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Peroxidized t-butyl perbenzoate production process
CN1763001A
China
Description
translated from
Technical Field
The invention relates to a production process of tert-butyl peroxybenzoate, belonging to the field of organic chemical industry.
Background
The traditional tert-butyl peroxybenzoate product in the current market is also named tert-butyl peroxybenzoate, which is abbreviated as: TBPB or CP-02, Properties: the colorless transparent liquid has aromatic flavor, melting point of 8.8C, boiling point of 124C, relative density of 1.043 and refractive index of 1.495-1.499(20C), is insoluble in water, soluble in common organic solvent, can be decomposed in water, is stable at room temperature, and has no corrosion to steel and aluminum. The application is as follows: used as organic synthetic raw material, and can be used as polymerization initiator of high-pressure polyethylene, polystyrene and polypropylene, etc., and rubber vulcanizing agent and drying accelerator of mixed paint. Because the raw material input amount of the original production process of the product is large, the yield of the finished product is low, and the impurities are increased due to more byproducts, such as tert-butyl hydroperoxide and di-tert-butyl hydroperoxide, and the product also contains a certain amount of iron ions, for example, the color of the product is changed when the product is placed at room temperature for no more than 15 days, so that the stability of the product quality is influenced.
Disclosure of Invention
The invention aims to provide a tert-butyl peroxybenzoate production process for ensuring stable product quality aiming at the quality condition.
In order to solve the existing technical problems, the specific technical scheme of the invention is as follows: a production process of tert-butyl peroxybenzoate comprises the following operation processes:
firstly, preparing acid: 71.4% by weight of 98% concentrated sulfuric acid; water 28.6 wt%.
Firstly, putting 98% concentrated sulfuric acid into a reaction kettle, then adding water under the cooling condition to ensure that the temperature is not higher than 80 ℃, and dripping for 60 minutes, wherein the speed is first high and then low, and the speed is determined according to the temperature. After the dropwise addition, the mixture was cooled to room temperature. 70 percent dilute sulfuric acid is obtained for standby.
Secondly, esterification: 30.6-35 wt% of tert-butyl alcohol; 70% dilute sulfuric acid 65-69.4 wt%.
Putting the tert-butyl alcohol into a reaction kettle, dripping 70% dilute sulfuric acid into the reaction kettle, pumping the frozen brine into an interlayer of the reaction kettle for circulating circulation of a circulating pump, and controlling the temperature of the frozen brine to be between 30 and 34 ℃. And (4) obtaining the esterified liquid for later use after the dripping is finished.
Thirdly, synthesis: 31.4 to 37.8 weight percent of 27.5 percent of hydrogen peroxide; 62.2 to 68.6 weight percent of esterification liquid.
Adding 27.5% hydrogen peroxide into the reaction kettle, adding the esterification solution dropwise, and controlling the temperature to be 34-38 deg.C with frozen saline water. Stirring for 30 minutes after the dropwise addition is finished, standing for 10 hours, and then removing lower layer diluted acid to obtain crude tert-butyl, namely crude tert-butyl hydroperoxide for later use.
Esterification liquid hydrogen peroxide crude tert-butyl hydroperoxide di-tert-butyl hydroperoxide water
Fourthly, preparing sodium salt: 25.8-26.8 wt% of 30% liquid alkali; coarse tertiary 20.7-23.7 wt%; 50.5-52.5 wt% of water.
Firstly, 30 percent of liquid caustic soda is put into a reaction kettle filled with water, the temperature of the reaction kettle is controlled by utilizing frozen saline water, all the crude caustic soda is dripped into the reaction kettle, and the temperature is controlled between 15 ℃ and 20 ℃. Stirringfor 30 minutes after the dripping is finished, standing for 1 hour, wherein the lower layer is sodium salt, and the upper layer is a byproduct, namely water.
Crude tertiary liquid alkali sodium salt water
And V, condensation: 77.2-80 wt% of sodium salt; 20-22.8 wt% of benzoyl chloride.
Adding benzoyl chloride into a reaction kettle, cooling by using frozen saline, adding sodium salt dropwise at a temperature below 20 ℃, keeping the temperature for 1 hour at a temperature of between 15 and 20 ℃ after dropwise adding, standing for 1 hour, and then layering, wherein the upper layer is a crude product, and the lower layer is waste liquid.
Sodium salt benzoyl chloride crude sodium chloride
Sixth, washing and drying: 14.6-15% by weight of 30% liquid alkali; 78-80 wt% of water; 5-7.3 wt% of anhydrous sodium sulfate.
Respectively adding 30% liquid caustic soda and water into the reaction kettle, adding all the crude products, stirring for 20 minutes, and standing for 1 hour to remove lower-layer waste liquid. Washing with water for 2-3 times, removing upper layer wastewater, and adding anhydrous sodium sulfate (Na)2SO4) Stirring for 30 minutes and then carrying out suction filtration to obtain a finished product.
The chemical equipment is from Suzhou chemical equipment supply and marketing company; the chemical raw materials are from Suzhou chemical raw materials Co.
The invention has the advantages that:
1. the sodium salt is dripped into the benzoyl chloride, so that the temperature can be effectively controlled, the conversion rate of the main product is improved, the yield of the main product is increased, and the product quality is improved. The prior traditional process is to drop benzoyl chloride into sodium salt,generally, the cooling is not easy, and the temperature cannot be effectively controlled.
| Product unit | Appearance of the product | TBPB content% |
| Haoda plastification Co Ltd of Xuanxing City | Colorless or yellowish transparent liquid | 98 |
| The invention | Colorless or yellowish transparent liquid | 98.2 |
2. And the repeated cleaning is also a factor for reducing impurities and ensuring the quality.
Detailed Description
The first embodiment is as follows:
a production process of tert-butyl peroxybenzoate comprises the following operation processes:
firstly, preparing acid: 324 kg of 98% concentrated sulfuric acid is firstly put into a 1 ton acid-resistant reaction kettle, 130 kg of water is then added under the cooling condition, the temperature is not higher than 80 ℃, the dripping time is 60 minutes, and the mixture is cooled to the room temperature after the dripping is finished. 454 kg of dilute acid is obtained for standby.
Secondly, esterification: 200 kg of tert-butyl alcohol is put into a 1 ton esterification reaction kettle, 454 kg of the diluted acid is added dropwise, the frozen brine is injected into the interlayer of the reaction kettle for circulating circulation of a circulating pump, and the temperature of the frozen brine is controlled to be between 30 and 34 ℃. 654 kg of esterified liquid is obtained after the dripping is finished.
Thirdly, synthesis: 300 kg of hydrogen peroxide with the content of 27.5 percent is put into a 1 ton crude tertiary synthesis reaction kettle, 654 kg of the esterified liquid is dripped into the kettle, and the temperature of the esterified liquid is controlled between 34 ℃ and 38 ℃ by utilizing frozen saline water. Stirring for 30 minutes after the dropwise addition is finished, standing for 10 hours, and removing the lower layer of dilute acid to obtain 185 kg of crude tert-butyl acid for later use.
Fourthly, preparing sodium salt: 240 kg of liquid caustic soda with the content of 30 percent is put into a 1 ton ceramic reaction kettle filled with 470 kg of water, the temperature of the reaction kettle is controlled by utilizing frozen brine, 185 kg of crude caustic soda is dripped into the reaction kettle, and the temperature is controlled between 15 ℃ and 20 ℃. After the dropwise addition, the mixture was stirred for 30 minutes, and after standing for 1 hour, 800 kg of sodium salt was formed in the lower layer, and 39 kg of a by-product (water) was formed in the upper layer.
And V, condensation: adding 118 kg of benzoyl chloride into a 1-ton di-tert-synthesis reaction kettle, cooling by using frozen brine, taking out 400 kg of sodium salt, dropwise adding the sodium salt into the kettle at the temperature of below 20 ℃, keeping the temperature for 1 hour at 15-20 ℃ after dropwise adding, standing for 1 hour, layering, wherein the upper layer is 125 kg of crude product, and the lower layer is waste liquid (sodium chloride).
Sixth, washing and drying: 30 kg of 30% liquid caustic soda and 160 kg of water are respectively put into a 1 ton washing reaction kettle, 125 kg of crude product is added, the mixture is stirred for 20 minutes, and the mixture is kept still for 1 hour to remove lower-layer waste liquid. Washing with water for 2-3 times by the same method, removing upper layer wastewater, adding 12 kg of anhydrous sodium sulfate, stirring for 30 min, and vacuum filtering to obtain 120 kg of finished product.
Example two:
a production process of tert-butyl peroxybenzoate comprises the following operation processes:
firstly, preparing acid: 324 kg of 98% concentrated sulfuric acid is firstly put into a 1 ton acid-resistant reaction kettle, 130 kg of water is then added under the cooling condition, the temperature is not higher than 80 ℃, the dropping time is 60 minutes, the dropping speed is fast first and slow later, and the mixture is cooled to the room temperature after the dropping is finished. 454 kg of dilute acid is obtained for standby.
Secondly, esterification: 244 kg of tertiary butanol is put into a 1 ton esterification reaction kettle, 454 kg of diluted acid is added dropwise, and the temperature is controlled between 30 ℃ and 34 ℃ by utilizing frozen brine. 698 kg of esterified liquid is obtained after the dripping for standby.
Thirdly, synthesis: 420 kg of hydrogen peroxide with the content of 27.5 percent is put into a 1 ton crude tertiary synthesis reaction kettle, 698 kg of the esterification solution is added into the kettle dropwise, and the temperature is controlled between 34 ℃ and 38 ℃ by utilizing frozen brine. Stirring for 30 minutes after the dropwise adding is finished, standing for 10 hours, and removing lower layer diluted acid to obtain 220 kg of crude tertiary acid for later use.
Fourthly, preparing sodium salt: firstly, 240 kg of liquid caustic soda with the content of 30% is put into a 1-ton ceramic reaction kettle filled with 470 kg of water, the temperature of the reaction kettle is controlled by utilizing frozen brine, and crude tertiary 220 kg of caustic soda is dripped into the reaction kettle, and the temperature is controlled between 15 ℃ and 20 ℃. Stirring for 30 minutes after the dripping is finished, standing for 1 hour, wherein the lower layer is 800 kg of sodium salt, and the upper layer is 39 kg of a byproduct.
And V, condensation: 100 kg of benzoyl chloride is put into a 1-ton di-tert-synthesis reaction kettle, the temperature is reduced by using frozen brine, 400 kg of sodium salt is added into the kettle dropwise at the temperature of below 20 ℃, after the addition, the temperature is kept between 15 ℃ and 20 ℃ for 1 hour, the mixture is layered after standing for 1 hour, the upper layer is 125 kg of crude product, and the lower layer is waste liquid (sodium chloride).
Sixth, washing and drying: 30 kg of 30% liquid caustic soda and 160 kg of water are respectively put into a 1 ton washing reaction kettle, 125 kg of crude product is added, the mixture is stirred for 20 minutes, and the mixture is kept still for 1 hour to remove lower-layer waste liquid. Washing with water for 2-3 times by the same method, removing upperlayer wastewater, adding 10 kg of anhydrous sodium sulfate, stirring for 30 min, and vacuum filtering to obtain 120 kg of finished product.
Example three:
a production process of tert-butyl peroxybenzoate comprises the following operation processes:
firstly, preparing acid: firstly putting 228 kg of 98% concentrated sulfuric acid into a 1 ton acid-resistant reaction kettle, then adding 92 kg of water under the cooling condition to ensure that the temperature is not higher than 80 ℃, dropwise adding for 60 minutes at a slow speed and a fast speed, and cooling to room temperature after dropwise adding. 320 kg of dilute acid is obtained for standby.
Secondly, esterification: 200 kg of tert-butyl alcohol is put into a 1 ton esterification reaction kettle, 320 kg of diluted acid is added dropwise, and the temperature is controlled between 30 ℃ and 34 ℃ by utilizing frozen brine. 520 kg of esterified liquid is obtained after the dripping is finished for standby.
Thirdly, synthesis: 300 kg of hydrogen peroxide with the content of 27.5 percent is put into a 1 ton crude tertiary synthesis reaction kettle, 520 kg of the esterification solution is added into the kettle dropwise, and the temperature is controlled between 34 ℃ and 38 ℃ by utilizing frozen brine. Stirring for 30 minutes after the dropwise addition is finished, standing for 10 hours, and removing the lower layer of dilute acid to obtain 185 kg of crude tert-butyl acid for later use.
Fourthly, preparing sodium salt: 240 kg of liquid caustic soda with the content of 30 percent is put into a 1 ton ceramic reaction kettle filled with 470 kg of water, the temperature of the reaction kettle is controlled by utilizing frozen brine, 185 kg of crude caustic soda is dripped into the reaction kettle, and the temperature is controlled between 15 ℃ and 20 ℃. After the dropwise addition, the mixture was stirred for 30 minutes, and after standing for 1 hour, 800 kg of sodium salt was formed in the lower layer, and 39 kg of a by-product (water) was formed in the upper layer. And V, condensation: adding 118 kg of benzoyl chloride into a 1-ton di-tert-synthesis reaction kettle, cooling by using frozen saline (3% calcium chloride solution), dropwise adding 400 kg of sodium salt into the kettle at the temperature of below 20 ℃, preserving heat for 1 hour at the temperature of between 15 and 20 ℃ after dropwise adding, standing for 1 hour, layering, wherein the upper layer is 125 kg of crude product, and the lower layer is waste liquid.
Sixth, washing and drying: 30 kg of 30% liquid caustic soda and 160 kg of water are respectively put into a 1 ton washing reaction kettle, 125 kg of crude product is added, the mixture is stirred for 20 minutes, and the mixture is kept still for 1 hour to remove lower-layer waste liquid. Washing with water for 2-3 times by the same method, removing upper layer wastewater, adding 15 kg of anhydrous sodium sulfate, stirring for 30 min, and vacuum filtering to obtain 120L of finished product.
Claims (1)
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Claims (1)
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1. A production process of tert-butyl peroxybenzoate is characterized by comprising the following steps: the operation process of the process is as follows:
A. acid preparation: 71.4% by weight of 98% concentrated sulfuric acid; water 28.6 wt%.
Firstly, putting 98% concentrated sulfuric acid into a reaction kettle, then adding water under the cooling condition to ensure that the temperature is not higher than 80 ℃, and dripping for 60 minutes, wherein the speed is first high and then low, and the speed is determined according to the temperature. After the dropwise addition, the mixture was cooled to room temperature. 70 percent dilute sulfuric acid is obtained for standby.
B. Esterification: 30.6-35 wt% of tert-butyl alcohol; 70% dilute sulfuric acid 65-69.4 wt%.
Putting the tert-butyl alcohol into a reaction kettle, dripping 70% dilute sulfuric acid into the reaction kettle, pumping the frozen brine into an interlayer of the reaction kettle for circulating circulation of a circulating pump, and controlling the temperature of the frozen brine to be between 30 and 34 ℃. And (4) obtaining the esterified liquid for later use after the dripping is finished.
C. Synthesizing: 31.4 to 37.8 weight percent of 27.5 percent of hydrogen peroxide; 62.2 to 68.6 weight percent of esterification liquid.
Adding 27.5% hydrogen peroxide into the reaction kettle, adding the esterification solution dropwise, and controlling the temperature to be 34-38 deg.C with frozen saline water. Stirring for 30 minutes after the dropwise addition is finished, standing for 10 hours, and then removing lower layer diluted acid to obtain crude tert-butyl, namely crude tert-butyl hydroperoxide for later use.
Esterification liquid hydrogen peroxide crude tert-butyl hydroperoxide di-tert-butyl hydroperoxide water
D. Preparing sodium salt: 25.8-26.8 wt% of 30% liquid alkali; coarse tertiary 20.7-23.7 wt%; 50.5-52.5 wt% of water.
Firstly, 30 percent of liquid caustic soda is put into a reaction kettle filled with water, the temperature of the reaction kettle is controlled by utilizing frozen saline water, all the crude caustic soda is dripped into the reaction kettle, and the temperature is controlled between 15 ℃ and 20 ℃. Stirring for 30 minutes after the dripping is finished, standing for 1 hour, wherein the lower layer is sodium salt, and the upper layer is a byproduct, namely water.
Crude tertiary liquid alkali sodium salt water
E. Condensation: 77.2-80 wt% of sodium salt; 20-22.8 wt% of benzoyl chloride.
Adding benzoyl chloride into a reaction kettle, cooling by using frozen saline, adding sodium salt dropwise at a temperature below 20 ℃, keeping the temperature for 1 hour at a temperature of between 15 and 20 ℃ after dropwise adding, standing for 1 hour, and then layering, wherein the upper layer is a crude product, and the lower layer is waste liquid.
Sodium salt benzoyl chloride crude sodium chloride
F. Washing and drying: 14.6-15% by weight of 30% liquid alkali; 7880 wt.% water; 5-7.3 wt% of anhydrous sodium sulfate.
Respectively adding 30% liquid caustic soda and water into the reaction kettle, adding all the crude products, stirring for 20 minutes, and standing for 1 hour to remove lower-layer waste liquid. Washing with water for 2-3 times by the same method, removing upper layer wastewater, adding a certain amount of anhydrous sodium sulfate, stirring for 30 min, and vacuum filtering to obtain the final product.