CN208747971U - A kind of alkyl esterification method production glyphosate solvent recovering system based on B-grade condensation - Google Patents
A kind of alkyl esterification method production glyphosate solvent recovering system based on B-grade condensation Download PDFInfo
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- CN208747971U CN208747971U CN201820570684.2U CN201820570684U CN208747971U CN 208747971 U CN208747971 U CN 208747971U CN 201820570684 U CN201820570684 U CN 201820570684U CN 208747971 U CN208747971 U CN 208747971U
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Abstract
The utility model relates to the alkyl esterification methods based on B-grade condensation to produce glyphosate solvent recovering system, and tail gas condenser one is connect with tail gas condenser two, and tail gas condenser two is connect with methanol dimethoxym ethane solution pans；Tail gas condenser one is connect with aqueous solution collecting tank, and aqueous solution collecting tank is connect with level-one rectifying column, and level-one rectifier bottoms are connected to sewage plant；Return tank one is connect with methanol dimethoxym ethane solution pans；Two-stage rectification tower is connected to first dimethoxym ethane finished pot through return tank two, and two-stage rectification tower bottom is connected to methanol finished pot.Its recovery process is the dilute methanol in dilute methanol solution collecting tank, goes to level-one rectifying column, and level-one rectifying column gas returns to return tank through condenser condensation, is sent to methanol dimethoxym ethane solution pans；It is pumped into two-stage rectification tower, the extraction of two-stage rectification tower is pumped toward dimethoxym ethane finished pot, and bottom liquid goes to methanol finished pot after condenser condenses.2.0t is reduced compared to liquid phase recovery process ton glyphosate steam consumption, safety and energy-saving benefit are significant.
Description
Technical field
The invention belongs to the solvent recovery technical fields of alkyl esterification method production glyphosate, and in particular to one kind is cold based on second level
Solidifying alkyl esterification method produces glyphosate solvent recovering system.
Background technique
Glyphosate is a kind of efficient, low toxicity, wide spectrum, natural disposition of going out, nonselective herbicide, has excellent biological nature.
Country's glyphosate mainstream production technology has two lines at present: alkyl esterification method and iminodiacetic acid (salt) acid system.External production technology
It is then mainly the iminodiacetic acid (salt) acid system of Monsanto Chemicals, the prevailing technology that China produces glyphosate is alkyl esterification method.Alkane
Base ester method and predominantly glycine-dialkyl phosphite method separately have the chloroethene that glyphosate is produced using monoxone as starting material
Acid-alkyl esterification method and glycine-Trimethyl phosphite method etc. minority's route.
Glyphosate solvent recovery process brief introduction
It is that water, dimethoxym ethane, methanol, hydrogen chloride and chloromethanes are mixed that alkyl esterification method glyphosate synthesis solution, which hydrolyzes tail gas main component,
Object is closed, the removal process of the tail gas is referred to as solvent recovery in glyphosate industry.
The Synthesis liquid refers to by methanol, paraformaldehyde (or other formaldehyde sources), glycine (or using monoxone as starting point
Other raw materials of raw material), the raw material such as dimethylphosphite (or other alkyl phosphates) obtain through depolymerization, condensation, esterification
The main component arrived is the mixed solution of the organic phosphorus intermediates (glyphosate precursor) such as N- methoxyalkyl ester methyl glycine.
Solvent recovery tradition recycles there are two types of routes:
1, first is that liquid phase recycles route, it may be assumed that main component is water, dimethoxym ethane, methanol, hydrogen chloride and chloromethanes glyphosate water
Solution tail gas is condensed through Multistage graphite condenser, and fixed gas goes to the recycling of chloromethanes device, water, dimethoxym ethane, methanol, chlorine in tail gas
Change hydrogen and obtains acid dilute methanol through condensation liquefaction, it is neutralized except neutral dilute methanol is obtained after de-chlorine hydride, for by dimethoxym ethane
(A)-methanol (B)-water (C) composition ternary mixes liquid mixed system.Wherein the volatility of A, B, C successively reduce, three components
It is separated using two-stage tower, specially successively isolates A, B from tower top according to the sequence of component relative volatility size, had
Body process are as follows: first order column overhead distillates component A, and tower bottom mixed liquor is B+C, and B+C enters second level tower and is further separated into B
(overhead distillate) and C (tower bottoms).
This method is easy to operate high but have the shortcomings that height relies on graphite condenser, intrinsic safety difference and energy consumption:
It is the sour gas containing a large amount of hydrogen chloride that the process route, which hydrolyzes tail gas, so height relies on graphite condenser.And graphite condenses
Device not temperature variation resistant, not withstand pressure, leaks it so enduring to the fullest extent in graphite condenser using the glyphosate gas-liquid of this glyphosate process route
Hardship, equipment investment is big, maintenance cost is high；Leakage causes acidic materials and organic matter to enter chilled water and circulating water in condenser
System, corrodes chilled water and circulation, chilled water fire risk, causes essential safety degree low, environmental protection pressure is big；Condensation
Leakage also results in chilled water and seals in dilute methanol system in device, increases dilute methanol treating capacity and operating cost.In addition, this method process
In, material is by " condensation, condenses gasification again " multiple phase transformation, so energy consumption is very high, it is uneconomical.
2, second is that gas phase recycles route, it may be assumed that main component is water, dimethoxym ethane, methanol, hydrogen chloride and chloromethanes glyphosate water
Tail gas is solved through, with removing hydrogen chloride gas, residual exhaust is by dimethoxym ethane (A)-methanol (B)-water (C)-chloromethanes (D) in gas phase
The quaternary mixed gaseous mixed system of composition, is separated through two stage rectification tower and condenser, specially high according to component boiling point
Low sequence successively isolates C, B, detailed process from tower bottom are as follows: first order tower tower bottom isolates C, and tower top isolates component A
+B+D；A+B+D enters second level tower and is further separated into B (tower bottoms) and A+D (overhead distillate), and A+D is cold through condenser
It is solidifying to be separated into A (condensate liquid) and D (fixed gas).
This method mutually tails off, low energy consumption, but haves the shortcomings that operation stability is poor: first is that hydrolysis tail gas removes de-chlorine hydride
The quaternary mixes liquid system that remaining tail gas is made of dimethoxym ethane (A)-methanol (B)-water (C)-chloromethanes (D) after gas,
Opposite liquid phase route, material total amount is big, and logistics load is big (being 1.5 times of liquid phase), and chloromethanes component ratio (accounts for tail gas total amount greatly
30%), lead to recovery system fluctuation of service.In the case of especially shutting off power in emergency, a large amount of dimethoxym ethanes (A), methanol (B), chlorine
Methane (D) material system is from urgent pressure relief system discharging decompressing, and therefore, there are larger safe and environment-friendly hidden danger for operation stability difference.
Summary of the invention
In view of the above problems and defect, the present invention provides a kind of alkyl esterification method glyphosate solvent recovery new equipments
And technique, the hidden danger leaked in graphite condenser is thoroughly eliminated compared to Traditional liquid phase recovery process, compares conventional gas-phase recovery process
Safety and stability is improved, to reach the mesh that essential safety is high, stable and operation convenience, energy saving economy are taken into account
's.
For achieving the above object, the invention adopts the following technical scheme:
A kind of alkyl esterification method based on B-grade condensation produces glyphosate solvent reclaimer, specifically include tail gas neutralizing tower,
Liquid caustic soda tank, dilute liquid alkali tank, level-one tail gas condenser, second level tail gas condenser, aqueous solution collecting tank, methanol dimethoxym ethane solution are collected
Tank, level-one rectifying column, two-stage rectification tower, compressor one, compressor 22, compressor three.
In the alkyl esterification method production glyphosate solvent recovering system based on B-grade condensation, B-grade condensation refers to from grass
Glyphosate tail gas after the neutralized tower of sweet phosphine hydrolysis system neutralizes is separated through I and II tail gas condenser point condensed in two stages, point
It Fen Li not aqueous solution (main component is water) and methanol dimethoxym ethane solution (main component is methanol, dimethoxym ethane).
Glyphosate hydrolyzing tail gas feeding pipe couples with tail gas neutralizing tower lower part.Tail gas neutralizing tower top also passes through liquid
Alkali supplement pipeline is connect with liquid caustic soda tank, and tail gas neutralizing tower lower part also produces pipeline by dilute liquid alkali and couples with dilute liquid alkali tank.Thin liquid
Alkali tank is connect by feeding pipe with tail gas neutralizing tower top, and forms circulation by pump.
Tail gas neutralizing tower top is coupled by feeding pipe with level-one tail gas condenser；The level-one tail gas condensing
Device, second level tail gas condenser are sequentially connected in series connection by feeding pipe；Between the tail gas neutralizing tower and level-one tail gas condenser,
Compressor one, compressor two are respectively arranged between level-one tail gas condenser and second level tail gas condenser and after secondary condenser
2, compressor three.
It illustrates, the level-one tail gas condenser, second level tail gas condenser difference in the B-grade condensation system are at least
One condenser, but it is not limited to an only condenser.When every level-one tail gas condenser has more, can by parallel or series or
The mode combined in series and parallel couples.
Level-one tail gas condenser lower part is coupled by feeding pipe with aqueous solution collecting tank, the liquid phase of first-stage condenser
Blanking goes to aqueous solution collecting tank by the feeding pipe.Second level tail gas condenser lower part passes through feeding pipe and methanol first
The connection of acetal solution collecting tank, the liquid phase blanking of secondary condenser are gone to methanol dimethoxym ethane solution by the feeding pipe and are collected
Tank.
The tail gas (containing gas is not coagulated through condenser is condensed) successively passes through tail gas neutralizing tower, compressor one, level-one tail
Gas condenser, compressor two, second level tail gas condenser, the incoagulability tail gas from second level tail gas condenser contract with from methanol first
The tail gas of aldehyde solution collecting tank through compressor three goes to Chloromethane recovery device after converging.
The aqueous solution collecting tank, methanol dimethoxym ethane solution collecting tank top are respectively arranged with pressure-equalizing pipe.Aqueous solution
The pressure-equalizing pipe on collecting tank top is connected with aqueous solution collecting tank and the outlet of level-one tail gas condenser respectively, and methanol solution is collected
The pressure-equalizing pipe on tank top is connected with methanol solution collecting tank and the outlet of second level tail gas condenser respectively.
The aqueous solution collecting tank is coupled by feeding pipe with level-one rectifier, and the methanol dimethoxym ethane solution is received
Collection tank is connect by feeding pipe with two-stage rectification tower top, and feeding pipe described herein is respectively arranged with valve 1, valve 2, with
Realize throttling, decompression.
The level-one rectifying column, two-stage rectification tower tower top pass through feeding pipe and be connected with condenser and reflux in turn
Tank, and be connected to form reflux with tower top by reflux pump, while the bottom of each tower is equipped with reboiler.
The return tank of the level-one rectifying tower is equipped with discharge nozzle, and it is molten that the discharge nozzle other end is attached to methanol dimethoxym ethane
Liquid collecting tank top successively couples discharging pump, check-valves, condenser, methanol dimethoxym ethane solution specifically by feeding pipe and receives
Collect tank.Level-one rectifying tower bottom is boiled again is additionally provided with waste water extraction mouth, connects after condenser with station at dirt.
The return tank of the two-stage rectification tower tower is equipped with discharge nozzle, and the discharge nozzle other end is attached to dimethoxym ethane finished product
Tank.Two-stage rectification tower tower bottom is boiled again is additionally provided with methanol extraction mouth, is connected to methanol finished pot.
The another object of the present invention alkyl esterification method that there is provided a kind of based on above system produces glyphosate solvent recovery work
Skill, specific steps and feature are as follows:
What it is from glyphosate hydrolysis post includes the mixture and liquid of hydrogen chloride, chloromethanes, methanol, dimethoxym ethane, vapor
It is 7-14 that alkali enters tail gas neutralizing tower to be neutralized to pH together, removes the acid ingredient in tail gas, then carry out through I and II condenser
Pressure control, fractional condensaion separation, condensate liquid go to aqueous solution collecting tank, methanol dimethoxym ethane solution collecting tank respectively；Aqueous solution is collected
Tank, the aqueous solution in methanol dimethoxym ethane solution collecting tank, methanol dimethoxym ethane solution carry out rectification and purification processing after depressurizing again；It does not coagulate
Property gas goes to Chloromethane recovery device.
Glyphosate hydrolyzing tail gas of the present invention is from glyphosate hydrolysis post including hydrogen chloride, chloromethanes, first
Alcohol, dimethoxym ethane, vapor mixture also contain a small amount of dimethoxym ethane 10- wherein predominantly water 40-45%, methanol 25-35%
15%, chloromethanes 10-15% and micro hydrogen chloride 0.1-2%；In technique of the invention, 43%, methanol 30% are detected, also
Contain a small amount of dimethoxym ethane 13%, chloromethanes 13% and micro hydrogen chloride 1%.
Specific step is as follows:
Step 1: the glyphosate hydrolyzing tail gas from glyphosate hydrolysis kettle enters tail gas neutralizing tower together with liquid alkaline and is neutralized to
PH is 7-14, the acid ingredient in tail gas is removed, then carry out pressure control, fractional condensaion through I and II condenser, by water therein
And methanol, dimethoxym ethane are condensed respectively, are separated, condensate liquid goes to aqueous solution collecting tank, methanol dimethoxym ethane solution collecting tank respectively.
(1) the pressure control embodiment are as follows:
Pass through the subsystem where 1#, 2# compressor control first-stage condenser, aqueous solution collecting tank and its pressure-equalizing pipe
Pressure is denoted as P1 in 0.1-0.3MPa.
By where 2#, 3# compressor control secondary condenser, methanol dimethoxym ethane solution collecting tank and its pressure-equalizing pipe
Subsystem pressure in 0.1-0.4MPa, be denoted as P2.
(2) the fractional condensaion embodiment are as follows:
First-stage condenser pressure P1 is controlled in 0.1-0.3MPa range, control system temperature T meets: T1 (methanol saturation) <
When T < T1 (water saturation), the water in tail gas is condensed, and methanol, dimethoxym ethane, chloromethanes do not condense, and water condensation is laggard
Enter aqueous solution surge tank, uncooled methanol, dimethoxym ethane, chloromethanes tail gas, which continue to go to secondary condenser, further to be condensed.
Secondary condenser pressure P2 meets in 0.1-0.4MPa range, control system temperature T: T2 (chloromethanes saturation) < T
When < T2 (dimethoxym ethane saturation), methanol, dimethoxym ethane in tail gas are condensed, and chloromethanes does not condense, methanol, dimethoxym ethane
Enter methanol dimethoxym ethane solution surge tank after condensation, uncooled chloromethanes tail gas continues to go to Chloromethane recovery device processing.
Step 2: aqueous solution collecting tank, the aqueous solution in methanol dimethoxym ethane solution collecting tank, methanol dimethoxym ethane solution, respectively
Level-one rectifying column, two-stage rectification tower are gone to after expenditure and pressure, carry out rectification and purification.It is specific as follows:
(1) material in aqueous solution collecting tank enters level-one rectifier, material decompression after throttling is decompressed to normal pressure
Its boiling point reduces afterwards, gasifies in tower.Level-one the top of the distillation column gas condenses through condenser and returns to level-one rectifier column reflux tank, and one
Liquid in grade rectifier column reflux tank pumps to form reflux through level-one rectifier column reflux, and another way is past through the extraction pumping of level-one rectifying column
Methanol dimethoxym ethane solution collecting tank.Level-one rectifying column bottom liquid goes to Sewage Disposal.The temperature control of level-one rectifier bottoms
100 ± 5 DEG C are made as, the temperature control on top is 65 ± 3 DEG C.
(2) material in methanol dimethoxym ethane solution collecting tank enters two-stage rectification tower top after throttling is decompressed to normal pressure,
Its boiling point reduces after material decompression, gasifies in tower.Two-stage rectification column overhead gas returns to two-stage rectification tower through condenser condensation
Return tank, the liquid in two-stage rectification tower return tank is formed through two-stage rectification tower reflux pump to flow back, and another way is through two-stage rectification tower
Extraction is pumped toward dimethoxym ethane finished pot.Two-stage rectification tower bottom liquid goes to methanol finished pot after condenser condenses.Second level essence
The temperature control for evaporating tower bottom is 65 ± 5 DEG C, and the temperature control on top is 42 ± 3 DEG C.
Beneficial effect
The present invention provides a kind of, and the alkyl esterification method based on B-grade condensation produces glyphosate solvent reclaimer and technique, both
It solves the defect that Traditional liquid phase recovery process height relies on graphite condenser, and solves the operation of conventional gas-phase recovery process not
Stable problem also has both energy conservation, economic feature, improves the essence peace of glyphosate hydrolyzing tail gas system and solvent recovery
Entirely, stability and economy.First is that thoroughly having eliminated the graphite condenser highly relied in Traditional liquid phase recovery process, avoid
What is leaked in condenser leads to this glyphosate professional problem of chilled water COD high；Two are reduction of system pressure, avoid tradition
The problem that gas phase recovery process logistics load is big, system pressure is big；Third is that reducing solvent by pressure control condensation, decompression gasification technology
The energy consumption of recycling, compares liquid phase recovery process, and ton glyphosate steam consumption reduces 2.0t.
Detailed description of the invention
Fig. 1 is that the present invention is based on the alkyl esterification methods of B-grade condensation to produce glyphosate solvent reclaimer figure, wherein 1. grass are sweet
Phosphine hydrolyzes tail gas tank, 2. liquid caustic soda tanks, 3. dilute liquid alkali tanks, 4. tail gas neutralizing towers, 5. compressors one, 6. tail gas condensers one, 7. pressures
Contracting machine two, 8. aqueous solution collecting tanks, 9. level-one rectifying columns, 10. condensers one, 11. reboilers one, 12. return tanks one, 13. first
Alcohol dimethoxym ethane solution pans, 14. two-stage rectification towers, 15. condensers two, 16. reboilers two, 17. return tanks two, the contracting of 18. first
Aldehyde finished pot, 19. methanol finished pots, 20. sewage plants, 21. tail gas condensers one, 22. compressors three, 23. pressure-equalizing pipes one,
24. pressure-equalizing pipe two.
Specific embodiment
Embodiment 1
A kind of alkyl esterification method production glyphosate solvent recovering system based on B-grade condensation, including tail gas condenser 1, tail
Gas condenser 2 21, aqueous solution collecting tank 8, level-one rectifying column 9, methanol dimethoxym ethane solution pans 13, two-stage rectification tower 14,
The glyphosate hydrolyzing tail gas pretreatment system of alkyl esterification method production is connect through compressor 1 with tail gas condenser 1；
One 6 one tunnel of tail gas condenser is connect through compressor 27 with tail gas condenser 2 21, and tail gas condenser 2 21 is through pipeline
It is connect with methanol dimethoxym ethane solution pans 13；
One 6 another way of tail gas condenser is connect with aqueous solution collecting tank 8, and aqueous solution collecting tank 8 is through pipeline and level-one rectifying
The connection of 9 top of tower, 9 top of level-one rectifying column are connect through condenser 1 with return tank 1, the connection of 9 bottom of level-one rectifying column
To sewage plant 20；
Return tank 1 is connect with methanol dimethoxym ethane solution pans 13；
Methanol dimethoxym ethane solution pans 13 are connect through pipeline with two-stage rectification tower 14, and 14 top of two-stage rectification tower is through condensing
Device 2 15 is connect with return tank 2 17, and return tank 2 17 is connected to first dimethoxym ethane finished pot 18, the connection of 14 bottom of two-stage rectification tower
To methanol finished pot 19.
The glyphosate hydrolyzing tail gas pretreatment system of the alkyl esterification method production includes glyphosate hydrolyzing tail gas tank 1, liquid
Alkali tank 2, dilute liquid alkali tank 3, tail gas neutralizing tower 4；
The glyphosate hydrolyzing tail gas tank 1 couples through pipeline with 4 lower part of tail gas neutralizing tower, liquid caustic soda tank 2 through pipeline with it is dilute
Liquid caustic soda tank 3 is connect with 4 top of tail gas neutralizing tower again after connecting, and 4 bottom of tail gas neutralizing tower connect formation with dilute liquid alkali tank 3 and is recycled back to
Road.
4 top of tail gas neutralizing tower is connect through compressor 1 with tail gas condenser 1；
Tail gas condenser 1 is connected to compressor 27 after pressure-equalizing pipe one converges with aqueous solution collecting tank 8 and connect；
Tail gas condenser 2 21 and methanol dimethoxym ethane solution pans 13 are connected to compression after pressure-equalizing pipe two converges
Machine 3 22, compressor 3 22 are connected to chloromethanes collecting tank.
The dilute liquid alkali tank 3 is connect through pipeline with aqueous solution collecting tank 8；
The tail gas condenser 6 is at least one, and when being multiple, multiple tail gas condensers 6 connect in parallel or series.
9 top of the level-one rectifying column is connect through condenser 1 with return tank 1, return tank 1 through pipeline and
The connection of one 10 top of condenser, forms circulation loop；14 top of two-stage rectification tower is connect through condenser 2 15 with return tank 2 17,
Return tank 2 17 is connect through pipeline with 2 15 top of condenser, forms circulation loop.
One 10 bottom of condenser is provided with reboiler 1, and one 10 bottom of condenser is provided with reboiler 2 16.
Embodiment 2
What it is from glyphosate hydrolysis post includes the mixture and liquid of hydrogen chloride, chloromethanes, methanol, dimethoxym ethane, vapor
It is 7-14 that alkali enters tail gas neutralizing tower to be neutralized to pH together, removes the acid ingredient in tail gas, then carry out through I and II condenser
Pressure control, fractional condensaion separation, condensate liquid go to aqueous solution collecting tank, methanol dimethoxym ethane solution collecting tank respectively；Aqueous solution is collected
Tank, the aqueous solution in methanol dimethoxym ethane solution collecting tank, methanol dimethoxym ethane solution carry out rectification and purification processing after depressurizing again；It does not coagulate
Property gas goes to Chloromethane recovery device.Steps are as follows:
Step 1: the glyphosate hydrolyzing tail gas from glyphosate hydrolysis kettle enters tail gas neutralizing tower together with liquid alkaline and is neutralized to
PH is 7-14, the acid ingredient in tail gas is removed, then carry out pressure control, fractional condensaion through I and II condenser, by water therein
And methanol, dimethoxym ethane are condensed respectively, are separated, condensate liquid goes to aqueous solution collecting tank, methanol dimethoxym ethane solution collecting tank respectively.
The pressure control embodiment are as follows:
Pass through the subsystem where 1#, 2# compressor control first-stage condenser, aqueous solution collecting tank and its pressure-equalizing pipe
Pressure is denoted as P1 in 0.1-0.3MPa.The specific boundary of the subsystem is 1# compressor outlet, 2# compressor inlet, valve 1.
By where 2#, 3# compressor control secondary condenser, methanol dimethoxym ethane solution collecting tank and its pressure-equalizing pipe
Subsystem pressure in 0.1-0.4MPa, be denoted as P2.The specific boundary of the subsystem be 2# compressor outlet, 3# compressor into
Mouth, valve 2, check-valves 1.
The fractional condensaion embodiment are as follows:
By water, methanol, dimethoxym ethane, chloromethanes physical property it is found that under a certain pressure, saturation temperature size order
Are as follows: water > methanol > dimethoxym ethane > chloromethanes.Under a certain pressure, exhaust temperature T is controlled by condenser to gradually reduce, work as tail
When temperature degree is down under the respective saturation temperature of water, methanol, dimethoxym ethane, water, methanol, dimethoxym ethane are condensed respectively, are separated.
Water, methanol, dimethoxym ethane, chloromethanes saturation temperature, saturated vapour pressure data see the table below:
Specific embodiment are as follows:
1. corresponding pressure is lauched, the saturation temperature of methanol, dimethoxym ethane when the control pressure of first-stage condenser is P1 above-mentioned
Degree is denoted as T1 (water saturation), T1 (methanol saturation), T1 (dimethoxym ethane saturation).Control system pressure P1 in 0.1-0.3MPa range,
When system temperature T meets: when T1 (water saturation) > T > T1 (methanol saturation), the water in tail gas is condensed, and methanol, first contract
Aldehyde, chloromethanes do not condense, and realize the separation of the water and methanol, dimethoxym ethane, chloromethanes in tail gas, enter after water condensation water-soluble
Liquid surge tank, uncooled methanol, dimethoxym ethane, chloromethanes tail gas, which continue to go to secondary condenser, further to be condensed.
Illustrative example: when selected system pressure P1 is in 0.3MPa, system temperature T is in 95-134 DEG C of range, then in tail gas
Water condense, and methanol, dimethoxym ethane, chloromethanes do not condense, and realize water and methanol, dimethoxym ethane, chloromethane in tail gas
The separation of alkane.When selected system pressure is in 0.2MPa, system temperature T1 is controlled in 84-122 DEG C of range, then is equally reached above-mentioned
Separating effect.
2. when the control pressure of secondary condenser is P2 above-mentioned, methanol under corresponding pressure, dimethoxym ethane, chloromethanes it is full
T2 (methanol saturation), T2 (dimethoxym ethane saturation), T2 (chloromethanes saturation) are denoted as with temperature.P2 is in 0.1- for control system pressure
0.4MPa range, when control system temperature T meets: when T2 (chloromethanes saturation) < T < T2 (dimethoxym ethane saturation), in tail gas
Methanol, dimethoxym ethane condense, and chloromethanes does not condense, and realize the separation of the methanol, dimethoxym ethane and chloromethanes in tail gas,
Enter methanol dimethoxym ethane solution surge tank after methanol, dimethoxym ethane condensation, uncooled chloromethanes tail gas continues to go to chloromethanes time
Receiving apparatus processing.
Illustrative example: when selected system pressure P is in 0.4MPa, control system temperature T is at 13-88 DEG C, then in tail gas
Methanol, dimethoxym ethane condense, and chloromethanes does not condense, and realize the separation of the methanol, dimethoxym ethane and chloromethanes in tail gas.
When selected system pressure P is in 0.3MPa, control system temperature T is at 5-78 DEG C, then the methanol in tail gas, dimethoxym ethane occur cold
It is solidifying, and chloromethanes does not condense, and realizes the separation of the methanol, dimethoxym ethane and chloromethanes in tail gas.
It should be noted that as normal pressure condenses this special operation condition as P=0.1MPa.
2, step 2: aqueous solution collecting tank, the aqueous solution in methanol dimethoxym ethane solution collecting tank, methanol dimethoxym ethane solution, point
Level-one rectifying column, two-stage rectification tower are not gone to after expenditure and pressure, carries out rectification and purification.It is specific as follows:
Material in aqueous solution collecting tank enters level-one rectifier after expenditure and pressure, its boiling point drops after material decompression
It is low, gasify in tower.Level-one the top of the distillation column gas returns to level-one rectifier column reflux tank through condenser condensation, and level-one rectifying column returns
Liquid in stream tank pumps to form reflux through level-one rectifier column reflux, and another way is pumped through the extraction of level-one rectifying column toward methanol dimethoxym ethane
Solution collecting tank.Level-one rectifying column bottom liquid goes to Sewage Disposal.The temperature control of level-one rectifier bottoms is 100 ± 5
DEG C, the temperature control on top is 65 ± 3 DEG C.
Material in methanol dimethoxym ethane solution collecting tank enters two-stage rectification tower top after expenditure and pressure, after material decompression
Its boiling point reduces, and gasifies in tower.Two-stage rectification column overhead gas returns to two-stage rectification tower return tank, second level through condenser condensation
Liquid in rectifier column reflux tank is formed through two-stage rectification tower reflux pump to flow back, and another way is pumped through the extraction of two-stage rectification tower toward first
Acetal finished pot.Two-stage rectification tower bottom liquid goes to methanol finished pot after condenser condenses.The temperature of two-stage rectification tower bottom
Degree control is 65 ± 5 DEG C, and the temperature control on top is 42 ± 3 DEG C.
It should be noted that in one, two rectifying columns material after decompression boiling point reduce, only by self heat realize ebullition, gasification and
Rectifying separation, when normal operation, does not need in addition to supplement steam, to realize energy conservation.The reboiler only drives for the first time or is
Raw steam is supplemented when temperature of uniting is too low on a small quantity.When selected system pressure P is in 0.4MPa, control system temperature T at 13-88 DEG C,
Compared to traditional handicraft, on the basis of methanol, dimethoxym ethane moisture, content quality index are up to standard, ton glyphosate solvent recovery steam list
Consumption decline 2.02t, it is low about to compare a kind of alkyl esterification method glyphosate solvent recovering system (being denoted as 1# process system) steam mono-consumption
0.7t。
It is illustrated, a kind of heretofore described alkyl esterification method glyphosate solvent recovery system based on B-grade condensation
It unites (being denoted as 2# process system), (is denoted as 1# technique system with a kind of alkyl esterification method glyphosate solvent recovering system declared simultaneously
System), a kind of maximum difference of the alkyl esterification method glyphosate solvent recovering system (being denoted as 3# process system) based on three-level condensation exists
It is specific to distinguish are as follows: 1. to operate convenience: 1# process system in the operation convenience of rectifying separation and the difference of energy conservation and economy
> 2# process system > 3# process system；2. energy conservation and economy: 3# process system > 2# process system > 1# process system.Tool
It is flexibly selected in body production process in combination with production requirement and operation preference.
Claims (6)
1. a kind of alkyl esterification method based on B-grade condensation produces glyphosate solvent recovering system, including tail gas condenser one (6), tail
Gas condenser two (21), aqueous solution collecting tank (8), level-one rectifying column (9), methanol dimethoxym ethane solution pans (13), second level essence
Evaporate tower (14), which is characterized in that
The glyphosate hydrolyzing tail gas pretreatment system of alkyl esterification method production is connect through compressor one (5) with tail gas condenser one (6)；
Tail gas condenser one (6) is connect through compressor two (7) with tail gas condenser two (21) all the way, tail gas condenser two (21) warp
Pipeline is connect with methanol dimethoxym ethane solution pans (13)；
Tail gas condenser one (6) another way is connect with aqueous solution collecting tank (8), and aqueous solution collecting tank (8) is through pipeline and level-one essence
The connection of tower (9) top is evaporated, is connect through condenser one (10) with return tank one (12) at the top of level-one rectifying column (9), level-one rectifying column
(9) bottom is connected to sewage plant (20)；
Return tank one (12) is connect with methanol dimethoxym ethane solution pans (13)；
Methanol dimethoxym ethane solution pans (13) are connect through pipeline with two-stage rectification tower (14), through cold at the top of two-stage rectification tower (14)
Condenser two (15) is connect with return tank two (17), and return tank two (17) is connected to first dimethoxym ethane finished pot (18), two-stage rectification tower
(14) bottom is connected to methanol finished pot (19).
2. the alkyl esterification method described in claim 1 based on B-grade condensation produces glyphosate solvent recovering system, which is characterized in that
The glyphosate hydrolyzing tail gas pretreatment system of the alkyl esterification method production includes glyphosate hydrolyzing tail gas tank (1), liquid caustic soda tank
(2), dilute liquid alkali tank (3), tail gas neutralizing tower (4)；
The glyphosate hydrolyzing tail gas tank (1) couples through pipeline with tail gas neutralizing tower (4) lower part, liquid caustic soda tank (2) through pipeline with
It is connect again with tail gas neutralizing tower (4) top after dilute liquid alkali tank (3) connection, tail gas neutralizing tower (4) bottom is connect with dilute liquid alkali tank (3)
Form circulation loop.
3. the alkyl esterification method as claimed in claim 2 based on B-grade condensation produces glyphosate solvent recovering system, which is characterized in that
It is connect through compressor one (5) with tail gas condenser one (6) at the top of tail gas neutralizing tower (4)；
Tail gas condenser one (6) and aqueous solution collecting tank (8) are connected to compressor two (7) even after pressure-equalizing pipe one converges
It connects；
Tail gas condenser two (21) and methanol dimethoxym ethane solution pans (13) are connected to compression after pressure-equalizing pipe two converges
Machine three (22), compressor three (22) are connected to chloromethanes collecting tank.
4. the alkyl esterification method as claimed in claim 2 based on B-grade condensation produces glyphosate solvent recovering system, which is characterized in that
Dilute liquid alkali tank (3) is connect through pipeline with aqueous solution collecting tank (8)；
The tail gas condenser one (6) is at least one, and when being multiple, multiple tail gas condensers one (6) connect in parallel or series
It connects.
5. the alkyl esterification method described in claim 1 based on B-grade condensation produces glyphosate solvent recovering system, which is characterized in that
It is connect through condenser one (10) with return tank one (12) at the top of level-one rectifying column (9), return tank one (12) is through pipeline and condenser
The connection of one (10) top, forms circulation loop；At the top of two-stage rectification tower (14) even through condenser two (15) and return tank two (17)
It connects, return tank two (17) is connect through pipeline with two-stage rectification tower (14) top, forms circulation loop.
6. the alkyl esterification method described in claim 1 based on B-grade condensation produces glyphosate solvent recovering system, which is characterized in that
Level-one rectifying column (9) bottom is provided with reboiler one (11), and two-stage rectification tower (14) bottom is provided with reboiler two (16).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409532A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method production glyphosate solvent recovering system and technique based on B-grade condensation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409532A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method production glyphosate solvent recovering system and technique based on B-grade condensation |
| CN108409532B (en) * | 2018-04-20 | 2023-07-11 | 湖北泰盛化工有限公司 | System and process for recycling solvent for producing glyphosate by alkyl ester method based on secondary condensation |
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