CN104045512A - Production technology for synthesizing m-bromotoluene - Google Patents

Abstract

A production technology for synthesizing m-bromotoluene relates to the technical field of the chemical industry. The technology comprises the following steps: adding 95% ethanol into an enamel reaction kettle, starting a stirrer for stirring, adding concentrated sulfuric acid and 3-bromo-aminomethyl, uniformly stirring, mixing sodium nitrite with an aqueous solution, adding the obtained solution into the reaction kettle, adding ether washed copper powder, heating, reacting until no bubbles appear and the material liquid becomes yellow from red brown, distilling, washing, separating and purifying the obtained water phase, drying, filtering, rectifying to obtain a colorless product, that is, an m-bromotoluene finished product, packaging and warehousing. The technology has the advantages of convenient and simple preparation, environmental protection, no pollution, easily available materials, less equipment investment, high purity and convenient operation, and the prepared m-bromotoluene has the advantages of good use effect, safety and reliability.

Description

The production technique that a kind of m-bromotoluene is synthetic

Technical field

The present invention relates to chemical technology field, be specifically related to the synthetic production technique of a kind of m-bromotoluene.

Background technology

M-bromotoluene is a kind of colourless or light yellow transparent liquid, water insoluble, is dissolved in acetone and chloroform, and miscible with ethanol, ether and benzene, it is mainly used in organic synthesis raw material; As solvent; Medical material, the medicine of production for treating arthralgia.But itself is poisonous for m-bromotoluene, and its toxicity is large compared with toluene, has narcoticness, can make nervous center poisoning; Irritant,, must, strictly control, there is the problems such as yield is low, not high pollution of purity is serious in industrial production m-bromotoluene so wait in the preparation in skin irritation and mucous membrane, and production technique is comparatively complicated, is difficult to meet human wants at present.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of purity high, the production technique that the simple m-bromotoluene of preparation technology is synthetic.

Technical problem to be solved by this invention realizes by the following technical solutions:

The production technique that m-bromotoluene is synthetic, is characterized in that: comprise following processing step,

A. the ethanol of choosing 620-630kg95% adds in reactor, and turn on agitator stirs.

B. take the vitriol oil of 360-370kg and the bromo-aminomethyl phenyl of the 3-of 240-260kg, add in the reactor in step a and to open chilled brine cooling, continue to stir, until mixture stirs.

C. take the Sodium Nitrite of 140-150kg and the water mixing wiring solution-forming of 250-270kg is for subsequent use.

D. in the time that reactor temperature is down to 10 DEG C in step b, the mixing solutions of preparing in step c is dropped in reactor, keep temperature≤10 DEG C, continue stirring reaction 20min.

E. after taking the copper powder of 35kg and adopting ether to wash, add in the reactor in steps d.

F. open steam and heat, nitrogen is emitted, and maintain the temperature at 40-60 DEG C of reaction 20min, and then temperature is risen to 80-100 DEG C, continue reaction until overflow without bubble, feed liquid is after reddish-brown becomes yellow, and reaction finishes.。

G. in step f, add 2000L water, then directly pass into water vapour and distill, then overhead product is collected in water-and-oil separator, until while producing without oily matter, stop distillation, overhead product is left standstill to 1h, water is taken out in layering.

H. the oil phase in step g is adopted 10.0% sodium hydroxide solution 100L to wash 2 times, and then divide again water purification phase after washing 1 time with 5.0% sodium carbonate solution 100L.

I. after the oil phase after treatment in step h being dried with Calcium Chloride Powder Anhydrous, filter filtering solids, be then a bromine first toluene finished product by carrying out obtaining colorless product after rectifying in remaining feed liquid suction rectifying still, packaging warehouse-in.

The described still of answering is enamel reaction still.

The invention has the beneficial effects as follows: the present invention is easy to prepare simple, and environment friendly and pollution-free, raw material is easy to get, and facility investment is few, and purity is high, convenient operation, the m-bromotoluene result of use of preparation is good, safe and reliable.

Embodiment

For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.

Embodiment 1

The production technique that m-bromotoluene is synthetic, comprises following processing step,

A. the ethanol of choosing 620kg95% adds in enamel reaction still, and turn on agitator stirs.

B. take the vitriol oil of 360kg and the bromo-aminomethyl phenyl of the 3-of 240kg, add in the enamel reaction still in step a and to open chilled brine cooling, continue to stir, until mixture stirs.

C. take the Sodium Nitrite of 140kg and the water mixing wiring solution-forming of 250kg is for subsequent use.

D. in the time that temperature is down to 10 DEG C in enamel reaction still in step b, the mixing solutions of preparing in step c is dropped in enamel reaction still, keep temperature≤10 DEG C, continue stirring reaction 20min.

E. after taking the copper powder of 35kg and adopting ether to wash, add in the enamel reaction still in steps d.

F. open steam and heat, nitrogen is emitted, and maintain the temperature at 40 DEG C of reaction 20min, and then temperature is risen to 80 DEG C, continue reaction until overflow without bubble, feed liquid is after reddish-brown becomes yellow, and reaction finishes.。

G. in step f, add 2000L water, then directly pass into water vapour and distill, then overhead product is collected in water-and-oil separator, until while producing without oily matter, stop distillation, overhead product is left standstill to 1h, water is taken out in layering.

H. the oil phase in step g is adopted 10.0% sodium hydroxide solution 100L to wash 2 times, and then divide again water purification phase after washing 1 time with 5.0% sodium carbonate solution 100L.

I. after the oil phase after treatment in step h being dried with Calcium Chloride Powder Anhydrous, filter filtering solids, be then a bromine first toluene finished product by carrying out obtaining colorless product after rectifying in remaining feed liquid suction rectifying still, packaging warehouse-in.

Embodiment 2

The production technique that m-bromotoluene is synthetic, comprises following processing step,

A. the ethanol of choosing 624kg95% adds in enamel reaction still, and turn on agitator stirs.

B. take the vitriol oil of 368kg and the bromo-aminomethyl phenyl of the 3-of 250kg, add in the enamel reaction still in step a and to open chilled brine cooling, continue to stir, until mixture stirs.

C. take the Sodium Nitrite of 148kg and the water mixing wiring solution-forming of 260kg is for subsequent use.

D. in the time that temperature is down to 10 DEG C in enamel reaction still in step b, the mixing solutions of preparing in step c is dropped in enamel reaction still, keep temperature≤10 DEG C, continue stirring reaction 20min.

E. after taking the copper powder of 35kg and adopting ether to wash, add in the reactor in steps d.

F. open steam and heat, nitrogen is emitted, and maintain the temperature at 50 DEG C of reaction 20min, and then temperature is risen to 90 DEG C, continue reaction until overflow without bubble, feed liquid is after reddish-brown becomes yellow, and reaction finishes.。

G. in step f, add 2000L water, then directly pass into water vapour and distill, then overhead product is collected in water-and-oil separator, until while producing without oily matter, stop distillation, overhead product is left standstill to 1h, water is taken out in layering.

H. the oil phase in step g is adopted 10.0% sodium hydroxide solution 100L to wash 2 times, and then divide again water purification phase after washing 1 time with 5.0% sodium carbonate solution 100L.

I. after the oil phase after treatment in step h being dried with Calcium Chloride Powder Anhydrous, filter filtering solids, be then a bromine first toluene finished product by carrying out obtaining colorless product after rectifying in remaining feed liquid suction rectifying still, packaging warehouse-in.

More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (2)

1. the synthetic production technique of m-bromotoluene, is characterized in that: comprise following processing step,

A. the ethanol of choosing 620-630kg95% adds in reactor, and turn on agitator stirs.

B. take the vitriol oil of 360-370kg and the bromo-aminomethyl phenyl of the 3-of 240-260kg, add in the reactor in step a and to open chilled brine cooling, continue to stir, until mixture stirs.

C. take the Sodium Nitrite of 140-150kg and the water mixing wiring solution-forming of 250-270kg is for subsequent use.

D. in the time that reactor temperature is down to 10 DEG C in step b, the mixing solutions of preparing in step c is dropped in reactor, keep temperature≤10 DEG C, continue stirring reaction 20min.

E. after taking the copper powder of 35kg and adopting ether to wash, add in the reactor in steps d.

F. open steam and heat, nitrogen is emitted, and maintain the temperature at 40-60 DEG C of reaction 20min, and then temperature is risen to 80-100 DEG C, continue reaction until overflow without bubble, feed liquid is after reddish-brown becomes yellow, and reaction finishes.。

G. in step f, add 2000L water, then directly pass into water vapour and distill, then overhead product is collected in water-and-oil separator, until while producing without oily matter, stop distillation, overhead product is left standstill to 1h, water is taken out in layering.

H. the oil phase in step g is adopted 10.0% sodium hydroxide solution 100L to wash 2 times, and then divide again water purification phase after washing 1 time with 5.0% sodium carbonate solution 100L.

I. after the oil phase after treatment in step h being dried with Calcium Chloride Powder Anhydrous, filter filtering solids, be then a bromine first toluene finished product by carrying out obtaining colorless product after rectifying in remaining feed liquid suction rectifying still, packaging warehouse-in.

2. the synthetic production technique of a kind of m-bromotoluene according to claim 1, is characterized in that: the described still of answering is enamel reaction still.