CN104163828A - Mechanical device for producing dimethyl phosphite - Google Patents
Mechanical device for producing dimethyl phosphite Download PDFInfo
- Publication number
- CN104163828A CN104163828A CN201310184203.6A CN201310184203A CN104163828A CN 104163828 A CN104163828 A CN 104163828A CN 201310184203 A CN201310184203 A CN 201310184203A CN 104163828 A CN104163828 A CN 104163828A
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- reaction kettle
- methyl alcohol
- dimethylphosphite
- phosphorus trichloride
- rectifying tower
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Abstract
The invention discloses a mechanical device for producing dimethyl phosphite. The device belongs to the field of fine chemical engineering. The mechanical device comprises a methyl alcohol ejector, a phosphorus trichloride ejector, an esterification reaction kettle, a neutralizing tank, a rectifying tower and a dimethyl phosphite storage tank, and is characterized in that the methyl alcohol ejector is provided with a methyl alcohol inlet; a first pipeline is arranged between the methyl alcohol ejector and the esterification reaction kettle; the phosphorus trichloride ejector is provided with a phosphorus trichloride inlet; a second pipeline is arranged between the phosphorus trichloride ejector and the esterification reaction kettle; the esterification reaction kettle is provided with a gas outlet; a first conveyer is arranged between the esterification reaction kettle and the neutralizing tank; the neutralizing tank is provided with an ammonia inlet; a second conveyer is arranged between the neutralizing tank and the rectifying tower; the rectifying tower is provided with an ammonium chloride outlet; a first slurry pump and a pipeline are arranged between the rectifying tower and the dimethyl phosphite storage tank; the first slurry pump is a steel-lined polytetrafluoroethylene slurry pump; all the pipelines are polytetrafluoroethylene pipelines; and all the conveyers are scrapper conveyers.
Description
Technical field
The invention belongs to field of fine chemical, relate in particular to a kind of mechanism of producing dimethylphosphite.
Background technology
Dimethylphosphite, molecular formula is C2H7O3P, and molecular weight is 110.05, and outward appearance is colourless transparent liquid, slightly fragrance, boiling point is 170 DEG C, relative density is 1.20, water-soluble, is soluble in most organic solvents such as alcohol, ether.Dimethylphosphite preparation method is made by methyl alcohol and phosphorus trichloride direct reaction, concrete mode has: have solvent reaction and solvent-free reaction, concrete grammar has vapour-liquid reaction, the reaction of vapour vapour, interruption method, continuous processing etc., and because this reaction is violent thermopositive reaction, speed of response is fast, moment completes, interruption method frequent operation, labour intensity is large, and the production cycle is long, plant factor is low, and throughput is restricted.The present invention adopts solvent-free continuous steam vapour method to produce dimethylphosphite, total recovery can reach 85-92%, product purity is more than 96%, the key of the method is to make phosphorus trichloride fully contact with methyl alcohol, can application sprayers meet this requirement, it is acid that the dimethylphosphite crude product of gained is, and needs to use ammonia neutralization, and the by-product ammonium chloride of neutralization can be through processing and be used as fertilizer again.The present invention is a kind of mechanism of producing dimethylphosphite, this device is taking methyl alcohol injector, phosphorus trichloride injector, reaction kettle of the esterification, neutralization tank, rectifying tower, dimethylphosphite storage tank as equipment, taking methyl alcohol, phosphorus trichloride, ammonia as raw material, make dimethylphosphite by operations such as esterification, neutralization, rectifying, the major advantage that this device is produced dimethylphosphite is: the equipment of use for general-purpose equipment, the production time is short, product purity is high, yield is high, can be mass.Dimethylphosphite can be directly used in synthetic organic phosphorous insecticide Trichlorphon, omethoate, phosfolan_methyl, herbicide glyphosate on agricultural chemicals, also can be used for synthetic other phosphorous intermediates, in addition, it is also a kind of important organic synthesis raw material, for the production of organophosphorus acid type inhibiter, dye additive and flame retardant for textile; As lubricating oil additive, tackiness agent and some organic synthesis intermediate.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of mechanism of producing dimethylphosphite, this device is taking methyl alcohol injector, phosphorus trichloride injector, reaction kettle of the esterification, neutralization tank, rectifying tower, dimethylphosphite storage tank as equipment, taking methyl alcohol, phosphorus trichloride, ammonia as raw material, make dimethylphosphite by operations such as esterification, neutralization, rectifying.
The technical solution used in the present invention is:
A mechanism of producing dimethylphosphite, comprising: methyl alcohol injector, phosphorus trichloride injector, reaction kettle of the esterification, neutralization tank, rectifying tower, dimethylphosphite storage tank; It is characterized in that: methyl alcohol injector is provided with methyl alcohol import, between methyl alcohol injector and reaction kettle of the esterification, be provided with the first pipeline, phosphorus trichloride injector is provided with phosphorus trichloride import, between phosphorus trichloride injector and reaction kettle of the esterification, be provided with second pipe, reaction kettle of the esterification is provided with pneumatic outlet, between reaction kettle of the esterification and neutralization tank, be provided with the first transfer roller, neutralization tank is provided with ammonia import, between neutralization tank and rectifying tower, be provided with second conveyor, rectifying tower is provided with ammonium chloride outlet, between rectifying tower and dimethylphosphite storage tank, is provided with the first shurry pump and pipeline.
Further technical scheme of the present invention is:
The first described shurry pump is steel lining polytetrafluoro shurry pump.
Described whole pipelines are polytetrafluoro pipeline.
Described whole transfer rollers are scraper conveyor.
The invention has the beneficial effects as follows: a kind of mechanism of producing dimethylphosphite is provided, and the advantage of this device is: the equipment of use is general-purpose equipment, rational in infrastructure, with short production cycle, product purity is high, can be mass; Dimethylphosphite is of many uses, on agricultural chemicals, can be directly used in synthetic organic phosphorous insecticide,, other phosphorous intermediates; Also for the production of organophosphorus acid type inhibiter, additives for plastics, lubricating oil additive, tackiness agent, dye additive and fire retardant.
Brief description of the drawings:
If Fig. 1 is structure iron of the present invention.
Embodiment
Further illustrate the particular content that uses this mechanism to produce dimethylphosphite most preferred embodiment below in conjunction with accompanying drawing:
(1) produce the mechanism of dimethylphosphite, comprising: methyl alcohol injector 1, phosphorus trichloride injector 2, reaction kettle of the esterification 3, neutralization tank 4, rectifying tower 5, dimethylphosphite storage tank 6, it is characterized in that: methyl alcohol injector 1 is provided with methyl alcohol import 7, between methyl alcohol injector 1 and reaction kettle of the esterification 3, be provided with the first pipeline 8, phosphorus trichloride injector is provided with phosphorus trichloride import 6, between phosphorus trichloride injector 2 and reaction kettle of the esterification 3, be provided with second pipe 10, reaction kettle of the esterification 3 is provided with pneumatic outlet 11, between reaction kettle of the esterification 3 and neutralization tank 4, be provided with the first transfer roller 12, neutralization tank 4 is provided with ammonia import 13, between neutralization tank 4 and rectifying tower 5, be provided with second conveyor 14, rectifying tower 5 is provided with ammonium chloride outlet 15, between rectifying tower 5 and dimethylphosphite storage tank 6, be provided with the first shurry pump and pipeline 16, the first described shurry pump is steel lining polytetrafluoro shurry pump, described whole pipelines are polytetrafluoro pipeline, described whole transfer rollers are scraper conveyor.
(2) methyl alcohol is sent into methyl alcohol injector 1 by the methyl alcohol import 7 on methyl alcohol injector 1, phosphorus trichloride is sent into phosphorus trichloride injector 2 by the phosphorus trichloride import 9 on phosphorus trichloride injector 2, the agitator that starts reaction kettle of the esterification 3 stirs, methyl alcohol injector 1 by methyl alcohol by being arranged at the first pipeline 8 between methyl alcohol injector 1 and reaction kettle of the esterification 3, phosphorus trichloride by be arranged at second pipe 10 between phosphorus trichloride injector 2 and reaction kettle of the esterification 3 simultaneously by methyl alcohol and phosphorus trichloride with the vaporific reaction kettle of the esterification 3 that sprays into slowly, the mol ratio of straying quatity is methyl alcohol: phosphorus trichloride=3:1, exothermic heat of reaction, control temperature of reaction in reaction kettle of the esterification 3 between 48-52 DEG C by controlling the straying quatity of methyl alcohol, the solid that reaction finishes to obtain in rear reaction kettle of the esterification 3 is dimethylphosphite crude product, gas is byproduct hydrogen chloride, methyl chloride, byproduct hydrogen chloride, methyl chloride uses it for anything else by the outlet 11 discharge collections that are arranged on reaction kettle of the esterification 3, solid phosphorous acid dimethyl ester crude product is sent into neutralization tank 4 by the first transfer roller 12 being arranged between reaction kettle of the esterification 3 and neutralization tank 4.
3. add appropriate ammonia to neutralize dimethylphosphite crude product by the ammonia import 13 being arranged on neutralization tank 4, for avoiding reaction violent, the speed that adds of ammonia is wanted slowly, when in tune neutralization tank, the pH value of material is for 6.5-7.5, stop, the interior material of neutralization tank 4 is the mixture of dimethylphosphite and ammonium chloride.
4. material in neutralization tank is sent into rectifying tower 5 rectifying by the second conveyor 14 being arranged between neutralization tank 4 and rectifying tower 5, in the time that temperature is 170-175 DEG C, dimethylphosphite all distillates, dimethylphosphite gets product after it is cooling, ammonium chloride is successfully separated to be improved the outlet that is arranged on rectifying tower 5 and discharges, and dimethylphosphite becomes after liquid by being arranged at and between rectifying tower 5 and dimethylphosphite storage tank 6, is provided with the first shurry pump and pipeline 16 and sends into dimethylphosphite storage tank 6 and store.
Claims (4)
1. a mechanism of producing dimethylphosphite, comprising: methyl alcohol injector (1), phosphorus trichloride injector (2), reaction kettle of the esterification (3), neutralization tank (4), rectifying tower (5), dimethylphosphite storage tank (6), it is characterized in that: methyl alcohol injector (1) is provided with methyl alcohol import (7), between methyl alcohol injector (1) and reaction kettle of the esterification (3), be provided with the first pipeline (8), phosphorus trichloride injector is provided with phosphorus trichloride import (6), between phosphorus trichloride injector (2) and reaction kettle of the esterification (3), be provided with second pipe (10), reaction kettle of the esterification (3) is provided with pneumatic outlet (11), between reaction kettle of the esterification (3) and neutralization tank (4), be provided with the first transfer roller (12), neutralization tank (4) is provided with ammonia import (13), between neutralization tank (4) and rectifying tower (5), be provided with second conveyor (14), rectifying tower (5) is provided with ammonium chloride outlet (15), between rectifying tower () 5 and dimethylphosphite storage tank (6), be provided with the first shurry pump and pipeline (16).
2. a kind of mechanism of producing dimethylphosphite as claimed in claim 1, is characterized in that: the first described shurry pump is steel lining polytetrafluoro shurry pump.
3. a kind of mechanism of producing dimethylphosphite as claimed in claim 1, is characterized in that: described whole pipelines are polytetrafluoro pipeline.
4. a kind of mechanism of producing dimethylphosphite as claimed in claim 1, is characterized in that: described whole transfer rollers are scraper conveyor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310184203.6A CN104163828A (en) | 2013-05-19 | 2013-05-19 | Mechanical device for producing dimethyl phosphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310184203.6A CN104163828A (en) | 2013-05-19 | 2013-05-19 | Mechanical device for producing dimethyl phosphite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104163828A true CN104163828A (en) | 2014-11-26 |
Family
ID=51907829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310184203.6A Pending CN104163828A (en) | 2013-05-19 | 2013-05-19 | Mechanical device for producing dimethyl phosphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104163828A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107722053A (en) * | 2017-10-20 | 2018-02-23 | 河南红东方化工股份有限公司 | A kind of rectificating method of dimethylphosphite |
-
2013
- 2013-05-19 CN CN201310184203.6A patent/CN104163828A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107722053A (en) * | 2017-10-20 | 2018-02-23 | 河南红东方化工股份有限公司 | A kind of rectificating method of dimethylphosphite |
| CN107722053B (en) * | 2017-10-20 | 2020-02-21 | 河南红东方化工股份有限公司 | Rectification method of dimethyl phosphite |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141126 |