CN204737902U - Formalin is process units of sweet phosphine raw materials of production of material glycine method grass - Google Patents
Formalin is process units of sweet phosphine raw materials of production of material glycine method grass Download PDFInfo
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- CN204737902U CN204737902U CN201520364749.4U CN201520364749U CN204737902U CN 204737902 U CN204737902 U CN 204737902U CN 201520364749 U CN201520364749 U CN 201520364749U CN 204737902 U CN204737902 U CN 204737902U
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Abstract
The utility model discloses a formalin is process units of sweet phosphine raw materials of production of material glycine method grass, including formaldehyde deacidification device, pre -heater, reaction unit, dehydration column and reaction rectifying column, formaldehyde deacidification device is equipped with the formalin entry to be connected with pre -heater and reaction unit in proper order, reaction unit is equipped with the auxiliary agent entry, and pipeline and dehydration column entry linkage are passed through to the top, the top of dehydration column is equipped with the export of rare formaldehyde, and the bottom is passed through the pipeline and is connected with the reaction rectifying column. The utility model discloses and the depolymerization of having overcome paraformaldehyde is chronic, and equipment area is big, the high scheduling problem of material cost, for general formalin, have higher yield, and the waste water treatment volume is little, energy consumption is low.
Description
Technical field
The utility model belongs to derived energy chemical technical field, particularly relates to production equipment and the processing method of glyphosate.
Background technology
Glyphosate, chemical name is N-((phosphonomethyl)) glycine, is current widely used a kind of weedicide.Since eighties of last century 70 mid-nineties 90 commercialization, due to the herbicidal performance of its brilliance, range of application constantly expands.
The method bibliographical information of synthesizing glyphosate has multiple, as iminodiacetic acid (salt) acid system, phosphonous acid dialkyl group ester process, chloromethyl phosphonic acid method, phosphorous test etc., but really realizes industrialized method mainly iminodiacetic acid (salt) acid system and dialkyl phosphite method at present.
Glycine method adopts paraformaldehyde as raw material, but paraformaldehyde itself is without chemically reactive, mainly utilize paraformaldehyde depolymerization city monomer formaldehyde could be used for reaction, with paraformaldehyde do raw material mainly paraformaldehyde be pressed powder, be convenient to storage and transport, do not adopt formaldehyde solution too high as moisture content in raw material mainly formaldehyde solution, unfavorable to reaction, and wastewater treatment capacity in system can be caused to increase, and energy expenditure is high.
Therefore be prepared by raw material with paraformaldehyde, mainly there is following problem: 1) the formaldehyde depolymerization time is long, the depolymerization of paraformaldehyde needs 2 ~ 3 days aborning; 2) due to the needs of formaldehyde depolymerization, the mode that formaldehyde depolymerization adopts multi-stage stirred tank to connect usually, floor space is large, and facility investment is large, and power consumption is large; 3) paraformaldehyde is raw material, and the price of paraformaldehyde is high relative to formaldehyde solution, and raw materials cost is high.
Summary of the invention
Goal of the invention: for above-mentioned existing Problems existing and deficiency, the purpose of this utility model is to provide the process unit that a kind of formaldehyde solution is raw material production glyphosate by using glycine raw material, formaldehyde solution with more cheap 37 ~ 50% is basic raw material, and the depolymerization time overcoming paraformaldehyde is long, the problems such as occupation area of equipment is large, raw materials cost is high; Relative to general formaldehyde solution, have higher yield, and wastewater treatment capacity is little, ability consumes low.
Technical scheme: in order to solve the problems of the technologies described above, the utility model is by the following technical solutions: a kind of formaldehyde solution is the process unit of the production glyphosate by using glycine raw material of raw material, comprise formaldehyde deacidifying device, preheater, reaction unit, dehydration tower and reactive distillation column, described formaldehyde deacidifying device is provided with formaldehyde solution entrance, and be connected with preheater and reaction unit successively, described reaction unit is provided with auxiliary entrance, and top is connected with dehydration tower entrance by pipeline; The top of described dehydration tower is provided with the outlet of rare formaldehyde, and bottom is connected with reactive distillation column by pipeline.
Further improvement, described reactive distillation column comprises the stripping section of bottom and the absorber portion on top, and absorber portion is also provided with methyl alcohol spray inlet.
As preferably, described reaction unit is the storage tank that stirs of band or tower.
Beneficial effect: compared with prior art, the utility model to overcome depolymerization time of paraformaldehyde long, the problems such as occupation area of equipment is large, raw materials cost is high; Relative to general formaldehyde solution, have higher yield, and wastewater treatment capacity is little, energy expenditure is low.
Accompanying drawing explanation
Fig. 1 is the production technique apparatus structure schematic diagram of glyphosate by using glycine raw material described in the utility model.
Wherein, deacidifying device 1, preheater 2, reaction unit 3, dehydration tower 4, reactive distillation column 5.
Embodiment
Below in conjunction with the drawings and specific embodiments, illustrate the utility model further, these embodiments should be understood and be only not used in restriction scope of the present utility model for illustration of the utility model, after having read the utility model, the amendment of those skilled in the art to the various equivalent form of value of the present utility model has all fallen within the application's claims limited range.
The device of the processing method of producing glyphosate by using glycine described in the utility model, comprise formaldehyde deacidifying device, preheater, reaction unit, dehydration tower and reactive distillation column, described formaldehyde deacidifying device is provided with formaldehyde solution entrance, and be connected with preheater and reaction unit successively, described reaction unit is provided with auxiliary entrance, and top is connected with dehydration tower entrance by pipeline; The top of described dehydration tower is provided with the outlet of rare formaldehyde, and bottom is connected with reactive distillation column by pipeline.Concrete technology method is as follows:
37 ~ 50% formaldehyde solutions market bought or produces, carry out depickling process through the fixed-bed reactor of filling sorbent material, after depickling process, solution acid content is 1 ~ 10ppm; Sorbent material is mainly silica gel or macropore weak basic anion exchange resin etc., controls reaction velocity 1 ~ 5h
-1, enter the speed of deacidifying device according to 0.001 ~ 0.2m/s.Concrete structure is fixed-bed reactor, filling gel or macropore weak basic anion exchange resin etc. in reactor, and weighting agent adopts water cap as grid, in case stopping leak dew.
Formaldehyde solution after depickling process is by after being preheating to 60 ~ 100 DEG C, enter reaction unit and auxiliary etc. again and carry out abundant hybrid reaction, reacted component due to density ratio water little, after leaving standstill, reaction unit upper strata light liquid is through Liquid transfer to dehydration tower, and due to the thermolysis effect of reaction product, dehydration tower controls vacuum operating, moisture is deviate from by dewatering unit top, is sent in reactive distillation column bottom dewatering unit by liquid organic phase e Foerderanlage.Reaction unit can be the storage tank of the band whipping appts of plural serial stage, also can be tower, and tower must ensure that top is with relatively large liquid phase separation space.For preventing carrying oxymethylene polymerization blocking secretly in dehydration overhead water, be rectifying bottom dehydration tower, top is for absorbing; Water is that light constituent directly enters absorber portion by rectifying section top, and absorber portion can adopt the rare formaldehyde solution bottom reaction unit.Auxiliary can be the monohydroxy-alcohol of 8 to 11 for carbonatoms, dibasic alcohol, (auxiliary of 8 to 11 carbon atoms can be polymerized with formaldehyde and obtains transient intermediate phenols, be insoluble in water, and there is depolymerization reduction at about 160 DEG C, carbonatoms is too high makes the too high balance affecting depolymerization reaction of de-polymerization temperature), it can be preferably diisopropyl ether, dimethyl formamide, ethylene glycol, isopropylcarbinol, one or more mixture in 4-methyl-2-amylalcohol or hexalin, wherein especially with diisopropyl ether and ethylene glycol, thus make the depolymerization time at 140 ~ 200 degrees Celsius, depolymerization is more thorough, yield is higher.Alkylphenol is may also be through overtesting.
Reaction unit is mainly reactive distillation column, the region residence time long Reaction Separation being beneficial to formaldehyde and auxiliary system of major control tower reactor section 140 ~ 200 DEG C, thus formaldehyde can depart from by reaction system, and the transformation efficiency that formaldehyde departs from is high, because the formaldehyde gas detached 100 ~ 120 DEG C time is easily polymerized in tower, therefore adopt methanol eddy to absorb formaldehyde, thus top obtains the methanol solution of formaldehyde, as the raw material of glyphosate by using glycine, thus the depolymehzation process of paraformaldehyde can be avoided.Then with the methanol solution of formaldehyde and glycine for raw material, and prepare the methanol solvate of reaction two, under triethylamine is catalytic condition, be obtained by reacting the triethylamine salt of hydroxymethylglycinate; Obtain the triethylamine salt of glyphosphonic acid dialkyl again with dialkyl phosphite through condensation reaction, eventually pass hydrochloric acid hydrolysis and obtain glyphosate.The technique of follow-up preparing glyphosate by glycin method is prior art.
Above production method mainly includes deacidifying device, reaction unit, dewatering unit, reactive distillation column.In major control index charging formaldehyde, acid content can not more than 1000ppm, reaction controlling temperature of reaction 80 ~ 100 DEG C, reaction time 1 ~ 5h, dehydration tower red-tape operati pressure 20 ~ 100KPa (A), service temperature controls 60 ~ 100 DEG C, raw material tower controls pressure-fired, and tower top service temperature controls 40 ~ 80 DEG C.
Claims (3)
1. one kind take formaldehyde solution as the process unit of raw material production glyphosate by using glycine raw material, it is characterized in that: comprise formaldehyde deacidifying device, preheater, reaction unit, dehydration tower and reactive distillation column, described formaldehyde deacidifying device is provided with formaldehyde solution entrance, and be connected with preheater and reaction unit successively, described reaction unit is provided with auxiliary entrance, and top is connected with dehydration tower entrance by pipeline; The top of described dehydration tower is provided with the outlet of rare formaldehyde, and bottom is connected with reactive distillation column by pipeline.
2. process unit according to claim 1, is characterized in that: described reactive distillation column comprises the stripping section of bottom and the absorber portion on top, and absorber portion is also provided with methyl alcohol spray inlet.
3. process unit according to claim 1, is characterized in that: described reaction unit is the storage tank that stirs of band or tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520364749.4U CN204737902U (en) | 2015-06-01 | 2015-06-01 | Formalin is process units of sweet phosphine raw materials of production of material glycine method grass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201520364749.4U CN204737902U (en) | 2015-06-01 | 2015-06-01 | Formalin is process units of sweet phosphine raw materials of production of material glycine method grass |
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| CN204737902U true CN204737902U (en) | 2015-11-04 |
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| CN201520364749.4U Active CN204737902U (en) | 2015-06-01 | 2015-06-01 | Formalin is process units of sweet phosphine raw materials of production of material glycine method grass |
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