Environmental-friendly method for preparing bromine-based alkyl

An environmentally friendly, bromoalkane technology, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of high production cost, poor recycling, and low content, and reduce production safety hazards , Guarantee occupational safety and health, and be easy for industrial application

Inactive Publication Date: 2012-11-07
连云港海水化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of the product is generally low, and the solvent is difficult to handle, which is not easy to recycle, which increases the production cost
[0005] To sum up, the existing method and technology will cause certain pollution to the environment due to the backward technology, obsolete equipment and high production cost of the product, and the product yield is low and the content is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a four-necked flask equipped with a condensation collection device, a stirrer, a thermometer and a constant pressure dropping funnel, add 200 g of 48% (mass concentration, the same below) hydrobromic acid (accounting for about 1 / 5 of the volume of the container), and start Stir the device, and heat up, weigh 48% hydrobromic acid 614g and 99% n-butanol 272g simultaneously, the two are uniformly mixed and placed in the constant pressure dropping funnel. Prepare saturated aqueous sodium carbonate solution. When the temperature in the four-necked flask rises to 108°C, open the constant pressure dropping funnel and drop the mixed solution at a constant speed, raise the temperature to keep the temperature in the bottle at 120-125°C, open the condenser to cool down and receive bromobutane. Put the bromobutane crude product at rest for 2 hours, separate layers, take the lower oil phase, wash with saturated aqueous sodium carbonate solution, the pH value is 8, wash with water...

Embodiment 2

[0031] In a four-necked flask equipped with a condensation collecting device, a stirrer, a thermometer and a constant pressure dropping funnel, add 300 g of 40% hydrobromic acid (accounting for about 1 / 3 of the volume of the container), start the stirring device, and heat up, while Weigh 738g of 40% hydrobromic acid and 284g of 95% n-butanol to prepare saturated aqueous sodium carbonate solution. When the temperature in the four-neck flask rises to 115°C, hydrobromic acid and n-butanol solution are added dropwise at the same time (to ensure that HBr and CH 3 CH 2 CH 2 CH 2 The feed molar ratio of OH is 1:1), the temperature is raised to keep the temperature in the bottle at 125-130°C, and bromobutane is received by condensation. Put the bromobutane crude product at rest for 1.5 hours, separate layers, take the lower layer of oil phase, wash with saturated aqueous sodium carbonate solution, the pH value is 8, wash with water twice, the pH value is 7, and dry through molecula...

Embodiment 3

[0033] In a four-necked flask equipped with a condensation collecting device, a stirrer, a thermometer and a constant pressure dropping funnel, add 300 g of 49% hydrobromic acid (accounting for about 1 / 3 of the volume of the container), start the stirring device, and heat up, while Weigh 394g of 60% hydrobromic acid and 218g of 99% n-butanol and mix them uniformly to prepare saturated aqueous sodium carbonate solution. When the temperature in the four-neck flask rises to 120°C, add the mixture of hydrobromic acid and n-butanol solution dropwise, raise the temperature to keep the temperature in the flask at 130-135°C, and condense to receive bromobutane. Put the bromobutane crude product at rest for 3 hours, separate layers, take the lower oil phase, wash with saturated aqueous sodium carbonate solution, the pH value is 8, wash twice with water, the pH value is 7, and dry through molecular sieves to obtain bromobutane with a yield of 93 %, the content is 99.2%, and the mass fra...

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Abstract

The invention discloses an environmental-friendly method for preparing bromine-based alkyl. The method comprises the steps as follows: adding a hydrobromic acid solution in a reaction vessel in advance, and then preheating until steam is generated; and slowly adding the mixture of the hydrobromic acid solution and an ethanol solution into the reaction vessel or slowly adding both in a separated way at the same time, as for the former way, during the adding process, heating the reaction vessel to 100-140 DEG C to cause reaction so as to prepare bromine-based alkyl, wherein the ethanol solution is the normal butanol solution or the methanol solution; and bromine-based alkyl is bromobutane or bromomethane. According to the invention, poisonous and harmful raw materials are reduced from the source, which reduces potential safety hazards during production and ensures the occupational safety and health of staff. During the process, no waste gas is generated, no solid waste is discharged, and waste water can be recycled after being subjected to neutralization and desalting processing, as a result, zero discharge of 'the three wastes' is realized, and the purpose of environment protection is achieved. Therefore, the method has the advantages of low cost, simplicity in operation, and easiness in industrialization application.

Description

technical field [0001] The invention belongs to the field of reagent preparation, and in particular relates to an environmentally friendly method for preparing bromoalkane. Background technique [0002] Bromobutane, also known as bromobutane, bromobutane, n-bromobutane, 1-bromobutane, is a colorless and transparent liquid that can be used as a solvent, an alkylating agent and an intermediate in organic synthesis; It can be used as a raw material for plastic ultraviolet absorbers and plasticizers; as a raw material for medicine; as a raw material for dyes and for preparing functional pigments; as an intermediate raw material for semiconductors; as a raw material for organic synthesis. [0003] Methyl bromide, also known as methyl bromide or methyl bromide, is a colorless, odorless liquid. It has a strong fumigation effect and can kill various harmful organisms efficiently and broadly. [0004] According to the current literature reports, most domestic manufacturers adopt th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/075C07C17/16
Inventor 章庚柱李备战吉玲
Owner 连云港海水化工有限公司
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