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3-(N-nitroso-N-phenyl hydroxylamine) aluminum salt preparation method

A phenylhydroxylamine ammonium salt, nitroso technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry and other directions, can solve problems such as no literature reports in industrialized preparation

Active Publication Date: 2010-05-12
INSIGHT HIGH TECH (BEIJING) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been described as a complex analysis product in analytical chemistry for a long time, but its industrial preparation as a polymerization inhibitor has not been reported in the literature

Method used

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  • 3-(N-nitroso-N-phenyl hydroxylamine) aluminum salt preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 42.0 grams (0.11 moles) of aluminum nitrate nonahydrate, dissolve it in 600 milliliters of water, put it into a 2000 milliliter reaction bottle, add 200 milliliters of methanol, and keep the solution temperature at 22-25 ° C. Weigh another 50.0 grams (0.32 moles) Dissolve N-nitroso-N-phenylhydroxylamine ammonium salt in 450 ml of water, add it dropwise to the reaction bottle for 1 hour, and soon a white precipitate will precipitate out. After the dropwise addition, raise the temperature of the reaction solution to 50-60°C , and 100 milliliters of sodium dihydrogen phosphate-disodium hydrogen phosphate buffer solution (pH value 6.8) was added dropwise at a concentration of 3.5%, and the pH value was stabilized between 5.5 and 5.7, and stirred for 2 hours. Then the temperature was cooled to room temperature, and the solid was suction filtered. The filter cake was washed with 100 ml of water to obtain an off-white solid, which was dried in an oven at 100°C for 2 hours...

Embodiment 2

[0022] Weigh 42.0 g (0.11 moles) of aluminum nitrate nonahydrate, dissolve it in 600 ml of water, put it into a 2000 ml reaction flask, add 200 ml of methanol, and keep the solution temperature at 22-25°C. Another 50.0 g (0.32 mol) of N-nitroso-N-phenylhydroxylamine ammonium salt was weighed and dissolved in 450 ml of water, and added dropwise into the reaction flask over 1 hour, and a white precipitate precipitated out soon. After the dropwise addition, raise the temperature of the reaction solution to 50-60° C., and add 100 ml of 3.5% concentration of acetic acid-sodium acetate buffer solution (pH 6.8) dropwise, the pH value is stabilized at 5.5-5.7, and stir for 2 hours. Then the temperature was lowered to room temperature, the solid was filtered with suction, and the filter cake was washed with 100 ml of water to obtain an off-white solid, which was dried in an oven at 100° C. for 2 hours to yield 42.1 g, with a yield of 89.5%. The melting point of the product is 167-169°C...

Embodiment 3

[0026] Polymerization inhibition effect test

[0027] Test formula table one

[0028] Test procedure: Prepare a certain amount of samples according to the formula, and test the fluidity D under the condition of 20±1°C 0 , put the sample in a dark box and put it in an oven at 80°C. Test the fluidity D of the placed sample at 20±1°C t .

[0029] Fluidity rate of change = (D 0 -D t ) / D 0 *100%

[0030] The influence of the polymerization inhibitor on the thermal storage stability is measured by the rate of change of fluidity, the greater the rate of change, the more unstable it is.

[0031] See GB / T14624.3-93 for fluidity test method. Table I

[0032] name

[0033] name

[0034] test results

[0035] Table II

[0036] Thermal storage time

[0037]As can be seen from the results shown in Table 2: the addition of a polymerization inhibitor in the black ink has a significant promotion effect on the stability of the formula, and after 72 hours...

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Abstract

The present invention relates to a preparation method of tri-(N-nitroso - N-phenyl hydroxylamine) aluminum salt as shown in formula (1). In the method, aluminum nitrate and N-nitroso-N-phenyl hydroxylamine ammonium salt are used for the decomposition reaction in the mixed solvent of alcohol; the buffer solution is used for controlling the pH value of the reaction solution to be 5.5 to 5.7; the compound of formula (1) can be prepared at a high collection rate.

Description

technical field [0001] The present invention relates to a method for preparing tris(N-nitroso-N-phenylhydroxylamine) aluminum salt. Background technique [0002] The tris(N-nitroso-N-phenylhydroxylamine) aluminum salt is one of the important assistants for the storage stability of the UV-curable ink composition. Japanese patent publication JP86-103150A describes its use effect: the stability of the formulation at a temperature of 80-90°C can meet the requirements of the product use process and viscosity performance, and the formulation of hydroquinone monomethyl ether as a reference product was prepared and used in the same way. Conditions will cloud and gel. Tris(N-nitroso-N-phenylhydroxylamine) aluminum salt can accept a little free radicals generated by free radical photoinitiators due to heat, light and other reasons, thereby preventing the initiation of acrylate monomer polymerization and gelation It can effectively prolong the shelf life of ink products. It has been...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C243/04C07C241/00
Inventor 罗鹏赵文超闫庆金邵俊峰
Owner INSIGHT HIGH TECH (BEIJING) CO LTD
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