Method for preparing formaldehyde-free non-ironing resin
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A non-ironing resin and formaldehyde technology, applied in textiles and papermaking, fiber treatment, plant fiber, etc., can solve the problems of uneasy reaction, poor crosslinking, and low activity, and achieve good effect, small loss of fabric strength, and good use effect Good results
Active Publication Date: 2017-03-15
中国纺织科学研究院江南分院
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The non-ironing resin invented by this patent contains four hydroxyl groups on the two nitrogen heterocycles, that is, each nitrogen heterocycle contains only two hydroxyl groups, and these two hydroxyl groups are less reactive and are not easy to interact with the hydroxyl groups on the cellulose fibers. Reaction, poor cross-linking, unsatisfactory non-iron effect
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preparation Embodiment 1
[0026] (1) Add 72.5g glyoxal (40%) aqueous solution to a 250mL round-bottomed flask, adjust the pH value of the sodium hydroxide aqueous solution to 5-5.5, add 32g urea, stir and heat up to 45°C, keep the reaction for 4 hours, drop to 20°C, let stand for 12 hours, filter the solid, and dry in vacuum.
[0027] (2) Add 150g of absolute ethanol to a 500mL round-bottomed flask, add the above dried solid into ethanol, add 100g of epichlorohydrin after dissolving, adjust the pH value of the sodium hydroxide solution and maintain it at 11-12,45 ℃ heat preservation reaction for 5 hours, hydrochloric acid aqueous solution to adjust the pH = about 7, vacuum distillation to remove ethanol, add 150mL of water to obtain a formaldehyde-free non-iron resin solution.
preparation Embodiment 2
[0029] (1) Add 200g of glyoxal (40%) aqueous solution to a 500mL round bottom flask, adjust the pH value of the sodium carbonate aqueous solution to 5-5.5, add 85g of urea, heat up to 50°C, keep the reaction for 3 hours, and drop to 15°C , let stand for 8h, filter the solid, and dry in vacuum.
[0030] (2) Add 500g of absolute ethanol to a 1L round-bottomed flask, add the above-mentioned dried solids into ethanol, add 306g of glycidol after dissolving, adjust the pH value of the sodium hydroxide solution and maintain it at 10-11, and keep it warm at 50°C After reacting for 4 hours, adjust the pH of the aqueous hydrochloric acid solution to 6-7, distill off the ethanol under reduced pressure, and add 450 mL of water to obtain a formaldehyde-free, easy-care resin aqueous solution.
[0031] product testing:
[0032] The formaldehyde-free and easy-care resin solution prepared in Example 1-2 has an appearance of light yellow to brown transparent liquid without unpleasant odor, and...
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Abstract
The invention relates to a method for preparing formaldehyde-free non-ironing resin, and belongs to the technical field of dyeing-and-printing-industry cotton-fabric post-finishing agents. The method is characterized by including the following steps that (1) urea and a glyoxal solution are reacted for 1 hour to 5 hours under the conditions that pH is 4 to 8, and the temperature is 30 DEG C to 80 DEG C, the temperature is reduced, then the product is standing at the room temperature lower than or equal to 20 DEG C, and a solid intermediate product dyhydroxyl ethylene urea is obtained; (2) the solid dyhydroxyl ethylene urea is dissolved in absolute ethyl alcohol with the mass accounting for 2 times to 5 times of that of the solid dyhydroxyl ethylene urea, then active-group-containing substances are added, wherein the molar ratio of the solid dyhydroxyl ethylene urea to the active-group-containing substances is 1:2-1:3, the mixture is reacted for 1 hour to 6 hours under the conditions that pH is 8 to 12, and the temperature is 30 DEG C to 60 DEG C, the pH of a solution is adjusted to be about 7, ethyl alcohol is removed in a reduced-pressure-distillation mode, a proper amount of water is added, the concentration is adjusted to be the required concentration, and a formaldehyde-free non-ironing resin solution is obtained. According to the formaldehyde-free non-ironing resin solution prepared with the method, the non-ironing finishing effect is good, and the fabric strength losses are small.
Description
[0001] Technical field: [0002] The invention relates to a preparation method of a formaldehyde-free non-ironing resin, which belongs to the technical field of finishing agents for cotton fabrics in the dyeing and finishing industry. [0003] Background technique: [0004] N-methylolamide resins are commonly used in non-ironing finishing of cotton fabrics, especially 2D resins. These resins are cheap, easy to obtain raw materials, and have good non-ironing effects. However, formaldehyde will be released during processing and wearing, which seriously endangers the human body. healthy. Although the release of formaldehyde can be reduced by methods such as etherification, it cannot be free of formaldehyde. [0005] In recent years, with the improvement of people's quality of life and the enhancement of environmental awareness, formaldehyde-free has become the development direction and research hotspot of durable non-ironing resins, and many kinds of non-formaldehyde non-ironing ...
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