from the group consisting of: (i) D z H where D H is as previously defined and z varies from 3 to 8; and (ii) M'D xx H D yy M' where M', D H , and D are as previously defined and xx is greater than 20 and yy is either 0 or greater than 20; with (b) an M' rich silicone compound comprising M' where M' is as previously defined, wherein when said M' rich compound additionally comprises D, T, or Q groups, D is as previously defined, T=R 4 SiO 3/2 with R 4 being independently selected from the group of one to forty carbon atom monovalent hydrocarbon radicals, and Q=SiO 4/2 where the molar ratio of silicon atoms in the M' groups in said M' rich silicone compound to the sum of the silicone atoms in the M', D, T, and Q groups in said M' rich silicone compound is 0.04 or greater; in the presence of a catalyst selected from the group consisting of acid washed clays, zeolites, ion exchange resins and linear phosphonitrilic halides and (c) heating the mixture of said hydrogen containing siloxane and said M' rich silicone compound to a temperature ranging from 20° C. to 200° C.