CN103922887A - Desorption process of methanol-containing hydrochloric acid - Google Patents
Desorption process of methanol-containing hydrochloric acid Download PDFInfo
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- CN103922887A CN103922887A CN201410179898.3A CN201410179898A CN103922887A CN 103922887 A CN103922887 A CN 103922887A CN 201410179898 A CN201410179898 A CN 201410179898A CN 103922887 A CN103922887 A CN 103922887A
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- hydrochloric acid
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- calcium chloride
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Abstract
The invention discloses a desorption process of methanol-containing hydrochloric acid. The desorption process comprises the following steps that the hydrochloric acid which contains 31% by weight of 0.3% methanol and a calcium chloride solution from a flash tank are mixed and then enter from the top of a desorption tower, a tower bottom solution is circularly heated through a reboiler, and a mixed solution positioned at the top of the desorption tower is filled in the desorption tower and generates a gas-liquid high-efficiency mass transfer process on the surface of an inner part; desorbed chlorine hydride and a methanol gas sequentially enter a first-stage condenser and a second-stage condenser from the top of the desorption tower to condense entrained water vapors; the dried chlorine hydride and the methanol gas pass through a demister and then are delivered into a chloromethane synthesis device for the synthesis of chloromethane; and a dilute calcium chloride solution enters the flash tank to be concentrated in the desorption tower bottom, the flash tank is connected with the thermosyphon natural-circulation reboiler, excessive water is evaporated by the flash tank and then sufficiently condensed by using the condenser and enters a waste water collection tank, and then waste water is subjected to lixiviating neutralizing treatment. The desorption process disclosed by the invention has the advantages of convenience for operation, cost reduction and energy conservation.
Description
Technical field
The present invention relates to a kind of de-technique of analysing containing methanolic hydrochloric acid.
Background technology
After separating out hydrogenchloride with 31% hydrochloric acid is de-in the synthesis technique of methyl chloride and through heating the methanol gas of vaporization, under catalyst action, react production methyl chloride.Concentrated hydrochloric acid after de-analysing tower reactor diluted acid except as absorption liquid for absorption cycle is applied mechanically again of hydrogenchloride, generally all to carry out alkali neutralizing treatment, because methyl chloride building-up reactions can not transform completely, still have unreacted hydrogenchloride and methyl alcohol to exist on the other hand, form by product: containing methanolic hydrochloric acid.This by product proportion is larger, generally all to select to recycle: as selected the conventional de-method of analysing of hydrochloric acid, but containing methanolic hydrochloric acid, difficulty is recycled, major cause is conventional de-analyse method and have limitation, take off and analyse in process at hydrochloric acid, along with tower reactor concentration of hydrochloric acid reduces gradually, hydrogenchloride can form binary azeotrope with water, hydrogenchloride can not be isolated from water, and concentration is still at 15%(W/W) more than; As tower bottoms is continued to cyclically utilizing, not only can dilute hydrochloric acid material concentration, increase the de-energy consumption of analysing, and uneven because of the turnover of system material, there is the phenomenon of raw material swell-warehouse; As by direct tower bottoms neutralizing treatment, because of waste water saltiness is high can not biochemical degradation, bring burden to wastewater treatment.Therefore, conventionally de-analyse method and can not be applicable to production requirement.
Summary of the invention
The object of the invention is in order to overcome above deficiency, a kind of easy to operate, de-technique of analysing containing methanolic hydrochloric acid of reducing cost, save energy is provided.
Object of the present invention is achieved through the following technical solutions: a kind of de-technique of analysing containing methanolic hydrochloric acid, comprises the following steps:
A, after mixing with from the calcium chloride solution of flash tank containing the hydrochloric acid of 31% (Wt) of methyl alcohol 0.3%, enter from desorption tower used top, wherein the weight ratio of hydrochloric acid and calcium chloride solution is 1.0:2.5-3.5, tower reactor solution carries out thermal siphon natural circulation heating by reboiler, and the mixed solution at desorption tower used top, at desorption tower used interior filler and internals surface, gas liquid high-efficiency mass transfer process occurs;
B, de-hydrogenchloride and the methanol gas of separating out enter first-stage condenser and secondary condenser successively from desorption tower used top, carry out respectively that one-level is cooling and secondary is cooling, by the water vapor condensation of carrying secretly;
C, dry hydrogenchloride and methanol gas are sent into methyl chloride synthesizer after mist eliminator, synthetic for methyl chloride;
D, at desorption tower used still, it is concentrated that rare calcium chloride solution enters flash tank, and flash tank is connected with thermal siphon natural circulation reboiler, and excessive water is flashed tank and evaporates away, carry out abundant condensation with condenser afterwards and enter wastewater collection tank, afterwards by waste water lixiviating neutralizing treatment.
Further improvement of the present invention is: the calcium chloride solution concentration through flash tank is greater than 50%.
Further improvement of the present invention is: desorption tower used interior working pressure span of control is at 0-2Barg.
The present invention compared with prior art has the following advantages:
The present invention adopts that the degree of depth is de-analyses method, and its technical process is smooth and easy, only need on biochemical treatment facility, increase a small amount of input, same production capacity, raw material consumption only for conventional take off analyse 50%; And by product has obtained utilization containing methanolic hydrochloric acid, has not only reduced raw material consumption cost, reduced the link of logistics transportation and artificial handling and the investment of other overhead charges simultaneously; Utilize simultaneously and produce a large amount of steam that produce when formaldehyde and carry out that the degree of depth is de-to be analysed, the thermal source of whole production line is fully used, and has reduced the working cost of circulating water steam.
brief description of the drawings:
Fig. 1 is schema of the present invention;
Number in the figure: 1-flash tank, 2-are desorption tower used, 3-reboiler, 4-first-stage condenser, 5-secondary condenser, 6-mist eliminator, 7-thermal siphon natural circulation reboiler, 8-condenser, 9-wastewater collection tank.
embodiment:
in order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
The present invention, containing de-a kind of embodiment of analysing technique of methanolic hydrochloric acid, comprises the following steps:
A, after mixing with from the calcium chloride solution of flash tank 1 containing the hydrochloric acid of 31% (Wt) of methyl alcohol 0.3%, enter from desorption tower used 2 tops, wherein the weight ratio of hydrochloric acid and calcium chloride solution is 1.0:2.5-3.5, calcium chloride solution concentration through described flash tank 1 is greater than 50%, desorption tower used interior working pressure span of control is at 0-2Barg, tower reactor solution carries out thermal siphon natural circulation heating by reboiler 3, and the mixed solution at desorption tower used 2 tops, at desorption tower used 2 interior fillers and internals surface, gas liquid high-efficiency mass transfer process occurs;
B, de-hydrogenchloride and the methanol gas of separating out enter first-stage condenser 4 and secondary condenser 5 successively from desorption tower used 2 tops, carry out respectively that one-level is cooling and secondary is cooling, by the water vapor condensation of carrying secretly;
C, dry hydrogenchloride and methanol gas are sent into methyl chloride synthesizer after mist eliminator 6, synthetic for methyl chloride;
D, at desorption tower used still, rare calcium chloride solution enters flash tank 1 and concentrates, and flash tank 1 is connected with thermal siphon natural circulation reboiler 7, and excessive water is flashed tank 1 and evaporates away, carry out abundant condensation with condenser 8 afterwards and enter wastewater collection tank 9, afterwards by waste water lixiviating neutralizing treatment.
Contain methanolic hydrochloric acid and want to serve as raw material recycled, must ensure again that hydrochloric acid takes off the waste water energy processing after analysing simultaneously, on operational path is selected, must adopt the hydrochloric acid degree of depth to take off and analyse.The de-essence of analysing technological principle of the degree of depth is to carry heating up in a steamer principle of operation, be mixed into desorption tower used by hydrochloric acid and the broken agent of boiling, control after the pressure that de-analysis system is suitable, due to breaking of hydrochloric acid and water azeotropic point, methyl alcohol in salt acid starting material and hydrogenchloride is de-separating out from solution in the lump, desorption tower used end dilution the broken agent solution that boils regulates to flow to after the flash concentration that circulates in flash tank by breaking the agent recycle pump that boils by liquid level difference and delivers to desorption tower and recycle, the waste water steaming from flash system, hydrogen chloride content is very low, conventionally at 0.8%(W/W) below, methyl alcohol is less than 0.1%, because of waste water composition single, in organism, only there is methyl alcohol, can be through cooling, in alkali, enter comprehensive adjustment pond dilution chlorine ion concentration with rear waste water producing with other device, the processing of deactivation mud method biochemical degradation, the final qualified discharge of waste water energy.
The present invention adopts that the degree of depth is de-analyses method, and its technical process is smooth and easy, only need on biochemical treatment facility, increase a small amount of input, same production capacity, raw material consumption only for conventional take off analyse 50%; And by product has obtained utilization containing methanolic hydrochloric acid, has not only reduced raw material consumption cost, reduced the link of logistics transportation and artificial handling and the investment of other overhead charges simultaneously; Utilize simultaneously and produce a large amount of steam that produce when formaldehyde and carry out that the degree of depth is de-to be analysed, the thermal source of whole production line is fully used, and has reduced the working cost of circulating water steam.Utilization to the by-product of methyl chloride containing methanolic hydrochloric acid, accomplishes discharged wastewater met the national standard, to reach the object of economic benefit and environmental benefit doulbe-sides' victory.
Claims (3)
1. containing the de-technique of analysing of methanolic hydrochloric acid, it is characterized in that: comprise the following steps:
A, after mixing with from the calcium chloride solution of flash tank (1) containing the hydrochloric acid of 31% (Wt) of methyl alcohol 0.3%, enter from desorption tower used (2) top, wherein the weight ratio of hydrochloric acid and calcium chloride solution is 1.0:2.5-3.5, tower reactor solution carries out thermal siphon natural circulation heating by reboiler (3), and the mixed solution at described desorption tower used (2) top is filler and internals surface generation gas liquid high-efficiency mass transfer process in described desorption tower used (2);
B, de-hydrogenchloride and the methanol gas of separating out enter first-stage condenser (4) and secondary condenser (5) successively from described desorption tower used (2) top, carry out respectively one-level cooling cooling with secondary, by the water vapor condensation of carrying secretly;
C, dry hydrogenchloride and methanol gas are sent into methyl chloride synthesizer after mist eliminator (6), synthetic for methyl chloride;
D, at desorption tower used still, it is concentrated that rare calcium chloride solution enters flash tank (1), described flash tank (1) is connected with thermal siphon natural circulation reboiler (7), excessive water is evaporated away by described flash tank (1), use afterwards condenser (8) to carry out abundant condensation and enter wastewater collection tank (9), afterwards by waste water lixiviating neutralizing treatment.
2. a kind of de-technique of analysing containing methanolic hydrochloric acid according to claim 1, is characterized in that: the calcium chloride solution concentration through described flash tank (1) is greater than 50%.
3. a kind of de-technique of analysing containing methanolic hydrochloric acid according to claim 1, is characterized in that: desorption tower used interior working pressure span of control is at 0-2Barg.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410179898.3A CN103922887A (en) | 2014-04-30 | 2014-04-30 | Desorption process of methanol-containing hydrochloric acid |
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| CN201410179898.3A CN103922887A (en) | 2014-04-30 | 2014-04-30 | Desorption process of methanol-containing hydrochloric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671208A (en) * | 2015-02-09 | 2015-06-03 | 大丰市天生药业有限公司 | Preparation device and technology for hydrogen chloride-methanol solution |
| CN105692554A (en) * | 2016-01-18 | 2016-06-22 | 广西柳化氯碱有限公司 | Method and equipment for producing high-concentration anhydrous hydrogen chloride methanol solution |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440015A (en) * | 2008-11-27 | 2009-05-27 | 山东东岳氟硅材料有限公司 | Method for producing methane chloride by using dilute hydrochloric acid |
| CN202989013U (en) * | 2012-12-25 | 2013-06-12 | 南通江天化学品有限公司 | Chloromethane production device |
-
2014
- 2014-04-30 CN CN201410179898.3A patent/CN103922887A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440015A (en) * | 2008-11-27 | 2009-05-27 | 山东东岳氟硅材料有限公司 | Method for producing methane chloride by using dilute hydrochloric acid |
| CN202989013U (en) * | 2012-12-25 | 2013-06-12 | 南通江天化学品有限公司 | Chloromethane production device |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671208A (en) * | 2015-02-09 | 2015-06-03 | 大丰市天生药业有限公司 | Preparation device and technology for hydrogen chloride-methanol solution |
| CN104671208B (en) * | 2015-02-09 | 2017-05-17 | 盐城市大丰区天生联合药业有限公司 | Preparation device and technology for hydrogen chloride-methanol solution |
| CN105692554A (en) * | 2016-01-18 | 2016-06-22 | 广西柳化氯碱有限公司 | Method and equipment for producing high-concentration anhydrous hydrogen chloride methanol solution |
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Application publication date: 20140716 |