US5068383A — Catalyzed redistribution of polyorganosiloxanes

Claim 1

Independent Claim 111 words

A process for the redistribution of chlorosiloxanes, the process comprising: (A) contacting a monodispersed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.m SiR.sub.2 Cl where each R is independently selected from a group consisting of hydrogen, and alkyl and substituted alkyl radicals of one to six carbon atoms, and m is an integer from one to 100; with a catalyst which facilitates redistribution of the chlorosiloxane, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a polydispersed redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.m' SiR.sub.2 Cl, where R is as previously described and m' is a mean value equivalent to m.

Claim 2

Dependent Claim 111 words

A process for the redistribution of chlorosiloxanes, the process comprising: (A) contacting a monodispersed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.m SiR.sub.2 Cl where each R is independently selected from a group consisting of hydrogen, and alkyl and substituted alkyl radicals of one to six carbon atoms, and m is an integer from one to 100; with a catalyst which facilitates redistribution of the chlorosiloxane, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a polydispersed redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.m' SiR.sub.2 Cl, where R is as previously described and m' is a mean value equivalent to m.

Claim 3

Dependent Claim 11 words

A process according to claim 1, where the catalyst is alumina.

Claim 4

Dependent Claim 10 words

A process according to claim 1, where R is methyl.

Claim 5

Dependent Claim 22 words

A process according to claim 1, where each R is a radical independently selected from a group consisting of methyl and 3,3,3-trifluoropropyl.

Claim 6

Dependent Claim 21 words

A process according to claim 1, where each R is independently selected from a group consisting of hydrogen atoms and methyl.

Claim 7

Dependent Claim 15 words

A process according to claim 1, where m is an integer from four to 25.

Claim 8

Dependent Claim 21 words

A process according to claim 1, where the process is conducted at a temperature of about 25° C. to 60° C.

Claim 9

Dependent Claim 15 words

A process according to claim 1, where R is methyl and the catalyst is alumina.

Claim 10

Dependent Claim 149 words

A process for the redistribution of chlorosiloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.x SiR.sub.2 Cl, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and x is a mean value of one to 5000, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than x; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than x.

Claim 11

Dependent Claim 149 words

A process for the redistribution of chlorosiloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.x SiR.sub.2 Cl, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and x is a mean value of one to 5000, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than x; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than x.

Claim 12

Dependent Claim 11 words

A process according to claim 9, where the catalyst is alumina.

Claim 13

Dependent Claim 10 words

A process according to claim 9, where R is methyl.

Claim 14

Dependent Claim 21 words

A process according to claim 9, where each R is independently selected from a group consisting of methyl and 3,3,3-trifluoropropyl radicals.

Claim 15

Dependent Claim 21 words

A process according to claim 9, where each R is independently selected from a group consisting of hydrogen atoms and methyl.

Claim 16

Dependent Claim 16 words

A process according to claim 9, where x is seven to 1000 and y is zero.

Claim 17

Dependent Claim 21 words

A process according to claim 9, where the process is conducted at a temperature of about 25° C. to 60° C.

Claim 18

Dependent Claim 15 words

A process according to claim 9, where the catalyst is alumina and R is methyl.

Claim 19

Dependent Claim 23 words

A process according to claim 9, where the catalyst is alumina, R is methyl, x is seven to 1000, and y is zero.

Claim 20

Dependent Claim 149 words

A process for the redistribution of hydroxysiloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising hydroxysiloxanes of formula HO(SiR.sub.2 O).sub.x SiR.sub.2 OH, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and x is a mean value of one to 5000, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than x; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than x+2y.

Claim 21

Dependent Claim 149 words

A process for the redistribution of hydroxysiloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising hydroxysiloxanes of formula HO(SiR.sub.2 O).sub.x SiR.sub.2 OH, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and x is a mean value of one to 5000, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than x; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, activated carbon, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than x+2y.

Claim 22

Dependent Claim 11 words

A process according to claim 18, where the catalyst is alumina.

Claim 23

Dependent Claim 10 words

A process according to claim 18, where R is methyl.

Claim 24

Dependent Claim 21 words

A process according to claim 18, where each R is independently selected from a group consisting of methyl and 3,3,3-trifluoropropyl radicals.

Claim 25

Dependent Claim 21 words

A process according to claim 18, where each R is independently selected from a group consisting of hydrogen atoms and methyl.

Claim 26

Dependent Claim 16 words

A process according to claim 18, where x is seven to 1000 and y is zero.

Claim 27

Dependent Claim 21 words

A process according to claim 18, where the process is conducted at a temperature of about 25° C. to 60° C.

Claim 28

Dependent Claim 15 words

A process according to claim 18, where the catalyst is alumina and R is methyl.

Claim 29

Dependent Claim 23 words

A process according to claim 18, where the catalyst is alumina, R is methyl, x is seven to 1000, and y is zero.

Claim 30

Dependent Claim 147 words

A process for the redistribution of cyclic siloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising cyclic siloxanes of formula (SiR.sub.2 O).sub.j, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and j is a mean value of three to 50, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than j; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than j.

Claim 31

Dependent Claim 147 words

A process for the redistribution of cyclic siloxanes, the process comprising: (A) contacting a first polydispersed mixture comprising cyclic siloxanes of formula (SiR.sub.2 O).sub.j, where each R is independently selected from a group consisting of hydrogen, alkyl and substituted alkyl radicals of one to six carbon atoms, and j is a mean value of three to 50, with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.y SiR.sub.2 Cl, where R is as previously described and y is a mean value of zero to less than j; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes, the catalyst selected from a group consisting of alumina, silica-alumina, zeolite, and acid clay; and (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.z SiR.sub.2 Cl, where R is as previously described and z is a mean value greater than y and less than j.

Claim 32

Dependent Claim 11 words

A process according to claim 27, where the catalyst is alumina.

Claim 33

Dependent Claim 10 words

A process according to claim 27, where R is methyl.

Claim 34

Dependent Claim 21 words

A process according to claim 27, where each R is independently selected from a group consisting of hydrogen atoms and methyl.

Claim 35

Dependent Claim 16 words

A process according to claim 27, where j is 3 to 10 and y is zero.

Claim 36

Dependent Claim 21 words

A process according to claim 27, where the process is conducted at a temperature of about 25° C. to 60° C.

Claim 37

Dependent Claim 15 words

A process according to claim 27, where the catalyst is alumina and R is methyl.

Claim 38

Dependent Claim 23 words

A process according to claim 27, where the catalyst is alumina, R is methyl, j is 3 to 10, and y is zero.

Claim 39

Dependent Claim 190 words

A three-stage process for preparing cyclic siloxanes, the process comprising: (A) contacting a first mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.x SiR.sub.2 Cl, where each R is independently selected from a group consisting of hydrogen atoms, and alkyl and substituted alkyl radicals of one to six carbon atoms and x is a mean value of one to 5000; with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.p SiR.sub.2 Cl, where R is as previously described and p is a mean value of zero to 7; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes; (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.o SiR.sub.2 Cl where R is as previously described and o is a mean value within a range of greater than zero and less than seven; (C) hydrolyzing the redistributed mixture of chlorosiloxanes to form a hydrolysate comprising cyclic siloxanes of formula (R.sub.2 SiO).sub.q, where R is as previously described and q is a mean value of three to 25, and chlorosiloxanes; (D) separating the cyclic siloxanes from the chlorosiloxanes; and (E) recycling the chlorosiloxanes as a feed to step (A).

Claim 40

Dependent Claim 190 words

A three-stage process for preparing cyclic siloxanes, the process comprising: (A) contacting a first mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.x SiR.sub.2 Cl, where each R is independently selected from a group consisting of hydrogen atoms, and alkyl and substituted alkyl radicals of one to six carbon atoms and x is a mean value of one to 5000; with a second mixture comprising chlorosilanes and chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.p SiR.sub.2 Cl, where R is as previously described and p is a mean value of zero to 7; in the presence of a catalyst which facilitates redistribution of chlorosiloxanes; (B) forming a redistributed mixture comprising chlorosiloxanes of formula Cl(SiR.sub.2 O).sub.o SiR.sub.2 Cl where R is as previously described and o is a mean value within a range of greater than zero and less than seven; (C) hydrolyzing the redistributed mixture of chlorosiloxanes to form a hydrolysate comprising cyclic siloxanes of formula (R.sub.2 SiO).sub.q, where R is as previously described and q is a mean value of three to 25, and chlorosiloxanes; (D) separating the cyclic siloxanes from the chlorosiloxanes; and (E) recycling the chlorosiloxanes as a feed to step (A).

Claim 41

Dependent Claim 24 words

A process according to claim 35, where the catalyst is selected from a group consisting of alumina, silicaalumina, zeolite, activated carbon, and acid clay.

Claim 42

Dependent Claim 11 words

A process according to claim 35, where the catalyst is alumina.

Claim 43

Dependent Claim 10 words

A process according to claim 35, where R is methyl.

Claim 44

Dependent Claim 21 words

A process according to claim 35, where each R is independently selected from a group consisting of hydrogen atoms and methyl.

Claim 45

Dependent Claim 15 words

A process according to claim 35, where the catalyst is alumina and R is methyl.

Claim 46

Dependent Claim 31 words

A process according to claim 35, where the contacting of the first mixture and the second mixture with the catalyst occurs at a temperature of about 25° C. to 60° C.

Claim 47

Dependent Claim 18 words

A process according to claim 35, where hydrolysis of the redistributed mixture is conducted in a fixed-bed reactor.

Claim 48

Dependent Claim 36 words

A process according to claim 35, where separating the cyclic siloxanes from the chlorosiloxanes is effected by gravitational separation into a siloxane phase and an aqueous hydrogen chloride phase and the siloxane phase is flash distilled.

Claim 49

Dependent Claim 22 words

A process according to claim 35, where the catalyst is selected from a group consisting of alumina, silica-alumina, zeolite, and acid clay.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1994-11-25	1995-05-27	1995-11-26	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1998-11-25	1999-05-27	1999-11-26	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2002-11-25	2003-05-27	2003-11-26	$7700.00	Window Closed / Lapsed

Catalyzed redistribution of polyorganosiloxanes

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