DE1594904B - Process for refining fiber material containing or consisting of cellulose - Google Patents

Description

low temperatures due to insufficient solubility of the catalyst system according to the main patent application may occur.

British patent 456 307 describes a process for finishing textiles with urea-formaldehyde reaction products in the presence of a catalyst combination of ammonium salts and organic acids with a low dissociation constant, post-curing at temperatures above 100 ^° C. being omitted. However, as can be seen from the comparative tests and the table, the advantageous results are only obtained if one works with the claimed catalyst combination and with the special N-methylol or N-methylol ether compounds mentioned in the claim, while the procedure of the citation is compared with this delivers significantly less favorable results.

In each case a bleached and mercerized cotton fabric with a square meter weight of about 120 g used. The liquor pick-up after padding is 70%. All padded Tissues are dried at 120 ° to 6 to 7% residual moisture and in the manner described in the example Way treated further.

Experiment 1 corresponds to example 1 of British patent specification 456 307: equipment with a mixture of

100 g / l urea (solid),
300 g / l 40% formaldehyde solution,
0.75 g / l ammonium chloride,

5 g / l succinic acid,
2 g / l oxethylated isooctylphenol as a wetting agent.

Experiment 2 corresponds to experiment 1, except that 300 g / l of 50% aqueous dimethylolpropylene urea solution are used for urea-formaldehyde used.

This experiment corresponds to the aminoplast component, but not to the catalyst

Lo sator composition of the present application.

Experiment 3: equipment with a mixture of 300 g / l 50% aqueous dimethylolpropyleneurea solution,
1.2 g / l oxalic acid,

5.6 g / l maleic acid,
4 g / l ammonium chloride,
2 g / l oxethylated isooctylphenol as

Wetting agents.
This attempt corresponds to the present application.

Experiment 4: equipment with a mixture of 300 g / l 50% aqueous dimethylolethylene

urea solution, 1.2 g / l oxalic acid,
5.6 g / l maleic acid,
4 g / l ammonium chloride,
7 g / l of a 25% strength aqueous solution of a

oxethylated polyamide.

This experiment corresponds to the example described in more detail below.

Untreated fabric

attempt
number 1

attempt
No. 2

Experiment No. 3

Experiment No. 4

Dry wrinkle angle according to DIN 53 890 der

Equipment (chain + weft)

Dry wrinkle angle according to DIN 53 890 one

Machine washable (at 95 ° C)

Wet wrinkles according to T ο ο t a 1 equipment

(Warp + weft)

Loss of tensile strength

Abrasion resistance measured in Accelerator

3 minutes 3000 rpm

225
120

210
8th%

28%

230
160

230
IS%

20%

265 255

295 25%

12%

255 240

290 28% -

15%

The parts and percentages given in the following example are units of weight. The parts by weight relate to parts of space like the kilogram to the liter.

example

A bleached and mercerized cotton fabric (poplin) with a weight of 125 g / m ² is impregnated with a solution of the following composition by padding:

300 parts of a 50% dimethylolethylene urea solution, 1.2 parts of oxalic acid, 5.6 parts of maleic acid, 4 parts of ammonium chloride and 7 parts of a 25% strength aqueous solution of an oxyethylated polyamide are used diluted with water to 1000 parts by volume. The liquor uptake is 75%.

After impregnation, the fabric is dried on the tenter frame at 110 ° C. to 5.5 to 6% residual moisture and then docked. The fabric dock is sealed with a polyethylene film and rotated for 24 hours at room temperature. The catalyst is then removed by alkali treatment in the cold and the fabric is ^{washed with soap / soda at 60 °} C. on a wide washing machine.

After drying, it has the following technological data:

Dry wrinkle angle after

DIN 53 890 warp + weft; 260 °

Wet crease angle after

Tootal warp + weft; 300 °

Loss of tensile strength 25%

In addition, 40 parts of a 40% strength aqueous dispersion of a copolymer are added to the padding liquor from 89 parts of acrylic acid n-butyl ester, 5 parts of butanediol diacrylate, 3 parts of N-methylol methacrylamide and 3 parts of acrylamide, with the same loss of tensile strength, even better drying properties are obtained and wet crease angles.

Claims (1)

Claim: Modification of the process for refining cellulose containing or consisting of fiber material with compounds containing N-methylol and / or N-methylol ether groups according to patent application P14 69 262.7-43 (German Auslegeschrift 1469262), characterized in that a water-soluble catalyst combination of a) one or more ^{strong or moderately strong acids which are not volatile up to 130 °} C. and b) one or more potent acidic salts are used in which components a) and b) are present in a weight ratio of 1: 1 to 5: 1. The patent application P 14 69 262.7-43 (German Auslegeschrift 1469 262) relates to a method for Refining of cellulose containing or consisting of fiber material with N-methylol and resp. or N-methylol ether compounds, which is characterized is that the material is impregnated with an aqueous solution or dispersion that is at least a substance of the formula R ₂ O-CH ₂ -N ' R ₄ and or or Rl2 wherein R ₁ and R _{2 are} hydrogen atoms or low molecular weight alkyl groups, R ₃ and R _{4 are} radicals of the formula R ₅
-C-, R ₆
the immediate or over R ₇ R9 - C—, —O— or —N - I.
R ₈ 35 45 are connected to one another, or, if R ₁ and R _{2 are} low molecular weight alkyl radicals, also hydrogen atoms, low molecular weight alkyl groups or low molecular weight alkoxymethyl groups, R ₅ , R ₇ , R ₁₀ and R _{11 are} hydrogen atoms or low molecular weight alkyl groups, R ₆ and R _{8 are} hydrogen atoms, hydroxyl groups, low molecular weight alkyl groups or low molecular weight alkoxyl groups, R _{9 is} a hydrogen atom, a low molecular weight alkyl group or a low molecular weight hydroxyalkyl group, R ₁₂ and R _{13 are} hydrogen atoms, low molecular weight alkyl groups or low molecular weight alkoxymethyl groups, A is a divalent aliphatic hydrocarbon radical having 2 to 8 carbon atoms and ζ is zero or 1, and contains a water-soluble catalyst combination of a smaller amount by weight of a non-volatile up to 130 ° C strong or moderately strong acid and a larger amount by weight of a potent acidic salt, the impregnated material to a moisture content of 10 to 35%, based on there s weight of ^ N-CH ₂ -OR ₁
I.
R ₃ R ₁₀ O-CH ₂ -N ^ ^ O -A-— C - N-CH- OR ₁₃ OR -H in the amorphous regions of cellulose and dried contained and it and leaves at a temperature up to 5O ⁰ C with the applied substances of the formula I or II or react. This method makes it possible in a single operation in a simple and reliable manner Fiber material that contains cellulose or consists of it to be equipped so that it has high to very high wet crease angles of 140 ° and more and average dry wrinkle angles of 110 ° and more. By variation It is in the hand of the process conditions, the height and difference of the wet and dry wrinkle angles adapt to the respective needs. In addition to the aforementioned advantages achieve particularly good abrasion and tear resistance of the material to be treated. It has now been found that equally good results can be achieved and additionally favorable solubility for the catalyst creates if, instead of according to the main patent to use a catalyst combination of such of a) one or more up to 13O ⁰ C nonvolatile strong or medium strong acids and b) one or more potent acidic salts are used in which components a) and b) are present in a weight ratio of 1: 1 to 5: 1, preferably 1: 1 to 2: 1. The acids and potent acid salts required for the catalyst combination are the same as those also come into consideration for the main patent application process. Also the others at that Process of the main patent application required or possible additives and procedural measures remain unchanged in the present proceedings. The present process gives the same advantageous results as that of the main patent application; but it also offers greater security against difficulties that, for example, occasionally occur