Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – At least one aryl ring which is part of a fused or bridged...
Reexamination Certificate
1999-12-16
2001-10-23
Gorr, Rachel (Department: 1711)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
At least one aryl ring which is part of a fused or bridged...
C528S045000, C528S070000, C528S073000, C524S839000, C525S124000, C525S452000, C525S528000, C008S115600, C008S115640, C008S192000
Reexamination Certificate
active
06306958
ABSTRACT:
The invention relates to aqueous dispersions comprising a compound having blocked isocyanate groups in the molecule, to a process for preparing such dispersions and to the use of said dispersions to treat fiber materials.
Aqueous dispersions comprising compounds having blocked isocyanate groups are known and described, for example, in EP-A 196 309, EP-A 262 069, EP-A 537 578, and EP-A 872 503. In connection with the oil and water repellent finishing of fiber materials it is also known to use compounds having blocked isocyanate groups as extenders in combination with perfluoroalkyl-containing polymers in order to intensify the effects of the latter. This utility is described, for example, in EP-A 196 309, EP-A 537 578, and EP-A 872 503.
The prior art aqueous dispersions comprising compounds having blocked isocyanate groups have the disadvantage that when used together with perfluoroalkyl-containing polymers in order to obtain an oil and water repellent finish on cellulosic fiber materials they occasionally result in effects which are less than optimum, especially as regards the permanence of the effects following laundering and dry-cleaning operations.
It is an object of the present invention to provide aqueous dispersions comprising a compound which has blocked isocyanate groups in the molecule and which together with perfluoroalkyl-containing polymers allows an oil and water repellent finish to be obtained on cellulosic fiber materials, especially cotton, with effects which are good and above all permanent.
This object has been achieved by an aqeuous dispersion comprising at least two components A) and B), component A) being a compound containing two or more blocked isocyanate groups in the molecule, wherein component B) is a product obtainable by reacting a diepoxy compound of the formula (I)
G—O—(L—O)
y
—G (I)
or a mixture of compounds of the formula (I) with a diamine or polyamine of the formula (II)
H
2
N—(C
j
H
2j
NH)
z
—H (II)
or a mixture of compounds of the formula (II) in a proportion such that the molar ratio of the deployed glycidyl radicals G to the hydrogen atoms of the deployed amino groups is in the range from 2:1 to 1:4, preferably in the range from 1:1 to 1:2, with particular preference in the range from 1:1 to 1:1.1, and subsequently reacting the resulting reaction product with an acid in a proportion such that the ratio of moles of nitrogen to equivalents of acid is in the range from 1:0.25 to 1:2, the above radicals and indices independently of one another having the following definitions:
G=glycidyl radical (2,3-epoxy-1-propyl radical)
L=divalent radical of formula (CO)c
1
—E
d
—(CO)c
2
E=divalent aromatic, aliphatic or araliphatic hydrocarbon radical of 1-18 carbon atoms uninterrupted or interrupted by one or more oxygen atoms; preferably an aliphatic radical of 1-8 carbon atoms or an aromatic radical of 6-24 carbon atoms
c
1
and c
2
independently of one another=0 or 1
d=0 or 1
and c
1
, c
2
and d are not all simultaneously 0 when y=1
j=0 or 2-10
y=0 or 1
z=1-3; but z=1 if j=0.
The aqueous dispersions of the invention have the following advantages:
1. good mechanical and thermal stability
2. together with even relatively small amounts of known perfluoroalkyl-containing polymers already used for textile finishing they allow an oil and water repellent finish to be obtained on cellulose fiber materials, especially cotton, with good effects including permanence after laundering and dry-cleaning operations
3. good running properties when used in textile finishing.
Components A) suitable for the aqueous dispersions of the invention are, as already mentioned at the outset, known and described for example—with no claim to completeness—in the abovementioned references. Blocked aliphatic, alicyclic or aromatic di-, tri- or polyisocyanates are suitable. The compounds suitable for blocking isocyanate groups are also known to the skilled worker. The compounds suitable as component A) can be obtained inter alia, for example, by simultaneous or successive reaction of one or more di- or polyisocyanates with one or more compounds having functional groups which react with isocyanate groups and subsequent reaction of the remaining free isocyanate groups with known blocking agents, preferably with ketone oximes—examples being acetone oxime or butanone oxime—or mixtures thereof. Further suitable blocking agents are described in the literature. The property common to all suitable blocking agents is that they result in reversible blocking of the isocyanate groups; that is, the blocking agent is bonded chemically to the isocyanate group at room temperature and is cleaved off at elevated temperatures. Aqueous dispersions of compounds A) are also known to the skilled worker.
Components B) present in the aqueous dispersions of the invention are also known per se. They are obtainable by reacting a diepoxy compound of the formula (I)
G—O—(L—O)
y
—G (I)
or a mixture of compounds of the formula (I) with a diamine or polyamine of formula (II)
H
2
N—(C
j
H
2j
NH)
z
—H (II)
or a mixture of compounds of the formula (II) in the stated proportion with cooling and subsequently reacting the resulting reaction product with an acid in the stated proportion, the radicals and indices indicated having the stated definition. Preference is given to compounds B) in which the diepoxy compound used corresponds to the formula G—O—E—O—G; particular preference to those in which E is a divalent aliphatic radical of 2-6 carbon atoms or a divalent aromatic radical of 6-18 carbon atoms, especially the radical p—C
6
H
4
—(CH
3
)C(CH
3
)—p—C
6
H
4
—. Likewise preferred are compounds B) prepared using a diamine of 2-6 carbon atoms, especially hexamethylene diamine. In the preparation of compounds B) the acid used is preferably either an organic acid, especially acetic acid, or a strong inorganic acid, such as sulfuric acid, phosphoric acid and, in particular, hydrochloric acid. However, other acids can also be used. It is advantageous for the acid to be added rapidly.
The dispersions of the invention can be obtained by mixing a dispersion of a compound A) with a solution of a compound B). Preferred, however, are dispersions of the invention prepared by jointly dispersing components A) and B) with the aid, for example, of a high-speed stirrer; particularly preferred dispersions of the invention are those which following the dispersing operation are converted into fine dispersions by homogenization. The homogenization can be carried out, for example, with a high-pressure homogenizer machine (e.g., from the manufacturer Manton-Gaulin) at a pressure of from 100 to 500 bar, preferably from 200 to 300 bar. When dispersed individually, or in the case of the stated preferred joint dispersing operation, components A) are preferably used in the form of solutions in organic solvents. Examples of suitable solvents are esters, ketones, alcohols, aromatic hydrocarbons, mono-, di-, tri- and tetraglycols of ethylene glycol or propylene glycol and also the alkyl ethers thereof or the esters thereof. Not only dispersing and, if desired, mixing, but also high-pressure homogenizing, can be carried out at normal or elevated temperature. Excessively low temperatures carry with them the risk of a precipitation of product from the dispersion; the upper temperature limit is determined by the boiling point of the water/solvent mixture. It is preferred to operate at 20-40° C.; high-pressure homogenization is judiciously conducted with cooling. After the dispersion comprising components A) and B) has been obtained, it is preferred to remove any organic solvent present, by means, for example, of distillation, under either atmospheric or reduced pressure. The solvent-free aqueous dispersions obtained in this way feature the advantages not only of eco-friendliness and a high flash point but also of increased stability.
The dispersions of the invention comprise components A) and B) advantageously in a weight ratio from
Artner Wilhelm
Dirschl Franz
Gaugenrieder Heinz
Ludemann Simpert
Mosch Franz
Ciba Specialty Chemicals Corporation
Gorr Rachel
Mansfield Kevin T.
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