Title of Invention	A PROCESS FOR REGENERATION OF CELLULOSE FROM A VISCOSE SOLUTION IN A SPIN BATH AND AN AMPHOTERIC SURFACTANT.
Abstract	The present invention relates to a process for regeneration of cellulose from a viscose solution in a spin bath, wherein the viscose solution is brought in contact with a spin bath containing an amphoteric surfactant having the general formula RNA (CnH2nNA) x-1A (I) where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents hydrogen, an alifatic group with 1-24 carbon a,oms or a BOOCCmH2m-group, where m is a number from 1-3, B is hydrogen or a salt-forming cation, n is a number from 2-3, x is 1- 8, and the number of BOOCCmH2m.- groups are from 1 to x + 2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45.

Title of Invention

A PROCESS FOR REGENERATION OF CELLULOSE FROM A VISCOSE SOLUTION IN A SPIN BATH AND AN AMPHOTERIC SURFACTANT.

Abstract

The present invention relates to a process for regeneration of cellulose from a viscose solution in a spin bath, wherein the viscose solution is brought in contact with a spin bath containing an amphoteric surfactant having the general formula RNA (CnH2nNA) x-1A (I) where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents hydrogen, an alifatic group with 1-24 carbon a,oms or a BOOCCmH2m-group, where m is a number from 1-3, B is hydrogen or a salt-forming cation, n is a number from 2-3, x is 1- 8, and the number of BOOCCmH2m.- groups are from 1 to x + 2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45.

Full Text	USE OF AN AMPHOTERIC SURFACTANT AS A VISCOSE SPIN BATH ADDITIVE The present invention relates to a method of reducing the clogging of nozzles and slits and diminishing the formation of deposits in the spin bath system in the process of making viscose filamentary and film materials by using an amphoteric surfactant. When regenerating cellulose material in an acidic spin bath containing zinc sulphate clogging disturbancies are frequent. The origins of the clogging material are different. One and the most important source are solid byproducts, i.e. elementary sulphur and zinc sulphide, which are formed when the dissolved xanthogenated celluloses are regenerated to cellulose and carbon disulphide. Other examples of by-products are hemicelluloses and resins derived from the cellulosic raw material itself and trans-fered to the spin bath where they cause deposits. One method of reducing these disadvantages is to add cationic surface active compounds to the spinning baths. Thus, in Japanese Patent No. 48006409 it is suggested to add N,N'-polyoxy-ethylene-N-long chain-alkyl alkylene-diamines and N,N',N"-polyoxyethylene-N-long chain-alkyl alkylene-triamines into the spin bath as dispersants for sulphur particles which cause blockages in spinning nozzles. The long-chain alkyl group contains from 10 to 20 carbon atoms. The number of oxyethylene groups are from 1 to 8 for each substitution position and their sum is from 2 to 10. However, this additives have a rather limited ability to disperse sulphur, especially when the amounts thereof is high. In Japanese Patent Application No. 54101916 it is suggested to add polyoxyethylene alkyl mono- and diamide polyalkylene polyamines to further reduce the clogging of nozzles. Examples of the used polyalkylene polyamines are triethylene tetramine and tetraethylene pentamine. The number of carbon numbers in the fatty acids used for preparing the said compounds is preferably from 12 to 22, while the number of ethylene oxide groups in the molecule is from 6 to 12. Although these polyamines have a good dispersing effect they have a serious drawback since they are not stable in hot acid solutions and are hydrolyzed at high temperature in the spin bath. Consequently, after some time their effect is essentially reduced. The degradation of the additive can be compensated by addition of higher dosages of the additives. However in practice the resulting products of the hydrolysis, i.e. the fatty acids produced especially during reconditioning of the spin bath enhances the clogging. Together with elementary sulphur and/or zinc sulphide and resins they form black particles, which are very difficult to disperse. It has now been found that not only the disturbancies of clogging materials in the spin bath are essentially diminished but also the quality of the fibers formed in the spin bath is improved by using an amphoteric surfactant having the formula RNA ( CnH2nNA ) X.XA (I) where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents a hydrogen, an alifatic group with 1-24 carbon atoms, or B00CCmH2m-groups, where rn is a number from 1-3, B is hydrogen or a salt forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCC groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45, as a viscose spin bath additive. The amphoteric surfactant has an excellent anticlogging effect, since it is a good dispersant and prevent or reduce precipitation in the spin bath. In addition it has a low foaming and is very stable in comparison with the amide compounds disclosed in JP Patent Application No. 54101916. Since the additive keeps the openings in the spinneret free from clogging materials, the filaments and films formed collect less solid particles, whereby the discolouration is reduced and the fiber or film strenght improved. The maintainance of the spin bath is also simplyfied, since the amphoteric surfactant is stable in ordinary working-up-processes of the spin bath and the spin bath solution can be recirculated after the removal of an excess of the by-products including sodium sulphate obtained in the spin bath. The amount of the amphoteric compound in the spin bath may be varied within wide limits but is normally added in an amount of 0.5-5000 ppm, preferably from 2 to 1500 ppm, to a spin bath containing 5-15% by weight H2S04, 15-30% by weight of Na2S04 and 0-7% by weight of ZnS04. The amphoteric surfactant with formula I preferably contains one or two aliphatic groups, R and A, with a total of 8 to 40 carbon atoms, preferably from 10 to 36 carbon atoms. Preferably R is a hydrocarbon group with 8-24 carbon atoms, and most preferably 10-22 carbon atoms. B is normally a mono- or divalent, preferably a monovalent cation, m is preferably a number 1 or 2. Most preferred amphoteric surfactants of the formula I are those having the formula where R, A and x have the meaning mentioned in formula I and Ax is a hydrogen or a group BOOCCJH2 where B and m have the meaning mentioned in formula I. These additives are easy to produce and have excellent dispersing ability. Normally at least 50% of all substituents A and Ax are the group BOOCCmH2m-. The amphoteric surfactant where m is 1 are preferred, since they exhibit low foaming. Low foaming is also supported by the presence of at least one R group with 14-22 carbon atoms. This is of benefit in the sequent treatment of the fiber and film material. The present invention also relates to a process for regeneration of cellulose from a viscose solution, in which process the viscose solution is brought into contact with a spin bath containing from 0.5 to 5000 ppm of an amphoteric surfactant according to formula I. Preferably the amphoteric surfactant has the formula II. The spin bath has normally a temperature of from 40°C to 60°C and contains in addition to the amphoteric surfactant from 5 to 15% by weight of H2S04/ from 15 to 30% by weight of Na2S04 and from 0-7% by weight of ZnS04. The cellulose regenerated may have the form of fibers or films or any other conventional shape. The invention is further illustrated by the following examples. Example 1. Degradation kinetics of two spin bath additives were evaluated in a spin bath with the composition 9,5% H2S04/ 23% Na2S04/ 0,4% ZnS04 and 67,1% H20 at different temperatures stated in the tables below. One of the additives was an amide condensate of tetraethylene pentamine and a tallow fatty acid ethoxylated with 10 moles ethylene oxide per mol amide, hereinafter referred to as Compound B. Compound B is a typical representative of an additive in the Japanese Patent Application No. 54101916. The other additive was an oleoampho-polycarboxyglycinate, RNA ( CnH2nNA ) X_XA where R is a C18-hydrocarbon group derived from oleic fatty acid, x is 4, n is 3, and A is the group BOOCC^H^ , where B is a sodium cation and m is 1, hereinafter referred to as Compound 1. It is a typical representative of an amphoteric surfactant according to this invention. The content of Compound B in the spin bath was analyzed by using the dye Orange II. This dye and the cationic surfactant were reacted and the complex formed was extracted into chloroform. Then the amount of the complex in the chloroform phase was spectrofotometrically determined at a wave length of 488 nm. The amphoteric surfactant, Compound 1, was analyzed by first concentrating the surfactant on a Dionex On Guard-RP column followed by eluation in an aqueous alkaline acetonitrile solution. The concentration of the amphoteric surfactant was then determined by an HPLC method under the following conditions: Column, Hamilton PRP-1; Detection, UV 230 nm; Mobil phase, Gradient of acetonitrile in alkaline water; Flow rate, 1 ml/min. All data are presentated below in Table 1 and 2, respectively. The figures show the residual non-degraded amount of From the results it is evident that the stability in hot spin bath is much lower for the amide type of spin bath additive (Compound B) than for the additive according to the invention (Compound 1). Examples 2-4. Precipitation prevention and dispersing capacities of some spin bath additives were determined according to the following procedure. 21 ml of a solution containing 0.25 M Na2S203/ 0.15 M Na2CS3 and 0.25 M Na2S was dropwise added during stirring into a polypropylene vessel containing 1 liter of a spin bath. The spin bath had a composition of 10% H2S04/ 20% Na2S04/ 1% ZnS04 and 69% H20. Its temperature was 50°C The stirrer was made of glass with a propellar of platinum. After the addition the transmittance of the bath was measured after predetermined times in a spectrophotometer at the wave length of 450 nm in a glass cuvette. During the whole test the stirring was kept constant at 300 rpm. After 270 minutes the test was interrupted and the weight of the stirrer was measured in order to determine the amount of material precipitated on the stirrer. The precipitation preventing and dispersing additives were added in different amounts to the spin bath before the start of adding the 21 ml solution to the spin bath solution. The following additives were used. Compound A. A compound having the formula (EO)yH C18-alkyl N(EO)x-C3H6N (E0)s H where EO is ethyleneoxy and the sum of x, y and z is 10, in accordance with the amine compounds disclosed in the Japanese Patent No. 48006409. Compound B. Same compound as in Example 1. Compound l. Same compound as in Example 1. Compound 2. Tallowamphopolycarboxyglycinate with the formula I, where R is a tallow fatty alkyl group, x is 4, n is 3 and A is B00CCmH2m-, where B is sodium and m is 1. Compound 3. Tallowamphopolycarboxypropionic acid with the formula I, where R, A, n, and x have the same meanings as in Compound 2, and m is 2 and B is hydrogen. The tests performed and the results obtained are shown in Table 3 below. Table 3. Time, Transmittancey % min " ■ ■ 1 '" ' \| 1 " ! [ 1 [ 1 1 1 1 Com- -AAB112233 3 3 pound Amount 5 25 5 5 25 5 25 5 25 250 500 ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm 0 100 100 100 100 100 100 100 100 100 100 100 100 30 57 71 67 39 75 93 86 77 84 71 76 79 60 52 41 48 25 31 37 36 44 35 41 56 54 120 47 38 42 32 28 12 36 15 26 16 34 26 270 45 41 30 36 30 5 30 12 20 4 10 10 Dry weight of precipitation on Pt-stirrer, mg 270 182 80 40 21 0.1 0.2 0.0 3.3 0.0 1.7 1.3 0.9 Table 3. Time, Transmittancey % min " ■ ■ 1 '" ' \| 1 " ! [ 1 [ 1 1 1 1 Com- -AAB112233 3 3 pound Amount 5 25 5 5 25 5 25 5 25 250 500 ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm 0 100 100 100 100 100 100 100 100 100 100 100 100 30 57 71 67 39 75 93 86 77 84 71 76 79 60 52 41 48 25 31 37 36 44 35 41 56 54 120 47 38 42 32 28 12 36 15 26 16 34 26 270 45 41 30 36 30 5 30 12 20 4 10 10 Dry weight of precipitation on Pt-stirrer, mg 270 182 80 40 21 0.1 0.2 0.0 3.3 0.0 1.7 1.3 0.9 It is evident that the spin bath additives in accordance with the present invention have an improved ability to disperse solid and colloidal particles and to prevent the precipitation thereof in comparison with the spin bath additive disclosed in the Japanese Patent No. 48006409 and Japanese Patent Application No. 54101916. Examples 5-14. The tests in these examples were performed as in example 2 but with the exeption that the additives used were as follows. Compound 4. Compound 4 has the formula I, where R is a C12-C14 derived coco alkyl group, x is 2, n is 3, and A is the group BOOCCmH2m-/ where B is sodium and m is 1. Compound 5. As Compound 4, but x is 3. Compound 6. Compound 6 is as Compound 4, but m is 2, x is 4 and B is hydrogen. Compound 7. Compound 7 has the formula I, where R is a C18 derived tallow fatty alkyl group, x is 4, n is 3, and A is the group BOOCC, where B is sodium„and m is 1. Compound 8. Compound 8 is as Compound 7, but x is 5. Compound 9. Compound 9 is as Compound 7, but x is 6. Compound 10. Compound 10 is as Compound 7, but m is 2 and B is hydrogen. Compound 11. Compound 11 is as Compound 8, but m is 2 and B is hydrogen. Compound 12. Compound 12 is as Compound 9, but m is 2 and B is hydrogen. The amounts added of compounds 4-12 are stated in the table below. The precipitation and dispersing tests gave the following results. From the results obtained it is evident that the amphoteric compounds according to the invention exhibit an unexpected improvement regarding precipitation inhibitation and dispersion ability. We C L A I M S 1. Use of an amphoteric surfactant having the general formula where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents hydrogen, an alifatic group with 1-24 carbon atoms or a BOOCCtnH2m-group, where m is a number from 1-3, B is hydrogen or a salt-forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCCmH2m-groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45, as a viscose spin bath additive, 2. Use according to claim 1, wherein the bath contains from 5 to 15% by weight of H2S04/ from 15 to 30% by weight of Na2S04 and from 0 to 7% by weight of ZnS04. 3. Use according to claim 1 or 2 wherein the amphoteric surfactant is present in an amount of from 0.5 to 5000 ppm in the spin bath. 4. Use according to claim 1, 2 or 3 wherein the amphoteric surfactant has the formula where R, A and x have the meaning mentioned in formula I, and Ax is a hydrogen or the group BOOCC^H^, where B and m has the meaning mentioned in formula I. 5. Use according to claim 1, 2, 3 or 4, wherein the amphoteric surfactant is added as a dispersant and precipitation reducing additive. 6. Use according to claim 5 of the amphoteric surfactant to reducing the clogging of nozzles and slits in the process of making viscose filamentary and film material. 7. A process for regeneration of cellulose from a viscose solution in a spin bath characterized in that the viscose solution is brought in contact with a spin bath containing from 0.5 to 5000 ppm of an amphoteric surfactant having the formula I defined in claim 1. 8. A process according to claim 7 characterized in that the spin bath solution contains from 5- to 15% by weight of H2S04/ from 15 to 30% by weight of Na2SQ4 and from 0-7% by weight of ZnS04. 9. A process according to claim 7 or 8, characterized in that the amphoteric surfactant has the formula where R, A and x have the meaning mentioned in formula I, and Ax is a hydrogen or the group BOOCC^a/ where B and m has the meaning mentioned in formula I. 10. A process for regeneration of cellulose from a viscose solution in a spin bath substantially as herein described with reference to the examples. SUMMARY The present invention relates to a method of reducing the clogging of nozzles and slits and diminishing the formation of deposits in the spin bath system in the process of making viscose filamentary and film materials by using an amphoteric surfactant having the formula where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents a hydrogen, an alifatic group with 1-24 carbon atoms, or BOOCCmH2m-groups, where m is a number from 1-3, B is hydrogen or a salt forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCCJH^-groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45. The amphoteric surfactant has an excellent anticlogging effect, since it is a good dispersant and prevent or reduce precipitation in the spin bath. In addition it has a low foaming and is very stable.

Full Text

USE OF AN AMPHOTERIC SURFACTANT AS A VISCOSE SPIN BATH ADDITIVE
The present invention relates to a method of reducing the clogging of nozzles and slits and diminishing the formation of deposits in the spin bath system in the process of making viscose filamentary and film materials by using an amphoteric surfactant.
When regenerating cellulose material in an acidic spin bath containing zinc sulphate clogging disturbancies are frequent. The origins of the clogging material are different. One and the most important source are solid byproducts, i.e. elementary sulphur and zinc sulphide, which are formed when the dissolved xanthogenated celluloses are regenerated to cellulose and carbon disulphide. Other examples of by-products are hemicelluloses and resins derived from the cellulosic raw material itself and trans-fered to the spin bath where they cause deposits. One method of reducing these disadvantages is to add cationic surface active compounds to the spinning baths. Thus, in Japanese Patent No. 48006409 it is suggested to add N,N'-polyoxy-ethylene-N-long chain-alkyl alkylene-diamines and N,N',N"-polyoxyethylene-N-long chain-alkyl alkylene-triamines into the spin bath as dispersants for sulphur particles which cause blockages in spinning nozzles. The long-chain alkyl group contains from 10 to 20 carbon atoms. The number of oxyethylene groups are from 1 to 8 for each substitution position and their sum is from 2 to 10. However, this additives have a rather limited ability to disperse sulphur, especially when the amounts thereof is high.
In Japanese Patent Application No. 54101916 it is suggested to add polyoxyethylene alkyl mono- and diamide polyalkylene polyamines to further reduce the clogging of nozzles. Examples of the used polyalkylene polyamines are triethylene tetramine and tetraethylene pentamine. The number of carbon numbers in the fatty acids used for preparing the said compounds is preferably from 12 to 22, while

the number of ethylene oxide groups in the molecule is from 6 to 12. Although these polyamines have a good dispersing effect they have a serious drawback since they are not stable in hot acid solutions and are hydrolyzed at high temperature in the spin bath. Consequently, after some time their effect is essentially reduced.
The degradation of the additive can be compensated by addition of higher dosages of the additives. However in practice the resulting products of the hydrolysis, i.e. the fatty acids produced especially during reconditioning of the spin bath enhances the clogging. Together with elementary sulphur and/or zinc sulphide and resins they form black particles, which are very difficult to disperse.
It has now been found that not only the disturbancies of clogging materials in the spin bath are essentially diminished but also the quality of the fibers formed in the spin bath is improved by using an amphoteric surfactant having the formula
RNA ( CnH2nNA ) X.XA (I) where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents a hydrogen, an alifatic group with 1-24 carbon atoms, or B00CCmH2m-groups, where rn is a number from 1-3, B is hydrogen or a salt forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCC groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45, as a viscose spin bath additive. The amphoteric surfactant has an excellent anticlogging effect, since it is a good dispersant and prevent or reduce precipitation in the spin bath. In addition it has a low foaming and is very stable in comparison with the amide compounds disclosed in JP Patent Application No. 54101916. Since the additive keeps the openings in the spinneret free from clogging materials, the filaments and films formed collect less solid particles, whereby the discolouration is reduced and the fiber or film strenght improved. The maintainance of the spin bath is also simplyfied, since the amphoteric surfactant is stable in

ordinary working-up-processes of the spin bath and the spin bath solution can be recirculated after the removal of an excess of the by-products including sodium sulphate obtained in the spin bath. The amount of the amphoteric compound in the spin bath may be varied within wide limits but is normally added in an amount of 0.5-5000 ppm, preferably from 2 to 1500 ppm, to a spin bath containing 5-15% by weight H2S04, 15-30% by weight of Na2S04 and 0-7% by weight of ZnS04.
The amphoteric surfactant with formula I preferably contains one or two aliphatic groups, R and A, with a total of 8 to 40 carbon atoms, preferably from 10 to 36 carbon atoms. Preferably R is a hydrocarbon group with 8-24 carbon atoms, and most preferably 10-22 carbon atoms. B is normally a mono- or divalent, preferably a monovalent cation, m is preferably a number 1 or 2.
Most preferred amphoteric surfactants of the formula I are those having the formula

where R, A and x have the meaning mentioned in formula I and Ax is a hydrogen or a group BOOCCJH2 where B and m have the meaning mentioned in formula I. These additives are easy to produce and have excellent dispersing ability. Normally at least 50% of all substituents A and Ax are the group BOOCCmH2m-. The amphoteric surfactant where m is 1 are preferred, since they exhibit low foaming. Low foaming is also supported by the presence of at least one R group with 14-22 carbon atoms. This is of benefit in the sequent treatment of the fiber and film material.
The present invention also relates to a process for regeneration of cellulose from a viscose solution, in which process the viscose solution is brought into contact with a spin bath containing from 0.5 to 5000 ppm of an amphoteric surfactant according to formula I. Preferably the amphoteric surfactant has the formula II. The spin bath has normally a temperature of from 40°C to 60°C and contains in addition to the amphoteric surfactant from 5 to 15% by weight of H2S04/

from 15 to 30% by weight of Na2S04 and from 0-7% by weight of ZnS04. The cellulose regenerated may have the form of fibers or films or any other conventional shape.
The invention is further illustrated by the following examples.
Example 1.
Degradation kinetics of two spin bath additives were evaluated in a spin bath with the composition 9,5% H2S04/ 23% Na2S04/ 0,4% ZnS04 and 67,1% H20 at different temperatures stated in the tables below.
One of the additives was an amide condensate of tetraethylene pentamine and a tallow fatty acid ethoxylated with 10 moles ethylene oxide per mol amide, hereinafter referred to as Compound B. Compound B is a typical representative of an additive in the Japanese Patent Application No. 54101916. The other additive was an oleoampho-polycarboxyglycinate, RNA ( CnH2nNA ) X_XA where R is a C18-hydrocarbon group derived from oleic fatty acid, x is 4, n is 3, and A is the group BOOCC^H^ , where B is a sodium cation and m is 1, hereinafter referred to as Compound 1. It is a typical representative of an amphoteric surfactant according to this invention.
The content of Compound B in the spin bath was analyzed by using the dye Orange II. This dye and the cationic surfactant were reacted and the complex formed was extracted into chloroform. Then the amount of the complex in the chloroform phase was spectrofotometrically determined at a wave length of 488 nm. The amphoteric surfactant, Compound 1, was analyzed by first concentrating the surfactant on a Dionex On Guard-RP column followed by eluation in an aqueous alkaline acetonitrile solution. The concentration of the amphoteric surfactant was then determined by an HPLC method under the following conditions: Column, Hamilton PRP-1; Detection, UV 230 nm; Mobil phase, Gradient of acetonitrile in alkaline water; Flow rate, 1 ml/min. All data are presentated below in Table 1 and 2, respectively.
The figures show the residual non-degraded amount of

From the results it is evident that the stability in hot spin bath is much lower for the amide type of spin bath additive (Compound B) than for the additive according to the invention (Compound 1).
Examples 2-4.
Precipitation prevention and dispersing capacities of some spin bath additives were determined according to the following procedure.
21 ml of a solution containing 0.25 M Na2S203/ 0.15 M Na2CS3 and 0.25 M Na2S was dropwise added during stirring into a polypropylene vessel containing 1 liter of a spin bath. The spin bath had a composition of 10% H2S04/ 20% Na2S04/ 1% ZnS04 and 69% H20. Its temperature was 50°C The stirrer was made of glass with a propellar of platinum. After the addition the transmittance of the bath was measured after predetermined times in a spectrophotometer at the wave length of 450 nm in a glass cuvette. During the whole test the stirring was kept constant at 300 rpm. After 270

minutes the test was interrupted and the weight of the stirrer was measured in order to determine the amount of material precipitated on the stirrer.
The precipitation preventing and dispersing additives were added in different amounts to the spin bath before the start of adding the 21 ml solution to the spin bath solution.
The following additives were used.
Compound A.
A compound having the formula
(EO)yH
C18-alkyl N(EO)x-C3H6N
(E0)s H where EO is ethyleneoxy and the sum of x, y and z is 10, in accordance with the amine compounds disclosed in the Japanese Patent No. 48006409.
Compound B.
Same compound as in Example 1.
Compound l.
Same compound as in Example 1.
Compound 2.
Tallowamphopolycarboxyglycinate with the formula I, where R is a tallow fatty alkyl group, x is 4, n is 3 and A is B00CCmH2m-, where B is sodium and m is 1.
Compound 3.
Tallowamphopolycarboxypropionic acid with the formula I, where R, A, n, and x have the same meanings as in Compound 2, and m is 2 and B is hydrogen.
The tests performed and the results obtained are shown in Table 3 below.

Table 3.
Time, Transmittancey %
min
" ■ ■ 1 '" ' | 1 " ! [ 1 [ 1 1 1 1
Com- -AAB112233 3 3
pound
Amount 5 25 5 5 25 5 25 5 25 250 500
ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm
0 100 100 100 100 100 100 100 100 100 100 100 100
30 57 71 67 39 75 93 86 77 84 71 76 79
60 52 41 48 25 31 37 36 44 35 41 56 54
120 47 38 42 32 28 12 36 15 26 16 34 26
270 45 41 30 36 30 5 30 12 20 4 10 10
Dry weight of precipitation on Pt-stirrer, mg
270 182 80 40 21 0.1 0.2 0.0 3.3 0.0 1.7 1.3 0.9
Table 3.
Time, Transmittancey %
min
" ■ ■ 1 '" ' | 1 " ! [ 1 [ 1 1 1 1
Com- -AAB112233 3 3
pound
Amount 5 25 5 5 25 5 25 5 25 250 500
ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm
0 100 100 100 100 100 100 100 100 100 100 100 100
30 57 71 67 39 75 93 86 77 84 71 76 79
60 52 41 48 25 31 37 36 44 35 41 56 54
120 47 38 42 32 28 12 36 15 26 16 34 26
270 45 41 30 36 30 5 30 12 20 4 10 10
Dry weight of precipitation on Pt-stirrer, mg
270 182 80 40 21 0.1 0.2 0.0 3.3 0.0 1.7 1.3 0.9
It is evident that the spin bath additives in accordance with the present invention have an improved ability to disperse solid and colloidal particles and to prevent the precipitation thereof in comparison with the spin bath additive disclosed in the Japanese Patent No. 48006409 and Japanese Patent Application No. 54101916.
Examples 5-14.
The tests in these examples were performed as in example 2 but with the exeption that the additives used were as follows.
Compound 4.
Compound 4 has the formula I, where R is a C12-C14 derived coco alkyl group, x is 2, n is 3, and A is the group BOOCCmH2m-/ where B is sodium and m is 1.
Compound 5.
As Compound 4, but x is 3.
Compound 6.
Compound 6 is as Compound 4, but m is 2, x is 4 and B is hydrogen.
Compound 7.
Compound 7 has the formula I, where R is a C18

derived tallow fatty alkyl group, x is 4, n is 3, and A is the group BOOCC, where B is sodium„and m is 1.
Compound 8.
Compound 8 is as Compound 7, but x is 5.
Compound 9.
Compound 9 is as Compound 7, but x is 6.
Compound 10.
Compound 10 is as Compound 7, but m is 2 and B is hydrogen.
Compound 11.
Compound 11 is as Compound 8, but m is 2 and B is hydrogen.
Compound 12.
Compound 12 is as Compound 9, but m is 2 and B is hydrogen.
The amounts added of compounds 4-12 are stated in the table below. The precipitation and dispersing tests gave the following results.

From the results obtained it is evident that the amphoteric compounds according to the invention exhibit an unexpected improvement regarding precipitation inhibitation and dispersion ability.

We C L A I M S
1. Use of an amphoteric surfactant having the general
formula

where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents hydrogen, an alifatic group with 1-24 carbon atoms or a BOOCCtnH2m-group, where m is a number from 1-3, B is hydrogen or a salt-forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCCmH2m-groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45, as a viscose spin bath additive,
2. Use according to claim 1, wherein the bath contains from 5 to 15% by weight of H2S04/ from 15 to 30% by weight of Na2S04 and from 0 to 7% by weight of ZnS04.
3. Use according to claim 1 or 2 wherein the amphoteric surfactant is present in an amount of from 0.5 to 5000 ppm in the spin bath.
4. Use according to claim 1, 2 or 3 wherein the amphoteric surfactant has the formula

where R, A and x have the meaning mentioned in formula I, and Ax is a hydrogen or the group BOOCC^H^, where B and m has the meaning mentioned in formula I.
5. Use according to claim 1, 2, 3 or 4, wherein the amphoteric surfactant is added as a dispersant and precipitation reducing additive.
6. Use according to claim 5 of the amphoteric surfactant to reducing the clogging of nozzles and slits in the process of making viscose filamentary and film material.
7. A process for regeneration of cellulose from a viscose solution in a spin bath characterized in that the viscose solution is brought in contact with a spin bath containing from 0.5 to 5000 ppm of an amphoteric surfactant having the formula I defined in claim 1.
8. A process according to claim 7 characterized in that

the spin bath solution contains from 5- to 15% by weight of H2S04/ from 15 to 30% by weight of Na2SQ4 and from 0-7% by weight of ZnS04.
9. A process according to claim 7 or 8, characterized in
that the amphoteric surfactant has the formula

where R, A and x have the meaning mentioned in formula I, and Ax is a hydrogen or the group BOOCC^a/ where B and m has the meaning mentioned in formula I.
10. A process for regeneration of cellulose from a viscose
solution in a spin bath substantially as herein described
with reference to the examples.

SUMMARY
The present invention relates to a method of reducing the clogging of nozzles and slits and diminishing the formation of deposits in the spin bath system in the process of making viscose filamentary and film materials by using an amphoteric surfactant having the formula
where R represents a hydrogen or an alifatic group with 1-24 carbon atoms, each A represents a hydrogen, an alifatic group with 1-24 carbon atoms, or BOOCCmH2m-groups, where m is a number from 1-3, B is hydrogen or a salt forming cation, n is a number from 2-3, x is 1-8, and the number of BOOCCJH^-groups are from 1 to x+2, with the provision that the total number of carbon atoms in the aliphatic groups is from 8 to 45. The amphoteric surfactant has an excellent anticlogging effect, since it is a good dispersant and prevent or reduce precipitation in the spin bath. In addition it has a low foaming and is very stable.

Documents:

mas-1998-1540-abstract.pdf

mas-1998-1540-claims duplicate.pdf

mas-1998-1540-claims original.pdf

mas-1998-1540-correspondance others.pdf

mas-1998-1540-correspondance po.pdf

mas-1998-1540-description complete duplicate.pdf

mas-1998-1540-description complete original.pdf

mas-1998-1540-form 1.pdf

mas-1998-1540-form 26.pdf

mas-1998-1540-form 3.pdf

mas-1998-1540-other documents.pdf

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Patent Number

204433

Indian Patent Application Number

1540/MAS/1998

PG Journal Number

26/2007

Publication Date

29-Jun-2007

Grant Date

21-Feb-2007

Date of Filing

10-Jul-1998

Name of Patentee

AKZO NOBEL N.V

Applicant Address

P O BOX 9300,,NL-6800, SB ARNHEM,,NETHERLAND

Inventors:

#	Inventor's Name	Inventor's Address
1	BJUR,KENT	SLANBARSGATAN 15, S-444 42 STENUNGSUND
2	CASSEL,ANDERS	ILLERSTIGEN 2, S-471 60 MYGGENAS,
3	STRANDBERG,MARGRETH	KOPPERSVAGEN 58, S-444 42 STENUNGSND

PCT International Classification Number

D01F2/10

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	9702703-1	1997-07-14	Sweden