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Ureido-ethane sulfinate and preparation method thereof

A technology for ureidoethane sulfinate and dithionite, which is applied in the field of ureidoethane sulfinate and its preparation, can solve problems such as yield reduction, achieve mild reaction, simple production process, The effect of short production cycle

Active Publication Date: 2012-01-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Filby et al. used thiols to oxidize sulfinates by weak oxidants at lower temperatures. However, Marvel et al. pointed out that when thiols were in excess, sulfinates could react with thiols to form disulfides, which reduced the yield.

Method used

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  • Ureido-ethane sulfinate and preparation method thereof
  • Ureido-ethane sulfinate and preparation method thereof
  • Ureido-ethane sulfinate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Specific steps are as follows:

[0028] Raw materials and formula (unit-kg):

[0029] Sodium dithionite: 40.5 kg

[0030] Glyoxal (40% content): 33.7 kg

[0031] Urea: 13kg

[0032] Sodium hydroxide: 0.8 kg

[0033] Ethylene glycol: 0.4 kg

[0034] H 2 O: 11.6 kg.

[0035] Process steps and process parameters: slowly add glyoxal into a reactor containing ethylene glycol, sodium dithionite, 0.7 kg of sodium hydroxide and water, control the temperature below 10°C, stir at a rotational speed of 50r / min, and complete the feeding Then the temperature was raised to 15°C, urea and 0.1 kg of sodium hydroxide were added after the reaction for 30min, the temperature was raised to 50°C after the addition of the materials, and after the reaction for 35min, the white ureidoethane with a purity of 86% was obtained by vacuum drying. Sodium sulfinate powder. At 25℃: under the condition of 5.0g / L reducing agent, its reduction potential is -14mV; under the condition of 5.0g / L red...

Embodiment 2

[0037] Specific steps are as follows:

[0038] Raw materials and formula (unit-kg):

[0039] Zinc dithionite: 43 kg

[0040] Glyoxal (40% content): 29.5 kg

[0041] Urea: 12.2 kg

[0042] Sodium carbonate: 1.9 kg

[0043] Propylene Glycol: 0.2 kg

[0044] H 2 O: 13.2 kg.

[0045] Process steps and process parameters: slowly add glyoxal into the reactor containing propylene glycol, zinc dithionite, 1.5 kg of sodium carbonate and water, control the temperature below 10°C, stir at a rotational speed of 200r / min, and complete the feeding Then the temperature will be raised to 20°C, urea and 0.4 kg of sodium carbonate will be added after the reaction for 50min, and the temperature will be raised to 55°C after the addition of the material. After 60min of reaction, vacuum-dried to obtain white ureidoethane with a purity of 88%. Zinc sulfinate powder. At 25℃: under the condition of 5.0g / L reducing agent, its reduction potential is -13mV; under the condition of 5.0g / L reducing ...

Embodiment 3

[0047] Specific steps are as follows:

[0048] Raw materials and formula (unit-kg):

[0049] Potassium hydrosulfite: 36.5 kg

[0050] Glyoxal (40% content): 29.7 kg

[0051] Urea: 13.5 kg

[0052] Potassium carbonate: 2.2 kg

[0053] Butanediol: 0.3 kg

[0054] H 2 O: 17.8 kg.

[0055] Process steps and process parameters: slowly add glyoxal into a reactor containing butanediol, potassium dithionite, 1.9 kg of potassium carbonate and water, control the temperature to be below 10 °C, stir at a rotational speed of 65 r / min, and feed After the completion, the temperature was raised to 25°C, and urea and 0.3 kg of potassium carbonate were added after the reaction for 60min. After adding the material, the temperature was raised to 60°C. After the reaction for 70min, the white ureidoethane with a purity of 86% was obtained by vacuum drying. Potassium sulfinate powder. At 25℃: under the condition of 5.0g / L reducing agent, its reduction potential is -18mV; under the condition of...

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Abstract

The invention provides a ureido-ethane sulfinate and a preparation method thereof, wherein the ureido-ethane sulfinate is white powder and has good chemical stability; and the preparation method comprises the following steps: hyposulphite is used for reacting with oxalic aldehyde and carbamide in alkaline condition to synthesize the ureido-ethane sulfinate. The product of the invention does not generate hazardous and noxious sulfur dioxide, formaldehyde or hydrogen sulphide gas at high temperature and in alkaline condition, and simultaneously has very high negative reduction potential; the chemical property of the prepared product is similar to that of formaldehydesulfoxylate as far as possible; and the product solves the problem of the existing reducing agents such as rongalite C and rongalite that sulfur dioxide, formaldehyde and other hazardous and noxious gases are released at high temperature and in alkaline condition.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and particularly relates to a ureidoethane sulfinate and a preparation method thereof. Background technique [0002] In the chemical and printing and dyeing industries, the reducing agent is a chemical auxiliary with a large amount and a wide range of applications. At present, the reducing agents used at home and abroad mainly include hydrosulfite, sodium sulfide, white powder and thiourea dioxide. However, the hydrosulfite will spontaneously ignite, especially after it absorbs moisture, it will naturally heat up and burn, and the storage stability is very poor. Sodium sulfide is used as a reducing agent to discharge sulfides in wastewater that exceed the standard and are difficult to biodegrade; while in practical applications, thiourea dioxide is difficult to control its reducibility, which will lead to excessive reduction of some dyes, which will affect the color fastness in the light, and produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C313/04
Inventor 刘明华刘剑锋蒋晓丽
Owner FUZHOU UNIV