Improved preparation method of dimethylol dihydroxy ethylene urea

A technology of dimethylol dihydroxyethylene urea and formaldehyde, which is applied in the fields of fiber treatment, textiles and papermaking, organic chemistry, etc., and can solve the problem of etherification modification reaction, poor storage stability, and glyoxal conversion rate that affect the product , High-concentration product stability and reactivity are rarely involved in issues such as high conversion rate, stable reaction and good stability

Active Publication Date: 2015-06-17
浙江震东新材料有限公司
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  • 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.
[0004] 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 dihydroxy ethylene urea
  • Improved preparation method of dimethylol dihydroxy ethylene urea
  • Improved preparation method of dimethylol dihydroxy ethylene urea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] In a 1-liter four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser, add 290 g of glyoxal (content 40%), then add 126 g of urea (content 99%), and stir to dissolve at 35°C. Then add 0.12 g of methanesulfonic acid (content 70%) and 0.60 g of sodium methanesulfonate (content 98%), and react at 40 °C for 2 hours; then add 0.20 g of sodium methanesulfonate, heat up to 55 °C, The reaction was continued for 2 hours. The residual amount of glyoxal was determined (see Table 1 for the results).

[0053] 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 for 1-2 hours. Aminoethanol was added to the formaldehyde solution in advance), and the reaction was continued at 50 ° C for 4 hours to obtain a light yellow transparent liquid. Determinatio...

Embodiment 2

[0056] In a 1L four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser, add 290 g of glyoxal (content 40%), then add 130 g of urea (content 99%), and stir to dissolve at 35°C. Then add 0.21 g of ethyl sulfonic acid (content 70%), 0.82 g of sodium ethyl sulfonate (content 98%), and react at 40°C for 2 hours; The reaction was continued for 2 hours. The residual amount of glyoxal was determined (see Table 1 for the results).

[0057] Then add 2.8 g of disodium hydrogen phosphate, 0.20 g of sodium dihydrogen phosphate, and dropwise add a mixture of 300 g of formaldehyde solution (37%) and 2.5 g of dimethylaminoethanol and 1.5 g of diethylaminopropanol for 1-2 hours (dimethylaminoethanol). Aminoethanol and diethylaminopropanol were added to the formaldehyde solution in advance), and the reaction was continued at 55°C for 3 hours to obtain a light yellow transparent liquid. Determination of active group methylol formaldehyde content (the results are...

Embodiment 3

[0060] In a four-necked round-bottomed flask equipped with a stirrer, a thermometer and a condenser, add 290 g of glyoxal (content 40%), then add 130 g of urea (content 99%), and stir to dissolve at 35°C. Then add 0.30 g of benzenesulfonic acid (content 80%), 0.80 g of sodium benzenesulfonate (content 98%), and react at 40°C for 2 hours; then add 0.45g of sodium benzenesulfonate, heat up to 50°C, and continue reaction 2 Hour. The residual amount of glyoxal was determined (see Table 1 for the results).

[0061] Then add 2.8g of dipotassium hydrogen phosphate, 0.20g of potassium dihydrogen phosphate, and dropwise add a mixture of 300g of formaldehyde solution (37%) and 2.5g of dimethylaminoethanol and 1.5g of diethylaminopropanol for 1-2 hours (dimethylaminoethanol). Aminoethanol and diethylaminopropanol were added to the formaldehyde solution in advance), and the reaction was continued at 55°C for 3 hours to obtain a light yellow transparent liquid. Determination of active gr...

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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-iron finishing agent in the field of textile functional finishing, more particularly to a preparation method of dimethylol dihydroxyethylene urea. technical background [0002] Cotton fabrics are favored by people because of their softness, comfort, breathability, and good hygroscopicity, but they have the disadvantage of being easy to shrink and wrinkle. Resin finishing of cotton fabric can achieve the effect of anti-shrinkage and anti-wrinkle. At present, the commonly used resin finishing agents are divided into two categories: low-formaldehyde finishing agents and aldehyde-free finishing agents. The formaldehyde-free finishing agent is safe and environmentally friendly, and conforms to the current development trend, but the cotton fabrics finished with it have low resilience, which is difficult to meet the requirements of shrinkage and wrinkle resistance of pure cotton fabrics, and th...

Claims

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Application Information

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Patent Type & Authority Applications(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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