CN101342441A - Method for treating tail gas of acyl chlorination - Google Patents
Method for treating tail gas of acyl chlorination Download PDFInfo
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- CN101342441A CN101342441A CNA200810147129XA CN200810147129A CN101342441A CN 101342441 A CN101342441 A CN 101342441A CN A200810147129X A CNA200810147129X A CN A200810147129XA CN 200810147129 A CN200810147129 A CN 200810147129A CN 101342441 A CN101342441 A CN 101342441A
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Abstract
The invention relates to a processing method of thionyl chloride acyl-chlorinated tail gas. Mixed tail gas produced by a acyl chlorinating process contains hydrogen chloride and sulfur dioxide; the sulfur dioxide is liquefied under a certain temperature condition; the incondensable hydrogen chloride and a little sulfur dioxide are absorbed in two stages by water; the absorbed tail gas in a first stage is pure hydrogen chloride gas; after being absorbed in a second stage, the qualified chlorhydric acid is obtained; first-stage falling film absorption liquid is resolved by heating; then the tail gas is sent to a liquefying process again; the liquid sulfur dioxide can be canned as a product; or after being vaporized, the liquid sulfur dioxide is absorbed by 30 percent of sodium hydroxide solution to obtain sodium sulfite aqueous solution which is further dried after low temperature crystallization or distillation to obtain 97 percent of sodium sulfite solid. With the method, the hydrogen chloride, the sulfur dioxide and a little thionyl chloride produced by an acyl chlorination synthetic process can be separated out to obtain the chlorhydric acid and the pure sodium sulfite solid. The processing method of the thionyl chloride acyl-chlorinated tail gas of the invention is capable of effectively recovering the thionyl chloride acyl-chlorinated tail gas, which has the advantages of safety process and easy control.
Description
Technical field
The present invention relates to a kind of processing method of thionyl chloride tail gas of acyl chlorination, realize separating, obtain hydrochloric acid and pure sodium sulfite solid by hydrogen chloride, sulfur dioxide and a spot of thionyl chloride that this method can produce the chloride building-up process.
Background technology
Acyl chlorides is the important intermediate of producing pyrethroid, and preparation process is to obtain the mixed tail gas of course of reaction by-product hydrogen chloride and sulfur dioxide by thionyl chloride and chrysanthemumic acid reaction.The common processing method of manufacturing enterprise is directly to absorb tail gas with liquid caustic soda now, obtains the waste water of high saliferous, with carrying out biochemical treatment after a large amount of clear water dilutions, does so not only and can not effectively reclaim the accessory substance of chloride process, and produce a large amount of waste water.Therefore need a kind of new technology effectively to reclaim the accessory substance of this course of reaction.
Summary of the invention
Processing method of the present invention can effectively reclaim the thionyl chloride tail gas of acyl chlorination, and process safety is easy to control.The tail gas that chloride produces is through condensation liquefaction, and the method that adopts secondary to absorb realizes sulfur dioxide and hydrogen chloride gas to separate.The concentration of mentioning among the present invention is mass percent concentration.
The technical solution adopted in the present invention is as follows:
Sulfur dioxide liquefaction after tail gas of acyl chlorination is lowered the temperature in the gas liquefaction device, the hydrogen chloride of incoagulability is carried a spot of sulfur dioxide water secretly and carry out the one-level falling film absorption in first grade absorption tower, hydrogen chloride reaches capacity very soon, the hydrogen chloride that continues to feed overflows from the aqueous solution and obtains pure hydrogen chloride gas, and sulfur dioxide continues to be dissolved in the water because concentration is lower; The hydrogen chloride gas that overflows from first grade absorption tower water again carries out obtaining 30～35% hydrochloric acid after the secondary falling film absorption two-level absorption tower.The one-level absorption liquid is warming up to 90～95 ℃ and resolves in Analytic Tower, and the gas of parsing enters the tail gas liquefying plant, and desorbed solution returns first grade absorption tower as lyosoption.
Liquid sulfur dioxide makes product or heat up vaporization in the sulfur dioxide vaporizer after can be canned, sulfur dioxide gas feeds 30% sodium hydroxide solution absorption, obtain sodium sulfite aqueous solution, low temperature crystallization or distillation generate the sodium sulfite crystal, in centrifugal device, separate, moisture is removed in oven dry, obtains 97% sodium sulfite solid.
In this technical process, mixed tail gas is cooled in the boiling point of sulfur dioxide, generally can be controlled in-10～-50 ℃, is controlled at-20～-30 ℃ usually.Usually contain sulfur dioxide 1～2% in the hydrogen chloride gas of incoagulability.The concentration of sulfur dioxide need be controlled in 8% in the one-level absorption liquid, and optimum control is 3～5%, and one-level falling film absorption temperature is 20～30 ℃ in the first grade absorption tower.Too high can the overflowing equally of content of sulfur dioxide enters the absorption of hydrogen chloride secondary in the one-level absorption liquid, and the content of hydrochloric acid is reclaimed in final influence.
The concentration of sulfur dioxide preferably is controlled at 3～5% in the described one-level absorption liquid, and when reaching this concentration, the one-level absorption liquid can begin extraction, and adds water according to produced quantity; To guarantee that the content of sulfur dioxide of overflowing is 0 from first grade absorption tower.
The preference temperature that secondary absorbs is 20～30 ℃, and the ultimate density of absorption liquid is controlled at 30～35%.
Alkali absorbs with 30% NaOH as absorbing medium, absorbs 0～10 ℃ of temperature, and process has more sodium sulfite solid to separate out, logical sulfur dioxide gas is to neutral, this absorption liquid decrease temperature crystalline, the temperature of crystallization is at-5～15 ℃ usually, and optimum temperature is 0～5 ℃.
Extract the another kind of method of sodium sulfite, directly water is steamed the sodium sulfite solid that obtains white powdery.Still-process may have the part sodium sulfite and be oxidized to sodium sulphate, and process need carries out secluding air, can be with nitrogen protection or vacuum distillation.
The concentration of mentioning among the present invention is mass percent concentration.
The hydrogen chloride, the sulfur dioxide that adopt method of the present invention the chloride building-up process can be produced are realized separating, and obtain hydrochloric acid and pure sodium sulfite solid.Method of the present invention directly absorbs the accessory substance of the more effective recovery chloride of tail gas method process than liquid caustic soda in the prior art, and process safety is easy to control, and avoids producing a large amount of waste water, reduces environment is polluted.
Description of drawings
The process chart that Fig. 1 absorbs for the thionyl chloride tail gas of acyl chlorination. Dioxy after tail gas of acyl chlorination is lowered the temperature in the gas liquefaction device Change sulphur liquefaction, the hydrogen chloride of incoagulability is carried a small amount of sulfur dioxide water secretly and carry out one-level falling film absorption, chlorine in first grade absorption tower Change hydrogen and reach capacity very soon, the hydrogen chloride that continues to pass into overflows from the aqueous solution and obtains pure hydrogen chloride gas, and sulfur dioxide Because concentration is lower, continues to be dissolved in the water; The hydrogen chloride gas that overflows from first grade absorption tower again water advances two-level absorption tower Obtain 30～35% hydrochloric acid after the row secondary falling film absorption. Contain sulfur dioxide and 10% left side about 3～5% in the one-level absorption liquid Right hydrogen chloride, this absorption liquid is warming up to 90～95 ℃ and resolves in Analytic Tower, and the gas of parsing enters the tail gas liquefying plant, separates Analyse liquid and return first grade absorption tower as lyosoption.
Liquid sulfur dioxide makes product or the vaporization that heats up after can be canned in the sulfur dioxide vaporizer, sulfur dioxide gas passes into 30% sodium hydroxide solution absorbs, and obtains sodium sulfite aqueous solution, and low temperature crystallization or distillation generate the sodium sulfite crystal, from Separate in the center device, moisture is removed in oven dry, obtains 97% sodium sulfite solid.
The specific embodiment
Be specific embodiments of the invention below:
The absorption and separation of embodiment 1 hydrogen chloride gas
The tail gas of acyl chlorination of dichlor chrysanthemic acid enters the tail gas cooling system continuously, and system temperature is controlled at-25 ℃, detects tail gas, and sulfur dioxide is 1.3%, and hydrogen chloride is 98.7%, and liquid sulfur dioxide content is greater than 99%.Hydrogen chloride gas enters one-level falling film absorption system, and absorbing temperature is 20～23 ℃.Content of sulfur dioxide raises gradually in the one-level absorption liquid, when content of sulfur dioxide reaches 5%, begins to have sulfur dioxide gas to occur in the tail gas that overflows, and the one-level absorption liquid begins extraction, and adds water according to produced quantity.The testing result content of sulfur dioxide is 0 in the tail gas that overflows.Hydrogen chloride gas enters secondary and absorbs, and absorbs 20～22 ℃ of temperature, obtains 30～35% hydrochloric acid.
The absorption and separation of embodiment 2 hydrogen chloride gas
The tail gas of acyl chlorination of dichlor chrysanthemic acid enters the tail gas cooling system continuously, and system temperature is controlled at-30 ℃, detects the tail gas of on-condensible gas, and sulfur dioxide is 0.8%, and hydrogen chloride is 99.2%, and liquid sulfur dioxide content is greater than 99%.Hydrogen chloride gas enters one-level falling film absorption system, and absorbing temperature is 20～23 ℃.Content of sulfur dioxide raises gradually in the one-level absorption liquid, and sulfur dioxide is increased to and began extraction one-level absorption liquid at 4% o'clock, and adds water according to produced quantity.The testing result content of sulfur dioxide is 0 in the tail gas that overflows.Hydrogen chloride gas enters secondary and absorbs, and absorbs 20～22 ℃ of temperature, obtains 30～35% hydrochloric acid.
The preparation of embodiment 3 sodium sulfites
Sulfur dioxide liquid is warming up to 0 ℃, there is gas to emit gradually, in the sodium hydroxide solution with this gas feeding 30%, the continuous pH value that passes to system is 6～7, and the sodium sulfite aqueous solution that obtains enters crystal system, is cooled to 2 ℃, be incubated after 30 minutes, centrifugal, to moisture less than 0.2%, analyzing content is 97.9% with oven for drying
The preparation of embodiment 4 sodium sulfites
Get the sodium sulfite aqueous solution that embodiment 3 obtains, the band vacuum is to 10mmHg, and with steam intensification precipitation to 80 ℃, sample analysis content is 97.2%.
The preparation of embodiment 5 sodium sulfites
Get the sodium sulfite aqueous solution that embodiment 3 obtains, normal pressure heats up and dewaters, and process is with feeding nitrogen protection, and continuous taking off to 150 ℃ obtains white crystals thing sodium sulfite, and analyzing content is 97.3%.
The parsing of embodiment 6 one-level absorption liquids
The one-level absorption liquid that embodiment 2 obtains is warming up to 90 ℃ and resolves in Analytic Tower, and desorption gas enters the absorption and separation system, resolves the residue analysis, and containing sulfur dioxide is 0.1%, and containing hydrogen chloride is 1.3%; This desorption gas enters the tail gas liquefying plant, and this desorbed solution returns first grade absorption tower as lyosoption.
Claims (10)
1, a kind of method of handling the thionyl chloride tail gas of acyl chlorination mainly comprises following operating procedure:
(1) sulfur dioxide liquefaction after tail gas of acyl chlorination is lowered the temperature in the gas liquefaction device, the hydrogen chloride of incoagulability is carried a spot of sulfur dioxide water secretly and carry out the one-level falling film absorption in first grade absorption tower, hydrogen chloride reaches capacity very soon, the hydrogen chloride that continues to feed overflows from the aqueous solution and obtains pure hydrogen chloride gas, and sulfur dioxide continues to be dissolved in the water because concentration is lower; The hydrogen chloride gas that overflows from first grade absorption tower water again carries out obtaining hydrochloric acid after the secondary falling film absorption two-level absorption tower; Described one-level absorption liquid heats up and resolves in Analytic Tower, and the gas of parsing enters the tail gas liquefying plant, and desorbed solution returns first grade absorption tower as lyosoption;
(2) Ye Tai sulfur dioxide makes product after can be canned, or the vaporization that in the sulfur dioxide vaporizer, heats up, sulfur dioxide gas feeds sodium hydroxide solution and absorbs, obtain sodium sulfite aqueous solution, low temperature crystallization or distillation generate the sodium sulfite crystal, separate in centrifugal device, moisture is removed in oven dry, obtains the sodium sulfite solid.
2, the temperature range of tail gas of acyl chlorination cooling is-10～-50 ℃ in the method according to claim 1, described step (1); The concentration of sulfur dioxide is controlled in 8% in the described one-level absorption liquid; Described carrying out in two-level absorption tower obtains 30～35% hydrochloric acid after the secondary falling film absorption; Described one-level absorption liquid is warming up to 90～95 ℃ and resolves in Analytic Tower; Sulfur dioxide gas feeds 30% sodium hydroxide solution absorption in the described step (2); Moisture is removed in described oven dry, obtains 97% sodium sulfite solid.
3, the temperature range of tail gas of acyl chlorination cooling is-20～-30 ℃ in the method according to claim 2, described step (1).
4, the temperature that one-level absorbs in the method according to claim 1, described step (1) is 20～30 ℃.
5, the concentration optimum control of sulfur dioxide is 3～5% in the one-level absorption liquid in the method according to claim 2, step (1), and when reaching described concentration, the one-level absorption liquid begins extraction, and adds water according to produced quantity.
6, the temperature that secondary absorbs in the method according to claim 1, described step (1) is 20～30 ℃.
7, method according to claim 1, the temperature that described NaOH absorbs sulfur dioxide is 0～10 ℃.
8, method according to claim 1, the low temperature crystallization temperature of described sodium sulfite is-5～15 ℃.
9, method according to claim 8, the low temperature crystallization temperature of described sodium sulfite is 0～5 ℃.
10, method according to claim 1 adopts nitrogen protection or vacuum distillation in the still-process of described sodium sulfite.
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| CN102093197A (en) * | 2009-12-14 | 2011-06-15 | 烟台氨纶股份有限公司 | Method for preparing aromatic dimethyl chloride |
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Effective date of registration: 20201123 Address after: 225009 No. 39, Wenfeng Road, Yangzhou, Jiangsu Patentee after: JIANGSU YANGNONG CHEMICAL Co.,Ltd. Patentee after: JIANGSU YOUTH CHEMICAL Co.,Ltd. Patentee after: JIANGSU YOUJIA PLANT PROTECTION Co.,Ltd. Address before: 225009 No. 39, Wenfeng Road, Yangzhou, Jiangsu Patentee before: JIANGSU YANGNONG CHEMICAL Co.,Ltd. Patentee before: JIANGSU YOUTH CHEMICAL Co.,Ltd. |