CN107722053A - A kind of rectificating method of dimethylphosphite - Google Patents
A kind of rectificating method of dimethylphosphite Download PDFInfo
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- CN107722053A CN107722053A CN201710981883.2A CN201710981883A CN107722053A CN 107722053 A CN107722053 A CN 107722053A CN 201710981883 A CN201710981883 A CN 201710981883A CN 107722053 A CN107722053 A CN 107722053A
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- Prior art keywords
- dimethylphosphite
- rectifying
- column
- distillation column
- rectifying column
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- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004821 distillation Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000009835 boiling Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 9
- 230000032050 esterification Effects 0.000 claims abstract description 8
- 238000005886 esterification reaction Methods 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 8
- 150000002148 esters Chemical class 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 8
- 239000000498 cooling water Substances 0.000 description 6
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000005562 Glyphosate Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 2
- 229940097068 glyphosate Drugs 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004836 Glue Stick Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- DLQDGVZAEYZNTG-UHFFFAOYSA-N dimethyl hydrogen phosphite Chemical compound COP(O)OC DLQDGVZAEYZNTG-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CWXVDJFKMQCYFG-UHFFFAOYSA-N n-dimethoxyphosphoryl-1,3-dithiolan-2-imine Chemical group COP(=O)(OC)N=C1SCCS1 CWXVDJFKMQCYFG-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006561 solvent free reaction Methods 0.000 description 1
- 239000006273 synthetic pesticide Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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 Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
- C07F9/142—Esters of phosphorous acids with hydroxyalkyl compounds without further substituents on alkyl
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of rectificating method of dimethylphosphite, comprise the following steps：Thick ester enters rectifying still to raw material after abundant reaction in reaction kettle of the esterification, and first rectifying column and Second distillation column, continuation heating first rectifying column and Second distillation column are set at the top of rectifying still；First rectifying column first collects the low-boiling-point substance in material in low-boiling-point substance storage tank, and bottom of towe discharge liquor is entered Second distillation column and further separated；Vacuum pump set is opened, is concentrated under reduced pressure, the dimethylphosphite of high-purity is collected in product storage tank, tower bottoms is high-boiling components.Present invention process flow is simple, the production time is short, product purity height, high income, can be low with continuous production, cost, fuel availability is high, substantially without discharge, environmental pollution is small, operation is safe, labor intensity is low, efficiency is high, good product quality, beneficial to industrialization.
Description
Technical field
The invention belongs to the synthetically prepared field of medicine intermediate, and in particular to a kind of rectifying side of dimethylphosphite
Method.
Background technology
Dimethylphosphite, molecular formula C2H7O3P, molecular weight 110.05, outward appearance are colourless transparent liquid, slightly fragrance, boiling
Point is 170 DEG C, and relative density 1.20 is dissolved in water, is soluble in most organic solvents such as alcohol, ether.It is commonly used for lube oil additive, glue
Stick and some organic synthesis intermediates.For synthetic pesticide flolimat, phosfolan_methyl and herbicide glyphosate etc..With
It is quite varied on the way.Production scale with domestic alkyl esterification method glyphosate constantly expands, anxious to the demand of dimethylphosphite
Increase severely and add.The process for purification of traditional batch fractionating is faced with severe tests.
The synthesis of dimethylphosphite has less document, industrially most of directly to react system with methanol and phosphorus trichloride
, while accessory substance is hydrogen chloride and chloromethanes.Production process includes esterification deacidification, the work such as product purification and tail gas absorption recovery
Sequence.The thick ester of gained is in addition to containing low-boiling-point substances such as methanol after esterification deacidification, also containing high-boiling components such as the methyl esters of accessory substance phosphorous acid one,
Need to further it refine.Concrete mode has：Have a solvent reaction and solvent-free reaction, specific method have vapour-liquid reaction, the reaction of vapour vapour,
Disconnected method, continuity method etc., because the reaction is violent exothermic reaction, reaction speed is fast, and moment completes, step-wise process frequent operation,
Labor intensity is big, and the production cycle is grown, and utilization rate of equipment and installations is low, and production capacity is restricted.Because reactant composition is complicated, and it is mixed
The boiling point of compound is high, and corrosivity is strong, and separating difficulty is big, and high energy consumption, disposal ability is low, and equipment is numerous and jumbled, it is difficult to adapt to large-scale
Industrialized production.
These are unfavorable for industrialized production and improve product quality, it is necessary to develop that a kind of technological process is simple, the production time
It is short, product purity height, high income, can be low with continuous production, cost, fuel availability is high, substantially without discharge, environmental pollution it is small,
Operation is safe, and labor intensity is low, efficiency is high, the rectificating method of good product quality.
The content of the invention
It is an object of the invention to provide a kind of rectificating method of dimethylphosphite.
Based on above-mentioned purpose, this invention takes following technical scheme：
A kind of rectificating method of dimethylphosphite, comprises the following steps：（a）Raw material fully reacts in reaction kettle of the esterification；（b）
At the top of rectifying still, first rectifying column and Second distillation column are set；（c）Continuation heats first rectifying column and Second distillation column；
（d）Material rectifying；（e）First rectifying column first collects the low-boiling-point substance in material in low-boiling-point substance storage tank, and bottom of towe discharge liquor is entered
Second distillation column further separates；（f）Vacuum pump set is opened, is concentrated under reduced pressure, the dimethylphosphite of high-purity is collected into production
In product storage tank, tower bottoms is high-boiling components.Present invention process flow is simple, the production time is short, product purity height, high income, can
It is low with continuous production, cost, fuel availability is high, substantially without discharge, environmental pollution is small, operation is safe, work is strong
Spend that low, efficiency is high, good product quality, beneficial to industrialization.
A kind of rectificating method of above-mentioned dimethylphosphite, the top of rectifying still set first rectifying column and the second rectifying
Tower, the filler in first rectifying column are glass filler, and tower height is 4~6m, and the filler in Second distillation column is regular ceramics, tower
A height of 8~10m.
A kind of rectificating method of above-mentioned dimethylphosphite, the king-post internal diameter of first rectifying column are 45cm, the second rectifying
The king-post internal diameter of tower is 50cm.
A kind of rectificating method of above-mentioned dimethylphosphite, the charging of the discharging opening and Second distillation column of first rectifying column
Mouth connection, bottom are designed with groove, ensure that material stops 8~10min in groove.
A kind of rectificating method of above-mentioned dimethylphosphite, first rectifying column and Second distillation column rectifying tubular body are set
Temperature control equipment, and reflux ratio adjuster are equipped with, is arranged near discharging opening, can be realized by adjusting different temperature
Adjust split ratio.
Above-mentioned reflux ratio adjuster, the reflux ratio of first rectifying column is 40~50：60~70, the backflow of Second distillation column
Than for 10~20：90~100.
The rectificating method of above-mentioned a kind of dimethylphosphite, using a water circulation vavuum pump and two Roots vacuums
Pump, carry out being composed in series a set of vacuum pump set, not only substantially increase vacuum, and slow down corrosion of the material to equipment.
Present invention saves production cost, daily cost-saved 22373.04 yuan of expense；The rectifying of dimethylphosphite
Yield improves 8 ﹪, and content improves 5 ﹪, obtains the ﹪ of content 99 product；The residual quantity of high-boiling components phosphorous acid dimethyl ester by
8 ﹪ originally or so, drop to 2~3 ﹪.
The present invention uses vacuum continuous rectification, significantly reduces the tower reactor of de- low boiling distillation and de- height boiling rectifying column
Temperature, reduce energy expenditure, almost without the discharge of waste water and gas, environmental pollution is small, and equipment investment is low, convenient operation, production
Product purity is high, steady quality, and working environment is friendly, and efficiency is high, and device realizes zero-emission, met green without evaporating, emitting, dripping or leaking of liquid or gas
The requirement of color clean manufacturing, beneficial to industrialization continuous production.
Embodiment
Technical scheme is described in further detail below by way of specific embodiment, but the protection model of the present invention
Enclose and be not limited thereto.
Embodiment 1
A kind of rectificating method of dimethylphosphite,
Comprise the following steps that：
By volume 1:0.9 ratio adds methanol 1800L and phosphorus trichloride 1620 with 71L/min and 50L/min flow velocity respectively
Enter reaction kettle of the esterification, open stirring, slowly heating, it is anti-to raw material by sample tap, sampling TLC detections after reacting a period of time
Should be complete, reaction obtains dimethylphosphite crude product after terminating.
Completely reacted thick ester is put into rectifying is carried out in rectifying still.（First rectifying column tower height 4m, Second distillation column 8m）
Stirring is opened, slowly heating, when first rectifying column and Second distillation column reach design temperature, open the condensation of first rectifying column top
The cooling water of gas, while the cooling circulating hot water of Second distillation column top condenser is opened, start vacuum system, open the first essence
The reflux ratio adjuster of tower is evaporated, regulation reflux ratio is 50：60 regulations, carry out de- low boiling rectifying in first rectifying column first.Tower top
The condensed cooler of low-boiling-point substance steam of outflow is condensed into liquid, and a part returns to first rectifying column, another part as backflow
Enter low-boiling-point substance storage tank as product is distillated.After reaction 2 hours, the cooling water when first rectifying column overhead condensation gas is closed, it is open-minded
The cooling water of Second distillation column top condensing gas, opens the reflux ratio adjuster of Second distillation column, and regulation reflux ratio is 20：90, enter
Enter the de- further rectifying of height boiling rectifying column.The condensed device of high-purity dimethylphosphite steam of tower top outflow is condensed into liquid,
A part returns to rectifying still as backflow, and another part enters dimethylphosphite finished pot as product.Control rectifying still man set
Interior steam pressure≤0.05Mpa, 146 DEG C of distillation end point temperature, distillation vacuum are steamed to tower top aneroid in 0.097 more than Mpa
Body flows out, and terminates distillation.The ﹪ of content 99.3 of sampling analysis dimethylphosphite, the ﹪ of yield 97.6, vinasse phosphorous acid
The ﹪ of content 2.4 of dimethyl ester.
Embodiment 2
A kind of rectificating method of dimethylphosphite,
Comprise the following steps that：
By volume 1:0.9 ratio is by methanol 1800L and phosphorus trichloride 1620L phosphorus trichlorides respectively with 71L/min and 50L/min
Flow velocity add reaction kettle of the esterification, open stirring, slowly heating, after reacting a period of time, by sample tap, sampling TLC detections,
Complete to raw material reaction, reaction obtains dimethylphosphite crude product after terminating.
Completely reacted thick ester is put into rectifying is carried out in rectifying still.（First rectifying column tower height 5m, Second distillation column 9m）
Stirring is opened, slowly heating, when first rectifying column and Second distillation column reach design temperature, open the condensation of first rectifying column top
The cooling water of gas, while the cooling circulating hot water of Second distillation column top condenser is opened, start vacuum system, open the first essence
The reflux ratio adjuster of tower is evaporated, regulation reflux ratio is 45：65 regulations, carry out de- low boiling rectifying in first rectifying column first.Tower top
The condensed cooler of low-boiling-point substance steam of outflow is condensed into liquid, and a part returns to first rectifying column, another part as backflow
Enter low-boiling-point substance storage tank as product is distillated.After reaction 2 hours, the cooling water when first rectifying column overhead condensation gas is closed, it is open-minded
The cooling water of Second distillation column top condensing gas, opens the reflux ratio adjuster of Second distillation column, and regulation reflux ratio is 15：95, enter
Enter the de- further rectifying of height boiling rectifying column.The condensed device of high-purity dimethylphosphite steam of tower top outflow is condensed into liquid,
A part returns to rectifying still as backflow, and another part enters dimethylphosphite finished pot as product.Control rectifying still man set
Interior steam pressure≤0.05Mpa, 146 DEG C of distillation end point temperature, distillation vacuum are steamed to tower top aneroid in 0.097 more than Mpa
Body flows out, and terminates distillation.The ﹪ of content 99.5 of sampling analysis dimethylphosphite, the ﹪ of yield 98.4, vinasse phosphorous acid
The ﹪ of content 2.2 of dimethyl ester.
Claims (9)
1. a kind of rectificating method of dimethylphosphite, it is characterised in that comprise the following steps：Raw material fills in reaction kettle of the esterification
Thick ester enters rectifying still after point reaction, sets first rectifying column and Second distillation column at the top of rectifying still, and continuation heats the
One rectifying column and Second distillation column；First rectifying column first collects the low-boiling-point substance in material in low-boiling-point substance storage tank, bottom of towe row
Go out liquid and enter Second distillation column and further separate；Vacuum pump set is opened, is concentrated under reduced pressure, the dimethylphosphite of high-purity is collected
In product storage tank, tower bottoms is high-boiling components.
2. the rectificating method of a kind of dimethylphosphite according to claim 1, it is characterised in that in first rectifying column
Filler is glass filler, and tower height is 4~6m, and the filler in Second distillation column is regular ceramics, and tower height is 8~10m.
A kind of 3. rectificating method of dimethylphosphite according to claim 1, it is characterised in that the tower of first rectifying column
Column internal diameter is 45cm, and the king-post internal diameter of Second distillation column is 50cm.
4. the rectificating method of a kind of dimethylphosphite according to claim 1, it is characterised in that first rectifying column goes out
Material mouth connects with the charging aperture of Second distillation column, and bottom is designed with groove, ensures that material stops 8~10min in groove.
5. the rectificating method of a kind of dimethylphosphite according to claim 1, it is characterised in that first rectifying column and
Two rectifying column rectifying tubular bodies are provided with temperature control equipment, and reflux ratio adjuster, are arranged near discharging opening, can be with
Regulation split ratio is realized by adjusting different temperature.
6. reflux ratio adjuster according to claim 3, it is characterised in that the reflux ratio of first rectifying column is 40~50：60
~70, the reflux ratio of Second distillation column is 10~20：90~100.
7. the rectificating method of a kind of dimethylphosphite according to claim 1, it is characterised in that using a water circulation
Vavuum pump and two Roots vaccum pumps, carry out being composed in series a set of vacuum pump set, not only increase vacuum, and slow down material
Corrosion to equipment.
8. the rectificating method of a kind of dimethylphosphite according to claim 1, it is characterised in that dimethylphosphite
Rectification yield improves 8 ﹪, and content improves 5 ﹪, obtains the ﹪ of content 99 product.
A kind of 9. rectificating method of dimethylphosphite according to claim 1, it is characterised in that high-boiling components phosphorous acid
The residual quantity of dimethyl ester drops to 2~3 ﹪ by 8 original ﹪ or so.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710981883.2A CN107722053B (en) | 2017-10-20 | 2017-10-20 | Rectification method of dimethyl phosphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710981883.2A CN107722053B (en) | 2017-10-20 | 2017-10-20 | Rectification method of dimethyl phosphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107722053A true CN107722053A (en) | 2018-02-23 |
| CN107722053B CN107722053B (en) | 2020-02-21 |
Family
ID=61212279
Family Applications (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256311A (en) * | 2019-05-24 | 2019-09-20 | 潍坊加华化工有限公司 | A kind of methyl thioglycolate process for refining |
| CN111978348A (en) * | 2020-07-09 | 2020-11-24 | 洪湖市一泰科技有限公司 | Method for comprehensively utilizing methyl phosphinic acid diethyl ester rectification kettle residue |
| CN112791680A (en) * | 2020-12-24 | 2021-05-14 | 华阳新材料科技集团有限公司 | A nickel phosphorus complex synthesis system for adiponitrile production |
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|---|---|---|---|---|
| US5344951A (en) * | 1993-03-16 | 1994-09-06 | Ethyl Petroleum Additives, Inc. | Production of alkyl phosphites |
| CN202924944U (en) * | 2012-10-12 | 2013-05-08 | 徐州江海源精细化工有限公司 | Novel device for producing dimethyl phosphite |
| CN104163828A (en) * | 2013-05-19 | 2014-11-26 | 新沂市汉菱生物工程有限公司 | Mechanical device for producing dimethyl phosphite |
| CN105713037A (en) * | 2016-03-19 | 2016-06-29 | 安徽东至广信农化有限公司 | Production technology of dimethyl phosphite |
| CN105753898A (en) * | 2016-03-19 | 2016-07-13 | 安徽东至广信农化有限公司 | Rectification method of dimethyl phosphite |
| CN107163077A (en) * | 2017-06-27 | 2017-09-15 | 徐州江海源精细化工有限公司 | A kind of dimethylphosphite method of purification |
-
2017
- 2017-10-20 CN CN201710981883.2A patent/CN107722053B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5344951A (en) * | 1993-03-16 | 1994-09-06 | Ethyl Petroleum Additives, Inc. | Production of alkyl phosphites |
| CN202924944U (en) * | 2012-10-12 | 2013-05-08 | 徐州江海源精细化工有限公司 | Novel device for producing dimethyl phosphite |
| CN104163828A (en) * | 2013-05-19 | 2014-11-26 | 新沂市汉菱生物工程有限公司 | Mechanical device for producing dimethyl phosphite |
| CN105713037A (en) * | 2016-03-19 | 2016-06-29 | 安徽东至广信农化有限公司 | Production technology of dimethyl phosphite |
| CN105753898A (en) * | 2016-03-19 | 2016-07-13 | 安徽东至广信农化有限公司 | Rectification method of dimethyl phosphite |
| CN107163077A (en) * | 2017-06-27 | 2017-09-15 | 徐州江海源精细化工有限公司 | A kind of dimethylphosphite method of purification |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256311A (en) * | 2019-05-24 | 2019-09-20 | 潍坊加华化工有限公司 | A kind of methyl thioglycolate process for refining |
| CN111978348A (en) * | 2020-07-09 | 2020-11-24 | 洪湖市一泰科技有限公司 | Method for comprehensively utilizing methyl phosphinic acid diethyl ester rectification kettle residue |
| CN112791680A (en) * | 2020-12-24 | 2021-05-14 | 华阳新材料科技集团有限公司 | A nickel phosphorus complex synthesis system for adiponitrile production |
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| CN107722053B (en) | 2020-02-21 |
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