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Process for preparing stilbene-based compound

A technology of stilbene and dinitrostilbene, which is applied in the field of preparation of stilbene compounds, can solve problems such as environmental pollution, achieve the effects of reducing preparation time and cost, and shortening oxidation reaction time

Inactive Publication Date: 2017-05-17
IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the use of transition metals as catalysts can increase the conversion rate, the selectivity is only maintained between 60-80%, and waste liquid containing heavy metals will be generated, causing environmental pollution

Method used

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  • Process for preparing stilbene-based compound
  • Process for preparing stilbene-based compound
  • Process for preparing stilbene-based compound

Examples

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preparation example Construction

[0019] The invention provides a preparation method of stilbene compound, by controlling alkali metal hydroxide, water, organic solvent, and p-nitrotoluene-2-sulfonic acid (p-nitrotoluene-2-sulfonic acid, NTS) (or Salts) in a specific range of ratios can shorten the oxidation reaction time (can be completed in about 30 minutes) and promote the stilbene High reaction conversion and selectivity (both reaction conversion and selectivity can reach more than 90%). In this way, in addition to greatly reducing the preparation time and cost of the stilbene compound, the amount of waste liquid produced in the preparation of the stilbene compound can be reduced and heavy metal pollution can be avoided.

[0020] According to an embodiment of the present invention, the present invention provides a method for preparing a stilbene compound, for example, a method for preparing a stilbene compound having a structure represented by formula (I)

[0021]

[0022] where M 1 Can be H, Na, or K...

Embodiment 1

[0038] Add 567 parts by weight of dimethyl sulfoxide (dimethyl sulfoxide, DMSO) into a reaction flask, then add 100 parts by weight of p-nitrotoluene-2-sulfonic acid (p-nitrotoluene-2-sulfonic acid, NTS) (solid) Add it into the reaction bottle and stir until the p-nitrotoluene-o-sulfonic acid is completely dissolved, and prepare the first solution with a weight concentration of 15 wt%. Then, the above solution was poured into the oxidation tank, and at the same time, the air was introduced (flow rate was about 250mL / min). Next, take another reaction bottle, add 14 parts by weight of water, and then add 19 parts by weight of sodium hydroxide (NaOH) into the water and stir until the sodium hydroxide is completely dissolved to prepare a second solution with a weight concentration of 57 wt%.

[0039] Then, the second solution was added during the high-speed stirring of the first solution (the second solution was added dropwise and completely added within 5 minutes), and the first ...

Embodiment 2

[0041] Add 567 parts by weight of dimethyl sulfoxide (DMSO) into a reaction flask, then add 100 parts by weight of p-nitrotoluene sulfonic acid (NTS) (solid) into the reaction flask and stir until p-nitrotoluene ortho The sulfonic acid is completely dissolved and prepared into a first solution with a weight concentration of 15wt%. Next, pour the above solution into the oxidation tank. Next, take another reaction bottle, add 33 parts by weight of water, then add 22 parts by weight of sodium hydroxide (NaOH) into water and stir until the sodium hydroxide is completely dissolved, and prepare a second solution with a weight concentration of about 40 wt%.

[0042] Then, the first solution was evenly stirred with an emulsifying homogenizer (homogenizer), and at the same time, air (flow rate was about 400mL / min) and the second solution (the second solution was added dropwise and added completely within 5 minutes), And fully mix the first solution and the second solution. After reac...

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Abstract

A process for preparing a stilbene-based compound is provided. The structure of the stilbene-based compound is shown as a formula (I), wherein M1 is H, Na or K. The process includes steps of subjecting a first solution to mixing treatment, feeding air into the first solution, mixing a second solution with the first solution in the mixing treatment step, and performing oxidation to obtain a third solution containing the stilbene-based compound shown as the formula (I), wherein the first solution comprises a compound shown as a formula (II) and a compound shown as a formula (III) in which R1 and R2 are C1-C4 alkyl independently, and M2 is H, Na or K, and the second solution comprises water and an alkaline metal hydroxide. The process can shorten oxidation reaction time in a case that oxygen is adopted as an oxidant and no heavy metal catalyst or phase transfer catalyst is added, and increases the reaction conversion rate and selectivity of the stilbene-based compound.

Description

technical field [0001] The present invention relates to a preparation method of stilbene compound, more particularly to a preparation method of 4,4'-dinitrostilbene-2,2'disulfonic acid or its salts. Background technique [0002] 4,4'-diaminostilbene-2,2'-disulfonic acid (4,4'-diaminostilbene-2,2'-disulfonic acid, DSD) is a key raw material for optical brighteners for paper, and can also be used in many Production of non-toxic dyes. [0003] 4,4'-Dinitrostilbene-2,2'disulfonic acid (4,4'-dinitrostilbene-2,2'-disulfonic acid, DNS) is 4,4'-diaminostilbene-2 , an important intermediate in the production of 2'disulfonic acid. 4,4'-Dinitrostilbene-2,2'disulfonic acid can be prepared by oxidation of p-nitrotoluene sulfonic acid (NTS). At present, the oxidants used in the industry to oxidize p-nitrotoluene orthosulfonic acid to 4,4'-dinitrostilbene-2,2'disulfonic acid can be divided into bleach water (hypochlorous acid), chlorine gas, and air . Although the use of hypochlorous ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/40C07C303/22C07C303/32
CPCC07C303/22C07C303/32C07C309/40
Inventor 张雅茹叶国良张学明
Owner IND TECH RES INST