Aqueous solutions of optical bleaches

FIELD: textile fabrics, paper.

SUBSTANCE: aqueous solutions are related to toluylene optical bleaches and may be used in production of chalk overlay paper of high whiteness. Aqueous solutions contain at least one optical bleach, polyvinyl alcohol, having extent of hydrolysis over 75% and Brookfield viscosity of 2-40 mPa·s, and water. This composition may be used for paper coating. It may be applied on paper after its moulding to produce chalk overlay paper.

EFFECT: provision of stability in storage of aqueous solutions of toluylene optical bleaches and simplified method for production of chalk overlay paper.

9 cl, 3 tbl, 3 ex

 

The present invention relates to stable storage water solutions stilinovich optical brighteners with polyvinyl alcohols which can be used directly by the paper manufacturers.

It is well known that white and, thus, the attractiveness of the coated paper can be improved by the addition of optical brighteners to the coating composition. To meet the demand higher for white coated paper, there is a need for more efficient optical brighteners.

WO 96/00221 describes the bleachers on the basis tetrasulfonated stilbene derived from amino acids, for use in paper, textiles and detergents. Polyvinyl alcohols are included in the list of additives that are, as indicated, improve the operational characteristics of the bleachers when applied to the surface of the paper.

WO 98/42685 describes the bleachers on the basis hexachlorophane stilbene, manufactured using certain amino acids, without connection WO 96/00221. Also describes how the fluorescent whitening of a paper surface coating of bleach as part of the composition pigmented coatings, which also includes polyvinyl alcohol as a water-soluble shared binding or protection of the aqueous colloid.

EP 1355004 describes the use of certain stilinovich brighteners, which are not derived from amino acids, bleaching aqueous coating compositions comprising at least one latex binder and at least one differing from it in shared synthetic binder. Polyvinyl alcohols are listed as the preferred synthetic shared binder.

The patent application of Japan Kokai 62-106965 describes some of the bleach-based hexachlorophane stilbene derived from amino acids. Stated that bleach is very effective for the fluorescent whitening of paper and can be applied to the surface of the paper as part of the solution for gluing or compositions pigmented coating. Polyvinyl alcohol is listed as a possible component of the solution for sizing.

Even though from the prior art it is known that polyvinyl alcohol, among other compounds, may increase the bleaching action, up to this time, the manufacturer of paper, if you wish to use the specified alcohol, had to add it separately in the coating composition. Therefore, there is still a need to simplify the method of obtaining bleached coated paper.

It has been unexpectedly discovered that can be made is to be stable during storage solutions consisting essentially of telenovela optical Brightener and polyvinyl alcohol, which can be used directly by the paper manufacturer, as they can be diluted with water and/or to measure directly in the composition for coating to obtain a coated paper is particularly high whiteness.

Thus, the invention provides aqueous optical Brightener consisting essentially of

(a) at least one optical Brightener of formula (1)

in which

M represents hydrogen, alkali metal atom, ammonium or a cation derived from an amine, preferably hydrogen or sodium, most preferably, sodium,

n is 1 or 2, and

X is a natural or synthetic amino acid, which was removed a hydrogen atom of an amino group;

(b) polyvinyl alcohol having a degree of hydrolysis of more than 75% and a viscosity Brookfield 2-40 MPa·s (4% wt./mass. aqueous solution at 20°C); and

(c) water.

Optical brighteners, for which n is 1, the group of SO3M preferably is in position 4 of the phenyl ring.

Optical brighteners, for which n is 2, groups a, SO3M are preferably in positions 2, 5 phenyl rings.

Examples of amino acids that can on what to teach X, are alanine, 2-aminobutyric acid, asparagine, aspartic acid, S-carboxymethylcysteine, cysteine acid, cysteine, glutamic acid, glutamine, glycine, iminodiacetate acid, isoleucine, leucine, methionine, N-methyltaurine, norleucine, Norvaline, phenylalanine, 2-phenylglycine, pipecolinate acid, Proline, sarcosine, serine, taurine, threonine and valine. When the amino acid contains a chiral center, you can use either optical isomer or racemic mixture.

Preferred amino acids are aspartic acid, glutamic acid and iminodiacetate acid.

Aqueous solutions can contain up to 10% of the mass. salt, typically sodium chloride, obtained as a by-product in the manufacture of optical Brightener.

Aqueous solutions may also contain one or more antifreeze agents, biocides, complexing agents, or other additives, and organic by-products formed in the manufacture of optical Brightener.

Polyvinyl alcohol preferably has a degree of hydrolysis equal to or greater than 80%, and the viscosity Brookfield 2-20 MPa·S.

Preferably, the mass ratio of polyvinyl alcohol to the optical Brightener is in the range from 0.01:1 to 1.5:1. More preferably, this ratio ranges from 0.03:1 to 1:1.

The water content in the solution, respectively, is at least such that the solution is still mixed and, preferably, easily erupt; in concentrated solutions, the concentration of optical Brightener is mostly in the range from 6 to 60%, preferably from 10 to 50 wt%. by weight of solution.

The pH value of aqueous solutions, preferably, is neutral to distinctly alkaline, in particular, in the range of pH 7 to 10. The pH value can, if necessary, adjust by adding M-relevant bases, such as hydroxides or carbonates of alkali metals, ammonia or amines.

The solution of the optical Brightener according to this invention are stable during storage and can be used directly as such, because they can be diluted with water and/or to measure directly in the composition for coating. Thus, a further object of the invention is the addition of solutions of bleach in the composition for coating to obtain a coated and optically bleached paper.

Thus, the invention also provides a method of obtaining optically bleached coated paper, at least, in the floor, where a composition for coating, described above, cover the paper after manufacture of paper.

Compositions for coating there is actually an are aqueous compositions which contain at least one binder and a white pigment, in particular, giving the opacity of the white pigment, and may optionally contain additional additives such as dispersing agents and antifoaming agents.

Although it is possible to obtain compositions for coatings that do not contain white pigments, the best white substrate for printing is made using the compositions of the opaque layers that contain 10-70% white pigment by weight. Such white pigments, as a rule, are inorganic pigments, such as aluminum silicate (kaolin, otherwise known as white clay), calcium carbonate (chalk), titanium dioxide, aluminum hydroxide, barium carbonate, barium sulfate or calcium sulfate (gypsum).

The binder can be any substance, usually used in the paper industry for the production of compositions for coatings, and may consist of a single binder or of a mixture of primary and secondary binders. The only or main binder preferably is a synthetic latex, typically strollerderby, vinyl acetate, styrene-acrylic, venerability or ethylenevinylacetate polymer. The secondary binder may constitute, for example, starch, carboxymethylcellulose, casein, soy polymers or poly is injuly alcohol.

The only or main binder is used in amounts typically in the range 5-25% of the mass. by weight of white pigment. The secondary binder is used in an amount typically in the range of 0.1-10% wt. by weight of white pigment.

The optical Brightener of formula (1) is used in amounts typically in the range of 0.01-1% wt. by weight of white pigment, preferably in the range of 0.05-0.5 wt%. by weight of white pigment.

EXAMPLES

The following examples explain the present invention in more detail. Unless stated otherwise, "%" and "parts" are mass; viscosity measured in 4% aqueous solution at 20°C using a Brookfield viscometer.

EXAMPLE of PREPARATION 1A

The solution of the optical Brightener 1a receive, mixing together

of 13.1 parts (0.01 mol) of an optical Brightener of the formula (4),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 98.5% and a viscosity Brookfield of 2.75 MPa·s, and

80,6 parts water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 1B

The solution of the optical Brightener 1b receive, mixing together

of 15.1 parts (0.01 mol) optical from the of elevates formula (5),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 98.5% and a viscosity Brookfield of 2.75 MPa·s, and

78,6 parts water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 1C

An example of comparison (without polyvinyl alcohol)

The solution of the optical Brightener 1c receive, mixing together

of 15.1 parts (0.01 mol) of an optical Brightener of the formula (5) and

84,9 parts of water. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 1D

An example of comparison representing the prior art (EP 1355004)

The solution of the optical Brightener 1d receive, mixing together

12,2 parts (0.01 mol) of an optical Brightener of the formula (6),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 98.5% and a viscosity Brookfield of 2.75 MPa·s, and

of 81.5 parts of water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 2A

The solution of the optical Brightener 2a receive the, mixing together

of 13.1 parts (0.01 mol) of an optical Brightener of the formula (4),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 85% and a viscosity Brookfield of 3.7 MPa·s, and

80,6 parts water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 2B

The solution of the optical Brightener 2b receive, mixing together

of 15.1 parts (0.01 mol) of an optical Brightener of the formula (5),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 85% and a viscosity Brookfield of 3.7 MPa·s, and

78,6 parts water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 2C

An example of comparison (without polyvinyl alcohol)

The solution of the optical Brightener 2c receive, mixing together

of 15.1 parts (0.01 mol) of an optical Brightener of the formula (5) and

84,9 parts of water. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

SAMPLE PREPARATION for 2D

An example of comparison representing the prior art (EP 1355004)

The solution optical otbelivanie what I get 2d, mixing together

12,2 parts (0.01 mol) of an optical Brightener of the formula (6),

of 6.3 parts of polyvinyl alcohol having a degree of hydrolysis of 85% and a viscosity Brookfield of 3.7 MPa·s, and

of 81.5 parts of water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 3A

The solution of the optical Brightener receive 3a, mixing together

18,9 part (of 0.0125 mol) of an optical Brightener of the formula (5),

1,2 parts of polyvinyl alcohol having a degree of hydrolysis of 85% and a viscosity Brookfield of 3.7 MPa·s, and

79,9 parts water

when heated to 90-95°C to obtain a clear solution which remains stable after cooling to room temperature. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

EXAMPLE of PREPARATION 3B

An example of comparison (without polyvinyl alcohol)

The solution of the optical Brightener 3b receive, mixing together

18,9 part (of 0.0125 mol) of an optical Brightener of the formula (5) and

81,1 parts of water. The pH value of the solution is regulated to 9.0 with sodium hydroxide.

APPLICATION EXAMPLE 1

Preparing a composition for coating containing 500 parts of chalk (commercially available under the trade name is of Hydrocarb 90 from OMYA), 500 parts of clay (commercially available under the trade name Kaolin SPS from IMERYS), 470 parts of water, 6 parts of a dispersant (sodium salt of polyacrylic acid, commercially available under the trade name Polysalz S from BASF), 200 parts of latex (copolymer of acrylic ester, commercially available under the trade name Acronal S320D from BASF) and 50 parts of 10% solution of carboxymethyl cellulose (commercially available under the trade name Finnfix 5,0 from Noviant) in water. The solids content of regulate to 60% by adding water, and regulate pH to 8-9 with sodium hydroxide.

Solutions 1a, 1b, 1c and 1d, manufactured as described in the preparation examples 1A, 1B, 1C and 1D, respectively, added in the concentration range from 0.5 to 4.0% for mixed compositions for coating. Then brightening composition for coating to be applied on commercial 75 g/m2the main sheet of white paper with a neutral sizing using an automatic device for coating with a rod wound with thread with the standard setting for the speed and the standard load on the rod. Then, the coated paper is dried for 5 minutes in a stream of hot air. The dried paper stand, then measure the CIE whiteness on the calibrated Elrepho spectrophotometer.

The table is a 1
Solution concentration (%)The CIE whiteness using a solution 1aThe CIE whiteness using a solution 1bThe CIE whiteness using a solution of 1c (comparison)The CIE whiteness using a solution of 1d (comparison)
0of 89.1of 89.1of 89.1of 89.1
0,5100,7101,398,398,3
1,0107,2106,4101,6104,6
2,0114,2114,2109,3110,9
4,0118,9121,4to 114.7117,5

APPLICATION EXAMPLE 2

Repeat the application example 1, using solutions 2a, 2b, 2c and 2d, prepared as described in preparation examples 2A, 2B, 2C and 2D, respectively the military.

Table 2
Solution concentration (%)The CIE whiteness using a solution 2aThe CIE whiteness using a solution 2bThe CIE whiteness when using a solution of 2c (comparison)The CIE whiteness using a solution of 2d (comparison)
0of 89.1of 89.1of 89.1of 89.1
0,5of 98.298,398,397,9
1,0106,8104,3101,6102,2
2,0111,2110,5109,3108,0
4,0114,8118,1to 114.7of 112.8

APPLICATION EXAMPLE 3

Preparing a composition for coating, sod is readuy 500 parts of chalk (commercially available under the trade name Hydrocarb 90 from OMYA), 500 parts of clay (commercially available under the trade name Kaolin SPS from IMERYS), 370 parts of water, 6 parts of a dispersant (sodium salt of polyacrylic acid, commercially available under the trade name Polysalz S from BASF), 200 parts of latex (copolymer of acrylic ester, commercially available under the trade name Acronal S320D from BASF) and 400 parts of a 20% solution of anionic potato starch (Perfectamyl A4692 from AVEBE B.A.) in water. The solids content of regulate to 60% by adding water, and regulate pH to 8-9 with sodium hydroxide.

Solutions 3a and 3b, are made as described in the preparation examples 3A and 3B, respectively, added in the concentration range from 0.5 to 4.0% for mixed compositions for coating. Then whitening composition for coating to be applied on commercial 75 g/m2the main sheet of white paper with a neutral sizing using an automatic device for coating with a rod wound with thread with the standard setting for the speed and the standard load on the rod. Then, the coated paper is dried for 5 minutes in a stream of hot air. The dried paper stand, then measure the CIE whiteness on the calibrated Elrepho spectrophotometer.

Table 3
To the concentrations of the solution (%) White CIE
when using a solution of 3a
White CIE
when using a solution of 3b (comparison)
087,987,9
0,599,4of 98.2
1,0106,4104,9
2,0114,8112,1
4,0of 123.2120,8

These results clearly show the surprising superiority of the white real solutions containing polyvinyl alcohol.

1. Aqueous optical Brightener consisting essentially of
(a) at least one optical Brightener of formula (1)

in which M represents hydrogen, alkali metal atom, ammonium or a cation derived from an amine,
n is 1 or 2, and
X is a natural or synthetic amino acid, which was removed a hydrogen atom of an amino group;
(b) polyvinyl alcohol having a degree of hydrolysis of more than 75% and a viscosity Brookfield 2-40 MPa·s; and
(c) water.

2. The solutions according to claim 1, the de
M represents hydrogen or sodium,
n is 1 or 2,
X represents aspartic acid, glutamic acid or iminoxyl acid, and
where polyvinyl alcohol has a degree of hydrolysis equal to or greater than 80%, and the viscosity Brookfield 2-20 MPa·S.

3. The solutions according to claim 1 or 2, where the mass ratio of polyvinyl alcohol to the optical Brightener is from 0.01:1 to 1.5:1 and where the concentration of the optical Brightener is from 6 to 60 wt.%.

4. The solution according to claim 3, where the mass ratio of polyvinyl alcohol to the optical Brightener is from 0.03:1 to 1:1, and where the concentration of the optical Brightener is from 10 to 50 wt.%.

5. The application of the solution according to any one of the preceding paragraphs in compositions for coating paper.

6. A method of obtaining a coated paper, where the composition for coating containing solution according to any one of the preceding paragraphs, is applied to the paper after manufacture of paper.

7. The method according to claim 6, where the composition for coating contains from 10 to 70 wt.% one or more white pigments.

8. The method according to claim 6 or 7, where the composition for coating contains the main connection on the basis of synthetic rubber latex selected from Starovoitova, vinyl acetate, styrene-acrylic, vinylgroover or ethylenevinylacetate polymer, or optionally a secondary binder, select the TES from starch, carboxymethylcellulose, casein, soy polymers or polyvinyl alcohol.

9. The method according to claim 6 or 7, where the main binder is used in an amount of 5 to 25 wt.% by weight of white pigment, where the secondary binder is used in an amount of from 0.1 to 10 wt.% by weight of white pigment, and where the optical Brightener of formula (1) is used in an amount of from 0.01 to 1 wt.% by weight of white pigment, preferably from 0.05 to 0.5 wt.% by weight of white pigment.



 

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