CN104130098A - Bromoethane production process - Google Patents
Bromoethane production process Download PDFInfo
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- CN104130098A CN104130098A CN201410319558.6A CN201410319558A CN104130098A CN 104130098 A CN104130098 A CN 104130098A CN 201410319558 A CN201410319558 A CN 201410319558A CN 104130098 A CN104130098 A CN 104130098A
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- Prior art keywords
- monobromethane
- hydrogen bromide
- water
- still
- bromoethane
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Abstract
The invention relates to the technical field of chemical industry, and particularly discloses a bromoethane production process. Raw materials comprise a hydrobromic acid base solution, sulfur dioxide, chlorine dioxide, ethanol and sodium bicarbonate. The production process comprises the following steps: removing free bromine from the hydrobromic acid base solution by using the sulfur dioxide and the chlorine dioxide; adding the ethanol for performing an esterification reaction to obtain a bromoethane crude solution; performing multi-stage condensation treatment; removing hydrobromic acid and water from the bromoethane crude solution, and performing condensation treatment; adding the sodium bicarbonate for rinsing; and repeatedly performing sedimentation, and drying sediment to obtain finished bromoethane. The production process disclosed by the invention has the advantages of simple and convenient preparation technology, environmental friendliness, freeness from pollution, high purity of a prepared finished product, convenience in operating a preparation process and small equipment investment. The prepared bromoethane has a good application effect, and is safe and reliable. The problems of low yield, low purity, severe pollution and the like in the conventional production method are solved.
Description
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Technical field
The present invention relates to chemical technology field, be specially monobromethane production technique.
Background technology
Monobromethane is colourless oil liquid.There are smell and the calcination taste of similar ether.Reveal and put air or see that light gradually becomes yellow.Volatile.Can with ethanol, ether, chloroform and most immiscible organic solvent.Relative density is 1.4612, and zero pour is-119 DEG C, and boiling point is 38.4 DEG C, and monobromethane is the important source material of organic synthesis.In agricultural, be used as the fumigating insecticide in storage cereal, warehouse and room etc.Monobromethane is to form by Potassium Bromide and freezing sulfuric acid and ethanol synthesis, is usually used in the ethylization of gasoline, refrigerant and narcotic.Purposes is very extensive, but current still more traditional mode of the method for industrial production monobromethane in this traditional production method, have the problems such as yield is low, not high pollution of purity is serious, and production technique is comparatively complicated, is difficult to meet human wants.
Summary of the invention
The object of this invention is to provide a kind of preparation technology simple, the monobromethane production technique that finished product purity is high, to solve the problem proposing in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
Monobromethane production technique, comprises the following steps:
(1) to adding liquid at the bottom of Hydrogen bromide in reactor, hydrobromic input amount is controlled between the 60%-75% of reactor capacity, and input Hydrogen bromide passes in advance dioxide peroxide and removes free bromine before feeding intake, and its chemical equation is as follows:
Br
2+SO
2+2H
2O→2HBr+H
2SO
4
(2) the logical steam of reacting kettle jacketing, when feed liquid in still is warming up to 120 DEG C, starts to add ethanol, carries out esterification, and its chemical equation is as follows:
CH
3CH
2OH+HBr→CH
3CH
2Br+H
2O
(3) reaction is steamed to thing (containing monobromethane, Hydrogen bromide and water), carry out multi-stage condensing processing, first step condensation is by Hydrogen bromide condensation and be back in reactor, and water-cooled condensation is discharged in second stage condensation, the third stage to level V with refrigerated water by monobromethane condensation, put into storage tank;
(4) monobromethane is squeezed into rinsing still, added water according to the mass ratio of 1:1, then add 0.5kg/t sodium bicarbonate and carry out rinsing, layering, draining;
(5) more than the monobromethane in rinsing still squeezed into being stirred 1h in the alkali lye still containing alkali lye, then more than sedimentation 1h, layering;
(6) monobromethane in alkali lye still is squeezed into header tank, then sedimentation;
(7) monobromethane in header tank is deviate from moisture through siccative (as discolour silica gel, sheet alkali, molecular sieve) for dewatering unit again, finally crosses title barrelling.
As further scheme of the present invention, before reactor feed, need to check equipment, pipeline, valve, instrument in advance, guarantee that all normally can feed intake.
As further scheme of the present invention, step (1), in the time deviating to dissociate bromine, first pumps into Hydrogen bromide sulfur dioxide treatment groove by the Hydrogen bromide in composite slot with magnetic drive pump, and the Hydrogen bromide amount in groove must not exceed groove molten long-pending 80%, and then open sulfurous gas needle type valve, control flow at 1-3m
3between/h, pass into sulfurous gas, open magnetic drive pump and play circulation, after 15min, start the test of KI test paper, when test, in sampling cup, add 250ml pure water, then, toward the Hydrogen bromide after 2 circulations in water tumbler and stir, test with KI test paper, if test paper table look (the light blue indigo plant that deepens), color illustrates that brominated amount is higher more deeply, continues to play circulation with magnetic drive pump, repeat a KI test paper test every 5min, until test paper nondiscoloration is standard.
As further scheme of the present invention, step (2) is in the time of esterification, need control temperature of reaction, pressure and ethanol flow, temperature is controlled at 120 DEG C ± 1 DEG C simultaneously, and vapor pressure must not be greater than 0.5Mpa, ethanol is according to the height adjust flux of required production output, the highlyest must not exceed 45L/h, and continue to drip Hydrogen bromide in still, liquid level in still is remained unchanged, every 1h inspection temperature, pressure and ethanol flow and reactor liquid level, keep normergic state.
As further scheme of the present invention, step (3), in the time of the condensation of the second stage, is surveyed primary condenser every 1h and is gone out water ph value, pH value illustrates that between 4-5 reaction is normal, pH value is less than explanation in 4 o'clock has Hydrogen bromide to take out of, can suitably regulate cooling water flow, makes sour water be back to reactor.
The present invention, compared with conventional art, has the following advantages:
Preparation technology of the present invention is simple and convenient, environment friendly and pollution-free, prepares gained finished product purity high, and preparation process convenient operation, and facility investment is few, and the monobromethane result of use of preparation is good, safe and reliable.
figure of description
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Monobromethane production technique, as shown in Figure 1, technical process is as follows:
(1) first equipment, pipeline, valve, instrument are checked, guarantee to add in all normal backward reactors liquid at the bottom of Hydrogen bromide, hydrobromic input amount is controlled between the 60%-75% of reactor capacity, input Hydrogen bromide passes in advance dioxide peroxide and removes free bromine before feeding intake, and its chemical equation is as follows:
Br
2+SO
2+2H
2O→2HBr+H
2SO
4
Except free bromine process is: first the magnetic drive pump of the Hydrogen bromide in composite slot is pumped into Hydrogen bromide sulfur dioxide treatment groove, it is molten long-pending 80% that the Hydrogen bromide amount in groove must not exceed groove, and then open sulfurous gas needle type valve, controls flow at 1-3m
3between/h, pass into sulfurous gas, open magnetic drive pump and play circulation, after 15min, start the test of KI test paper, when test, in sampling cup, add 250ml pure water, then, toward the Hydrogen bromide after 2 circulations in water tumbler and stir, with the test of KI test paper, if test paper table look (the light blue indigo plant that deepens), color illustrates that brominated amount is higher more deeply, continue to play circulation with magnetic drive pump, repeat a KI test paper test every 5min, until test paper nondiscoloration is standard, can drop in reactor;
(2) the logical steam of reacting kettle jacketing, when feed liquid in still is warming up to 120 DEG C, starts to add ethanol, carries out esterification, and its chemical equation is as follows:
CH
3CH
2OH+HBr→CH
3CH
2Br+H
2O
In esterification reaction process, need control temperature of reaction, pressure and ethanol flow simultaneously, temperature is controlled at 120 DEG C ± 1 DEG C, vapor pressure must not be greater than 0.5Mpa, and ethanol is according to the height adjust flux of required production output, the highlyest must not exceed 45L/h, and continue to drip Hydrogen bromide in still, liquid level in still is remained unchanged, and every 1h inspection temperature, pressure and ethanol flow and reactor liquid level, keep normergic state;
(3) reaction that contains monobromethane, Hydrogen bromide and water is steamed to thing, carry out multi-stage condensing processing, first step condensation is by Hydrogen bromide condensation and be back in reactor, water-cooled condensation is discharged in second stage condensation, the third stage to level V with refrigerated water by monobromethane condensation, in the time carrying out second stage condensation, survey primary condenser every 1h and go out water ph value, pH value illustrates that between 4-5 reaction is normal, pH value is less than explanation in 4 o'clock has Hydrogen bromide to take out of, can suitably regulate cooling water flow, make sour water be back to reactor;
(4) monobromethane is squeezed into rinsing still, added water according to the mass ratio of 1:1, then add 0.5kg/t sodium bicarbonate and carry out rinsing, layering, draining;
(5) more than the monobromethane in rinsing still squeezed into being stirred 1h in the alkali lye still containing alkali lye, then more than sedimentation 1h, layering;
(6) monobromethane in alkali lye still is squeezed into header tank, then sedimentation;
(7) monobromethane in header tank is deviate from moisture through siccative such as discolour silica gel, sheet alkali or molecular sieves for dewatering unit again, finally crosses title barrelling.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (4)
1. monobromethane production technique, is characterized in that, comprises the following steps:
(1) to adding liquid at the bottom of Hydrogen bromide in reactor, hydrobromic input amount is controlled between the 60%-75% of reactor capacity, and input Hydrogen bromide passes in advance dioxide peroxide and removes free bromine before feeding intake, and its chemical equation is as follows:
Br
2+SO
2+2H
2O→2HBr+H
2SO
4
(2) the logical steam of reacting kettle jacketing, when feed liquid in still is warming up to 120 DEG C, starts to add ethanol, carries out esterification, and its chemical equation is as follows:
CH
3CH
2OH+HBr→CH
3CH
2Br+H
2O
(3) reaction that contains monobromethane, Hydrogen bromide and water is steamed to thing, carry out multi-stage condensing processing, first step condensation is by Hydrogen bromide condensation and be back in reactor, and water-cooled condensation is discharged in second stage condensation, the third stage to level V with refrigerated water by monobromethane condensation, put into storage tank;
(4) monobromethane is squeezed into rinsing still, added water according to the mass ratio of 1:1, then add 0.5kg/t sodium bicarbonate and carry out rinsing, layering, draining;
(5) more than the monobromethane in rinsing still squeezed into being stirred 1h in the alkali lye still containing alkali lye, then more than sedimentation 1h, layering;
(6) monobromethane in alkali lye still is squeezed into header tank, then sedimentation;
(7) monobromethane in header tank is deviate from moisture through dewatering unit with siccative again, finally crosses title barrelling.
2. monobromethane production technique according to claim 1, it is characterized in that, step (1) is in the time deviating to dissociate bromine, first the Hydrogen bromide in composite slot is pumped into Hydrogen bromide sulfur dioxide treatment groove with magnetic drive pump, Hydrogen bromide amount in groove must not exceed groove molten long-pending 80%, and then open sulfurous gas needle type valve, control flow at 1-3m
3between/h, pass into sulfurous gas, open magnetic drive pump and play circulation, after 15min, start the test of KI test paper, when test, in sampling cup, add 250ml pure water, then, toward the Hydrogen bromide after 2 circulations in water tumbler and stir, test with KI test paper, if test paper table look, color illustrates that brominated amount is higher more deeply, continues to play circulation with magnetic drive pump, repeat a KI test paper test every 5min, until test paper nondiscoloration is standard.
3. monobromethane production technique according to claim 1, it is characterized in that, step (2) is in the time of esterification, and temperature is controlled at 120 DEG C ± 1 DEG C, and vapor pressure must not be greater than 0.5Mpa, ethanol is according to the height adjust flux of required production output, the highlyest must not exceed 45L/h, and continue to drip Hydrogen bromide in still, liquid level in still is remained unchanged, every 1h inspection temperature, pressure and ethanol flow and reactor liquid level, keep normergic state.
4. monobromethane production technique according to claim 1, it is characterized in that, step (3) is in the time carrying out second stage condensation, survey primary condenser every 1h and go out water ph value, pH value illustrates that between 4-5 reaction is normal, pH value is less than explanation in 4 o'clock has Hydrogen bromide to take out of, can suitably regulate cooling water flow, makes sour water be back to reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410319558.6A CN104130098A (en) | 2014-07-07 | 2014-07-07 | Bromoethane production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410319558.6A CN104130098A (en) | 2014-07-07 | 2014-07-07 | Bromoethane production process |
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|---|---|
| CN104130098A true CN104130098A (en) | 2014-11-05 |
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ID=51803007
Family Applications (1)
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|---|---|---|---|
| CN201410319558.6A Pending CN104130098A (en) | 2014-07-07 | 2014-07-07 | Bromoethane production process |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5138110A (en) * | 1990-03-13 | 1992-08-11 | Bromine Compounds Ltd. | Process for the preparation of alkyl-halides |
| CN102766012A (en) * | 2012-06-29 | 2012-11-07 | 连云港海水化工有限公司 | Environmental-friendly method for preparing bromoethane |
-
2014
- 2014-07-07 CN CN201410319558.6A patent/CN104130098A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5138110A (en) * | 1990-03-13 | 1992-08-11 | Bromine Compounds Ltd. | Process for the preparation of alkyl-halides |
| CN102766012A (en) * | 2012-06-29 | 2012-11-07 | 连云港海水化工有限公司 | Environmental-friendly method for preparing bromoethane |
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Application publication date: 20141105 |