CN103641748B - A kind of recycle by-product hydrochloric acid prepares the method for methylsulphonic acid - Google Patents
A kind of recycle by-product hydrochloric acid prepares the method for methylsulphonic acid Download PDFInfo
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Abstract
Recycle by-product hydrochloric acid prepares a method for methylsulphonic acid, it is characterized in that: the method adopting " hydrogenchloride → chlorine → methylsulphonic acid → hydrogenchloride ", by the by-product hydrochloric acid recycle in methylsulphonic acid preparation process, prepares methylsulphonic acid; Its advantage is: adopt by-product hydrochloric acid to prepare chlorine, and direct and Methyl disulfide is reacted, and avoids purchase, transports and store security risk and the logistics cost of hypertoxic chlorine; To the by-product hydrochloric acid digestibility and utilization on the spot sold be difficult to, and turn waste into wealth, become the main raw material(s) preparing methylsulphonic acid, achieve the recycle of chlorine element.Simultaneously, by the utilization of waste material of reacted for potassium permanganate oxidation tankage Manganse Dioxide, prepare Manganous chloride tetrahydrate, can be used for electrolytic manganese, greatly reduce production cost and the security risk of methylsulphonic acid, also eliminate the chlorine in methylsulphonic acid preparation and these two large restraining factors of by-product hydrochloric acid simultaneously.
Description
Technical field
The present invention relates to chemical technology field, a kind of recycle by-product hydrochloric acid prepares the method for methylsulphonic acid specifically.
Background technology
Methylsulphonic acid is a kind of important organic medicinal and pesticide intermediate, in the agricultural chemicals such as fomesafen, the synthesis of cephalosporin medicine, have very important application.Meanwhile, the main raw material of methylsulphonic acid or the current electronics finishing of widespread use the most.At present, the common method of producing methylsulphonic acid is the hydrolysis process of Methanesulfonyl chloride.This technique carries out wet oxidation with Methyl disulfide and chlorine, obtains Methanesulfonyl chloride, obtains methylsulphonic acid after Methanesulfonyl chloride hydrolysis.
Wherein, the wet process oxidation technology of Methanesulfonyl chloride, adopts chlorine and Methyl disulfide to carry out oxychlorination reaction in the emulsion of water.This reaction conditions is gentle, and yield is high, and the product purity obtained is high, operational safety, is the main method of current Methanesulfonyl chloride industry preparation.Owing to there being a large amount of sulfide resources within Chinese territory, make China become one of methylsulphonic acid production major country in the world, methylsulphonic acid exports to the countries and regions such as South East Asia, America and Europe and India in a large number.
Prepare the raw material chlorine required for methylsulphonic acid, generally from chlorine industry.Method is that the aqueous solution of sodium-chlor is carried out electrolytic reaction, obtains chlorine, and chlorine is liquid chlorine through purification and condensation, and liquid chlorine is stored in special liquid chlorine cylinder or liquid chlorine groove tank, through security devices such as special gasifications during use, operates comparatively loaded down with trivial details; Sodium chloride electrolysis legal system, for chlorine, needs to consume a large amount of electric energy, and meanwhile, electrolyzer investment is huge, and due to chlorine be severe poisonous chemicals, transport, store and use and all there is larger potential safety hazard.Meanwhile, because the transportation cost of chlorine is high, which dictates that the production of methylsulphonic acid near chlor-alkali factory, must limit the production of methylsulphonic acid.
Meanwhile, Methyl disulfide and preparation of chlorine Methanesulfonyl chloride and Methanesulfonyl chloride hydrolysis are prepared in the process of methylsulphonic acid and are all produced a large amount of by-product hydrochloric acids.Owing to there being the sulfide of trace in by-product hydrochloric acid, making by-product hydrochloric acid have stink, limit the use of by-product hydrochloric acid.And the sale of by-product hydrochloric acid is subject to the impact in season, in unsalable season, due to hydrochloric acid dull sale, seriously constrain the normal production of Methanesulfonyl chloride and methylsulphonic acid.Same problem also exists in the project of other by-product hydrochloric acids.Such as, the production of potassium sulfate will be subject to the restriction of by-product hydrochloric acid.
Therefore, in the production of methylsulphonic acid, the economy in raw material chlorine source, the problem of outlet of security and by-product hydrochloric acid are the determinatives of methylsulphonic acid manufacture.How by-product hydrochloric acid is carried out recycle, turn waste into wealth, reduce production cost and the security risk of methylsulphonic acid, there is very real meaning.
Summary of the invention
The object of the invention is to: the by-product hydrochloric acid in utilizing methylsulphonic acid to prepare prepares methylsulphonic acid, realizes the recycle of hydrochloric acid, reduce production cost and the security risk of methylsulphonic acid.
Recycle by-product hydrochloric acid prepares a method for methylsulphonic acid, and its step is as follows:
1. by-product concentrated hydrochloric acid, is utilized to prepare chlorine
In corrosion-resistant container, add by-product concentrated hydrochloric acid, be heated to 40 DEG C.Slowly add manganese dioxide powder, start and stir.Along with the consumption of hydrochloric acid, progressively raise temperature of reaction to 90 DEG C.Obtain chlorine and manganese chloride solution.Chlorine is overflowed, and the chlorine of effusion carries a small amount of hydrogenchloride and water vapour secretly, by the mixed gas of this effusion through glass or graphite condenser, the temperature of mixed gas is reduced, and collects phlegma, recycle.Main containing chlorine and hydrogenchloride in gained mixed gas.
Its reaction is as follows:
MnO
2+ 4H
++ Cl
-=Mn
2++ Cl
2(gas)+2H
2o
Described by-product concentrated hydrochloric acid, being the by-product hydrochloric acid in Methanesulfonyl chloride and methylsulphonic acid production process, also can be from other industrial by-product hydrochloric acid, the by-product concentrated hydrochloric acid in such as potassium sulfate production process.This by-product hydrochloric acid is without organic impurity, and purity is high, and source is sufficient.
Described Manganse Dioxide, from potassium permanganate oxidation technique tankage or other Manganse Dioxide of originating.
The temperature of reaction of hydrochloric acid and Manganse Dioxide is 40 DEG C-90 DEG C.Temperature is too high, and hydrogenchloride overflows in a large number; Temperature is too low, and be unfavorable for hydrochloric acid and Manganse Dioxide reaction, chlorine yields poorly.The mode progressively heated up is adopted to react.When beginning concentration of hydrochloric acid is higher, temperature should be low, and along with the reduction of concentration of hydrochloric acid, temperature progressively raises.
2., the preparation of Manganous chloride tetrahydrate
1. step is obtained manganese chloride solution reduction vaporization condensing crystal, obtain Manganous chloride tetrahydrate crystal.The gas of evaporation, after condensation, is dilute hydrochloric acid solution; This dilute hydrochloric acid solution recycles as chlorine hydride absorbent;
3., the preparation of Methanesulfonyl chloride
In reactor, add Methyl disulfide, saturated concentrated hydrochloric acid and emulsifying agent, stir, cool to less than 20 DEG C, the chlorine 1. obtained by step and chlorine hydride mixed gas body import reactor bottom reactor, obtain Methanesulfonyl chloride and by-product hydrogen chloride.
Described concentrated hydrochloric acid, mass percent should be greater than 37%.Its objective is and in reaction system, bring reactant with the form of hydrochloric acid into---water.Adopting the form of concentrated hydrochloric acid to bring water into, is react the hydrogen chloride gas produced meet water liberated heat to reduce the hydrogen chloride gas and chlorine carried secretly in passed into chlorine and Methyl disulfide.Said by-product concentrated hydrochloric acid, being the by-product hydrochloric acid in Methanesulfonyl chloride and methylsulphonic acid production process, also can be from other industrial by-product hydrochloric acid, the by-product concentrated hydrochloric acid in such as potassium sulfate production process.This by-product hydrochloric acid is without organic impurity, and purity is high, and source is sufficient.
Manganse Dioxide and concentrated hydrochloric acid are obtained by reacting chlorine, and chlorine directly imports after condensation, and in time by Methyl disulfide absorption reaction, namely chlorine produce and namely use; In order to chlorine is consumed utilization in time, the chlorination tank of two or more Methyl disulfide is set simultaneously, adopts the operation of major-minor still, when a chlorination tank is reacted to terminal, in time chlorine is switched to another chlorination tank and continues reaction.
Its reaction is as follows:
5Cl
2+CH
3SSCH
3+4H
2O=2CH
3SO
2Cl+8HCl
4., the preparation of methylsulphonic acid
Methanesulfonyl chloride step 3. obtained adds in reactor, continues to pass into saturated steam, be hydrolyzed under stirring, obtains methylsulphonic acid and by-product hydrogen chloride.
5., the preparation of by-product concentrated hydrochloric acid
By the by-product hydrogen chloride gas that 3. and 4. step obtains, by vapor-liquid separation after freezing, as utilized wire mesh demister to carry out purification process, absorption agent falling film absorption is then adopted to obtain the concentrated hydrochloric acid of 37%; By step 1. in the phlegma that obtains be merged into recycle in this concentrated hydrochloric acid.
Described absorption agent is the dilute hydrochloric acid solution that step is 2. obtained.
6. the concentrated hydrochloric acid, by step 5. obtained, together with supplementing the potassium sulfate by-product hydrochloric acid of interpolation, reacts with Manganse Dioxide, obtains chlorine, and circulation step 1. extremely 5..
Wherein, step 1.: due to concentrated hydrochloric acid and Manganse Dioxide reaction, a chlorine element part is converted into chlorine, and a part transfers Manganous chloride tetrahydrate to.Therefore, preparing methylsulphonic acid for realizing stablizing, also needing additionally to supplement a part of hydrochloric acid; The said extra hydrochloric acid supplemented is from other industrial by-product hydrochloric acid, and the by-product hydrochloric acid of preferably sulfuric acid potassium production process, this by-product hydrochloric acid is not containing organism, and purity is higher.
Wherein, step 1.: the chlorine tail gas of hydrochloric acid and Manganse Dioxide preparation effusion can carry a part of water vapour and hydrogenchloride effusion secretly.Hydrogenchloride and water vapour are for reaction not any disadvantageous effect of chlorine and Methyl disulfide, but, because chlorine has certain temperature, and can thermopositive reaction be there is in water vapour chance concentrated hydrochloric acid, and chlorine and Methyl disulfide are reacted and need be carried out at low temperatures, therefore, need to lower the temperature to chlorine tail gas.After cooling, the water vapour in tail gas and hydrogen chloride condensed are hydrochloric acid soln, and this phlegma is capable of circulation to be applied mechanically.
Wherein, step 3.: the water miscible liquid reaction needed of chlorine and Methyl disulfide is carried out at low temperatures.Hydrogenchloride in tail gas and chlorine and Methyl disulfide react the hydrogenchloride produced water-soluble time release a large amount of heat, therefore, the water miscible liquid of Methyl disulfide need be prepared by concentrated hydrochloric acid and Methyl disulfide, like this, just reduce or avoid the generation of hydrogenchloride Heat of fusion, reduce energy consumption.
Wherein, step 3.: the reaction process of Methyl disulfide and chlorine and Methanesulfonyl chloride hydrolysis are prepared in the process of methylsulphonic acid, produce a large amount of hydrogenchloride, through falling film absorption, obtain the concentrated hydrochloric acid of more than 37%, this concentrated hydrochloric acid recycle.
The square ratio juris that a kind of recycle of the present invention by-product hydrochloric acid prepares methylsulphonic acid is: the method adopting " hydrogenchloride → chlorine → methylsulphonic acid → hydrogenchloride ", utilize the by-product hydrochloric acid produced in methylsulphonic acid preparation process to be converted into methylsulphonic acid and produce necessary raw material chlorine, realize the conversion and cycle of " hydrochloric acid → chlorine → hydrochloric acid ".The present invention utilizes the by-product hydrochloric acid of methylsulphonic acid or the by-product hydrochloric acid in other sources and Manganse Dioxide to react, and obtain Manganous chloride tetrahydrate and chlorine, the Manganous chloride tetrahydrate of gained is the main raw material of electrolytic manganese.The chlorine obtained imports in the middle of the emulsion of Methyl disulfide after condensation, carries out oxychlorination, obtains Methanesulfonyl chloride and by-product hydrogen chloride, and Methanesulfonyl chloride continues hydrolysis and obtains methylsulphonic acid and by-product hydrogen chloride.Obtained by-product hydrogen chloride is carried out the absorption of falling liquid film water, obtain by-product concentrated hydrochloric acid.The by-product concentrated hydrochloric acid obtained is together with the by-product concentrated hydrochloric acid of supplementary interpolation, and Manganse Dioxide reaction, obtains Manganous chloride tetrahydrate and chlorine.The by-product hydrochloric acid that so just can circulate prepares methylsulphonic acid, simultaneously main raw material---the Manganous chloride tetrahydrate of by-product electrolytic manganese.
A kind of advantage utilizing by-product hydrochloric acid to prepare the method for methylsulphonic acid of the present invention is: adopt by-product hydrochloric acid to prepare chlorine, and direct and Methyl disulfide is reacted, and avoids purchase, transports and store security risk and the logistics cost of hypertoxic chlorine; To the by-product hydrochloric acid digestibility and utilization on the spot sold be difficult to, and turn waste into wealth, become the main raw material(s) preparing methylsulphonic acid, achieve the recycle of chlorine element.Simultaneously, by the utilization of waste material of reacted for potassium permanganate oxidation tankage Manganse Dioxide, prepare Manganous chloride tetrahydrate, can be used for electrolytic manganese, greatly reduce production cost and the security risk of methylsulphonic acid, also eliminate the chlorine in methylsulphonic acid preparation and these two large restraining factors of by-product hydrochloric acid simultaneously.
Embodiment
Come to be further described content of the present invention further below by some examples, but the present invention is not limited to following embodiment, anyly do not depart from spirit of the present invention and scope, and the amendment or change that it carries out equivalence is all encompassed among the scope of the claims of the present invention.
embodiment one:
Recycle by-product hydrochloric acid prepares a method for methylsulphonic acid, and its step is as follows:
1., in two enamel reaction stills, add the by-product hydrochloric acid that 250kg Methyl disulfide and 500kg concentration are the methylsulphonic acid of 37% respectively, pass into salt solution in chuck, cool to 15 DEG C, stand-by.In reactor tail gas pipeline, condenser and falling-film absorber are set, to purify and to absorb by-product hydrochloric acid.
The by-product hydrochloric acid 10000kg of the methylsulphonic acid of 37% is put into 15m
3reaction tank in, open stir, in pond, pass into water vapor, be heated to 50 DEG C.Slowly Manganse Dioxide is added in pond.Tail gas, after graphite condenser condensation, passes into Methyl disulfide water miscible liquid bottom one of them enamel reaction still through surge tank.Control rate of feeding and the chuck inner salt water circulating speed of Manganse Dioxide, the temperature of reaction of Methyl disulfide is controlled within 20 DEG C.Hydrogen chloride tail gas is falling film absorption after condensation cleaning.React 8 hours, sampling analysis, chlorination reaction is to terminal.
2., by chlorine be switched to another enamel still, continue to react with Methyl disulfide emulsion wherein.
3., by the enamel still being reacted to terminal leave standstill and isolate crude product Methanesulfonyl chloride in two hours, through rectification and purification, obtain the Methanesulfonyl chloride finished product 540kg of 99.8%.
4., by 540kg Methanesulfonyl chloride put in the enamel reaction still being provided with tail gas falling film absorbing device, open and stir, in reactor, pass into the water vapour of 140kg.Hydrogen chloride tail gas obtains the hydrochloric acid of 37% through falling film absorption.React after 5 hours, dechlorination, obtain water white 70.2% methylsulphonic acid solution 630kg.
5., 15m is treated
3reaction tank in when not having chlorine to overflow, be reacted to terminal, reaction solution taken out, reduction vaporization condensing crystal.Evaporated liquor graphite film-falling absorption tower absorbs, and obtains dilute hydrochloric acid solution.This dilute hydrochloric acid solution is for subsequent use as the absorption agent of hydrogenchloride.
Collect the 37% concentrated hydrochloric acid 4700kg. obtained, 4.2% dilute hydrochloric acid 2610kg.
embodiment two:
1., in two enamel reaction stills, add the by-product hydrochloric acid that 300kg Methyl disulfide and 600kg are the methylsulphonic acid of 37% from the concentration of embodiment one respectively, pass into salt solution in chuck, cool to 15 DEG C, stand-by.In reactor tail gas pipeline, condenser and falling-film absorber are set, to purify and to absorb by-product hydrochloric acid; The dilute hydrochloric acid solution of 4.2% of embodiment one collection is added in tourie.
The by-product hydrochloric acid 4700kg of the methylsulphonic acid of embodiment one 37% and 37% by-product hydrochloric acid of 5300kg Production of Potassium Sulphate are put into 15m
3reaction tank in, open stir, in pond, pass into water vapor, be heated to 40 DEG C.
Slowly Manganse Dioxide is added in pond.Tail gas, after graphite condenser condensation, passes into Methyl disulfide water miscible liquid bottom one of them enamel reaction still through surge tank.Control the intake of water vapour, make temperature of reaction slowly rise to 90 DEG C, control rate of feeding and the chuck inner salt water circulating speed of Manganse Dioxide, the temperature of reaction of Methyl disulfide is controlled within 20 DEG C.Hydrogen chloride tail gas is falling film absorption after condensation cleaning.
React 9 hours, sampling analysis, chlorination reaction is to terminal.
2., by chlorine be switched to another enamel still, continue to react with Methyl disulfide emulsion wherein.
3., by the enamel still being reacted to terminal leave standstill and isolate crude product Methanesulfonyl chloride in two hours, through rectification and purification, obtain the Methanesulfonyl chloride finished product 650kg of 99.8%.
4., by 650kg Methanesulfonyl chloride put in the enamel reaction still being provided with tail gas falling film absorbing device, open and stir, in reactor, pass into the water vapour of 180kg.Hydrogen chloride tail gas obtains the hydrochloric acid of 37% through falling film absorption.React after 6 hours, dechlorination, obtain water white 70.16% methylsulphonic acid solution 750kg.
embodiment three:
1., to 15m
3drop into methylsulphonic acid and the potassium sulfate by-product hydrochloric acid of 37% of 10000kg in reaction tank, water vapour is heated to 40 DEG C.
2., in enamel reaction still, drop into 550kg Methyl disulfide and 500kg potassium sulfate by-product 37% concentrated hydrochloric acid, be cooled to 20 DEG C.
3. 2500kg Manganse Dioxide, is slowly added to 15m
3in reaction tank, open steam, be slowly warmed up to 90 DEG C, by reaction end gas after graphite condenser cooling, then pass into through surge tank and fill in the enamel still of Methyl disulfide.
4., after 7 hours, to 15m
3reaction tank supplements the by-product hydrochloric acid of 2 ton 37%, and keeps temperature 60 C in pond---90 DEG C, continue reaction; After 15 hours, Manganse Dioxide feeds intake complete.
5., sampling analysis, Methyl disulfide reaction complete.Chlorine residue is switched to secondary still, and collect resultant of reaction crude product Methanesulfonyl chloride, rectification and purification, obtains 1200kg Methanesulfonyl chloride, and through gas chromatographic analysis, its content is 99.81%; The hydrogenchloride produced in chlorination process removes liquid through freezing, silk screen, absorbs with the evaporation condensate of Manganous chloride tetrahydrate.
6., by gained Methanesulfonyl chloride pass into 800kg water vapour, hydrolysis obtains methylsulphonic acid and hydrogenchloride.The evaporation condensate of hydrogenchloride Manganous chloride tetrahydrate absorbs, and collects the dilute hydrochloric acid 3600kg of 37.2% concentrated hydrochloric acid 6500kg and 4.5%; Collect methylsulphonic acid 1450kg, content is 70.11%.
Claims (1)
1. recycle by-product hydrochloric acid prepares a method for methylsulphonic acid, it is characterized in that: it comprises the steps:
1. by-product concentrated hydrochloric acid, is utilized to prepare chlorine
In corrosion-resistant container, add by-product concentrated hydrochloric acid, be heated to 40 DEG C, slowly add manganese dioxide powder, start and stir, along with the consumption of hydrochloric acid, progressively raise temperature of reaction to 90 DEG C, obtain chlorine and manganese chloride solution; Chlorine is overflowed, and the chlorine of effusion carries a small amount of hydrogenchloride and water vapour secretly, by the mixed gas of this effusion through glass or graphite condenser, the temperature of mixed gas is reduced, collect phlegma, recycle, main containing chlorine and hydrogenchloride in gained mixed gas;
Its reaction is as follows:
MnO
2+ 4H
++ Cl
-=Mn
2++ Cl
2(gas)+2H
2o
2., the preparation of Manganous chloride tetrahydrate
1. step is obtained manganese chloride solution reduction vaporization condensing crystal, obtain Manganous chloride tetrahydrate crystal, the gas of evaporation, after condensation, is dilute hydrochloric acid solution; This dilute hydrochloric acid solution recycles as chlorine hydride absorbent;
3., the preparation of Methanesulfonyl chloride
In reactor, add Methyl disulfide, saturated concentrated hydrochloric acid and emulsifying agent, stir, cool to less than 20 DEG C, the chlorine 1. obtained by step and chlorine hydride mixed gas body import reactor bottom reactor, obtain Methanesulfonyl chloride and by-product hydrogen chloride;
4., the preparation of methylsulphonic acid
Methanesulfonyl chloride step 3. obtained adds in reactor, continues to pass into saturated steam, be hydrolyzed under stirring, obtains methylsulphonic acid and by-product hydrogen chloride;
5., the preparation of by-product concentrated hydrochloric acid
By the by-product hydrogen chloride gas that 3. and 4. step obtains, by vapor-liquid separation after freezing, utilize wire mesh demister to carry out purification process, then adopt absorption agent falling film absorption to obtain the concentrated hydrochloric acid of 37%; By step 1. in the phlegma that obtains be merged into recycle in this concentrated hydrochloric acid;
6. the concentrated hydrochloric acid, by step 5. obtained, together with supplementing the potassium sulfate by-product hydrochloric acid of interpolation, reacts with Manganse Dioxide, obtains chlorine, and circulation step 1. extremely 5..
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| CN104860268A (en) * | 2015-06-04 | 2015-08-26 | 中南大学 | Method for cyclic utilization of chlorine gas and coproduction of manganese chloride in chloride pyridine production process |
| CN106336365A (en) * | 2016-08-27 | 2017-01-18 | 唐山威格化学工业有限公司 | Production process of electroplating grade methanesulfonic acid |
| CN108310914A (en) * | 2017-01-18 | 2018-07-24 | 湖北星火化工有限公司 | The purification method of methylsufonyl chloride tail gas |
| CN106866469A (en) * | 2017-01-18 | 2017-06-20 | 湖北星火化工有限公司 | The processing method of pyrovinic acid tail gas |
| CN106831501A (en) * | 2017-01-18 | 2017-06-13 | 湖北星火化工有限公司 | A kind of continuity method prepares the production system of methylsufonyl chloride |
| CN110452112B (en) * | 2018-12-03 | 2022-03-25 | 山东民基新材料科技有限公司 | Catalytic hydrogenation treatment process for chloro pivaloyl chloride rectification residual liquid |
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Effective date of registration: 20220706 Address after: 432400 No. 20, the third development road, Changjiang port, Yingcheng City, Xiaogan City, Hubei Province Patentee after: Hubei Xinghuo (Yingcheng) Chemical Co.,Ltd. Address before: 432900 Xinghuo Fine Chemical Industrial Park, Xiaochang County, Xiaogan City, Hubei Province Patentee before: HUBEI XINGHUO CHEMICAL Co.,Ltd. |