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Preparation method for allantoin derivative imidazolidinyl urea

A technology for producing imidazolidinyl urea and allantoin is applied in the field of preparation of allantoin derivative imidazolidinyl urea, and can solve problems such as unsatisfactory catalytic effect and the like

Inactive Publication Date: 2018-12-18
茆振斌
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of imidazolidinyl urea mainly includes dichloroacetic acid method, trichloroacetaldehyde method, cisbutanol ozonation method, oxalic acid electrolytic reduction method, and acetaldehyde oxidation method; and hydroxymethylation reactions, cyclization reactions and hydroxymethylation reactions need to be catalyzed by catalysts, but the existing catalysts generally have the defect of unsatisfactory catalytic effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0014] The invention provides a preparation method of allantoin derivative imidazolidinyl urea, comprising:

[0015] 1) Ultrasonic vibration of cobalt salt, soluble molybdate, nano-zinc oxide, urea, and starch in water to form a mixed system;

[0016] 2) The mixed system is subjected to a hydrothermal reaction, then filtered and dried to obtain a hydrothermal product;

[0017] 3) Calcining the hydrothermal product in the presence of protective gas to prepare the composite;

[0018] 4) Hydrolyze chloral, aluminum salt of N-nitrosobenzene, and water, then add urea, boric acid, and the compound to the system for cyclization reaction, and finally add acetaldehyde to the system for methylol Kylation reaction.

[0019] In step 1) of the present invention, the amount of each material can be selected within a wide range, but in order to further improve the yield of the preparation method, preferably, in step 1), cobalt salt, soluble molybdate, nano oxide The dosage ratio of zinc, u...

Embodiment 1

[0031] 1) Mix cobalt salt (cobalt stearate), soluble molybdate (sodium molybdate), nano zinc oxide (average particle size 20nm), urea, starch, water according to 1mmol: 1.1mmol: 0.09mmol: 2.5mmol: 70mg: 200mL dosage ratio for ultrasonic oscillation (ultrasonic frequency 25KHz, oscillation time 35min) to form a mixed system;

[0032] 2) The mixed system is subjected to hydrothermal reaction in a reactor (reaction temperature is 170°C, reaction time is 9h), then filtered and dried (drying temperature is 105°C, drying time is 5h) to obtain a hydrothermal product;

[0033] 3) In the presence of protective gas, the hydrothermal product was first incubated at 210°C for 1.5h, then heated to 290°C at a rate of 1°C / h and held for 1.5h, and finally cooled naturally to obtain complex A1.

Embodiment 2

[0035] 1) Mix cobalt salt (cobalt dichloride), soluble molybdate (ammonium molybdate), nano-zinc oxide (average particle size 20nm), urea, starch, water according to 1mmol: 1mmol: 0.05mmol: 2mmol: 50mg: 150mL volume ratio for ultrasonic vibration (ultrasonic frequency 20KHz, vibration time 40min) to form a mixed system;

[0036] 2) The mixed system is subjected to hydrothermal reaction in a reactor (reaction temperature is 160°C, reaction time is 10h), then filtered and dried (drying temperature is 100°C, drying time is 6h) to obtain a hydrothermal product;

[0037] 3) In the presence of protective gas, the hydrothermal product was first incubated at 200°C for 2h, then heated to 280°C at a rate of 0.8°C / h and held for 2h, and finally cooled naturally to obtain complex A2.

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Abstract

The invention discloses a preparation method for an allantoin derivative, i.e., imidazolidinyl urea. The preparation method comprises the following steps: 1) ultrasonically oscillating a cobalt salt,soluble molybdate, nanometer zinc oxide, urea and starch in water to form a mixed system; 2) subjecting the mixed system to a hydrothermal reaction, and carrying out filtration and drying so as to obtain a hydrothermal product; 3) calcining the hydrothermal product in the presence of protective gas to obtain a compound; and 4) hydrolyzing trichloroacetaldehyde, aluminum N-nitrosophenylhydroxylamine and water, then adding urea, boric acid and the compound into the system for a cyclization reaction, and finally adding acetaldehyde into the system for a hydroxymethylation reaction. The preparation method can realize high-yield preparation of the allantoin derivative imidazolidinyl urea.

Description

technical field [0001] The invention relates to a catalyst, in particular to a method for preparing an allantoin derivative imidazolidinyl urea. Background technique [0002] Imidazolidinyl urea is an allantoin derivative, which can be used in creams, shampoos, lotions, conditioners and other products. It can be used alone or in combination with parabens and IPBC to enhance its antiseptic effect. [0003] At present, the preparation of imidazolidinyl urea mainly includes dichloroacetic acid method, trichloroacetaldehyde method, cisbutanol ozonation method, oxalic acid electrolytic reduction method, and acetaldehyde oxidation method; The cyclization reaction and methylolation reaction need to be catalyzed by catalysts, but the existing catalysts generally have the defect of unsatisfactory catalytic effect. Contents of the invention [0004] The purpose of the present invention is to provide a preparation method of allantoin derivative imidazolidinyl urea, which can prepare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/88
CPCC07D233/88
Inventor 茆振斌
Owner 茆振斌