CN104190104B - A kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance - Google Patents
A kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance Download PDFInfo
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- CN104190104B CN104190104B CN201410425855.9A CN201410425855A CN104190104B CN 104190104 B CN104190104 B CN 104190104B CN 201410425855 A CN201410425855 A CN 201410425855A CN 104190104 B CN104190104 B CN 104190104B
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Abstract
The invention discloses a kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance, the equipment includes lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower, the tower top of the lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower is connected with condenser and return tank in turn by pipeline, and connect to form backflow by reflux pump with tower top, while the bottom of each tower is equipped with reboiler；The bottom of the lightness-removing column is provided with discharge nozzle and is connected with eparating methanol tower by discharging pump；The bottom of the eparating methanol tower also is provided with discharge nozzle and is connected with methanol eddy tower feeding mouth by discharging pump, and the backflow pump discharge of tower top is provided with arm, and is connected with pressurizing tower feeding mouth；The bottom of the pressurizing tower and methanol eddy tower is equipped with products export.Dimethoxym ethane in effectively refined recovery glyphosate accessory substance of the invention, reduces waste discharge and environmental pollution, and improves productivity effect and greatly improve glyphosate accessory substance added value, turn waste into wealth.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to the by-product of producing glyphosate by using glycine
The process for purification of dimethoxym ethane in thing.
Background technology
Glyphosate is a kind of broad spectrum organic phosphorus herbicide, be interior suction after a seed bud, conduct, go out raw nonselective herbicide,
There is excellent biological nature, other kind herbicides cannot replace at present.China produces the main flow work of glyphosate at present
Skill is glycine method (dialkyl phosphite method), is with glycine as initiation material, passes through with paraformaldehyde, dimethylphosphite
Addition, condensation, hydrolysis and glyphosate.Solvent methanol can generate dimethoxym ethane, mother liquor concentrations work in paraformaldehyde depolymehzation process
Skill, during reclaiming methyl alcohol, glyphosate per ton is while recyclable about 0.45 ton of dimethoxym ethane.Dimethoxym ethane is used as glyphosate production pair
Produce, its amount is very considerable, at present, this by-product is sold by manufacturer as general merchandise.Dimethoxym ethane content 85% or so, only
Make the occasion few in number such as solvent for paint, will such as be used for the higher industry of requirement, then there will be rectification process, further improve
Content.
Dimethoxym ethane, is colourless transparent liquid, has the smell of similar chloroform, and low boiling point, with excellent dissolubility and water phase
Dissolubility is good.It is novel solvent that State Environmental Protection Administration recommends.Concrete physical and chemical parameter is as follows：2 molecule of molecular formula CH2 (OCH3)
Amount：76.09, boiling point：42.3 DEG C, -17.8 DEG C of flash-point, density d 15/15.0.866；D20/20.0.861,237 DEG C of self-ignition point melt
- 104.8 DEG C of point, more stable to alkali, when heating together with watery hydrochloric acid, it is readily decomposed to formaldehyde and methyl alcohol.With ether, propyl alcohol, ketone
Etc. miscible；Energy dissolving resin and oils, solvability are stronger than ether, acetone；Nitrogen content can be dissolved with the azeotropic mixture of methyl alcohol
High nitrocellulose；32.3% (WT) is dissolved when 16 DEG C in water；Water dissolves 4.3% (WT) in dimethoxym ethane.
The technique of traditional production dimethoxym ethane, under under the concentrated sulfuric acid or acid resin catalyst catalysis, methyl alcohol is molten
Liquid and formalin carry out reactive distillation or intermittent reaction in synthetic tower, as methyl alcohol is liquid during reaction, reacts and generate
Thing dimethoxym ethane easily generates solution altogether with methyl alcohol, and solution is difficult to separate from dimethoxym ethane altogether, so as to affect product dimethoxym ethane
Quality.Unreacted methanol solution is directly discharged, cause material waste and waste water in methanol content too high, pollute ring
Border.
Content of the invention
Goal of the invention：For above-mentioned problem and defect, the invention provides a kind of producing glyphosate by using glycine
The dimethoxym ethane process for refining device and method of accessory substance, dimethoxym ethane in effectively refined recovery glyphosate accessory substance, reduce waste row
Put and environmental pollution, and improve productivity effect.
Technical scheme：For achieving the above object, the present invention is employed the following technical solutions：A kind of glycine method production grass
The dimethoxym ethane process for refining equipment of sweet phosphine accessory substance, including lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower, described de-
The tower top of light tower, eparating methanol tower, pressurizing tower and methanol eddy tower is connected with condenser and return tank in turn by pipeline, and leads to
Cross reflux pump to connect to form backflow with tower top, while the bottom of each tower is equipped with reboiler；The bottom of the lightness-removing column is provided with out
Expects pipe is simultaneously connected with eparating methanol tower by discharging pump；The bottom of the eparating methanol tower also is provided with discharge nozzle and by discharging pump and first
Alcohol reflux tower feeding mouth connects, and the backflow pump discharge of tower top is provided with arm, and is connected with pressurizing tower feeding mouth；The pressurizing tower
Products export is equipped with the bottom of methanol eddy tower.
The condenser connected at the top of the pressurizing tower is the reboiler for being located at eparating methanol tower bottom.
The eparating methanol tower bottom is provided with two reboilers, and one of reboiler is independent reboiler, and another boils again
Device thermal source is from pressurizing tower top gas.
Another object of the present invention there is provided a kind of dimethoxym ethane refining technique based on above-mentioned process equipment, including with
Lower step：
(1) after glyphosate accessory substance sends into lightness-removing column, rectifying is carried out in lightness-removing column, tower top outlet gas phase is obtained through supercooling
To dimethyl ether and monochloro methane mixture that content is 90～99%, a portion is back to lightness-removing column, remainder conduct
Accessory substance output；Wherein, the pressure in lightness-removing column is 0.8～1.5MPa, and tower top temperature is 40～55 DEG C, and column bottom temperature is 115
～130 DEG C；
(2), after the heavy constituent of lightness-removing column bottom of towe enters eparating methanol tower, further rectifying in eparating methanol tower is separated, and tower top is obtained
To the azeotropic constituent being made up of dimethoxym ethane and a small amount of methyl alcohol, and bottom of towe obtains the mixture that main component is methyl alcohol, and delivers to
Methanol eddy tower is further purified；The pressure of the eparating methanol tower is 0～0.2MPa, and tower top temperature is 40～55 DEG C, bottom of towe temperature
Spend for 70～85 DEG C；
(3) the azeotropic constituent at the top of eparating methanol tower is partly refluxed to eparating methanol tower, and remainder is sent into pressurizing tower and carried out
Compression rectification, from the dimethoxym ethane that bottom of towe obtains 99～99.9%；In the pressurizing tower pressure be 0.8～1.5MPa, temperature in tower
For 120～140 DEG C；
(4) eparating methanol tower bottom of towe obtains mixture and sends into methanol eddy tower being further fractionated, 95 are obtained from tower top～
99.5% methyl alcohol, used as accessory substance output；The methanol eddy pressure tower is 0～0.2MPa, and tower top temperature is 65～85 DEG C,
Column bottom temperature is 100～120 DEG C.
Further improve, the pressurizing tower tower top stream goes out gas phase and exchanged heat through the reboiler with eparating methanol tower tower bottom
After cooling, pressurizing tower is partly refluxed to, remainder sends into eparating methanol tower entrance.
Beneficial effect：Compared with prior art, the present invention has advantages below：Reclaim purification producing glyphosate by using glycine
Dimethoxym ethane in accessory substance, improves its economic benefits；Of the invention can by-product high concentration methanol, low boiling point solvent monochloro methane, two
Methyl ether.The dimethoxym ethane prepared using the invention market that compares adopts methyl alcohol, formaldehyde to prepare high-concentration methylal cost for raw material
Low with energy consumption.Patent of the present invention employs differential pressure rectifying thermal coupling, and the heat by the use of pressurizing tower overhead vapours is used as eparating methanol tower
Reboiler thermal source, greatly save heat, for the consumption of steam consumption and recirculated water has a larger lifting, and by tower
Top condenser and reboiler are combined into an equipment, effectively reduce equipment cost.
Description of the drawings
Fig. 1 is the structural representation of the refined production process equipment of dimethoxym ethane of the present invention.
Wherein, lightness-removing column 1, eparating methanol tower 2, pressurizing tower 3, methanol eddy tower 4, condenser 5, return tank 6, reflux pump 7, again
Boiling device 8.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is further elucidated with, it should be understood that these embodiments are merely to illustrate
The present invention rather than restriction the scope of the present invention, after the present invention has been read, those skilled in the art are each to the present invention's
The modification for planting the equivalent form of value falls within the application claims limited range.
As shown in figure 1, main component is 80～95% dimethoxym ethane and first in the accessory substance of producing glyphosate by using glycine
Alcohol, and a small amount of dimethyl ether, monochloro methane, water and poly- dimethoxym ethane, its are sent into de- light after metering as raw material A by pump
Tower, carries out rectifying in lightness-removing column, lightness-removing column system comprising conventional lightness-removing column, lightness-removing column top condenser, lightness-removing column return tank,
Lightness-removing column reflux pump, lightness-removing column reboiler and lightness-removing column bottom discharging pump.
In lightness-removing column, raw material enters the liquid of lightness-removing column return tank through a lightness-removing column reflux pump part through rectifying from tower top
Tower is back to, another part light component (mainly containing dimethyl ether, monochloro methane etc.) is directly as product output；Lightness-removing column bottom liquid
(mainly containing dimethoxym ethane, first alcohol and water etc.) is pumped to eparating methanol tower unit through the discharging of dehydrogenation bottom of towe.
Eparating methanol tower system includes conventional rectification device eparating methanol tower, and two separating methanol reboiler A/B, separating methanol tower top are cold
Condenser, separating methanol return tank and eparating methanol tower reflux pump.Separating methanol tower top is obtained methyl alcohol and is constituted with the azeotropic of dimethoxym ethane, by piptonychia
Alcohol reflux tank is back to tower through separating methanol reflux pump, a part, is partly into pressurizing tower；Pressurization Tower System is mainly comprising conventional
Rectifier unit pressurizing tower return tank, pressurizing tower reflux pump, pressurizing tower reboiler and pressurizing tower condenser as eparating methanol tower again
Boiling device, pressurization tower top obtain 70～85% or so dimethoxym ethane solution by the pressurized tower reflux pump of pressurizing tower return tank, and a part is returned
Tower is flow to, eparating methanol tower is partly into and is recycled.Pressurization tower bottom is sent outside for finished product high-concentration methylal, eparating methanol tower bottom
Portion's methyl alcohol and a small amount of heavy constituent, are pumped into 17 methanol distillation columns through eparating methanol tower bottom.Methanol distillation column unit includes conventional essence
Distillation unit methanol distillation column, methanol distillation column condenser, methanol distillation column return tank, methanol distillation column reflux pump, Methanol Recovery
Tower reboiler, Methanol Recovery bottom of towe pump, light component high concentration methanol are back to tower through methanol distillation column reflux pump, a part, and one
Part is produced as product, and bottom of towe restructuring 22 Methanol Recovery bottom of towe of lease making is pumped to the external world.
In above-mentioned technical process, lightness-removing column 0.6～1.2MPa of tower top pressure (g) is controlled, eparating methanol tower tower top pressure 0～
0.3MPa (g), pressurizing tower 0.8～1.6MPa of tower top pressure (g), methanol distillation column tower top pressure are 0～0.3MPa (g).More than
All of tower can adopt high-efficiency packing tower, and the plate efficiency in order to increase under pressurized condition can be adopted with lightness-removing column and pressurizing tower
Plate column.For the effectively utilizes of energy, the device is using the thermal source by the use of pressurizing tower overhead vapours as methanol distillation column.
The present invention mainly purifies the dimethoxym ethane in producing glyphosate by using glycine by-product dimethoxym ethane, improves its economy effect
Should.Energy by-product high concentration methanol of the invention, low boiling point solvent monochloro methane, dimethyl ether.The dimethoxym ethane phase prepared using the invention
Relatively market adopts that methyl alcohol, formaldehyde prepare high-concentration methylal cost for raw material and energy consumption is low.Patent of the present invention employs differential pressure
Rectifying thermal coupling, the heat by the use of pressurizing tower overhead vapours greatly save heat as the reboiler thermal source of eparating methanol tower, right
Consumption in steam consumption and recirculated water has larger lifting, and overhead condenser and reboiler are combined into an equipment,
Effectively reduce equipment cost.
Claims (5)
1. the dimethoxym ethane process for refining equipment of a kind of producing glyphosate by using glycine accessory substance, it is characterised in that：Including lightness-removing column,
Eparating methanol tower, pressurizing tower and methanol eddy tower, the tower top of the lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower lead to
Piping is connected with condenser and return tank in turn, and connects to form backflow by reflux pump with tower top, while the bottom of each tower
It is equipped with reboiler；The bottom of the lightness-removing column is provided with discharge nozzle and is connected with eparating methanol tower by discharging pump；The separating methanol
The bottom of tower also is provided with discharge nozzle and is connected with methanol eddy tower feeding mouth by discharging pump, and the backflow pump discharge of tower top is provided with
Arm, and be connected with pressurizing tower feeding mouth；The bottom of the pressurizing tower and methanol eddy tower is equipped with products export.
2. the dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance according to claim 1, its feature exist
In：The condenser connected at the top of the pressurizing tower is the reboiler for being located at eparating methanol tower bottom.
3. the dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance according to claim 2, its feature exist
In：The eparating methanol tower bottom is provided with two reboilers, and one of reboiler is independent reboiler, another reboiler thermal source
From pressurizing tower top gas.
4. a kind of dimethoxym ethane refining technique based on the arbitrary process equipment of claims 1 to 3, it is characterised in that include
Following steps：
(1) after glyphosate accessory substance sends into lightness-removing column, rectifying is carried out in lightness-removing column, tower top outlet gas phase is contained through supercooling
Dimethyl ether and the monochloro methane mixture for 90～99% is measured, a portion is back to lightness-removing column, and remainder is used as by-product
Produce go out；Wherein, the pressure in lightness-removing column is 0.8～1.5MPa, and tower top temperature is 40～55 DEG C, and column bottom temperature is 115～130
℃；
(2) after the heavy constituent of lightness-removing column bottom of towe enters eparating methanol tower, further rectifying separation in eparating methanol tower, tower top obtain by
Dimethoxym ethane and the azeotropic constituent of a small amount of methyl alcohol composition, and bottom of towe obtains the mixture that main component is methyl alcohol, and deliver to methyl alcohol
Reflux column is further purified；The pressure of the eparating methanol tower is 0～0.2MPa, and tower top temperature is 40～55 DEG C, and column bottom temperature is
70～85 DEG C；
(3) the azeotropic constituent at the top of eparating methanol tower is partly refluxed to eparating methanol tower, and remainder is sent into pressurizing tower and pressurizeed
Rectifying, from the dimethoxym ethane that bottom of towe obtains 99～99.9%；In the pressurizing tower, pressure is 0.8～1.5MPa, and in tower, temperature is 120
～140 DEG C；
(4) eparating methanol tower bottom of towe obtain mixture send into methanol eddy tower be further fractionated, obtain 95～99.5% from tower top
Methyl alcohol, used as accessory substance output；The methanol eddy pressure tower is 0～0.2MPa, and tower top temperature is 65～85 DEG C, column bottom temperature
For 100～120 DEG C.
5. dimethoxym ethane refining technique according to claim 4, it is characterised in that：The pressurizing tower tower top stream goes out gas phase warp
Crossing is carried out after heat exchange cooling with the reboiler of eparating methanol tower tower bottom, is partly refluxed to pressurizing tower, and remainder sends into separating methanol
Tower entrance.
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| CN104761430A (en) * | 2015-03-12 | 2015-07-08 | 赛鼎工程有限公司 | Process of varying-pressure thermal-coupling rectification separation of methylal from methanol |
| CN108997086A (en) * | 2018-08-31 | 2018-12-14 | 南通江山农药化工股份有限公司 | The purifying process of glyphosate by using glycine by-product dimethoxym ethane |
| CN110343034A (en) * | 2019-07-30 | 2019-10-18 | 安徽东至广信农化有限公司 | A kind of method of variable-pressure rectification recycling purification dimethoxym ethane |
| CN113429269B (en) * | 2021-07-29 | 2023-07-28 | 南通江山农药化工股份有限公司 | Methylal pressurization rectification purification process equipment |
| CN113828001B (en) * | 2021-10-29 | 2022-10-11 | 新疆晶硕新材料有限公司 | Separation system and separation method of chloromethane |
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| CN101225030B (en) * | 2007-01-15 | 2011-07-20 | 浙江新安化工集团股份有限公司 | Method for utilizing thermal energy during continuous synthesis of glyphosate |
| CN100509786C (en) * | 2008-04-18 | 2009-07-08 | 浙江金帆达生化股份有限公司 | Comprehensive process for tail gas in glyphosate production |
| EP2450336A1 (en) * | 2010-11-09 | 2012-05-09 | INEOS Paraform GmbH | Process for the production of pure methylal |
| CN102093176B (en) * | 2010-12-23 | 2014-07-30 | 南京师范大学 | Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk |
| CN204275534U (en) * | 2014-08-27 | 2015-04-22 | 江苏凯茂石化科技有限公司 | A kind of dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance |
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Denomination of invention: Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method Effective date of registration: 20170622 Granted publication date: 20170315 Pledgee: Jiangsu Wujin credit Company limited by guarantee Pledgor: Jiangsu Kaimao Chemical Technology Co., Ltd. Registration number: 2017990000474 |
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