CN109970790A - The extraction separating method and rectifier unit of dichloromethylphosphine - Google Patents
The extraction separating method and rectifier unit of dichloromethylphosphine Download PDFInfo
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- CN109970790A CN109970790A CN201910355096.6A CN201910355096A CN109970790A CN 109970790 A CN109970790 A CN 109970790A CN 201910355096 A CN201910355096 A CN 201910355096A CN 109970790 A CN109970790 A CN 109970790A
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- dichloromethylphosphine
- phosphorus trichloride
- rectifying column
- column
- extractant
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/52—Halophosphines
Abstract
The present invention relates to the extraction separating method of dichloromethylphosphine and rectifier units, belong to rectifying separation technology field.Present invention solves the technical problem that phosphorus trichloride purity is low when being that the prior art separates dichloromethylphosphine from phosphorus trichloride, flow back relatively high.The invention discloses the extraction separating methods of dichloromethylphosphine, extractant is added in the mixture containing phosphorus trichloride and dichloromethylphosphine, successively distillation obtains phosphorus trichloride and dichloromethylphosphine after mixing, recycled after the extractant recycling in remaining liq.Invention has the advantages that separative efficiency is high compared to traditional handicraft, reduces theoretical cam curve, reducing reflux ratio, the three wastes are few, operation energy consumption is low etc., is conducive to industrialized production.
Description
Technical field
The invention belongs to rectifying separation technology fields, and in particular to the extraction separating method of dichloromethylphosphine and rectifying dress
It sets.
Background technique
Dichloromethylphosphine can be used as high-efficiency low-toxicity steriland herbicide glufosinate-ammonium and the resistance of non-halogen methyl hypophosphorous acid esters
Fire the key intermediate of agent.Glufosinate-ammonium is the excellent substitute of paraquat, and the resolution ability of quick-acting and Weed Resistance is better than
Glyphosate；Non-halogen flame retardant has many advantages, such as that additive amount is few, the high and low cigarette of flame retarding efficiency, low toxicity, widely used.Therefore, it studies
High efficiency, low cost manufactures dichloromethylphosphine, is increasingly valued by people.
Currently, dichloromethylphosphine can use phosphorus trichloride and alchlor Solid phase synthesis, can also be used by methane
Pintsch process with phosphorus trichloride at 500 DEG C or more synthesizes.The former solid waste yield is big, and with quantity of three wastes, few, atom passes through the latter
The high advantage of Ji property, but energy consumption is larger, because of the conversion ratio of the reaction raw materials phosphorus trichloride only 20% or so, phosphorus trichloride and first
Base dichloride phosphine boiling point differs 7 DEG C, and it is very big that dichloromethylphosphine difficulty is separated from a large amount of phosphorus trichloride.
A kind of method of separation of extractive distillation dichloromethylphosphine is disclosed in CN 108659042A, with 1,1,2- trichlorine
Ethane or tetrachloro-ethylene are extractant, and phosphorus trichloride theoretical number of plates of rectifying tower is 90~120 pieces, and reflux ratio is 5:1~12:1,
Although reflux ratio is reduced, the phosphorus trichloride highest content of this method rectifying extraction is 97.2%, impure phosphorus trichloride
Make raw material for cracking reaction, through high temperature rear impurity coking, cracker is caused to block, block clearing of frequently stopping causes to produce
Discontinuity, operating cost increase.
Summary of the invention
Present invention solves the technical problem that when being that the prior art separates dichloromethylphosphine from phosphorus trichloride, phosphorus trichloride
Purity is low, flows back relatively high.
Technical proposal that the invention solves the above-mentioned problems is to provide the extraction separating method of dichloromethylphosphine, including as follows
Step: being added extractant in the mixture containing phosphorus trichloride and dichloromethylphosphine, and successively distillation obtains trichlorine after mixing
Change phosphorus and dichloromethylphosphine, recycled after the extractant recycling in remaining liq, the extractant is compoundOr at least one of sulfolane, wherein R1、R2、R3、R4、R5、R6It is each independently selected from hydrogen, methyl, second
Base, methoxyl group, ethyoxyl, halogen.
Wherein, extractant is preferably toluene, dimethylbenzene, trimethylbenzene, ortho-chlorotolu'ene, o-chloro-anisole, 1,2-dimethoxy benzene, ring
At least one of fourth sulfone.
Wherein, the additional amount of extractant is the 0.1%~150% of mixture quality.
Wherein, the additional amount of extractant is preferably the 1%~15% of mixture quality.
Wherein, after extractant being added in the mixture of phosphorus trichloride and dichloromethylphosphine, successively pass through phosphorus trichloride essence
Evaporate tower (I), dichloromethylphosphine rectifying column (II) rectifying, first obtain phosphorus trichloride from phosphorus trichloride rectifying column (I), then from
Dichloromethylphosphine rectifying column (II) obtains dichloromethylphosphine.
Wherein, the tower top temperature for distilling out phosphorus trichloride is 73~76 DEG C, and column bottom temperature is 90~120 DEG C, distills out first
The tower top temperature of base dichloride phosphine is 81~85 DEG C, and column bottom temperature is 125~210 DEG C.
Wherein, 73~76 DEG C of tower top temperature of phosphorus trichloride rectifying column (I), tower top pressure 0.1kPa~1KPa, overhead reflux
Than 1:1~15:1,90~120 DEG C of column bottom temperature, tower bottom pressure 10kPa~30KPa；Overhead reflux is than being preferably 1:1~5:1.
Wherein, 81~85 DEG C of tower top temperature of dichloromethylphosphine rectifying column (II), tower top pressure 0.1kPa~1KPa, tower top
Reflux ratio 1:1~2:1,125~210 DEG C of column bottom temperature, tower bottom pressure 3kPa~25KPa.
Invention additionally discloses the rectifying devices of dichloromethylphosphine extraction extraction separating method, including phosphorus trichloride rectifying column
(I), dichloromethylphosphine rectifying column (II) and extracting agent recovery device (III)；Two rectifying columns middle part be equipped with into
Material mouth, tower top connect condenser, and the liquid outlet of condenser is separately connected the column overhead and receives storage tank, phosphorus trichloride rectifying column
(I) feed inlet is connected in the middle part of bottom and dichloromethylphosphine rectifying column (II), dichloromethylphosphine rectifying column (II) bottom with
Extracting agent recovery device (III) is connected.
Wherein, phosphorus trichloride rectifying column (I), dichloromethylphosphine rectifying column (II) are plate column or packed tower.
Wherein, phosphorus trichloride rectifying column (I) theoretical cam curve is 70~110, and dichloromethylphosphine rectifying column (II) is theoretical
The number of plates is 25~45.
Wherein, the raw mixture feed entrance point of phosphorus trichloride rectifying column (I) phosphorus trichloride and dichloromethylphosphine is the
At 50~60 blocks of column plates, extractant feed position is located at the top of raw mixture feed inlet, dichloromethylphosphine rectifying column
(II) feed entrance point is at the 15th~22 block of column plate.
Beneficial effects of the present invention:
The present invention is used when rectifying separates dichloromethylphosphine from a large amount of phosphorus trichloridesAs extraction
Agent is taken, wherein R1、R2、R3、R4、R5、R6It is each independently hydrogen, methyl, ethyl, methoxyl group, ethyoxyl, halogen, to tri-chlorination
Phosphorus and dichloromethylphosphine are efficiently separated；It, can be in lower theoretical cam curve and reflux by way of two-tower rectification
Than in the case where, phosphorus trichloride of the purity 98% or more is obtained；The present invention has separative efficiency height compared to traditional handicraft, reduces
Theoretical cam curve reduces reflux ratio, the advantages such as the three wastes are few, operation energy consumption is low, is conducive to industrialized production.
Detailed description of the invention
Fig. 1 is the schematic diagram (equipment appurtenance is not limited to equipment in figure) of dichloromethylphosphine extracting rectifying device of the present invention,
Wherein (I) is phosphorus trichloride rectifying column, and auxiliary device includes condenser, reboiler, pump, pans etc., and (II) is methyl dichloro
Change phosphorus rectifying column, auxiliary device includes condenser, reboiler, pump etc., and (III) is wiped-film short-distance linkage, and auxiliary device includes
Receiving tank, pump etc..
Specific embodiment
The present invention provides the extraction separating method of dichloromethylphosphine, includes the following steps: containing phosphorus trichloride and first
Extractant is added in the mixture of base dichloride phosphine, successively distillation obtains phosphorus trichloride and dichloromethylphosphine after mixing, remaining
Recycled after extractant recycling in liquid, the extractant are compoundOr at least one in sulfolane
It plants, wherein R1、 R2、R3、R4、R5、R6It is each independently hydrogen, methyl, ethyl, methoxyl group, ethyoxyl, halogen.
Wherein, extractant is preferably toluene, dimethylbenzene, trimethylbenzene, ortho-chlorotolu'ene, o-chloro-anisole, 1,2-dimethoxy benzene, ring
At least one of fourth sulfone.
Wherein, the additional amount of extractant is the 0.1%~150% of mixture quality.
Wherein, the additional amount of extractant is preferably the 1%~15% of mixture quality.
Wherein, after extractant being added in the mixture of phosphorus trichloride and dichloromethylphosphine, successively pass through phosphorus trichloride essence
Evaporate tower (I), dichloromethylphosphine rectifying column (II) rectifying, first obtain phosphorus trichloride from phosphorus trichloride rectifying column (I), then from
Dichloromethylphosphine rectifying column (II) obtains dichloromethylphosphine.
Wherein, the tower top temperature for distilling out phosphorus trichloride is 73~76 DEG C, and column bottom temperature is 90~120 DEG C, distills out first
The tower top temperature of base dichloride phosphine is 81~85 DEG C, and column bottom temperature is 125~210 DEG C.
Further, energy consumption, raising separative efficiency are reduced in order to reach, while guarantees the purity of phosphorus trichloride, rectifying
Temperature, pressure, the reflux ratio of journey can be controlled in following ranges:
Wherein, 73~76 DEG C of tower top temperature of phosphorus trichloride rectifying column (I), tower top pressure 0.1kPa~1KPa, overhead reflux
Than caning be controlled in 1:1~15:1,90~120 DEG C of column bottom temperature, tower bottom pressure 10kPa~30KPa；Preferably, tower top returns
Stream ratio also can be controlled in 1:1~5:1.
Wherein, 81~85 DEG C of tower top temperature of dichloromethylphosphine rectifying column (II), tower top pressure 0.1kPa~1KPa, tower top
Reflux ratio can be controlled in 1:1~2:1, and 125~210 DEG C of column bottom temperature, tower bottom pressure 3kPa~25KPa.
Invention additionally discloses the rectifying devices of dichloromethylphosphine extraction extraction separating method, including phosphorus trichloride rectifying column
(I), dichloromethylphosphine rectifying column (II) and extracting agent recovery device (III)；Two rectifying columns middle part be equipped with into
Material mouth, tower top connect condenser, and the liquid outlet of condenser is separately connected the column overhead and receives storage tank, phosphorus trichloride rectifying column
(I) feed inlet is connected in the middle part of bottom and dichloromethylphosphine rectifying column (II), dichloromethylphosphine rectifying column (II) bottom with
Extracting agent recovery device (III) is connected.
Wherein, phosphorus trichloride rectifying column (I), dichloromethylphosphine rectifying column (II) are plate column or packed tower.
Wherein, phosphorus trichloride rectifying column (I) theoretical cam curve is 70~110, and dichloromethylphosphine rectifying column (II) is theoretical
The number of plates is 25~45.
Wherein, the raw mixture feed entrance point of phosphorus trichloride rectifying column (I) phosphorus trichloride and dichloromethylphosphine is the
At 50~60 blocks of column plates, extractant feed position is located at the top of raw mixture feed inlet, dichloromethylphosphine rectifying column
(II) feed entrance point is at the 15th~22 block of column plate.
Specifically, phosphorus trichloride rectifying column (I) is equipped with reboiler, for the heating of materials at bottom of tower, dichloromethylphosphine essence
It evaporates tower (II) and also is provided with reboiler, the heating for materials at bottom of tower.
Wherein, wiped-film short-distance linkage can be selected in extracting agent recovery device (III).
The present invention will be further explained by the following examples and explanation.
Embodiment 1
Stainless steel rectifying column of the experiment using a set of DN25, built-in θ ring wire packing, 3 meters of tower height (theoretical cam curve 70~
75), raw mixture group is divided into phosphorus trichloride 80.3%, dichloromethylphosphine 19%, and extractant is pseudocumene；
Extracting rectifying is carried out using continuous operation method, feedstock position is 1.5 meters of eminences, and pseudocumene feed inlet is higher by
Mixed liquor feed inlet 10cm, pseudocumene inlet amount be mixture 7%, control reflux ratio 1:1,110 DEG C of column bottom temperature, tower top
74 DEG C of temperature, tower top obtains the phosphorus trichloride that purity is 99%, and tower bottom obtains the mixture of dichloromethylphosphine and pseudocumene；
The mixture of dichloromethylphosphine and pseudocumene pump is continuously entered into other set DN25 stainless steel rectifying column
It is interior, built-in θ ring wire packing, 2 meters of tower height, feed entrance point be 1 meter of eminence, control reflux ratio be 1:1,170 DEG C of column bottom temperature, tower
83 DEG C of temperature of top, tower top obtains methyl dichloro phosphorus, and purity 98%, last materials at bottom of tower is by way of depressurizing wiped-film short-distance distillation
Recycle extractant pseudocumene, purity 99.0%.
Embodiment 2
Same as Example 1, Solvent quantity ratio replaces with 3%, and phosphorus trichloride separation process reflux ratio replaces with 3:
1, resulting phosphorus trichloride purity is 97.9%, and gained dichloromethylphosphine purity is 98.5%, and gained pseudocumene purity is
99.0%.
Embodiment 3
Same as Example 1, extractant replaces with sulfolane, and phosphorus trichloride separation process reflux ratio replaces with 2:1, methyl
Dichloride phosphine rectifying column bottom temperature is 210 DEG C, and resulting phosphorus trichloride purity is 98.7%, and gained dichloromethylphosphine purity is
97.6%, gained sulfolane purity is 99.1%.
Embodiment 4
Same as Example 1, extractant replaces with ortho-xylene, and phosphorus trichloride separation process reflux ratio replaces with 5:1, first
Base dichloride phosphine rectifying column bottom temperature is 145 DEG C, and resulting phosphorus trichloride purity is 98.0%, gained dichloromethylphosphine purity
It is 97.7%, gained ortho-xylene purity is 99.0%.
Embodiment 5
Same as Example 1, extractant replaces with ortho-chlorotolu'ene, and dichloromethylphosphine rectifying column bottom temperature is 165 DEG C, institute
The phosphorus trichloride purity obtained is 98.3%, and gained dichloromethylphosphine purity is 98.6%, and gained ortho-chlorotolu'ene purity is
98.6%.
Embodiment 6
Same as Example 1, extractant replaces with 1,2-dimethoxy benzene, and phosphorus trichloride separation process reflux ratio replaces with 5:1,
Dichloromethylphosphine rectifying column bottom temperature is 210 DEG C, and resulting phosphorus trichloride purity is 97.5%.Gained dichloromethylphosphine is pure
Degree is 98.2%, and gained 1,2-dimethoxy benzene purity is 99.1%.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
1. the extraction separating method of dichloromethylphosphine, it is characterised in that include the following steps: containing phosphorus trichloride and methyl
Extractant is added in the mixture of dichloride phosphine, successively distillation obtains phosphorus trichloride and dichloromethylphosphine, raffinate after mixing
Recycled after extractant recycling in body, the extractant are compoundOr at least one in sulfolane
It plants, wherein R1、R2、R3、R4、R5、R6It is each independently selected from hydrogen, methyl, ethyl, methoxyl group, ethyoxyl, halogen.
2. the extraction separating method of dichloromethylphosphine according to claim 1, it is characterised in that: the extractant is first
At least one of benzene, dimethylbenzene, trimethylbenzene, ortho-chlorotolu'ene, o-chloro-anisole, 1,2-dimethoxy benzene, sulfolane.
3. the extraction separating method of dichloromethylphosphine according to claim 1 or 2, it is characterised in that: the extractant
Additional amount be mixture quality 0.1%~150%；Preferably the 1%~15% of mixture quality.
4. the extraction separating method of described in any item dichloromethylphosphines according to claim 1~3, it is characterised in that: trichlorine
Change after extractant is added in the mixture of phosphorus and dichloromethylphosphine, successively passes through phosphorus trichloride rectifying column (I), methyl dichloro
Phosphine rectifying column (II) rectifying first obtains phosphorus trichloride from phosphorus trichloride rectifying column (I), then from dichloromethylphosphine rectifying column
(II) dichloromethylphosphine is obtained.
5. the extraction separating method of dichloromethylphosphine according to claim 4, it is characterised in that: distill out phosphorus trichloride
Tower top temperature be 73~76 DEG C, column bottom temperature be 90~120 DEG C, distill out dichloromethylphosphine tower top temperature be 81~85
DEG C, column bottom temperature is 125~210 DEG C.
6. the extraction separating method of dichloromethylphosphine according to claim 4 or 5, it is characterised in that: phosphorus trichloride essence
Evaporate 73~76 DEG C of tower top temperature of tower (I), tower top pressure 0.1kPa~1KPa；Overhead reflux ratio 1:1~15:1；Column bottom temperature 90~
120 DEG C, tower bottom pressure 10kPa~30KPa；Overhead reflux is than being preferably 1:1~5:1.
7. the extraction separating method of dichloromethylphosphine according to any one of claim 4 to 6, it is characterised in that: methyl
81~85 DEG C of tower top temperature of dichloride phosphine rectifying column (II), tower top pressure 0.1kPa~1KPa；Overhead reflux ratio 1:1~2:1；Tower
125~210 DEG C of bottom temperature, tower bottom pressure 3kPa~25KPa.
8. being used for the rectifier unit of the described in any item dichloromethylphosphine extraction separating methods of claim 1~7, feature exists
In: including phosphorus trichloride rectifying column (I), dichloromethylphosphine rectifying column (II) and extracting agent recovery device (III)；Described two
A rectifying column middle part be equipped with feed inlet, tower top connect condenser, the liquid outlet of condenser be separately connected the column overhead and
Storage tank is received, phosphorus trichloride rectifying column (I) bottom is connected with feed inlet in the middle part of dichloromethylphosphine rectifying column (II), methyl two
Phosphonium chloride rectifying column (II) bottom is connected with extracting agent recovery device (III).
9. the rectifier unit of the extraction and separation of dichloromethylphosphine according to claim 8, it is characterised in that: described three
Phosphorus chloride rectifying column (I), dichloromethylphosphine rectifying column (II) are plate column or packed tower；Phosphorus trichloride rectifying column (I) reason
It is 70~110 by the number of plates, dichloromethylphosphine rectifying column (II) theoretical cam curve is 25~45.
10. the rectifier unit of the extraction and separation of dichloromethylphosphine according to claim 9, it is characterised in that: described three
The raw mixture feed entrance point of phosphorus chloride rectifying column (I) phosphorus trichloride and dichloromethylphosphine is at the 50th~60 block of column plate,
Extractant feed position is located at the top of raw mixture feed inlet；Dichloromethylphosphine rectifying column (II) feed entrance point is the 15th
At~22 blocks of column plates.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563761A (en) * | 2019-09-11 | 2019-12-13 | 利尔化学股份有限公司 | Method for cleaning coking substance of methyl phosphine dichloride synthesis trapping system |
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| CN102286021A (en) * | 2011-06-16 | 2011-12-21 | 襄阳市布拉德化工科技有限公司 | Method for producing 2-carboxyethyl(phenyl)phosphinicacid |
| CN105732708A (en) * | 2016-02-01 | 2016-07-06 | 东营美利达新型材料科技有限公司 | Method for producing dichlorophenylphosphine |
| CN108659042A (en) * | 2018-06-22 | 2018-10-16 | 河北威远生物化工有限公司 | A kind of extraction separating method and extracting rectifying equipment of alkyl phosphorus dichloride |
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| WO2010066612A1 (en) * | 2008-12-10 | 2010-06-17 | Basf Se | Method for producing tricyclohexyl phosphonium hydrogen chloride |
| CN102286021A (en) * | 2011-06-16 | 2011-12-21 | 襄阳市布拉德化工科技有限公司 | Method for producing 2-carboxyethyl(phenyl)phosphinicacid |
| CN105732708A (en) * | 2016-02-01 | 2016-07-06 | 东营美利达新型材料科技有限公司 | Method for producing dichlorophenylphosphine |
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| CN110563761A (en) * | 2019-09-11 | 2019-12-13 | 利尔化学股份有限公司 | Method for cleaning coking substance of methyl phosphine dichloride synthesis trapping system |
| CN110563761B (en) * | 2019-09-11 | 2022-03-01 | 利尔化学股份有限公司 | Method for cleaning coking substance of methyl phosphine dichloride synthesis trapping system |
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