CN104190104A - Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method - Google Patents
Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method Download PDFInfo
- Publication number
- CN104190104A CN104190104A CN201410425855.9A CN201410425855A CN104190104A CN 104190104 A CN104190104 A CN 104190104A CN 201410425855 A CN201410425855 A CN 201410425855A CN 104190104 A CN104190104 A CN 104190104A
- Authority
- CN
- China
- Prior art keywords
- tower
- methanol
- pressurizing
- lightness
- eparating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 33
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 22
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 22
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000004471 Glycine Substances 0.000 title claims abstract description 14
- 238000007670 refining Methods 0.000 title claims abstract description 12
- 239000006227 byproduct Substances 0.000 title abstract description 9
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 309
- 238000010992 reflux Methods 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims description 18
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 12
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000470 constituent Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 230000006835 compression Effects 0.000 claims description 2
- 238000007906 compression Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005194 fractionation Methods 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 11
- 238000004821 distillation Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000002904 solvent Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000002363 herbicidal effect Effects 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229920002866 paraformaldehyde Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000066 reactive distillation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses process equipment and a process method for refining dimethoxymethane in byproducts produced in the production of glyphosate by a glycine method. The equipment comprises a light component removing tower, a methanol removing tower, a pressurizing power and a methanol reflux tower, wherein each tower top of the light component removing tower, the methanol removing tower, the pressurizing power and the methanol reflux tower is connected with a condenser and a reflux tank in sequence through pipelines, and reflux is formed by communicating a reflux pump with each tower top; meanwhile, a reboiler is arranged on the bottom of each tower bottom; the bottom of the light component removing tower is provided with a material discharge pipe and is connected with the methanol removing tower through a material discharging pump; the bottom of the methanol removing tower is also provided with a material discharging pipe and is connected with a material inlet of the methanol reflux tower through another material discharging pump; an outlet of the reflux pump at the tower top of the methanol removing tower is provided with a branch pipe and is connected with a material inlet of the pressurizing tower; product outlets are formed in the bottoms of both the pressurizing tower and the methanol reflux tower. According to the process equipment and the process method, the dimethoxymethane in the byproducts of the glyphosate is refined and recycled effectively, so that the waste emission and environment pollution are reduced, the production benefits are improved, the additional value of the byproduct of the glyphosate is greatly improved, and waste is turned into treasure.
Description
Technical field
The invention belongs to Chemical Manufacture Processes and apparatus technical field, relate generally to the process for purification of dimethoxym ethane in the accessory substance of producing glyphosate by using glycine.
Background technology
Glyphosate is a kind of broad spectrum organic phosphorus herbicide, is the interior raw nonselective herbicide of inhaling, conduct, go out after a kind of bud, has good biological nature, and other kind herbicide cannot replace at present.At present China to produce the main flow technique of glyphosate be glycine method (dialkyl phosphite method), be to take glycine as initiation material, with paraformaldehyde, dimethylphosphite through addition, condensation, hydrolysis and glyphosate.Solvent methanol, in paraformaldehyde solution collecting process, can generate dimethoxym ethane, and mother liquor concentration technology reclaims in the process of methyl alcohol, and glyphosate per ton is recyclable approximately 0. 45 tons of dimethoxym ethanes simultaneously.Dimethoxym ethane is as glyphosate production by-product, and its amount is very considerable, and at present, manufacturer sells this by-product as general merchandise.Dimethoxym ethane content, in 85% left and right, is only made the occasions few in number such as solvent for paint, as will be had rectification process for the industry of having relatively high expectations, further improves content.
Dimethoxym ethane, is colourless transparent liquid, has the smell of similar chloroform, and boiling point is low, has good dissolubility, good with water dissolubility.It is the novel solvent of State Environmental Protection Administration's recommendation.Concrete physical and chemical parameter is as follows: molecular formula CH2(OCH3) 2 molecular weight: 76. 09, and boiling point: 42. 3 ℃, flash-point-17. 8 ℃, density d 15/15. 0. 866; D20/20. 0. 861,237 ℃ of self-ignition points, fusing point-104.8 ℃, more stable to alkali, while heating, easily resolve into formaldehyde and methyl alcohol together with watery hydrochloric acid.Miscible with ether, propyl alcohol, ketone etc.; Energy dissolving resin and oils, solvability is stronger than ether, acetone; Can dissolve with the azeotropic mixture of methyl alcohol the nitrocellulose that nitrogen content is high; During 16 ° of C, in water, dissolve 32. 3% (WT); Water dissolves 4. 3% (WT) in dimethoxym ethane.
The technique of traditional production dimethoxym ethane, employing under the concentrated sulfuric acid or acid resin catalyst catalysis under, methanol solution and formalin are carried out reactive distillation or intermittent reaction in synthetic tower, during due to reaction, methyl alcohol is liquid, reaction product dimethoxym ethane and methyl alcohol easily generate solution altogether, solution is difficult for separating from dimethoxym ethane altogether, thereby affects the quality of product dimethoxym ethane.Unreacted methanol solution is directly discharged, and causes in the waste of material and waste water methanol content too high, contaminated environment.
Summary of the invention
Goal of the invention: for problem and the defect of above-mentioned existence, the invention provides a kind of dimethoxym ethane process for refining Apparatus and method for of producing glyphosate by using glycine accessory substance, effectively dimethoxym ethane in refine and reclaim glyphosate accessory substance, reduces waste discharge and environmental pollution, and has improved productivity effect.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance, comprise lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower, the tower top of described lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower is all connected with condenser and return tank in turn by pipeline, and by reflux pump, being communicated with formation backflow with tower top, the bottom of each tower is equipped with reboiler simultaneously; The bottom of described lightness-removing column is provided with discharge nozzle and is connected with eparating methanol tower by discharging pump; The bottom of described eparating methanol tower is also provided with discharge nozzle and is connected with methanol eddy tower feeding mouth by discharging pump, and the reflux pump of tower top outlet is provided with arm, and is connected with pressurizing tower feeding mouth; The bottom of described pressurizing tower and methanol eddy tower is equipped with products export.
The condenser that described pressurizing tower top connects is the reboiler that is located at eparating methanol tower bottom.
Another object of the present invention has been to provide a kind of dimethoxym ethane refining technique based on above-mentioned process equipment, specifically comprises the following steps:
(1) glyphosate accessory substance is sent into after lightness-removing column, carries out rectifying in lightness-removing column, and it is 90～99% dimethyl ether and monochloro methane mixture that tower top outlet gas phase obtains content through supercooling, and wherein a part is back to lightness-removing column, and remainder is as accessory substance output; Wherein, the interior pressure of lightness-removing column is 0.8～1.5MPa, and tower top temperature is 40～55 ℃, and column bottom temperature is 115～130 ℃;
(2) heavy constituent at the bottom of lightness-removing column tower enters after eparating methanol tower, in eparating methanol tower, further rectifying is separated, tower top obtains the azeotropic constituent being comprised of dimethoxym ethane and a small amount of methyl alcohol, and at the bottom of tower, obtains the mixture that main component is methyl alcohol, and delivers to methanol eddy tower and further purify; The pressure of described eparating methanol tower is 0～0.2MPa, and tower top temperature is 40～55 ℃, and column bottom temperature is 70～85 ℃;
(3) the azeotropic constituent at eparating methanol tower top is partly refluxed to eparating methanol tower, and remainder is sent into pressurizing tower and carried out compression rectification, at the bottom of tower, obtains 99～99.9% dimethoxym ethane; In described pressurizing tower, pressure is 0.8～1.5MPa, and in tower, temperature is 120～140 ℃;
(4) at the bottom of eparating methanol tower tower, obtain mixture and send into the further fractionation of methanol eddy tower, from tower, surely obtain 95～99.5% methyl alcohol, as accessory substance output; Described methanol eddy pressure tower is 0～0.2MPa, and tower top temperature is 65～85 ℃, and column bottom temperature is 100～120 ℃.
Further improve, described pressurizing tower overhead streams goes out gas phase after the reboiler with eparating methanol tower tower bottom carries out heat exchange cooling, is partly refluxed to pressurizing tower, and remainder is sent into eparating methanol tower entrance.
Beneficial effect: compared with prior art, the present invention has the following advantages: reclaim the dimethoxym ethane in purification producing glyphosate by using glycine accessory substance, improve its economic benefits; Energy by-product high concentration methanol of the present invention, low boiling point solvent monochloro methane, dimethyl ether.Use the dimethoxym ethane of this invention preparation compare market adopt methyl alcohol, formaldehyde for raw material prepare high-concentration methylal cost and energy consumption low.Patent of the present invention has adopted the coupling of differential pressure rectified heat, utilize the heat of pressurizing tower overhead vapours as the reboiler thermal source of eparating methanol tower, greatly saved heat, consumption for steam consumption and recirculated water all has larger lifting, and overhead condenser and reboiler are combined into an equipment, effectively reduce equipment cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of the refining 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, reboiler 8.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
As shown in Figure 1, in the accessory substance of producing glyphosate by using glycine, main component is 80～95% dimethoxym ethane and methyl alcohol, and a small amount of dimethyl ether, monochloro methane, water and poly-dimethoxym ethane, it sends into lightness-removing column as raw material A after metering by pump, in lightness-removing column, carry out rectifying, lightness-removing column system comprises discharging pump at the bottom of 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.
Lightness-removing column Raw enters lightness-removing column return tank through rectifying liquid from tower top is back to tower through a lightness-removing column reflux pump part, and another part light component (mainly containing dimethyl ether, monochloro methane etc.) is directly as product output; Liquid at the bottom of lightness-removing column (mainly containing dimethoxym ethane, first alcohol and water etc.) is delivered to eparating methanol tower unit through discharging pump at the bottom of dehydrogenation tower.
Eparating methanol tower system comprises conventional rectification device eparating methanol tower, two separating methanol reboiler A/B, separating methanol tower top condenser, separating methanol return tank and eparating methanol tower reflux pump.The azeotropic that separating methanol tower top obtains methyl alcohol and dimethoxym ethane forms, and by separating methanol return tank, through separating methanol reflux pump, a part is back to tower, and a part enters pressurizing tower; Pressurizing tower system mainly comprises conventional rectification device pressurizing tower return tank, pressurizing tower reflux pump, pressurizing tower reboiler and pressurizing tower condenser as the reboiler of eparating methanol tower, pressurization tower top obtain 70 ~ 85% left and right dimethoxym ethane solution by pressurizing tower return tank through pressurizing tower reflux pump, a part is back to tower, and a part enters eparating methanol tower and recycles.Pressurizing tower bottom is sent outside for finished product high-concentration methylal, and eparating methanol tower bottom methyl alcohol and a small amount of heavy constituent are pumped into 17 methanol distillation columns at the bottom of eparating methanol tower.Methanol distillation column unit comprises conventional rectification device methanol distillation column, methanol distillation column condenser, methanol distillation column return tank, methanol distillation column reflux pump, methanol distillation column reboiler, Methanol Recovery column bottoms pump, light component high concentration methanol is through methanol distillation column reflux pump, a part is back to tower, and a part is as product extraction, and at the bottom of tower, heavy constituent is pumped to the external world at the bottom of 22 methanol distillation columns.
In above-mentioned technical process, control lightness-removing column tower top pressure 0.6～1.2MPa (g), eparating methanol tower tower top pressure 0～0.3MPa (g), pressurizing tower tower top pressure 0.8～1.6MPa (g), methanol distillation column tower top pressure is 0～0.3MPa (g).All towers all can adopt high-efficiency packing tower above, for the plate efficiency increasing in pressurization situation can lightness-removing column and pressurizing tower employing plate column.For effective utilization of energy, this device adopts and utilizes pressurizing tower overhead vapours as the thermal source of methanol distillation column.
The present invention is mainly the dimethoxym ethane in purification producing glyphosate by using glycine by-product dimethoxym ethane, improves its economic benefits.Energy by-product high concentration methanol of the present invention, low boiling point solvent monochloro methane, dimethyl ether.Use the dimethoxym ethane of this invention preparation compare market adopt methyl alcohol, formaldehyde for raw material prepare high-concentration methylal cost and energy consumption low.Patent of the present invention has adopted the coupling of differential pressure rectified heat, utilize the heat of pressurizing tower overhead vapours as the reboiler thermal source of eparating methanol tower, greatly saved heat, consumption for steam consumption and recirculated water all 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 producing glyphosate by using glycine accessory substance, it is characterized in that: comprise lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower, the tower top of described lightness-removing column, eparating methanol tower, pressurizing tower and methanol eddy tower is all connected with condenser and return tank in turn by pipeline, and by reflux pump, being communicated with formation backflow with tower top, the bottom of each tower is equipped with reboiler simultaneously; The bottom of described lightness-removing column is provided with discharge nozzle and is connected with eparating methanol tower by discharging pump; The bottom of described eparating methanol tower is also provided with discharge nozzle and is connected with methanol eddy tower feeding mouth by discharging pump, and the reflux pump of tower top outlet is provided with arm, and is connected with pressurizing tower feeding mouth; The bottom of described 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, is characterized in that: the condenser that described pressurizing tower top connects is the reboiler that is located at eparating methanol tower bottom.
3. the dimethoxym ethane process for refining of producing glyphosate by using glycine accessory substance is equipped according to claim 2, it is characterized in that: described eparating methanol tower bottom is provided with two reboilers, wherein take individual reboiler as independent reboiler, and another reboiler thermal source is from pressurizing tower top gas.
4. the dimethoxym ethane refining technique based on the arbitrary described process equipment of claim 1～3, is characterized in that comprising the following steps:
(1) glyphosate accessory substance is sent into after lightness-removing column, carries out rectifying in lightness-removing column, and it is 90～99% dimethyl ether and monochloro methane mixture that tower top outlet gas phase obtains content through supercooling, and wherein a part is back to lightness-removing column, and remainder is as accessory substance output; Wherein, the interior pressure of lightness-removing column is 0.8～1.5MPa, and tower top temperature is 40～55 ℃, and column bottom temperature is 115～130 ℃;
(2) heavy constituent at the bottom of lightness-removing column tower enters after eparating methanol tower, in eparating methanol tower, further rectifying is separated, tower top obtains the azeotropic constituent being comprised of dimethoxym ethane and a small amount of methyl alcohol, and at the bottom of tower, obtains the mixture that main component is methyl alcohol, and delivers to methanol eddy tower and further purify; The pressure of described eparating methanol tower is 0～0.2MPa, and tower top temperature is 40～55 ℃, and column bottom temperature is 70～85 ℃;
(3) the azeotropic constituent at eparating methanol tower top is partly refluxed to eparating methanol tower, and remainder is sent into pressurizing tower and carried out compression rectification, at the bottom of tower, obtains 99～99.9% dimethoxym ethane; In described pressurizing tower, pressure is 0.8～1.5MPa, and in tower, temperature is 120～140 ℃;
(4) at the bottom of eparating methanol tower tower, obtain mixture and send into the further fractionation of methanol eddy tower, from tower, surely obtain 95～99.5% methyl alcohol, as accessory substance output; Described methanol eddy pressure tower is 0～0.2MPa, and tower top temperature is 65～85 ℃, and column bottom temperature is 100～120 ℃.
5. dimethoxym ethane refining technique according to claim 4, is characterized in that: described pressurizing tower overhead streams goes out gas phase after the reboiler with eparating methanol tower tower bottom carries out heat exchange cooling, is partly refluxed to pressurizing tower, and remainder is sent into eparating methanol tower entrance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410425855.9A CN104190104B (en) | 2014-08-27 | 2014-08-27 | A kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410425855.9A CN104190104B (en) | 2014-08-27 | 2014-08-27 | A kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104190104A true CN104190104A (en) | 2014-12-10 |
| CN104190104B CN104190104B (en) | 2017-03-15 |
Family
ID=52075557
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410425855.9A Active CN104190104B (en) | 2014-08-27 | 2014-08-27 | A kind of dimethoxym ethane process for refining device and method of producing glyphosate by using glycine accessory substance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104190104B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113429269A (en) * | 2021-07-29 | 2021-09-24 | 南通江山农药化工股份有限公司 | Pressurized rectification purification process equipment for methylal |
| CN113828001A (en) * | 2021-10-29 | 2021-12-24 | 新疆晶硕新材料有限公司 | A kind of separation system and separation method of methyl chloride |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225030A (en) * | 2007-01-15 | 2008-07-23 | 浙江新安化工集团股份有限公司 | A kind of method of thermal energy utilization in glyphosate continuous synthesis |
| CN101270077A (en) * | 2008-04-18 | 2008-09-24 | 浙江金帆达生化股份有限公司 | Comprehensive process for tail gas in glyphosate production |
| CN102093176A (en) * | 2010-12-23 | 2011-06-15 | 南京师范大学 | Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk |
| EP2450336A1 (en) * | 2010-11-09 | 2012-05-09 | INEOS Paraform GmbH | Process for the production of pure methylal |
| 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 |
-
2014
- 2014-08-27 CN CN201410425855.9A patent/CN104190104B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225030A (en) * | 2007-01-15 | 2008-07-23 | 浙江新安化工集团股份有限公司 | A kind of method of thermal energy utilization in glyphosate continuous synthesis |
| CN101270077A (en) * | 2008-04-18 | 2008-09-24 | 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 |
| CN102093176A (en) * | 2010-12-23 | 2011-06-15 | 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113429269A (en) * | 2021-07-29 | 2021-09-24 | 南通江山农药化工股份有限公司 | Pressurized rectification purification process equipment for methylal |
| CN113828001A (en) * | 2021-10-29 | 2021-12-24 | 新疆晶硕新材料有限公司 | A kind of separation system and separation method of methyl chloride |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104190104B (en) | 2017-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105712955B (en) | A kind of technological process of preparing epoxy chloropropane by epoxidation of propylene chloride | |
| CN104190104A (en) | Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method | |
| CN104098441A (en) | Technology and device system for producing dimethyl oxalate by high-pressure carbonylation of industrial synthesis gases and producing ethylene glycol through dimethyl oxalate hydrogenation | |
| CN107628946A (en) | The method and device of reactive distillation film device coupling production ethyl acetate in high purity | |
| CN103772145B (en) | A kind of separation method of acetone hydrogenation preparing isopropanol | |
| CN106431812A (en) | Method and device for separating methylbenzene-methanol-water azeotrope using extractive distillation | |
| CN105330514A (en) | Purification process for preparation of ethylene glycol from synthesis gas | |
| CN103274913A (en) | Method and device for producing methyl isobutyl ketone | |
| CN104926690A (en) | Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis | |
| CN101830788A (en) | Method for separating azeotropic mixture of ethyl methyl ketone and water through variable-pressure rectification | |
| CN103012332B (en) | Use the method for packing tower distillation separation of tetrahydrofuran-methanol-water solvent slop | |
| CN204275534U (en) | A kind of dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance | |
| CN101798265B (en) | Novel method for preparing vinyl acetate from bioethanol | |
| CN102557898A (en) | Method and device for preparing high-concentration methylal | |
| CN106349107B (en) | A kind of method and device of heterogeneous azeotropic rectification separating acetonitrile-triethylamine mixture | |
| CN103739486A (en) | Production method for ethyl acetate crude product | |
| CN103980115B (en) | A kind of method reclaiming sec-butyl acetate with high yield from the reaction product preparing sec-butyl acetate | |
| CN104761430A (en) | Process of varying-pressure thermal-coupling rectification separation of methylal from methanol | |
| CN108947774A (en) | A kind of method and device of separating isopropanol | |
| CN108299167A (en) | The method and apparatus for detaching polymethoxy dimethyl ether using next door tower | |
| CN108129328A (en) | A kind of preparation method of methyl triethyl ammonium chloride | |
| CN109646977A (en) | A kind of reactive distillation coupled and its preparing the application in formic acid | |
| CN104710285A (en) | Method for recycling ethylene glycol monomethyl ether | |
| CN104163832A (en) | Glyphosate continuous production device and glyphosate continuous production method | |
| CN101912693B (en) | Equipment and method for separating indole and biphenyl from wash oil fraction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
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 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20180411 Granted publication date: 20170315 |
|
| PP01 | Preservation of patent right | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20181011 Granted publication date: 20170315 |
|
| PD01 | Discharge of preservation of patent |