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Treatment method for oxidizing M-Na through hydrogen peroxide to pass through end point

A treatment method, the technology of hydrogen peroxide, applied in the direction of organic chemistry, etc., can solve the problems of reduced product yield purity, unqualified quality, waste of raw materials, etc., and achieve the effect of improving purity, low cost, and easy operation

Inactive Publication Date: 2020-04-21
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Indeed, in the normal production process, overoxidation will inevitably occur during operation, resulting in a decrease in the purity of the product yield, unqualified quality, and waste of raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Prepare 300ml of 6% M-Na solution in a 500ml three-necked flask, heat up to 35℃ and add dropwise a compound oxidant mixed with hydrogen peroxide and sulfuric acid while stirring. The molar ratio of hydrogen peroxide to sulfuric acid is 1.1:1, and the dropping rate is 3s. / Drop, drip until the PH value is below 6, the end point of the detection with cobalt oleate is green, and the end point of the detection is green, indicating that the end has been passed. If the post-processing is directly carried out, the purity and quality of the product will be seriously reduced.

[0027] Add 32% sodium hydroxide solution to the above-mentioned reaction solution that has passed the end point, adjust the pH of the solution to 8, then continue to add dropwise a compound oxidant mixed with hydrogen peroxide and sulfuric acid, adjust pH=6, and stir for 15 minutes The end point of detection with cobalt oleate was pink, and the finished DM was obtained by dehydration, washing and drying. The ...

Embodiment 2

[0029] Prepare 300ml of 8% M-Na solution in a 500ml three-necked flask, heat up to 42℃ and add dropwise a compound oxidant mixed with hydrogen peroxide and sulfuric acid while stirring. The molar ratio of hydrogen peroxide to sulfuric acid is 1.2:1, and the dropping rate is 2s. / Drop, drip until the PH value is below 6, use cobalt oleate to detect the end point of green, the test end of green indicates that the end has been passed, if the post-processing directly will cause serious product purity and quality degradation.

[0030] Add a 32% mass fraction of sodium hydroxide solution to the above-mentioned reaction solution that has passed the end point, adjust the pH of the solution to 8.5, and continue to add dropwise a compound oxidant mixed with hydrogen peroxide and sulfuric acid, adjust the pH=6.5, and stir for 15 minutes The end point of cobalt oleate detection was pink, and the finished product DM was obtained by dehydration, washing and drying. The yield of the finished pro...

Embodiment 3

[0033] Prepare 300ml of 10% M-Na solution in a 500ml three-necked flask, heat up to 50℃ and add dropwise a compound oxidant mixed with hydrogen peroxide and sulfuric acid while stirring. The molar ratio of hydrogen peroxide to sulfuric acid is 1.3:1, and the dropping rate is 1s. / Drop, drip until the PH value is below 6, the end point of the detection with cobalt oleate is green, and the end of the detection is green, indicating that the end has been passed. If the post-processing is directly carried out, the purity and quality of the product will be seriously reduced.

[0034] Add 32% sodium hydroxide solution to the above-mentioned reaction solution that has passed the end point, adjust the pH of the solution to 7, and stir for 15 minutes. Use cobalt oleate to detect that the end point is pink. Start dehydration, washing, and drying. The finished product DM has a yield of 97.8% and an initial melting point of 169.5°C by visual inspection.

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Abstract

The invention discloses a treatment method for oxidizing M-Na through hydrogen peroxide to pass through an end point, and belongs to the technical field of rubber accelerator production. The treatmentmethod comprises the following steps: dropwise adding alkali liquor into a reaction solution passing through an end point, adjusting the pH value of the solution to be greater than or equal to 8, then dropwise adding a mixed compound oxidant of hydrogen peroxide and sulfuric acid, adjusting the pH value of the solution to be 6-7, stirring the solution for 10 to 20 minutes, taking a product DM sample, detecting an end point by using cobalt oleate, wherein the color is pink at the end point, and dehydrating, washing and drying the product to obtain a finished product DM. The method is simple, convenient to operate and low in cost, the phenomenon that hydrogen peroxide oxidizes M-Na to pass through the end point is effectively treated, the purity and quality of the product can be remarkablyimproved, waste of raw materials is reduced, and remarkable economic benefits are achieved. Industrialization can be realized, and the bottleneck of hydrogen peroxide process development is thoroughlysolved.

Description

Technical field [0001] The invention relates to the technical field of rubber accelerator production, in particular to a treatment method for the end-point of the hydrogen peroxide oxidation of M-Na. Background technique [0002] At present, the main production processes for the production of rubber vulcanization accelerator DM at home and abroad are sodium nitrite method, oxygen oxidation method and hydrogen peroxide method. [0003] Although the cost of sodium nitrite method is low, but the quality is low, the nitrogen oxide produced is difficult to control, pollutes the environment, and is facing the situation of elimination. [0004] Although the oxygen oxidation method is an environmentally friendly process, it has a high cost, strict requirements on equipment, and high safety risks. [0005] Oxidation is carried out with a compound oxidant mixed with hydrogen peroxide and sulfuric acid, which is a clean and environmentally friendly process, and the yield and quality are both sat...

Claims

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Application Information

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IPC IPC(8): C07D277/78
CPCC07D277/78
Inventor 方雪山周福朋李硕郭焕宇齐步金唐士通
Owner SHANDONG SUNSINE CHEM