CN102241398B - Method and extraction machine for purifying carbon disulfide - Google Patents
Method and extraction machine for purifying carbon disulfide Download PDFInfo
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- CN102241398B CN102241398B CN201110122810A CN201110122810A CN102241398B CN 102241398 B CN102241398 B CN 102241398B CN 201110122810 A CN201110122810 A CN 201110122810A CN 201110122810 A CN201110122810 A CN 201110122810A CN 102241398 B CN102241398 B CN 102241398B
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- purification
- jolting
- dithiocarbonic anhydride
- carbon disulfide
- separating flask
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Abstract
The invention discloses a purification method of carbon disulfide. The purification method comprises the following steps: 1) mixing carbon disulfide to be extracted as well as concentrated sulfuric acid and paraformaldehyde used as extracting agents in a mass ratio of 1: (0.18-0.2): (0.018-0.02); 2) thoroughly shaking the mixed liquor; 3) stopping shaking, standing, discharging the lower acid layer after the mixed liquor is fully layered; 4) fully washing the upper-layer material in the step 3) with water, then standing and layering, and sucking upper-layer water; and 5) repeating the step 4). In addition, the invention also discloses an extraction machine for carbon disulfide purification. Through the purification method provided by the invention, the benzene content in carbon disulfide can be decreased from 1% to below 0.01% by once extraction purification, the consumption is small, the cost is low, and purified carbon disulfide can fully meet chromatographically pure indexes.
Description
Technical field
The present invention relates to the purification of organic chemical industry's product, specific equipment is used in the method for purification and the purification that particularly relate to a kind of dithiocarbonic anhydride.
Background technology
Chromatographically pure dithiocarbonic anhydride often uses as strippant in environmental protection tests, therefore the foreign matter content in the dithiocarbonic anhydride is required very sternly, and particularly benzene content must be less than just can using below 0.02%, otherwise can influence the accuracy of detected result.And benzene content can't use without purifying all between 0.9%～1% at all in the dithiocarbonic anhydride of selling in the market.
Purification dithiocarbonic anhydride generally adopts distillation method and extraction process at present.It is to utilize the difference of various boiling point substances to carry out the impurity separation that distillation method is purified, and there is following shortcoming in it: the material that 1, boiling point is close is difficult to thoroughly separate; 2, receive temperature in the still-process, heat up in a steamer the influence of speed fluctuation, be easy to cause mechanical entrapment, impurity is and then steamed together, influence separating effect and quality product.Facts have proved, adopt single flash purification dithiocarbonic anhydride not reach the chromatographically pure requirement at all.Through the repeated multiple times distillation, benzene content also can only be dropped to about 0.08% by 1% in the raw material, does not only reach the chromatographically pure index, and consumption is big, cost is high.In addition, because electrically heated is adopted in distillation, dithiocarbonic anhydride is again utmost point inflammable substance, and fire hazard is big, and is very dangerous.When using extraction process to purify; Use the vitriol oil-formaldehyde to be extraction agent, the ratio that proportion of raw materials is about dithiocarbonic anhydride, the vitriol oil, formaldehyde is 1: 0.15: 0.03 (mass ratio), 15～20 minutes standing demix of shaking out; Discard the acid layer; Stay the curing carbon-coating, with pure water washing 3～4 times, tell dithiocarbonic anhydride at last then as finished product.The problem that extraction process purification dithiocarbonic anhydride exists is: selecting the vitriol oil-formaldehyde for use is extraction agent; Though warp is purification by liquid extraction repeatedly; The content of benzene also can only drop to 0.05% in the dithiocarbonic anhydride, does not still reach the requirement of chromatographically pure index 0.02%, and raw materials consumption is big when repeatedly extracting in addition, cost is high.
Summary of the invention
The purpose of this invention is to provide a kind of consume little, cost is low, can satisfy the dithiocarbonic anhydride method of purification that environmental protection tests requires fully.
For this reason, technical scheme of the present invention is following:
A kind of method of purification of dithiocarbonic anhydride may further comprise the steps:
1) dithiocarbonic anhydride, the vitriol oil and Paraformaldehyde 96 being pressed mass ratio 1: 0.18～0.2: 0.018～0.02 mixes;
2) mixed solution is carried out shake well;
3) stop jolting, leave standstill, treat abundant layering after, emit the acid layer that is positioned at lower floor;
4) the upper strata material in the step 3) is fully washed, left standstill then, layering, the water on sucking-off upper strata;
5) repeating step 4).
Preferably, the mass ratio of said dithiocarbonic anhydride, the vitriol oil, Paraformaldehyde 96 is 1: 0.18: 0.018.
Said step 2) the jolting mode in is: rotate up and down with certain rotating speed, after the certain time, rotating is alternately changed once, continuous in this way jolting for some time.Preferred jolting mode is: PM rotation 30 is changeed, continue after 10 minutes rotating alternately conversion once, jolting 1 hour continuously in this way.
Preferably, during washing, the mass ratio of pure water and washings is 1: 3, and in step 5), the multiplicity of step 4) is 3～4 times.
A kind of extracter of dithiocarbonic anhydride purification usefulness; Comprise separating flask, separating flask support, motor, two-position controller and transmission rig; Said separating flask comprises bottle, be separately positioned on upper and lower fluid inlet of bottle and liquid outlet and be arranged on the venting port on bottle top; One vertical and be fixedly installed on the bottle side wall; This axle supports through said support rotationally, and said transmission rig makes the jolting in a certain way of said separating flask through motor and described axle under the control of said two-position controller.
Said transmission rig comprises the driving toothed gear that is installed on the motor output shaft, is installed in the follower gear and the chain that be connected said driving toothed gear and follower gear of said axle away from separating flask one end.
The concentration proportioning of extraction agent is very important; In this method of purification; With the vitriol oil-Paraformaldehyde 96 is that the principle of extraction agent is to utilize benzene in the environment of the vitriol oil, can sufficient chemical reaction take place with Paraformaldehyde 96; Generate a kind of red compound, and this compound is easy to be dissolved in fully in the vitriol oil, so just can from dithiocarbonic anhydride, benzene be extracted fully.
It is extraction agent that method of purification of the present invention is selected the vitriol oil-Paraformaldehyde 96 for use; Through single extraction purify the content can make benzene in the dithiocarbonic anhydride from 1% be reduced to below 0.01%, the dithiocarbonic anhydride main content can bring up to more than 99% from 97%; Not only consume little, cost is low; And can reach the chromatographically pure index fully, fully satisfied the environmental protection tests requirement.
Embodiment
Below in conjunction with specific embodiment dithiocarbonic anhydride method of purification of the present invention is elaborated.
At first as shown in Figure 1; The extracter of dithiocarbonic anhydride purification usefulness of the present invention comprises separating flask, separating flask support 21, motor 11, two-position controller 12 and transmission rig; The venting port 17 that said separating flask comprises bottle 10, is separately positioned on the upper and lower fluid inlet of bottle 18, liquid outlet 20 and is arranged on bottle top; Axle 16 is vertical and be fixedly installed on the sidewall of bottle 10; And supports rotationally through support 21, said transmission rig comprises the driving toothed gear that is installed on motor 11 output shafts (among the figure sign), is installed in 16 a follower gear 14 and the chain that is connected said driving toothed gear and follower gear 13 away from separating flask one end.Said transmission rig makes separating flask jolting in a certain way through motor 11 and axle 16 under the control of two-position controller 12.
Embodiment 1
Separating flask lower end drain hole joint door is closed, open upper end opening for feed joint door and venting joint door simultaneously.Inject about 20 liters dithiocarbonic anhydride raw material and about 2500 milliliters of the vitriol oil that contains 10% Paraformaldehyde 96 for preparing in advance from opening for feed, the ratio that above-mentioned each amount promptly is equivalent to dithiocarbonic anhydride, the vitriol oil, Paraformaldehyde 96 three is 1: 0.18: 0.018 (mass ratio of pure substance).
Close opening for feed joint door and venting joint door.The start jolting; Extracter changes, whenever replaces the conversion continuous jolting of mode once 1 hour at a distance from rotating in 10 minutes with PM 30 by pre-designed program, stops to leave standstill 30 minutes after the jolting; After treating abundant layering; Open upper end venting joint door, slowly emit red acid layer, close blowing joint door then from following drain hole.
Washing: open upper end opening for feed joint door and venting joint door, from opening for feed, inject the pure water (about 6000-7000 milliliter) that is equivalent to raw material 1/3, close opening for feed joint door and venting joint door.Start jolting 40 minutes stops jolting, leaves standstill half a hour, after the layering, opens charging joint door,, uses with quadrat method washing 3 times the water layer sucking-off with siphonage, get final product about 19 liters of chromatographically pure dithiocarbonic anhydride, productive rate is more than 95%.Product is through assay, and each item index all reaches the chromatographically pure standard.
Embodiment 2
Separating flask lower end drain hole joint door is closed, open upper end opening for feed joint door and venting joint door simultaneously.Inject about 20 liters dithiocarbonic anhydride raw material and about 2800 milliliters of the vitriol oil that contains 10% Paraformaldehyde 96 for preparing in advance from opening for feed, the ratio that above-mentioned each amount promptly is equivalent to dithiocarbonic anhydride, the vitriol oil, Paraformaldehyde 96 three is 1: 0.2: 0.02 (mass ratio of pure substance).
Close opening for feed joint door and venting joint door.The start jolting; Extracter changes, whenever replaces the conversion continuous jolting of mode once 1 hour at a distance from rotating in 10 minutes with PM 30 by pre-designed program, stops to leave standstill 30 minutes after the jolting; After treating abundant layering; Open upper end venting joint door, slowly emit red acid layer, close blowing joint door then from following drain hole.
Washing: open upper end opening for feed joint door and venting joint door, from opening for feed, inject the pure water (about 6000-7000 milliliter) that is equivalent to raw material 1/3, close opening for feed joint door and venting joint door.Start jolting 30 minutes stops jolting, leaves standstill half a hour, after the layering, opens charging joint door,, uses with quadrat method washing 4 times the water layer sucking-off with siphonage, get final product about 19 liters of chromatographically pure dithiocarbonic anhydride, productive rate is more than 95%.Product is through assay, and each item index all reaches the chromatographically pure standard.
Claims (8)
1. the method for purification of a dithiocarbonic anhydride may further comprise the steps:
1) dithiocarbonic anhydride, the vitriol oil and Paraformaldehyde 96 being pressed mass ratio 1: 0.18～0.2: 0.018～0.02 mixes;
2) mixed solution is carried out shake well;
3) stop jolting, leave standstill, treat abundant layering after, emit the acid layer that is positioned at lower floor;
4) the upper strata material in the step 3) is fully washed, left standstill then, layering, the water on sucking-off upper strata;
5) repeating step 4).
2. method of purification according to claim 1 is characterized in that: the mass ratio of said dithiocarbonic anhydride, the vitriol oil, Paraformaldehyde 96 is 1: 0.18: 0.018.
3. method of purification according to claim 1 is characterized in that step 2) in the jolting mode be: rotate up and down with certain rotating speed, after the certain time, rotating alternately conversion once, jolting for some time continuously in this way.
4. method of purification according to claim 1 is characterized in that step 2) in the jolting mode be: PM rotation 30 is changeed, continue after 10 minutes rotating alternately conversion once, jolting 1 hour continuously in this way.
5. method of purification according to claim 1 is characterized in that: during washing, the mass ratio of pure water and washings is 1: 3.
6. method of purification according to claim 1 is characterized in that: in step 5), the multiplicity of said step 4) is 3～4 times.
7. the extracter of a dithiocarbonic anhydride purification usefulness; It is characterized in that: comprise separating flask, separating flask support, motor, two-position controller and transmission rig; Said separating flask comprises bottle, be separately positioned on upper and lower fluid inlet of bottle and liquid outlet and be arranged on the venting port on bottle top; One vertical and be fixedly installed on the bottle side wall; This axle supports through said support rotationally, and said transmission rig makes the jolting in a certain way of said separating flask through motor and described axle under the control of said two-position controller.
8. extracter according to claim 7 is characterized in that: said transmission rig comprises the driving toothed gear that is installed on the motor output shaft, is installed in the follower gear and the chain that be connected said driving toothed gear and follower gear of said axle away from separating flask one end.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110122810A CN102241398B (en) | 2011-05-12 | 2011-05-12 | Method and extraction machine for purifying carbon disulfide |
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| CN201110122810A CN102241398B (en) | 2011-05-12 | 2011-05-12 | Method and extraction machine for purifying carbon disulfide |
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| CN102241398A CN102241398A (en) | 2011-11-16 |
| CN102241398B true CN102241398B (en) | 2012-08-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103364361B (en) * | 2013-04-09 | 2016-05-25 | 江苏国创环保科技有限公司 | A kind of infrared spectrophotometry that does not use oils in CFC class reagent Fast Measurement water |
| CN104649268A (en) * | 2015-02-09 | 2015-05-27 | 安建华 | Method suitable for purifying carbon disulfide in laboratory |
| CN105675380B (en) * | 2016-01-07 | 2018-06-15 | 浙江省海洋水产研究所 | A kind of portable separatory funnel example enrichment pre-processing device |
| CN105905901A (en) * | 2016-03-29 | 2016-08-31 | 江阴秋毫检测有限公司 | Carbon disulfide purification method |
| CN113786788A (en) * | 2021-08-24 | 2021-12-14 | 翱翔化工(鹤壁)有限公司 | Retort is used in carbon disulfide purification production |
| CN113562732A (en) * | 2021-08-24 | 2021-10-29 | 翱翔化工(鹤壁)有限公司 | Carbon disulfide production process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002000549A1 (en) * | 2000-06-28 | 2002-01-03 | Ege Kimya Sanayi Ve Ticaret A.S. | A process for the production of polymeric allotropes of sulfur |
| CN101189052A (en) * | 2005-04-07 | 2008-05-28 | 马寺松气体股份有限公司 | Fluid storage and purification method and system |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002000549A1 (en) * | 2000-06-28 | 2002-01-03 | Ege Kimya Sanayi Ve Ticaret A.S. | A process for the production of polymeric allotropes of sulfur |
| CN101189052A (en) * | 2005-04-07 | 2008-05-28 | 马寺松气体股份有限公司 | Fluid storage and purification method and system |
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Granted publication date: 20120829 Termination date: 20160512 |