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Preparation method for synthesizing p-dinitrobenzene from wet material

A technology for p-dinitrosobenzene and nitrosophenol is applied in the field of preparation of chemical raw material p-dinitrosobenzene, and can solve the problems of reduced rubber material quality, difficulty in removing by-products, dangerous use of raw materials, etc. The effect of low cost of raw materials, simple operation process and simplified process

Pending Publication Date: 2022-03-22
天元(杭州)新材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the embodiments of the present invention is to provide a method for synthesizing p-dinitrosobenzene with wet materials, which solves the problem of lower rubber material quality caused by difficult removal of by-products in the traditional technology, or complex synthesis process, high raw material cost, and low raw material quality. Potentially dangerous use of

Method used

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  • Preparation method for synthesizing p-dinitrobenzene from wet material
  • Preparation method for synthesizing p-dinitrobenzene from wet material
  • Preparation method for synthesizing p-dinitrobenzene from wet material

Examples

Experimental program
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Effect test

Embodiment 1

[0037] In the first step, add sodium nitrite (2.0mol, 137.99g) and sodium hydroxide (1.5mol, 60.12g) into 483mL of tap water, stir to dissolve them completely, then add phenol (1.0mol, 94.60g), and stir to dissolve Mixed solution 1 was obtained; concentrated sulfuric acid (3mol, 294.78g) was slowly added to 535mL ice water, stirred and diluted to obtain solution 2;

[0038] At an ambient temperature of 3°C, slowly (2 hours) drop solution 1 into solution 2, maintain the system temperature at 5°C, continue stirring for 2 hours after addition, filter and wash to obtain the intermediate p-nitrosophenol wet material;

[0039]In the second step, add hydroxylamine hydrochloride (2mol, 139.54g) into 109mL of tap water, stir and dissolve to obtain solution 3; at an ambient temperature of 42°C, add solution 3 (2 hours) dropwise to the intermediate p-nitrosophenol wet In the aqueous solution of the raw material, keep the temperature of the system at 40° C., continue to stir for 2 hours ...

Embodiment 2

[0044] In the first step, add sodium nitrite (1.0mol, 69.21g) and sodium hydroxide (1.5mol, 60.23g) into 483mL of tap water, stir to dissolve them completely, then add phenol (1.0mol, 94.52g), and stir to dissolve Mixed solution 1 was obtained; concentrated sulfuric acid (3mol, 294.03g) was slowly added to 535mL ice water, stirred and diluted to obtain solution 2;

[0045] At an ambient temperature of 3°C, slowly (2 hours) drop solution 1 into solution 2, maintain the system temperature at 5°C, continue stirring for 2 hours after addition, filter and wash to obtain the intermediate p-nitrosophenol wet material;

[0046] In the second step, add hydroxylamine hydrochloride (2mol, 139.02g) into 109mL tap water, stir and dissolve to obtain solution 3; at an ambient temperature of 42°C, add solution 3 (2 hours) dropwise to the intermediate p-nitrosophenol wet In the aqueous solution of the raw material, keep the system temperature at 40° C., continue to stir for 2 hours after the ...

Embodiment 3

[0052] In the first step, add sodium nitrite (2.0mol, 138.11g) and sodium hydroxide (1.0mol, 40.34g) into 483mL of tap water, stir to dissolve them completely, then add phenol (1.0mol, 94.42g), and stir to dissolve Mixed solution 1 was obtained; concentrated sulfuric acid (3mol, 294.12g) was slowly added to 535mL ice water, stirred and diluted to obtain solution 2;

[0053] At an ambient temperature of 3°C, slowly (2 hours) drop solution 1 into solution 2, maintain the system temperature at 5°C, continue stirring for 2 hours after addition, filter and wash to obtain the intermediate p-nitrosophenol wet material;

[0054] In the second step, add hydroxylamine hydrochloride (2mol, 139.24g) into 109mL of tap water, stir and dissolve to obtain solution 3; at an ambient temperature of 42°C, add solution 3 (2 hours) dropwise to the intermediate p-nitrosophenol wet In the aqueous solution of the raw material, keep the system temperature at 40° C., continue to stir for 2 hours after ...

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Abstract

The preparation method comprises the following steps: adding phenol into an aqueous solution of sodium nitrite and sodium hydroxide to prepare a mixed solution of sodium phenolate and sodium nitrite, dropwise adding the mixed solution into a sulfuric acid solution at a preset temperature, and carrying out stirring reaction, filtering and washing to prepare an intermediate p-nitrosophenol wet material; dropwise adding a hydroxylamine hydrochloride aqueous solution into the intermediate p-nitrosophenol wet material, stirring for reaction, filtering and washing to obtain a p-benzoquinone dioxime wet material; the preparation method comprises the following steps: dissolving a p-benzoquinone dioxime wet material in an aqueous solution of sodium hydroxide to obtain an alkaline p-benzoquinone dioxime solution, dropwise adding a dilute NaClO solution into the alkaline p-benzoquinone dioxime solution, stirring, reacting, filtering and washing to obtain a p-dinitrobenzene product. According to the method, the raw material cost is low, only water is involved as a reaction solvent in the whole process, the operation process is simple, a wet material intermediate does not need to be dried in the process, and the finally prepared p-dinitrosobenzene has excellent adhesive performance.

Description

technical field [0001] The invention belongs to the field of chemical raw material production, and in particular relates to a preparation method of chemical raw material p-dinitrosobenzene. Background technique [0002] P-dinitrosobenzene (1,4-dinitrosobenzene) is a vulcanizing agent with a brown powder or solid appearance. The alias of p-dinitrosobenzene is 1,4-p-dinitrosobenzene, with a molecular weight of 136.11 The melting point is 146.5°C and the density is 1.4175. It is mainly used for vulcanization and bonding of butyl rubber, natural rubber, styrene-butadiene rubber and other colloids. [0003] Rubber-metal composite parts combine the characteristics of rubber and metal, and have been widely used in automobile, machinery, national defense and other industries, and the firm bond between rubber and metal is the key to its reliability. With the advancement of science and technology and economic development, synthetic adhesives are increasingly replacing mechanical conn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/00C07C207/02C07C249/06C07C251/46C07C249/04C07C251/44C09J11/06
CPCC07C201/00C07C249/06C07C249/04C09J11/06C07C2601/16C08K5/32C07C207/02C07C251/46C07C251/44
Inventor 齐永新梁玉飞胡盼徐慧慧史哲肖丁元朱月吕德斌周正勇
Owner 天元(杭州)新材料科技有限公司
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