CN108147943A - A kind of carbon tetrachloride turns chloroform production technology - Google Patents
A kind of carbon tetrachloride turns chloroform production technology Download PDFInfo
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- CN108147943A CN108147943A CN201810053500.XA CN201810053500A CN108147943A CN 108147943 A CN108147943 A CN 108147943A CN 201810053500 A CN201810053500 A CN 201810053500A CN 108147943 A CN108147943 A CN 108147943A
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- chloroform
- carbon tetrachloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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Abstract
The invention discloses a kind of carbon tetrachloride to turn chloroform production technology, includes the following steps：S1：Raw material weighing：Activated carbon felt catalyst and carbon tetrachloride are weighed, and activated carbon felt catalyst and carbon tetrachloride are put into container and stored according to proportioning, wait to be used, S2：Hybrid reaction：Activated carbon felt catalyst described in S1 and carbon tetrachloride are added in reactor, and be passed through hydrogen in the reactor, carry out heating reaction, S3：Cooling：After the completion of the heating reaction described in S2, raw material is put into cooler and is cooled down, takes out raw material from cooler after the completion of cooling, chloroform sample, S4 is made：Rectifying：Chloroform sample described in S3 is put into, rectification process is carried out in rectifying device, chloroform just finished product is made.The present invention obtains analysis data, and analysis data are compared with preset data so that carry out control to the quality of chloroform, prevent underproof chloroform from entering market by the detection and analysis to chloroform sample.
Description
Technical field
Turn chloroform production technical field the present invention relates to carbon tetrachloride more particularly to a kind of carbon tetrachloride turns chloroform production work
Skill.
Background technology
Chloroform is organic synthesis raw material, is mainly used to produce freon, dyestuff and drug, medically, is commonly used for anaesthetizing
Agent can be used as the solvent and extractant of antibiotic, fragrance, grease, resin, rubber, and through retrieval, publication number CN1045090A's is special
Sharp file, which discloses, a kind of to be produced chlorinated product mixture by partial oxidation chloromethanes-dichloromethane mixture and prepares chloroform
Method, containing chloroform, chloromethanes, dichloromethane and a small amount of carbon tetrachloride or without carbon tetrachloride in generated mixture, wherein
The amount of dichloromethane is substantially equal to the amount in initial feed mixture, and the amount of carbon tetrachloride is equivalent to chloroform in product
Less than 0.1 mole.
But this preparation method is not easy to be detected analysis to chloroform obtained, is not easy to the quality of control product,
Therefore we have proposed a kind of carbon tetrachloride to turn chloroform production technology, for solving the above problems.
Invention content
Technical problems based on background technology, the present invention propose a kind of carbon tetrachloride and turn chloroform production technology.
A kind of carbon tetrachloride proposed by the present invention turns chloroform production technology, includes the following steps：
S1：Raw material weighing：Activated carbon felt catalyst and carbon tetrachloride are weighed according to proportioning, and by activated carbon felt catalyst and tetrachloro
Change carbon, which is put into container, to be stored, and is waited to be used；S2：Hybrid reaction：By the activated carbon felt catalyst and tetrachloro described in S1
Change carbon to be added in reactor, and be passed through hydrogen in the reactor, carry out heating reaction；S3：Cooling：When the heating described in S2
After the completion of reaction, raw material is put into cooler and is cooled down, take out raw material from cooler after the completion of cooling, chloroform is made
Sample；S4：Rectifying：Chloroform sample described in S3 is put into, rectification process is carried out in rectifying device, chloroform just finished product is made；
S5：Detection：After finished product at the beginning of the chloroform described in S4 is made, the first finished product of taking-up chloroform, which is put into storage tank, to be stored, and transport
Analysis is detected to finished product at the beginning of chloroform, and analysis data are recorded with check analysis instrument；S6：Data comparison：By S5
Described in analysis data compared with preset data, when data differences are larger, need to locate finished product at the beginning of chloroform in time
Reason, finished product meets the requirements at the beginning of chloroform, and chloroform is made；S7：Storage：Chloroform described in S6 is put into storage container and is carried out
Storage, and carry out encapsulation process.
Preferably, in the S1, when weighing activated carbon felt catalyst and carbon tetrachloride, one is put on weighing equipment first
Measuring cup, and weight at this time is recorded, activated carbon felt catalyst is put into measuring cup, is weighed according to proportioning, activated carbon felt is urged
After agent weighs, measuring cup is replaced, then put carbon tetrachloride into measuring cup and weigh.
Preferably, in the S2, reactor is tubular reactor, when carrying out heating reaction, needs to check pipe reaction
The air-tightness of device and pipeline, after confirming no leakage, to being heated in tubular reactor.
Preferably, in the S3, cooler is shell and tube cooler, after activated carbon felt catalyst and carbon tetrachloride reaction
Product sequentially through each baffling channel, is circuitously flow to and takes over outlet by the take over import on shell and tube cooler, and cooler is situated between
Matter is then flowed using two-tube-pass, i.e., cooler medium by water inlet through water cover is divided to enter half cooler tube and then from return water
The other half cooler tube of lid inflow enters opposite side and divides water cover and outlet pipe, and cold medium absorbs activity during two-tube-pass stream
The waste heat that charcoal felt catalyst and carbon tetrachloride mix products are released is discharged by water outlet.
Preferably, in the S4, rectifying device is rectifying column, has different volatility using each component in mixture,
That is this different property of the vapour pressure of each component at the same temperature, makes the light component in liquid phase be transferred in gas phase, and gas phase
In heavy constituent be transferred in liquid phase, so as to fulfill the purpose of separation.
Preferably, in the S5, check analysis instrument is gas chromatograph, by the sample of finished product at the beginning of chloroform in injection port
After gasification, chromatographic column is brought by carrier gas, the chromatographic column for there are different retention properties by sample component detaches each component, successively
Detector is imported, to obtain the detection signal of each component, according to the precedence for importing detector, by comparison, it is possible to distinguish
It is any component to go out, and analysis is detected to the concentration of finished product at the beginning of chloroform.
Preferably, it in the S7, when being stored to chloroform, should be sealed when preserving chloroform, shading is placed at shady and cool ventilation,
Far from kindling material, heat source, library temperature is no more than 30 DEG C, and holding container sealing is separately stored with bases, aluminium, edible chemical.
Preferably, in the S2, weighing equipment is electronic balance.
Beneficial effects of the present invention：By the detection and analysis to chloroform sample, obtain analysis data, and will analysis data with
Preset data are compared so that are carried out control to the quality of chloroform, prevented underproof chloroform from entering market.
Specific embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment
A kind of carbon tetrachloride is proposed in the present embodiment and turns chloroform production technology, is included the following steps：
S1：Raw material weighing：Activated carbon felt catalyst and carbon tetrachloride are weighed according to proportioning, and by activated carbon felt catalyst and tetrachloro
Change carbon, which is put into container, to be stored, and is waited to be used；S2：Hybrid reaction：By the activated carbon felt catalyst and tetrachloro described in S1
Change carbon to be added in reactor, and be passed through hydrogen in the reactor, carry out heating reaction；S3：Cooling：When the heating described in S2
After the completion of reaction, raw material is put into cooler and is cooled down, take out raw material from cooler after the completion of cooling, chloroform is made
Sample；S4：Rectifying：Chloroform sample described in S3 is put into, rectification process is carried out in rectifying device, chloroform just finished product is made；
S5：Detection：After finished product at the beginning of the chloroform described in S4 is made, the first finished product of taking-up chloroform, which is put into storage tank, to be stored, and transport
Analysis is detected to finished product at the beginning of chloroform, and analysis data are recorded with check analysis instrument；S6：Data comparison：By S5
Middle analysis data are compared with preset data, when data differences are larger, need to carry out timely processing to finished product at the beginning of chloroform, directly
It meets the requirements to finished product at the beginning of chloroform, chloroform is made；S7：Storage：Chloroform described in S6 is put into storage container and is stored,
And encapsulation process is carried out, the beneficial effects of the invention are as follows by the detection and analysis to chloroform sample, obtain analysis data, and will divide
Analysis data are compared with preset data so that are carried out control to the quality of chloroform, prevented underproof chloroform from entering market.
In the present embodiment, in S1, when weighing activated carbon felt catalyst and carbon tetrachloride, one is put on weighing equipment first
Measuring cup, and weight at this time is recorded, activated carbon felt catalyst is put into measuring cup, is weighed according to proportioning, activated carbon felt is urged
After agent weighs, measuring cup being replaced, then put carbon tetrachloride into measuring cup and weigh, in S2, reactor is tubular reactor,
When carrying out heating reaction, need to check the air-tightness of tubular reactor and pipeline, after confirming no leakage, in tubular reactor into
Row heating, in S3, cooler is shell and tube cooler, and the product after activated carbon felt catalyst and carbon tetrachloride reaction is by shell and tube
Take over import on cooler sequentially through each baffling channel, circuitously flow to and takes over outlet, and cooler medium is then using two-tube
Cheng Liudong, i.e. cooler medium are by water inlet through water cover is divided to enter half cooler tube and then flows into the other half from water return cover
Cooler tube enters opposite side and divides water cover and outlet pipe, cold medium during two-tube-pass stream, absorb activated carbon felt catalyst and
The waste heat that carbon tetrachloride mix products are released is discharged by water outlet, and in S4, rectifying device is rectifying column, utilizes each group in mixture
Point there is different volatility, i.e. this different property of the vapour pressure of each component at the same temperature, make the light component in liquid phase
It is transferred in gas phase, and the heavy constituent in gas phase is transferred in liquid phase, so as to fulfill the purpose of separation, in S5, check analysis instrument
Device is gas chromatograph, after the sample of finished product at the beginning of chloroform is gasified in injection port, brings chromatographic column by carrier gas, passes through sample sets
Dividing has the chromatographic column of different retention properties, detaches each component, imports detector successively, to obtain the detection signal of each component,
According to the precedence for importing detector, by comparison, it is possible to distinguish what component goes out is, the concentration of finished product at the beginning of chloroform is carried out
It tests and analyzes, in S7, when being stored to chloroform, should be sealed when preserving chloroform, shading is placed at shady and cool ventilation, far from kindling material, heat
Source, library temperature are no more than 30 DEG C, and holding container sealing is separately stored with bases, aluminium, edible chemical, and in S2, weighing equipment is electricity
Sub- balance, the beneficial effects of the invention are as follows by the detection and analysis to chloroform sample, obtaining analysis data, and will analysis data with
Preset data are compared so that are carried out control to the quality of chloroform, prevented underproof chloroform from entering market.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of carbon tetrachloride turns chloroform production technology, which is characterized in that includes the following steps：
S1：Raw material weighing：Activated carbon felt catalyst and carbon tetrachloride are weighed according to proportioning, and by activated carbon felt catalyst and tetrachloro
Change carbon, which is put into container, to be stored, and is waited to be used；
S2：Hybrid reaction：Activated carbon felt catalyst described in S1 and carbon tetrachloride are added in reactor, and in reactor
In be passed through hydrogen, carry out heating reaction；
S3：Cooling：After the completion of the heating reaction described in S2, raw material is put into cooler and is cooled down, after the completion of cooling
Raw material from cooler is taken out, chloroform sample is made；
S4：Rectifying：Chloroform sample described in S3 is put into, rectification process is carried out in rectifying device, chloroform just finished product is made；
S5：Detection：After finished product at the beginning of the chloroform described in S4 is made, the first finished product of taking-up chloroform, which is put into storage tank, to be stored,
And analysis is detected to finished product at the beginning of chloroform, and analysis data are recorded with check analysis instrument；
S6：Data comparison：It compares data are analyzed described in S5 with preset data, when data differences are larger, needs pair
Just finished product carries out timely processing to chloroform, and finished product meets the requirements at the beginning of chloroform, and chloroform is made；
S7：Storage：Chloroform described in S6 is put into storage container and is stored, and carries out encapsulation process.
2. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S1, weighs
When activated carbon felt catalyst and carbon tetrachloride, a measuring cup is put on weighing equipment first, and record weight at this time, it will be active
Charcoal felt catalyst is put into measuring cup, is weighed according to proportioning, after activated carbon felt catalyst weighs, replaces measuring cup, then by four
Chlorination carbon is put measuring cup into and is weighed.
3. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S2, reaction
Device is tubular reactor, when carrying out heating reaction, needs to check the air-tightness of tubular reactor and pipeline, confirms no leakage
Afterwards, to being heated in tubular reactor.
4. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S3, cooling
Device is shell and tube cooler, the product after activated carbon felt catalyst and carbon tetrachloride reaction by shell and tube cooler take over into
Mouthful, sequentially through each baffling channel, circuitously it flow to and takes over outlet, and cooler medium is then using two-tube-pass flowing, i.e. cooler
Medium by water inlet through divide water cover enter half cooler tube and then from water return cover flow into the other half cooler tube enter it is another
Water cover and outlet pipe are divided in side, and cold medium absorbs activated carbon felt catalyst and carbon tetrachloride mix products during two-tube-pass stream
The waste heat of releasing is discharged by water outlet.
5. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S4, rectifying
Equipment is rectifying column, has different volatility, the i.e. vapour pressure of each component at the same temperature using each component in mixture
This different property, make the light component in liquid phase be transferred in gas phase, and the heavy constituent in gas phase is transferred in liquid phase, so as to real
The purpose now detached.
6. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S5, examines
Analytical instrument is gas chromatograph, after the sample of finished product at the beginning of chloroform is gasified in injection port, brings chromatographic column by carrier gas, passes through
Sample component has the chromatographic column of different retention properties, detaches each component, imports detector successively, to obtain the detection of each component
Signal, according to the precedence for importing detector, by comparison, it is possible to distinguish what component goes out is, to the dense of finished product at the beginning of chloroform
Degree is detected analysis.
7. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S7, right
When chloroform stores, it should be sealed when preserving chloroform, shading is placed at shady and cool ventilation, and far from kindling material, heat source, library temperature is no more than 30 DEG C,
Holding container seals, and is separately stored with bases, aluminium, edible chemical.
8. a kind of carbon tetrachloride according to claim 1 turns chloroform production technology, which is characterized in that in the S2, weighs
Equipment is electronic balance.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045090A (en) * | 1987-11-10 | 1990-09-05 | 纳幕尔杜邦公司 | The preparation of chloroform |
| CN1051167A (en) * | 1989-10-10 | 1991-05-08 | 纳幕尔杜邦公司 | The hydrogenolysis of halocarbon |
| US5208393A (en) * | 1989-12-22 | 1993-05-04 | Ercros, S.A. | Process for the manufacture of chloroform |
| JPH05221890A (en) * | 1992-01-14 | 1993-08-31 | Toyo Kasei Kogyo Kk | Method for treating carbon tetrachloride |
| JPH06145079A (en) * | 1992-11-06 | 1994-05-24 | Tokuyama Soda Co Ltd | Production of chloroform |
| CN1109461A (en) * | 1993-11-04 | 1995-10-04 | 恩尼彻姆公司 | Preparation of CHCl3 by starting from CCl4 |
| CN1350885A (en) * | 2000-10-31 | 2002-05-29 | 舒德化学公司 | Catalyst for preparing chloroform by hydrogenation dechlorination of carbon tetrachloride |
| DE10228480A1 (en) * | 2002-06-26 | 2004-01-15 | Lii Europe Gmbh | Production of chloroform by selective hydrogenation of carbon tetrachloride with gaseous hydrogen comprises contact with finely divided particles of a Group VIII metal or copper on a porous support material in the presence of an activator |
| CN1636631A (en) * | 2003-10-08 | 2005-07-13 | 株式会社德山 | Catalyst for reduction of polychloralkane, producing process thereof and process for producing low-grade chloralkane |
| CN101362090A (en) * | 2008-09-28 | 2009-02-11 | 广东理文化工研发有限公司 | Catalyst for transferring the carbon tetrachloride into chloroform and preparation method thereof |
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-
2018
- 2018-01-19 CN CN201810053500.XA patent/CN108147943A/en active Pending
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|---|---|---|---|---|
| CN1045090A (en) * | 1987-11-10 | 1990-09-05 | 纳幕尔杜邦公司 | The preparation of chloroform |
| CN1051167A (en) * | 1989-10-10 | 1991-05-08 | 纳幕尔杜邦公司 | The hydrogenolysis of halocarbon |
| US5208393A (en) * | 1989-12-22 | 1993-05-04 | Ercros, S.A. | Process for the manufacture of chloroform |
| JPH05221890A (en) * | 1992-01-14 | 1993-08-31 | Toyo Kasei Kogyo Kk | Method for treating carbon tetrachloride |
| JPH06145079A (en) * | 1992-11-06 | 1994-05-24 | Tokuyama Soda Co Ltd | Production of chloroform |
| CN1109461A (en) * | 1993-11-04 | 1995-10-04 | 恩尼彻姆公司 | Preparation of CHCl3 by starting from CCl4 |
| CN1350885A (en) * | 2000-10-31 | 2002-05-29 | 舒德化学公司 | Catalyst for preparing chloroform by hydrogenation dechlorination of carbon tetrachloride |
| DE10228480A1 (en) * | 2002-06-26 | 2004-01-15 | Lii Europe Gmbh | Production of chloroform by selective hydrogenation of carbon tetrachloride with gaseous hydrogen comprises contact with finely divided particles of a Group VIII metal or copper on a porous support material in the presence of an activator |
| CN1636631A (en) * | 2003-10-08 | 2005-07-13 | 株式会社德山 | Catalyst for reduction of polychloralkane, producing process thereof and process for producing low-grade chloralkane |
| CN101362090A (en) * | 2008-09-28 | 2009-02-11 | 广东理文化工研发有限公司 | Catalyst for transferring the carbon tetrachloride into chloroform and preparation method thereof |
| CN102633591A (en) * | 2011-11-03 | 2012-08-15 | 常州大学 | Catalytic conversion technology for carbon tetrachloride |
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| 张霓等: "四氯化碳催化加氢制氯仿的实验研究", 《北京化工大学学报》 * |
| 陈春财: "国内外四氯化碳转化技术介绍", 《中国氯碱》 * |
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Application publication date: 20180612 |