CN105905901A - Carbon disulfide purification method - Google Patents
Carbon disulfide purification method Download PDFInfo
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- CN105905901A CN105905901A CN201610188927.1A CN201610188927A CN105905901A CN 105905901 A CN105905901 A CN 105905901A CN 201610188927 A CN201610188927 A CN 201610188927A CN 105905901 A CN105905901 A CN 105905901A
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- carbon disulfide
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a carbon disulfide purification method. The carbon disulfide purification method comprises 1, orderly adding CS2, concentrated H2SO4, concentrated HNO3 and glass beads or porcelain pieces into a four-mouth flask, installing a stirring device in a central opening of the four-mouth flask, inserting a thermometer into one side opening of the four-mouth flask, condenser pipes are inserted into two sides, communicating cooling water to the four-mouth flask, putting the four-mouth flask into a thermostat water bath kettle, carrying out heating along with stirring and cooling water feeding under the condition of a water bath temperature of 450-460 DEG C, 2, after the reaction, stopping stirring, removing the thermostat water bath kettle, carrying out cooling to the room temperature or less than room temperature through a cold water bath pot or an ice water bath pot, transferring a nitrification liquor into a separating funnel, separating a mixed acid in the lower layer, carrying out extraction washing on the CS2 in the separating funnel through deionized water and carrying out extraction washing through a NaCO3 solution, and 3, carrying out extraction washing through deionized water, carrying out waterless CaCl2 dehydration on the separated CS2, carrying out water bath distillation in a distillation flask and collecting a fraction so that CS2 is obtained. The carbon disulfide purification method realizes a stable and safe nitratlon reaction, greatly improves a nitratlon rate and nitratlon efficiency and greatly shortens nitratlon time.
Description
Technical field
The present invention relates to the method for purification of a kind of carbon disulfide, belong to technical field of chemistry.
Background technology
In prior art, use and measure CODCrReflux purify CS2, achieve preferable effect.
But, due to the defect of equipment for purifying, also bring some shortcomings to refining effect.As only by reflux course
Nitrating agent and CS2Contact, therefore nitrification efficiency is low, and the nitrification time is long.For another example with electric furnace heated water bath pot,
Be difficult to control temperature the most permanent, the most careless, water-bath temperature it is possible to more than 500 DEG C, easily cause nitrating agent with
CS2Run off from suitable for reading the going out of condenser pipe, cause CS2The rate of recovery be sometimes less than 50%.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the purification side of a kind of carbon disulfide
Method, makes the steady safety of nitration reaction, and digestion rate and nitrification efficiency are greatly improved, and the nitrification time is greatly shortened.
The technical scheme provided according to the present invention, the method for purification of described carbon disulfide, it is characterized in that, including
Following steps:
(1) in four mouthfuls of beam ground round-bottomed flasks, 300mL CS it is sequentially added into2, the dense H of 30mL2SO4、
10～20mL dense HNO3With several beades or broken ceramics, pacify at four mouthfuls of beam ground round-bottomed flask center port
Dress stirs, and a side port plugs in thermometer, and another two side port insert spherical condensation tube, connects cooling water, by four mouthfuls of standards
Ground round-bottomed flask is placed in thermostat water bath, and water-bath liquid level is higher than liquid level in four mouthfuls of beam ground round-bottomed flasks,
Boiling water bath power supply heats, and opens stirring simultaneously, opens cooling water, and mixing speed is by progressively accelerating, by water-bath slowly
Temperature is adjusted to 450 DEG C～460 DEG C；
(2) stirring reaction 20～30min after, stop stirring, remove thermostat water bath, change cold water bath or
Frozen water bath, is cooled to below room temperature or room temperature by the nitrification liquid that step (1) reaction obtains, is turned by nitrification liquid
Enter in 500mL separatory funnel, stand 15～20min, separate the nitration mixture of lower floor, be retained in separatory funnel
CS2Deionized water extraction is washed 2 times, then is the NaCO of 5% by mass percentage concentration3Solution extraction washes to neutralize
CS2The acid of middle remaining；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2
Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 480 DEG C～500 DEG C, collect
460 DEG C～the cut of 470 DEG C, obtain removing the CS of benzene homologues2。
Further, in described step (1) liquid temperature in four mouthfuls of beam ground round-bottomed flasks constant at 450 DEG C～
460℃。
Further, in described step (1) mixing speed according to CS2Backflow situation be controlled, keep
Brown color NO in spherical condensation tube2Height less than spherical condensation tube height 2/3～3/4.
Further, described step (2) extraction washes the NaCO separated3Solution reclaim after again with.
Further, when in described step (2), deionized water extraction is washed, deionized consumption is 100mL.
Further, NaCO in described step (2)3NaCO when solution extraction is washed3The consumption of solution is 150mL.
Further, the nitration mixture that described step (2) separates through separatory funnel reclaim after again with；Work as step
(1) use for reclaim again with nitration mixture time, in four mouthfuls of beam ground round-bottomed flasks, add 2～3mL
Dense HNO3。
Further, CaCl is also included2Recycling step: will step (3) be dehydrated after reclaim chlorine
Change calcium and be placed in the Muffle furnace of about 8000 DEG C calcination 10～20 minutes, obtain anhydrous calcium chloride, for next
Dehydration in secondary carbon disulfide purification process.
The method of purification of carbon disulfide of the present invention, it is possible to ensure that nitration reaction is carried out the most safely, disappear
Changing speed and nitrification efficiency is greatly improved, the nitrification time is greatly shortened, CS2Reaching import level, the rate of recovery is steady
It is scheduled on more than 90%.
Accompanying drawing explanation
Fig. 1 is for analyzing pure CS2Chromatogram.
Fig. 2 is import CS2Chromatogram.
Fig. 3 is the CS that embodiment 4 obtains2Chromatogram.
Detailed description of the invention
Below in conjunction with concrete drawings and Examples, the invention will be further described.
The dense H used in the embodiment of the present invention2SO4With dense HNO3It is respectively adopted the commercially available concentrated sulfuric acid and commercially available dense
Nitric acid, the concentration of the commercially available concentrated sulfuric acid is the H more than or equal to 70%2SO4The aqueous solution, commercially available red fuming nitric acid (RFNA)
Mass fraction be about 65%.
Embodiment 1: the method for purification of a kind of carbon disulfide, comprises the following steps:
(1) in tetra-mouthfuls of beam ground round-bottomed flasks of 500mL, it is sequentially added into 300mL analyzes pure CS2、30mL
Dense H2SO4, the dense HNO of 10mL3With several beades or broken ceramics, in four mouthfuls of beam ground round-bottomed flasks
Stirring is installed at the pit of the stomach, and a side port plugs in thermometer, and another two side port insert spherical condensation tube, connects cooling water, by four
Mouth beam ground round-bottomed flask is placed in thermostat water bath, and water-bath liquid level is higher than four mouthfuls of beam ground round-bottomed flasks
Interior liquid level, boiling water bath power supply heat, open stirring simultaneously, open cooling water, mixing speed by progressively accelerating slowly,
Water-bath temperature is adjusted to 450 DEG C, and the liquid temperature in four mouthfuls of beam ground round-bottomed flasks is constant at 450 DEG C；Described stirring
Speed is according to CS2Backflow situation be controlled, keep brown color NO in spherical condensation tube2Height do not surpass
Cross the 3/4 of spherical condensation tube height；
(2), after stirring reaction 20min, stop stirring, remove thermostat water bath, change cold water bath or frozen water
Bath, is cooled to below room temperature or room temperature by the nitrification liquid that step (1) reaction obtains, is proceeded to by nitrification liquid
In 500mL separatory funnel, standing 15min, separate the nitration mixture of lower floor, the nitration mixture separated through separatory funnel can
With reclaim after again with；The CS being retained in separatory funnel2Wash 2 times by 100mL deionized water extraction, then
It is the NaCO of 5% by 150mL mass percentage concentration3Solution extraction washes to neutralize CS2The acid of middle remaining, extraction is washed
The NaCO separated3Solution can reclaim after again with；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2
Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 480 DEG C, collect 460 DEG C
Cut, obtains removing the CS of benzene homologues2About 280mL；
Calcium chloride after above-mentioned steps (3) reclaims is placed in calcination 10 minutes in the Muffle furnace of about 8000 DEG C,
Obtain anhydrous calcium chloride, the dehydration in carbon disulfide purification process next time.
Embodiment 2: the method for purification of a kind of carbon disulfide, comprises the following steps:
(1) in tetra-mouthfuls of beam ground round-bottomed flasks of 500mL, it is sequentially added into 300mL analyzes pure CS2、30mL
Dense H2SO4, the dense HNO of 20mL3With several beades or broken ceramics, in four mouthfuls of beam ground round-bottomed flasks
Stirring is installed at the pit of the stomach, and a side port plugs in thermometer, and another two side port insert spherical condensation tube, connects cooling water, by four
Mouth beam ground round-bottomed flask is placed in thermostat water bath, and water-bath liquid level is higher than four mouthfuls of beam ground round-bottomed flasks
Interior liquid level, boiling water bath power supply heat, open stirring simultaneously, open cooling water, mixing speed by progressively accelerating slowly,
Water-bath temperature is adjusted to 460 DEG C, and the liquid temperature in four mouthfuls of beam ground round-bottomed flasks is constant at 460 DEG C；Described stirring
Speed is according to CS2Backflow situation be controlled, keep brown color NO in spherical condensation tube2Height do not surpass
Cross the 3/4 of spherical condensation tube height；
(2), after stirring reaction 30min, stop stirring, remove thermostat water bath, change cold water bath or frozen water
Bath, is cooled to below room temperature or room temperature by the nitrification liquid that step (1) reaction obtains, is proceeded to by nitrification liquid
In 500mL separatory funnel, standing 20min, separate the nitration mixture of lower floor, the nitration mixture separated through separatory funnel can
With reclaim after again with；The CS being retained in separatory funnel2Wash 2 times by 100mL deionized water extraction, then
It is the NaCO of 5% by 150mL mass percentage concentration3Solution extraction washes to neutralize CS2The acid of middle remaining, extraction is washed
The NaCO separated3Solution can reclaim after again with；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2
Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 500 DEG C, collect 470 DEG C
Cut, obtains removing the CS of benzene homologues2About 280mL；
Calcium chloride after above-mentioned steps (3) reclaims is placed in calcination 20 minutes in the Muffle furnace of about 8000 DEG C,
Obtain anhydrous calcium chloride, the dehydration in carbon disulfide purification process next time.
Embodiment 3: the method for purification of a kind of carbon disulfide, comprises the following steps:
(1) in tetra-mouthfuls of beam ground round-bottomed flasks of 500mL, it is sequentially added into 300mL analyzes pure CS2、30mL
Dense H2SO4, the dense HNO of 15mL3With several beades or broken ceramics, in four mouthfuls of beam ground round-bottomed flasks
Stirring is installed at the pit of the stomach, and a side port plugs in thermometer, and another two side port insert spherical condensation tube, connects cooling water, by four
Mouth beam ground round-bottomed flask is placed in thermostat water bath, and water-bath liquid level is higher than four mouthfuls of beam ground round-bottomed flasks
Interior liquid level, boiling water bath power supply heat, open stirring simultaneously, open cooling water, mixing speed by progressively accelerating slowly,
Water-bath temperature is adjusted to 455 DEG C, and the liquid temperature in four mouthfuls of beam ground round-bottomed flasks is constant at 455 DEG C；Described stirring
Speed is according to CS2Backflow situation be controlled, keep brown color NO in spherical condensation tube2Height do not surpass
Cross the 2/3 of spherical condensation tube height；
(2), after stirring reaction 25min, stop stirring, remove thermostat water bath, change cold water bath or frozen water
Bath, is cooled to below room temperature or room temperature by the nitrification liquid that step (1) reaction obtains, is proceeded to by nitrification liquid
In 500mL separatory funnel, standing 15min, separate the nitration mixture of lower floor, the nitration mixture separated through separatory funnel can
With reclaim after again with；The CS being retained in separatory funnel2Wash 2 times by 100mL deionized water extraction, then
It is the NaCO of 5% by 150mL mass percentage concentration3Solution extraction washes to neutralize CS2The acid of middle remaining, extraction is washed
The NaCO separated3Solution can reclaim after again with；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2
Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 490 DEG C, collect 465 DEG C
Cut, obtains removing the CS of benzene homologues2About 280mL；
Calcium chloride after above-mentioned steps (3) reclaims is placed in calcination 15 minutes in the Muffle furnace of about 8000 DEG C,
Obtain anhydrous calcium chloride, the dehydration in carbon disulfide purification process next time.
Embodiment 4: the method for purification of a kind of carbon disulfide, comprises the following steps:
(1) in tetra-mouthfuls of beam ground round-bottomed flasks of 500mL, it is sequentially added into 300mL analyzes pure CS2、45mL
The dense HNO of the nitration mixture of recycling, 2～3mL3With several beades or broken ceramics, grind four mouthfuls of standards
Mouth round-bottomed flask center port installs stirring, and a side port plugs in thermometer, and another two side port insert spherical condensation tube, connects
Four mouthfuls of beam ground round-bottomed flasks are placed in thermostat water bath by cooling water, and water-bath liquid level is higher than four mouthfuls of standards
Liquid level in ground round-bottomed flask, boiling water bath power supply heats, opens stirring simultaneously, open cooling water, mixing speed
By progressively accelerating slowly, water-bath temperature is adjusted to 460 DEG C, liquid temperature in four mouthfuls of beam ground round-bottomed flasks constant
460℃；Described mixing speed is according to CS2Backflow situation be controlled, keep brown color in spherical condensation tube
NO2Height less than spherical condensation tube height 3/4；
(2), after stirring reaction 30min, stop stirring, remove thermostat water bath, change cold water bath or frozen water
Bath, is cooled to below room temperature or room temperature by the nitrification liquid that step (1) reaction obtains, is proceeded to by nitrification liquid
In 500mL separatory funnel, standing 20min, separate the nitration mixture of lower floor, the nitration mixture separated through separatory funnel can
With reclaim after again with；The CS being retained in separatory funnel2Wash 2 times by 100mL deionized water extraction, then
It is the NaCO of 5% by 150mL mass percentage concentration3Solution extraction washes to neutralize CS2The acid of middle remaining, extraction is washed
The NaCO separated3Solution can reclaim after again with；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2
Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 500 DEG C, collect 470 DEG C
Cut, obtains removing the CS of benzene homologues2About 280mL；
Calcium chloride after above-mentioned steps (3) reclaims is placed in calcination 20 minutes in the Muffle furnace of about 8000 DEG C,
Obtain anhydrous calcium chloride, the dehydration in carbon disulfide purification process next time.
It is illustrated in figure 1 the pure CS of analysis2Chromatogram, be illustrated in figure 2 import CS2Chromatogram, as figure
3 show the CS that embodiment 4 obtains2Chromatogram.Nitrating agent (the H that embodiment 4 uses2SO4+HNO3)
It is the nitrating agent of the 35th recycling, shown in Fig. 1～Fig. 3, adds the nitrating agent of recycling
To CS2Refining effect the most fine.Although the amount that nitrating agent uses is little, but at batch purifying CS2
Time, the disposal of its spent acid still can't neglect, and discarded nitration mixture not only pollutes environment, too increases CS simultaneously2
Loss.Nitrification principle according to trace aromatic hydrocarbons, the nitrating agent separated is carried out recycling by the present invention,
Achieve nitrification effect good as adding new nitrating agent.In view of H in nitrifying process2SO4Will not damage
Losing, the loss of nitric acid is the most less, therefore, only need to add the dense HNO of 2～3mL during recycling3。
The invention have the advantages that
(1) present invention uses four mouthfuls of beam ground round-bottomed flasks that band stirs, thermostat water bath, double spherical cold
Solidifying pipe, nitrating agent and CS in stirring and reflux course2Haptoreaction, firing equipment uses thermostat water bath,
Stable temperature control, nitrification time≤30min, CS2The rate of recovery is stable more than 90%.Due to stirred
Journey greatly strengthen mixed acid nitrification agent and CS2The contact of middle impurity benzene homologues, nitrification efficiency is greatly improved,
The nitrification time significantly shortens；Double spherical condensation tubes ensure that CS in nitrifying process2Do not lose, therefore CS2Return
Yield is greatly improved.
(2) owing to the present invention is with stirring, thermometer in reactant liquor, also it is inserted with, therefore can be according to reaction liquid temperature
Control bath temperature.Test shows: when reaction liquid temperature reaches CS2Near boiling point, nitration reaction just can be normal
Carry out, at this moment, CS in double spherical condensation tubes2Backflow height pipe high 2/3～3/4, control this temperature,
Both ensure that nitration reaction was comparatively fast carried out, and avoided again reacting undue fierce and causing CS2Loss.
(3) in order to reduce in carbon disulfide purification process the harmful effect to environment as far as possible, the present invention will take off
The calcium chloride reclaimed after water is placed in calcination in Muffle furnace, can again prepare anhydrous calcium chloride, for next time
Carbon disulfide purification process is dehydrated.The absorption a small amount of carbon disulfide on calcium chloride becomes CO in calcination2
And SO2, the impact on environment is significantly lower than carbon disulfide.
It is respectively adopted the CS that embodiment 4 purifies2Benzene CS low with import2Make the diluent of standard benzene homologues, carry out
The mensuration of benzene homologues, measurement result is as shown in table 1.As shown in Table 1, (1) nitrating agent recycling reaches
35 times, CS2Refining effect the most fine；(2) CS purified by the method for the invention2Can replace completely
For import CS2Make solvent and the extractant of Determination of The Homologous Series of Benzene by Gas Ghromatography.
Table 1
Claims (8)
1. a method of purification for carbon disulfide, is characterized in that, comprises the following steps:
(1) in four mouthfuls of beam ground round-bottomed flasks, 300mL CS it is sequentially added into2, the dense H of 30mL2SO4, 10～the dense HNO of 20mL3With several beades or broken ceramics, installing stirring at four mouthfuls of beam ground round-bottomed flask center port, a side port plugs in thermometer, and another two side port insert spherical condensation tube, connect cooling water, being placed in thermostat water bath by four mouthfuls of beam ground round-bottomed flasks, water-bath liquid level heats higher than liquid level in four mouthfuls of beam ground round-bottomed flasks, boiling water bath power supply, open stirring simultaneously, opening cooling water, water-bath temperature, by progressively accelerating slowly, is adjusted to 450 DEG C～460 DEG C by mixing speed；
(2) after stirring reaction 20～30min, stop stirring, remove thermostat water bath, change cold water bath or frozen water bath, the nitrification liquid that step (1) reaction obtains is cooled to below room temperature or room temperature, nitrification liquid is proceeded in separatory funnel, stand 15～20min, separate the nitration mixture of lower floor, the CS being retained in separatory funnel2Deionized water extraction is washed 2 times, then is the NaCO of 5% by mass percentage concentration3Solution extraction washes to neutralize CS2The acid of middle remaining；
(3) NaCO is used3Solution extraction washes the CS after neutralization2Wash 2 times by deionized water extraction again, the CS separated2Through anhydrous CaCl2Reinject cucurbit after dehydration, distill in the water-bath of 480 DEG C～500 DEG C, collect 460 DEG C～the cut of 470 DEG C, obtain removing the CS of benzene homologues2。
2. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: in described step (1), the liquid temperature in four mouthfuls of beam ground round-bottomed flasks is constant at 450 DEG C～460 DEG C.
3. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: in described step (1), mixing speed is according to CS2Backflow situation be controlled, keep brown color NO in spherical condensation tube2Height less than spherical condensation tube height 2/3～3/4.
4. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: described step (2) extraction washes the NaCO separated3Solution reclaim after again with.
5. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: when in described step (2), deionized water extraction is washed, deionized consumption is 100mL.
6. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: NaCO in described step (2)3NaCO when solution extraction is washed3The consumption of solution is 150mL.
7. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: described step (2) after the nitration mixture that separatory funnel separates reclaims again with；When step (1) use for reclaim again with nitration mixture time, in four mouthfuls of beam ground round-bottomed flasks, add the dense HNO of 2～3mL3。
8. the method for purification of carbon disulfide as claimed in claim 1, is characterized in that: also include CaCl2Recycling step: the calcium chloride reclaimed after step (3) being dehydrated is placed in the Muffle furnace of about 8000 DEG C calcination 10～20 minutes, obtains anhydrous calcium chloride, the dehydration in carbon disulfide purification process next time.
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| CN201610188927.1A CN105905901A (en) | 2016-03-29 | 2016-03-29 | Carbon disulfide purification method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321576A (en) * | 2021-05-31 | 2021-08-31 | 成都市科隆化学品有限公司 | Benzene-free acetone and preparation method thereof |
| CN113336227A (en) * | 2021-05-31 | 2021-09-03 | 成都市科隆化学品有限公司 | Benzene-free carbon disulfide and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321576A (en) * | 2021-05-31 | 2021-08-31 | 成都市科隆化学品有限公司 | Benzene-free acetone and preparation method thereof |
| CN113336227A (en) * | 2021-05-31 | 2021-09-03 | 成都市科隆化学品有限公司 | Benzene-free carbon disulfide and preparation method thereof |
| CN113321576B (en) * | 2021-05-31 | 2023-06-13 | 成都市科隆化学品有限公司 | Non-propiophenone and preparation method thereof |
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