Preparation method of di-tert-butyl peroxide

A technology of di-tert-butyl peroxide and hydrogen peroxide, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc. low problems, to save raw materials, simplify operations, and provide production profits.

Inactive Publication Date: 2021-03-19
宁夏顺邦达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing production process route is long, the production cost is high, the reaction time is long, and the oxide yield is low
Moreover, the waste liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Using sulfuric acid and hydrogen peroxide as raw materials, put the hydrogen peroxide and sulfuric acid into the reactor, the mass ratio of the sulfuric acid to the hydrogen peroxide is 1:1.5, the mass % specific concentration of the sulfuric acid is 75, and the mass % of the hydrogen peroxide The specific concentration is 27, fully mixed under the condition of ice bath, and the temperature of the ice bath is maintained at 2 ~ -8 ° C to prepare the mixed solution, and continue to stir for 30 minutes;

[0022] Step 2: After vigorously stirring the mixed solution in step 1, add tert-butanol dropwise, and control the rate of addition to ensure that the reaction temperature does not exceed 5°C. The time for adding tert-butanol in step 2 is 90 minutes;

[0023] Step 3: after the dropwise addition, naturally rise to room temperature, and continue to stir for 4 hours to obtain a reaction crude product solution;

[0024] Step 4: Stand still, the step 4 is left to stand ...

Embodiment 2

[0027] Step 1: Using sulfuric acid and hydrogen peroxide as raw materials, put the hydrogen peroxide and sulfuric acid into the reactor, the mass ratio of the sulfuric acid to the hydrogen peroxide is 1:2, the mass % specific concentration of the sulfuric acid is 82, and the mass % of the hydrogen peroxide The specific concentration is 35, fully mixed under the condition of ice bath, and the temperature of the ice bath is maintained at 2 ~ -8 ° C to prepare a mixed solution, which is continuously stirred for 30 minutes;

[0028] Step 2: After vigorously stirring the mixed solution in step 1, add tert-butanol dropwise, and control the rate of addition to ensure that the reaction temperature does not exceed 5°C. The time for adding tert-butanol in step 2 is 90 minutes;

[0029] Step 3: after the dropwise addition, naturally rise to room temperature, and continue to stir for 4 hours to obtain a reaction crude product solution;

[0030] Step 4: Stand still. After standing still fo...

Embodiment 3

[0033] Step 1: Using sulfuric acid and hydrogen peroxide as raw materials, put the hydrogen peroxide and sulfuric acid into the reactor, the mass ratio of the sulfuric acid to the hydrogen peroxide is 1:3, the mass % specific concentration of the sulfuric acid is 90, and the mass % of the hydrogen peroxide The specific concentration is 45, fully mixed under the condition of ice bath, and the temperature of the ice bath is maintained at 2 ~ -8 ° C to prepare the mixed solution, and continue to stir for 30 minutes;

[0034] Step 2: After vigorously stirring the mixed solution in step 1, add tert-butanol dropwise, and control the rate of addition to ensure that the reaction temperature does not exceed 5°C. The time for adding tert-butanol in step 2 is 90 minutes;

[0035] Step 3: after the dropwise addition, naturally rise to room temperature, and continue to stir for 4 hours to obtain a reaction crude product solution;

[0036] Step 4: Stand still, the step 4 is left to stand fo...

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PUM

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Abstract

The invention discloses a preparation method of di-tert-butyl peroxide. The preparation method comprises the following steps of: adding hydrogen peroxide and sulfuric acid into a reaction kettle, sufficiently mixing the hydrogen peroxide and the sulfuric acid under an ice bath condition to obtain a mixed solution, and continuously stirring the mixed solution for 30 minutes; dropwise adding tert-butyl alcohol after violently stirring the mixed solution, controlling the dropwise adding speed, and ensuring that the reaction temperature does not exceed 5 DEG C; after dropwise adding the tert-butylalcohol, naturally heating the solution to room temperature, and continuously stirring the solution for 4 hours to obtain a reaction crude product solution; and making the solution stand still, introducing the solution into a liquid separation tank for liquid separation to obtain an upper-layer organic phase, washing the organic phase with a 30% NaOH solution, washing the organic phase with water, and drying the organic phase with anhydrous MgSO4 to obtain stimulated colorless liquid which is di-tert-butyl peroxide. The preparation method has the advantages of simplified operation, higher yield, shortened reaction time, effectively controlled reverse reaction decomposition and raw material-saving performance/ Waste gas mother liquor is recycled, so that raw materials are saved, the production cost is reduced; and the discharge of the waste liquor is reduced, the subsequent treatment cost is saved, and the environmental protection is achieved; and the sustainable development is realized, and the production profits of enterprises are greatly improved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of di-tert-butyl peroxide. Background technique [0002] Di-t-butyl peroxide, also known as di-t-butyl peroxide, initiator a, vulcanizing agent dTBP, is a colorless to light yellow transparent liquid, insoluble in water, and benzene, Miscible with organic solvents such as toluene and acetone. It is highly oxidizing, flammable, relatively stable at room temperature, and insensitive to impact. It is widely used as initiator and crosslinking agent in the field of polymer chemistry. With the development and application of fine chemical products, it is also used as a bleaching agent for grease and food, an additive for diesel oil and lubricating oil, a crosslinking agent for unsaturated polyester and silicone rubber, and a pour point depressant for transformers. [0003] The synthesis methods of di-tert-butyl include: base-catalyzed synthesis method,...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/16
CPCC07C407/00C07C409/16
Inventor 朱国成李振伟刘振余刘洋
Owner 宁夏顺邦达新材料有限公司
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