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Green and environment-friendly process for synthesizing bromoacetate by solvent-free method

A bromoacetate, green and environmentally friendly technology, applied in the field of chemical manufacturing, can solve the problems of difficult catalyst recovery, low production efficiency, poor safety, etc., and achieve the effects of avoiding occupational health hazards, improving production efficiency, and avoiding safety problems

Pending Publication Date: 2021-11-05
江苏沃德化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation method of existing BBAB, BBAE basically reacts in a large amount of organic inert solvents, and alcohol and bromoacetic acid are esterified under the action of a catalyst. Most of the catalysts are inorganic salts, p-toluenesulfonic acid, sulfuric acid, etc., and the production efficiency is not high , Catalyst recovery is difficult, high cost, high energy consumption, poor safety, more waste water, difficult to biochemical treatment (need to remove a large amount of reaction solvent after the reaction), the final yield of BBAB is only 66.75%

Method used

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  • Green and environment-friendly process for synthesizing bromoacetate by solvent-free method
  • Green and environment-friendly process for synthesizing bromoacetate by solvent-free method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of green environmental protection technology of solvent-free synthetic bromoacetate, comprises the steps:

[0020] 1) Mixing: Put 695kg of bromoacetic acid, 220kg of 1,4-butene diol and 2kg of sodium bisulfate into the reactor, start stirring, turn on the vacuum pump system to adjust the pressure to -0.085Mpa, and slowly heat to 50°C; 2) Reaction: After the reaction starts, slowly increase the reaction temperature to 95°C within 4.5 hours, and keep it for 1.4 hours, then take a sample for analysis; 3) Finished product: After the reaction is completed, cool down to room temperature, seal and filter the reaction solution, and transfer it to a dehydration kettle for use Maintain a high vacuum of -0.098Mpa at 75°C for 1.3h to obtain 820kg of 1,4-bis(bromoacetoxy)-2-butene as a brown oily liquid with a yield of 90.46%.

Embodiment 2

[0022] A kind of green environmental protection technology of solvent-free synthetic bromoacetate, comprises the steps:

[0023] 1) Mixing: Put 695kg of bromoacetic acid, 220kg of 1,4-butene diol and 2kg of sodium bisulfate into the reactor, start stirring, turn on the vacuum pump system to adjust the pressure to -0.085Mpa, and slowly heat to 50°C; 2) Reaction: After the reaction starts, slowly raise the reaction temperature to 95°C within 5.5 hours, and keep it for 1.8 hours, then take a sample for analysis; 3) Finished product: After the reaction is completed, cool down to room temperature, seal and filter the reaction solution, and transfer it to a dehydration kettle for use -0.098Mpa high vacuum was maintained at 78°C for 1.6h, and 820kg of 1,4-bis(bromoacetoxy)-2-butene was obtained as a brown oily liquid with a yield of 90.28%.

[0024] The parameter indexes of Embodiment 1 and Embodiment 2 are shown in the table below.

[0025]

[0026] A kind of green environmental...

Embodiment 3

[0029] A kind of green environmental protection technology of solvent-free synthetic bromoacetate, comprises the steps:

[0030] 1) Mixing: Put 695kg of bromoacetic acid, 155kg of ethylene glycol and 2kg of sodium bisulfate into the reactor, start stirring, turn on the vacuum pump system to adjust the pressure to -0.085Mpa, and slowly heat to 50°C; 2) Reaction: After the reaction starts , slowly raise the reaction temperature to 95°C within 5 hours, and keep it for 1.5 hours, and take samples for analysis; 3) Finished product: After the reaction is completed, cool down to room temperature, seal and filter the reaction solution, transfer it to the dehydration kettle and use -0.098Mpa high vacuum in the Keep at 75°C for 1.5h to obtain 750kg of 1,4-bis(bromoacetoxy)-2-butene as a brown oily liquid with a yield of 93%.

[0031] The parameter indexes of the second embodiment are shown in the table below.

[0032]

[0033] The invention is a green and environment-friendly proces...

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Abstract

The invention discloses a green and environment-friendly process for synthesizing bromoacetate by a solvent-free method, which comprises the following steps: 1) mixing: adding a certain amount of mixture into a reaction kettle, starting stirring, starting a vacuum pump system to adjust pressure, and slowly heating to a specified temperature; 2) reacting: after the reaction starts, slowly raising the reaction temperature to a specified temperature within a certain reaction time, keeping the temperature for a period of time, and sampling and analyzing; and 3) obtaining a finished product: after the reaction is finished, cooling to room temperature, sealing and filtering the reaction liquid, transferring into a dehydration kettle, and keeping for a period of time in high vacuum at a certain temperature to obtain a yellowish-brown oily liquid, namely the product. Safety problems and occupational health hazards caused in the solvent using process are avoided, sodium hydrogen sulfate is used as a catalyst, and the catalyst can be separated after being filtered after the reaction is completed and can be applied mechanically in batches; the method accords with the current green process development direction, improves the production efficiency, promotes the reaction, omits the washing process, and does not generate wastewater.

Description

technical field [0001] The invention relates to the field of chemical manufacturing, in particular to a green and environment-friendly process for synthesizing bromoacetate by a solventless method. Background technique [0002] Water systems such as industrial circulating cooling water, oil field reinjection water and paper industry have special and complex ecological environments, which are suitable for the growth and reproduction of various bacteria and algae microorganisms. The large-scale reproduction of these microorganisms will form slime, causing problems such as pipeline blockage, equipment corrosion, and water quality deterioration, causing huge economic losses to industrial production. Therefore, it is necessary to select excellent industrial water treatment antibacterial agents for sterilization treatment. [0003] 1,4-bis(bromoacetoxy)-2-butene (BBAB) and 2,2-bis(bromoacetoxy)ethane (BBAE) are highly efficient and environmentally friendly disinfectant and antiba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/63
CPCC07C67/08C07C69/63
Inventor 徐善泉储宇锋季敏周雪华
Owner 江苏沃德化工有限公司
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