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Improved preparation method of dimethylol dihydroxyethylene urea

A technology of dimethylol dihydroxyethylene urea and dihydroxyethylene urea, which is applied in the field of textile functional finishing, can solve the problems affecting the etherification modification reaction of products, the conversion rate of glyoxal, the stability of high-concentration products and the reactivity, etc. Rarely involve problems such as poor storage stability, etc., to achieve the effects of high conversion rate, good stability and stable reaction

Active Publication Date: 2017-04-19
浙江震东新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the 2D resin prepared by the traditional two-step method has poor storage stability at high concentrations, which affects the etherification modification reaction of the product.
[0005] For the two-step process, although many professional journals have reported the improvement of many synthetic methods, most of them are optimized from the raw material ratio, reaction temperature, reaction time and other conditions to reduce the formaldehyde content and increase the glyoxal conversion rate. , high-concentration product stability and reactivity are rarely involved

Method used

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  • Improved preparation method of dimethylol dihydroxyethylene urea
  • Improved preparation method of dimethylol dihydroxyethylene urea
  • Improved preparation method of dimethylol dihydroxyethylene urea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] In a 1-liter four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser tube, add 290 grams of glyoxal (40% content) and then 126 grams of urea (99% content), stirring and dissolving at 35°C. Then add 0.12g of methanesulfonic acid (content 70%), 0.60g of sodium methanesulfonate (content 98%), and react at 40°C for 2 hours; then add 0.20g of sodium methanesulfonate, heat up to 55°C, The reaction was continued for 2 hours. Determination of residual glyoxal (results in Table 1).

[0054] Then the reactant was cooled to 50°C, 2.6 g of disodium hydrogen phosphate and 0.16 g of sodium dihydrogen phosphate were added, and a mixture of 300 g of formaldehyde solution (37%) and 2.5 g of dimethylaminoethanol (dimethylaminoethanol) was added dropwise within 1-2 hours Add aminoethanol to the formaldehyde solution in advance), and continue the reaction at 50°C for 4 hours to obtain a light yellow transparent liquid. Determination of active group methylo...

Embodiment 2

[0057] In a 1L four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser tube, add 290 grams of glyoxal (content 40%), then add 130 grams of urea (content 99%), stir and dissolve at 35 °C. Then add 0.21g of ethylsulfonic acid (content 70%), sodium ethylsulfonate 0.82g (content 98%), and react at 40°C for 2 hours; then add 0.50g of sodium ethylsulfonate, heat up to 50°C, The reaction was continued for 2 hours. Determination of residual glyoxal (results in Table 1).

[0058] Then add 2.8 g of disodium hydrogen phosphate, 0.20 g of sodium dihydrogen phosphate, and dropwise add 300 g of formaldehyde solution (37%), 2.5 g of dimethylaminoethanol, and 1.5 g of diethylaminopropanol (dimethylaminopropanol) for 1-2 hours. Add aminoethanol and diethylaminopropanol to the formaldehyde solution in advance), and continue the reaction at 55°C for 3 hours to obtain a light yellow transparent liquid. Determination of active group methylol formaldehyde content (...

Embodiment 3

[0061] In a four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser tube, add 290 grams of glyoxal (content 40%), then add 130 grams of urea (content 99%), stir and dissolve at 35°C. Then add 0.30g of benzenesulfonic acid (content 80%), 0.80g of sodium benzenesulfonate (content 98%), and react for 2 hours at 40°C; then add 0.45g of sodium benzenesulfonate, heat up to 50°C, and continue the reaction for 2 hours Hour. Determination of residual glyoxal (results in Table 1).

[0062] Then add 2.8g of dipotassium hydrogen phosphate, 0.20g of potassium dihydrogen phosphate, and dropwise add 300g of formaldehyde solution (37%), 2.5g of dimethylaminoethanol, and 1.5g of diethylaminopropanol (dimethylaminopropanol) for 1-2 hours. Add aminoethanol and diethylaminopropanol to the formaldehyde solution in advance), and continue the reaction at 55°C for 3 hours to obtain a light yellow transparent liquid. Determination of active group methylol formaldehyde...

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Abstract

The invention provides a preparation method of dimethylol dihydroxy ethylene urea. The method comprises the following steps: 1, reacting urea with glyoxal in the presence of sulfonic acid and sulfonic acid alkali metal salt at 30-60DEG C for 3-6h to prepare a dihydroxy ethylene urea intermediate; and 2, reacting the dihydroxy ethylene urea intermediate obtained in step 1 with a formaldehyde and optional organic alcohol amine mixture in the presence of dialkali metal hydrogen phosphate and alkali metal dihydrogen phosphate at 40-60DEG C for 2-4h to obtain a target product. The preparation method has the advantages of stable reaction and high conversion rate, and the product has the advantages of high content of active groups, and strong responsivity.

Description

technical field [0001] The invention relates to an improved preparation method of a non-ironing finishing agent in the field of textile functional finishing, more specifically a preparation method of dimethylol dihydroxyethylene urea. [0002] technical background [0003] Cotton fabric is favored by people because of its softness, comfort, breathability, and good hygroscopicity, but it has the disadvantage of being easy to shrink and wrinkle. Resin finishing of cotton fabrics can achieve the effect of anti-shrinkage and anti-wrinkle. At present, commonly used resin finishing agents are divided into two categories: low aldehyde finishing agents and aldehyde-free finishing agents. Formaldehyde-free finishing agents are safe and environmentally friendly, and conform to the current development trend. However, the cotton fabrics treated with them have low resilience, which makes it difficult to meet the requirements of anti-shrinkage and anti-wrinkle for pure cotton fabrics, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/40D06M13/432
Inventor 李正雄顾喆栋
Owner 浙江震东新材料有限公司
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