US4196282A — Process for making a shapeable cellulose and shap…

Claim 1

Independent Claim 79 words

In a process for dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein a solution containing up to about 44% cellulose is prepared in a solvent for the cellulose comprising a tertiary amine N-oxide and from 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 2

Dependent Claim 79 words

In a process for dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein a solution containing up to about 44% cellulose is prepared in a solvent for the cellulose comprising a tertiary amine N-oxide and from 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 3

Dependent Claim 33 words

The process of claim 1 wherein the solution additionally contains an aprotic, organic, liquid, diluent which is compatible with the tertiary amine N-oxide and has a dipole moment larger than about 3.5 Debyes.

Claim 4

Dependent Claim 93 words

The process of claim 1 wherein the solvent is selected from the group consisting of N-methylmorpholine N-oxide with from about 5.5% to about 22% water, N,N-dimethylethanolamine N-oxide with from about 1.4% to about 12.5% water, N,N-dimethylbenzylamine N-oxide with from about 5.5% to about 17% water, N-methylhomopiperidine N-oxide with from 5.5% to about 20% water, N,N,N-triethylamine N-oxide with from about 7% to about 29% water, N,N-dimethylcyclohexylamine N-oxide with from 0.8% to about 21% water, N-methylpiperdine N-oxide with from about 2.6% to about 17.5% water and 2(2-hydroxypropoxy)-N-ethyl-N,N-dimethylamine N-oxide with from 5% to about 10% water.

Claim 5

Dependent Claim 19 words

The process of claim 1 wherein the solvent comprises N-methylmorpholine N-oxide and from about 5.5% to about 22% water.

Claim 6

Dependent Claim 19 words

The process of claim 1 wherein the solvent comprises N,N-dimethylethanolamine N-oxide and from about 1.4% to about 12.5% water.

Claim 7

Dependent Claim 18 words

The process of claim 1 wherein the solvent comprises N,N-dimethylcyclohexylamine N-oxide and from 0.8% to about 21% water.

Claim 8

Dependent Claim 183 words

In a process for dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein the solution is prepared with a solvent for the cellulose comprising a tertiary amine N-oxide selected from the group consisting of: (a) N,N,N-triethylamine N-oxide and (b) tertiary amine N-oxides having one or two of the valence bonds of the nitrogen substituted by a methyl residue and, where one methyl residue is present, the remaining valences are satisfied by a divalent radical forming a 5- to 7-membered ring structure having the N-atom in the ring; where two methyl residues are present, the remaining valence is satisfied by (1) a monovalent cyclic 5-, 6- or 7-membered residue which may be substituted only by methyl residues at the β- or ε-positions, or (2) by a radical which can form a pseudo-cyclic structure through interaction with the N-oxide functionality, and from 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 9

Dependent Claim 183 words

In a process for dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein the solution is prepared with a solvent for the cellulose comprising a tertiary amine N-oxide selected from the group consisting of: (a) N,N,N-triethylamine N-oxide and (b) tertiary amine N-oxides having one or two of the valence bonds of the nitrogen substituted by a methyl residue and, where one methyl residue is present, the remaining valences are satisfied by a divalent radical forming a 5- to 7-membered ring structure having the N-atom in the ring; where two methyl residues are present, the remaining valence is satisfied by (1) a monovalent cyclic 5-, 6- or 7-membered residue which may be substituted only by methyl residues at the β- or ε-positions, or (2) by a radical which can form a pseudo-cyclic structure through interaction with the N-oxide functionality, and from 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 10

Dependent Claim 156 words

In a process which comprises dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein the solution is prepared with a solvent for the cellulose comprising (1) a tertiary amine N-oxide having one of the following structures: ##STR9## where X is a radical chain completing a ring comprising 2 to 4 carbon atoms, R 1 and R 2 are H or methyl (Me); ##STR10## wherein Z is (i) a saturated or aromatic, unsaturated 5-, 6- or 7-membered ring which may be substituted only by methyl at the β- or ε-positions; or (ii) CH 2 CH 2 W where W can be OH, SH or NH 2 , or (2) N,N,N-triethylamine N-oxide and from about 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 11

Dependent Claim 156 words

In a process which comprises dissolving cellulose in a tertiary amine N-oxide solvent for the cellulose and thereafter shaping the solution and separating the cellulose from the tertiary amine N-oxide, the improvement wherein the solution is prepared with a solvent for the cellulose comprising (1) a tertiary amine N-oxide having one of the following structures: ##STR9## where X is a radical chain completing a ring comprising 2 to 4 carbon atoms, R 1 and R 2 are H or methyl (Me); ##STR10## wherein Z is (i) a saturated or aromatic, unsaturated 5-, 6- or 7-membered ring which may be substituted only by methyl at the β- or ε-positions; or (ii) CH 2 CH 2 W where W can be OH, SH or NH 2 , or (2) N,N,N-triethylamine N-oxide and from about 0.8% to about 29% by weight of water wherein the maximum water content in the solvent decreases substantially linearly with increase in cellulose content.

Claim 12

Dependent Claim 168 words

In a process for making a shaped cellulosic article which comprises preparing a tertiary amine N-oxide solution containing dissolved cellulose, the improvement which comprises dissolving cellulose in a solvent containing a tertiary amine N-oxide selected from the group consisting of N,N,N-triethylamine N-oxide and a tertiary amine N-oxide having a cyclic or pseudo-cyclic structure including a ring having a width less than about 5.15 A and a molecule having a dipole moment of at least about 4.5 Debyes mixed with an amount of water which liquefies the tertiary amine N-oxide at a temperature below its melting point and within the range of from 0.8% to about 29% by weight water based on the weight of the solvent to prepare a solution containing up to about 44% dissolved cellulose, the larger percentage of water being included in the solvent for preparing a solution containing the smaller percentage of cellulose and the maximum water content in the solvent decreasing substantially linearly as the percentage cellulose solids in the solution is increased.

Claim 13

Dependent Claim 168 words

In a process for making a shaped cellulosic article which comprises preparing a tertiary amine N-oxide solution containing dissolved cellulose, the improvement which comprises dissolving cellulose in a solvent containing a tertiary amine N-oxide selected from the group consisting of N,N,N-triethylamine N-oxide and a tertiary amine N-oxide having a cyclic or pseudo-cyclic structure including a ring having a width less than about 5.15 A and a molecule having a dipole moment of at least about 4.5 Debyes mixed with an amount of water which liquefies the tertiary amine N-oxide at a temperature below its melting point and within the range of from 0.8% to about 29% by weight water based on the weight of the solvent to prepare a solution containing up to about 44% dissolved cellulose, the larger percentage of water being included in the solvent for preparing a solution containing the smaller percentage of cellulose and the maximum water content in the solvent decreasing substantially linearly as the percentage cellulose solids in the solution is increased.

Claim 14

Dependent Claim 66 words

A process for preparing a solution containing cellulose dissolved in N-methylmorpholine N-oxide which is substantially free of undissolved cellulose and crystals of N-methylmorpholine N-oxide which comprises dissolving the cellulose in said tertiary amine N-oxide containing from about 5.5% to about 22% by weight water and with the weight of cellulose and water in relative amounts within the area of FIG. 5 between lines B and C.

Claim 15

Dependent Claim 66 words

A process for preparing a solution containing cellulose dissolved in N-methylmorpholine N-oxide which is substantially free of undissolved cellulose and crystals of N-methylmorpholine N-oxide which comprises dissolving the cellulose in said tertiary amine N-oxide containing from about 5.5% to about 22% by weight water and with the weight of cellulose and water in relative amounts within the area of FIG. 5 between lines B and C.

Claim 16

Dependent Claim 68 words

A process for preparing a solution containing cellulose dissolved in N,N-dimethylethanolamine N-oxide which is substantially free from crystals of said tertiary amine N-oxide and undissolved cellulose which comprises dissolving the cellulose in said tertiary amine N-oxide containing from about 1.4% to about 12.5% by weight water with the amounts of water and cellulose being within the area between lines B and C of FIG. 3 of the drawing.

Claim 17

Dependent Claim 68 words

A process for preparing a solution containing cellulose dissolved in N,N-dimethylethanolamine N-oxide which is substantially free from crystals of said tertiary amine N-oxide and undissolved cellulose which comprises dissolving the cellulose in said tertiary amine N-oxide containing from about 1.4% to about 12.5% by weight water with the amounts of water and cellulose being within the area between lines B and C of FIG. 3 of the drawing.

Claim 18

Dependent Claim 64 words

A process for preparing a solution containing cellulose dissolved in N,N-dimethylcyclohexylamine N-oxide which is substantially free from undissolved cellulose and crystals of said tertiary amine N-oxide which comprises dissolving the cellulose in said tertiary amine N-oxide and from 0.8% to about 21% water and with the relative amounts of water and cellulose being within the area of FIG. 4 between lines B and C.

Claim 19

Dependent Claim 64 words

A process for preparing a solution containing cellulose dissolved in N,N-dimethylcyclohexylamine N-oxide which is substantially free from undissolved cellulose and crystals of said tertiary amine N-oxide which comprises dissolving the cellulose in said tertiary amine N-oxide and from 0.8% to about 21% water and with the relative amounts of water and cellulose being within the area of FIG. 4 between lines B and C.

Claim 20

Dependent Claim 48 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N-methylmorpholine N-oxide and from about 5.5% to about 22% water with the relative amounts of cellulose and water being within the area between lines B and C of FIG. 5 of the drawing.

Claim 21

Dependent Claim 48 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N-methylmorpholine N-oxide and from about 5.5% to about 22% water with the relative amounts of cellulose and water being within the area between lines B and C of FIG. 5 of the drawing.

Claim 22

Dependent Claim 48 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N,N-dimethylethanolamine N-oxide and from about 1.4% to about 12.5% water with the relative amounts of water and cellulose being within the area between lines B and C of FIG. 3 of the drawing.

Claim 23

Dependent Claim 48 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N,N-dimethylethanolamine N-oxide and from about 1.4% to about 12.5% water with the relative amounts of water and cellulose being within the area between lines B and C of FIG. 3 of the drawing.

Claim 24

Dependent Claim 47 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N,N-dimethylcyclohexylamine N-oxide and from 0.8% to about 21% water with the relative amounts of water and cellulose within the area within the lines B and C of FIG. 4 of the drawing.

Claim 25

Dependent Claim 47 words

A solution adapted to be shaped to form a shaped article containing cellulose which comprises N,N-dimethylcyclohexylamine N-oxide and from 0.8% to about 21% water with the relative amounts of water and cellulose within the area within the lines B and C of FIG. 4 of the drawing.

Claim 26

Dependent Claim 134 words

In a method for making amorphous cellulose or cellulose having a cellulose structure II which comprises dissolving cellulose in a tertiary amine N-oxide solvent and separating the cellulose from said solvent, the improvement which comprises preparing a solution by dissolving cellulose of structure I in a solvent therefor containing N,N,N-triethylamine N-oxide or a tertiary amine N-oxide having a cyclic or pseudo-cyclic structure and water in an amount whereby the resulting solution is substantially free from undissolved cellulose and free from crystals of said tertiary amine N-oxide and from 0.8% to about 29% water based on the weight of the solution and wherein the maximum amount of water in the solution decreases substantially linearly with increase in cellulose content, said solution being prepared at a temperature below the melting point of the tertiary amine N-oxide.

Claim 27

Dependent Claim 134 words

In a method for making amorphous cellulose or cellulose having a cellulose structure II which comprises dissolving cellulose in a tertiary amine N-oxide solvent and separating the cellulose from said solvent, the improvement which comprises preparing a solution by dissolving cellulose of structure I in a solvent therefor containing N,N,N-triethylamine N-oxide or a tertiary amine N-oxide having a cyclic or pseudo-cyclic structure and water in an amount whereby the resulting solution is substantially free from undissolved cellulose and free from crystals of said tertiary amine N-oxide and from 0.8% to about 29% water based on the weight of the solution and wherein the maximum amount of water in the solution decreases substantially linearly with increase in cellulose content, said solution being prepared at a temperature below the melting point of the tertiary amine N-oxide.

Claim 28

Dependent Claim 95 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylcyclohexylamine N-oxide solvent containing from 0.8% to about 21% weight water with the amount of water in the solution being between amounts determined by solving the equations B=37.45-2.10 (% water) and C=33.57-3.28 (% water) with B and C being the percent by weight of cellulose dissolved in the solvent, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting shaped precipitated cellulose substantially free from N,N-dimethylcyclohexylamine N-oxide and drying the shaped precipitated cellulose.

Claim 29

Dependent Claim 95 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylcyclohexylamine N-oxide solvent containing from 0.8% to about 21% weight water with the amount of water in the solution being between amounts determined by solving the equations B=37.45-2.10 (% water) and C=33.57-3.28 (% water) with B and C being the percent by weight of cellulose dissolved in the solvent, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting shaped precipitated cellulose substantially free from N,N-dimethylcyclohexylamine N-oxide and drying the shaped precipitated cellulose.

Claim 30

Dependent Claim 97 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in N,N,-dimethylethanolamine N-oxide solvent containing from about 1.4% to about 12.5% by weight water and with the amount of water in the solution being between the amounts determined by solving the equations B=28.6-2.57 (% water) and C=21.59-2.59 (% water) with B and C being the percent by weight cellulose dissolved in the solvent, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N,N,-dimethylethanolamine N-oxide and drying the shaped cellulose.

Claim 31

Dependent Claim 97 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in N,N,-dimethylethanolamine N-oxide solvent containing from about 1.4% to about 12.5% by weight water and with the amount of water in the solution being between the amounts determined by solving the equations B=28.6-2.57 (% water) and C=21.59-2.59 (% water) with B and C being the percent by weight cellulose dissolved in the solvent, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N,N,-dimethylethanolamine N-oxide and drying the shaped cellulose.

Claim 32

Dependent Claim 97 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in a N-methylmorpholine N-oxide solvent containing from about 5.5% to about 22% water by weight with the amount of water in the solution being between the amounts determined by solving the equations B=34.69-1.695 (% water) C=32.38-2.21 (% water) with B and C being the percent by weight of cellulose dissolved in the solution, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Claim 33

Dependent Claim 97 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in a N-methylmorpholine N-oxide solvent containing from about 5.5% to about 22% water by weight with the amount of water in the solution being between the amounts determined by solving the equations B=34.69-1.695 (% water) C=32.38-2.21 (% water) with B and C being the percent by weight of cellulose dissolved in the solution, (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Claim 34

Dependent Claim 101 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylcyclohexylamine N-oxide solvent containing from 0.8% to about 21% by weight water with the amount of water in the solution being between amounts by solving the equations A=B+2.63√1.05+0.05 (% water).sup.2 and D=C-3.12√1.05+0.18 (% water-5.28).sup.2 with A and D being the percent by weight cellulose dissolved in the solution, B=37.45-2.10 (% water) and C=33.57-3.28 (% water) (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting shaped precipitated cellulose substantially free from N,N-dimethylcyclohexylamine N-oxide and drying the shaped precipitated cellulose.

Claim 35

Dependent Claim 101 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylcyclohexylamine N-oxide solvent containing from 0.8% to about 21% by weight water with the amount of water in the solution being between amounts by solving the equations A=B+2.63√1.05+0.05 (% water).sup.2 and D=C-3.12√1.05+0.18 (% water-5.28).sup.2 with A and D being the percent by weight cellulose dissolved in the solution, B=37.45-2.10 (% water) and C=33.57-3.28 (% water) (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting shaped precipitated cellulose substantially free from N,N-dimethylcyclohexylamine N-oxide and drying the shaped precipitated cellulose.

Claim 36

Dependent Claim 98 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylethanolamine N-oxide containing from about 1.4% to about 12.5% by weight water with the amount of water determined by solving the equations A=B+1.23√0.61+0.10 (% water-56.66).sup.2 and D=C-2.05√1.29+0.58 (% water-4.41).sup.2 with A and D being the percent by weight of cellulose dissolved in the solution and B=28.62- 2.57 (% water) C=21.59-2.59 (% water), (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Claim 37

Dependent Claim 98 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N,N-dimethylethanolamine N-oxide containing from about 1.4% to about 12.5% by weight water with the amount of water determined by solving the equations A=B+1.23√0.61+0.10 (% water-56.66).sup.2 and D=C-2.05√1.29+0.58 (% water-4.41).sup.2 with A and D being the percent by weight of cellulose dissolved in the solution and B=28.62- 2.57 (% water) C=21.59-2.59 (% water), (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Claim 38

Dependent Claim 79 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N-methylmorpholine N-oxide containing from about 5.5% to about 22% by weight water with the amount of water determined by solving the equations ##EQU1## with A and D being the percent by weight cellulose (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Claim 39

Dependent Claim 79 words

A process for making a shaped cellulose article which comprises (1) dissolving cellulose in an N-methylmorpholine N-oxide containing from about 5.5% to about 22% by weight water with the amount of water determined by solving the equations ##EQU1## with A and D being the percent by weight cellulose (2) shaping the resulting solution, and (3) precipitating the cellulose from the shaped solution, washing the resulting precipitated shaped, precipitated cellulose substantially free from N-methylmorpholine N-oxide and drying the shaped cellulose.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1983-04-01	1983-10-01	1984-04-01	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1987-04-01	1987-10-01	1988-04-01	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1991-04-01	1991-10-01	1992-04-01	$7700.00	Window Closed / Lapsed

Process for making a shapeable cellulose and shaped cellulose products

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